Download citation
Download citation
link to html
The title compound, Li+·CF3SO3-, has already been investigated by powder diffraction methods. We present in this work the single-crystal structure, which is in good agreement with the previous structure determination.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007462/cv6022sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007462/cv6022Isup2.hkl
Contains datablock I

CCDC reference: 170273

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](O-Li) = 0.003 Å
  • R factor = 0.029
  • wR factor = 0.078
  • Data-to-parameter ratio = 14.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 29.48 From the CIF: _reflns_number_total 1144 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1341 Completeness (_total/calc) 85.31% Alert B: < 90% complete (theta max?)
Author response: The data are over 99% complete to 26 degrees in theta.

0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991).

(I) top
Crystal data top
Li+·CF3SO3F(000) = 304
Mr = 156.01Dx = 2.135 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.0994 (6) ÅCell parameters from 500 reflections
b = 5.0410 (2) Åθ = 4–20.8°
c = 9.5320 (6) ŵ = 0.66 mm1
β = 90.370 (5)°T = 173 K
V = 485.27 (5) Å3Block, colourless
Z = 40.36 × 0.22 × 0.16 mm
Data collection top
Siemens CCD three-circle
diffractometer
1144 independent reflections
Radiation source: fine-focus sealed tube966 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 29.5°, θmin = 4.0°
Absorption correction: empirical
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.798, Tmax = 0.902k = 66
7664 measured reflectionsl = 1212
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.029Secondary atom site location: difference Fourier map
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0409P)2 + 0.2268P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
1144 reflectionsΔρmax = 0.38 e Å3
82 parametersΔρmin = 0.38 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S10.82387 (4)0.39249 (8)0.09187 (4)0.01597 (15)
C10.66103 (17)0.2386 (4)0.1016 (2)0.0247 (4)
Li11.1010 (3)0.1123 (6)0.0906 (3)0.0212 (6)
F10.57236 (12)0.4162 (3)0.13686 (15)0.0466 (4)
F20.62774 (11)0.1362 (3)0.02208 (13)0.0376 (3)
F30.66341 (12)0.0468 (3)0.19553 (13)0.0404 (4)
O10.85216 (14)0.4918 (3)0.22993 (14)0.0306 (3)
O20.90882 (11)0.1728 (3)0.05312 (13)0.0208 (3)
O30.80845 (13)0.5895 (3)0.01570 (14)0.0252 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0160 (2)0.0157 (2)0.0162 (2)0.00001 (15)0.00001 (15)0.00175 (17)
C10.0188 (8)0.0307 (11)0.0247 (10)0.0004 (8)0.0046 (7)0.0032 (8)
Li10.0241 (14)0.0213 (16)0.0184 (14)0.0011 (12)0.0013 (11)0.0020 (13)
F10.0242 (6)0.0514 (9)0.0644 (10)0.0118 (6)0.0148 (6)0.0015 (7)
F20.0294 (6)0.0488 (8)0.0347 (7)0.0179 (6)0.0045 (5)0.0039 (6)
F30.0386 (7)0.0426 (8)0.0401 (8)0.0087 (6)0.0110 (5)0.0176 (6)
O10.0358 (7)0.0349 (8)0.0211 (7)0.0033 (6)0.0037 (5)0.0114 (6)
O20.0175 (6)0.0188 (7)0.0262 (7)0.0019 (5)0.0011 (5)0.0056 (5)
O30.0265 (7)0.0207 (7)0.0285 (7)0.0042 (5)0.0016 (5)0.0065 (6)
Geometric parameters (Å, º) top
S1—O11.4351 (13)Li1—O3ii1.901 (3)
S1—O31.4351 (13)Li1—O2iii1.988 (3)
S1—O21.4500 (13)Li1—O21.995 (3)
S1—C11.8212 (18)Li1—Li1iii2.895 (6)
C1—F11.311 (2)O1—Li1iv1.873 (3)
C1—F31.318 (2)O2—Li1iii1.988 (3)
C1—F21.328 (2)O3—Li1ii1.901 (3)
Li1—O1i1.873 (3)
O1—S1—O3115.70 (9)O3ii—Li1—O2iii109.57 (16)
O1—S1—O2112.67 (8)O1i—Li1—O2116.93 (17)
O3—S1—O2114.08 (8)O3ii—Li1—O2106.35 (15)
O1—S1—C1106.05 (9)O2iii—Li1—O286.74 (12)
O3—S1—C1103.72 (8)O1i—Li1—Li1iii126.23 (19)
O2—S1—C1102.93 (8)O3ii—Li1—Li1iii115.09 (18)
F1—C1—F3109.63 (15)O2iii—Li1—Li1iii43.46 (9)
F1—C1—F2108.87 (15)O2—Li1—Li1iii43.28 (9)
F3—C1—F2108.73 (17)S1—O1—Li1iv176.61 (13)
F1—C1—S1109.93 (14)S1—O2—Li1iii134.49 (11)
F3—C1—S1109.55 (12)S1—O2—Li1130.38 (12)
F2—C1—S1110.11 (12)Li1iii—O2—Li193.26 (12)
O1i—Li1—O3ii118.68 (16)S1—O3—Li1ii139.93 (12)
O1i—Li1—O2iii113.97 (16)
O1—S1—C1—F161.21 (15)O1—S1—O2—Li138.74 (18)
O3—S1—C1—F161.12 (15)O3—S1—O2—Li195.81 (16)
O2—S1—C1—F1179.73 (13)C1—S1—O2—Li1152.52 (16)
O1—S1—C1—F359.32 (16)O1i—Li1—O2—S178.8 (2)
O3—S1—C1—F3178.35 (13)O3ii—Li1—O2—S156.5 (2)
O2—S1—C1—F359.20 (15)O2iii—Li1—O2—S1165.91 (14)
O1—S1—C1—F2178.86 (13)Li1iii—Li1—O2—S1165.91 (14)
O3—S1—C1—F258.81 (15)O1i—Li1—O2—Li1iii115.3 (2)
O2—S1—C1—F260.33 (15)O3ii—Li1—O2—Li1iii109.45 (18)
O1—S1—O2—Li1iii161.18 (16)O1—S1—O3—Li1ii52.0 (2)
O3—S1—O2—Li1iii64.27 (18)O2—S1—O3—Li1ii81.1 (2)
C1—S1—O2—Li1iii47.40 (18)C1—S1—O3—Li1ii167.7 (2)
Symmetry codes: (i) x+2, y1/2, z+1/2; (ii) x+2, y+1, z; (iii) x+2, y, z; (iv) x+2, y+1/2, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds