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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
CCDC reference: 170273
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (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
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
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).
Crystal data top
Li+·CF3SO3− | F(000) = 304 |
Mr = 156.01 | Dx = 2.135 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.0994 (6) Å | Cell parameters from 500 reflections |
b = 5.0410 (2) Å | θ = 4–20.8° |
c = 9.5320 (6) Å | µ = 0.66 mm−1 |
β = 90.370 (5)° | T = 173 K |
V = 485.27 (5) Å3 | Block, colourless |
Z = 4 | 0.36 × 0.22 × 0.16 mm |
Data collection top
Siemens CCD three-circle diffractometer | 1144 independent reflections |
Radiation source: fine-focus sealed tube | 966 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ω scans | θmax = 29.5°, θmin = 4.0° |
Absorption correction: empirical (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.798, Tmax = 0.902 | k = −6→6 |
7664 measured reflections | l = −12→12 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.029 | Secondary 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 reflections | Δρmax = 0.38 e Å−3 |
82 parameters | Δρmin = −0.38 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
S1 | 0.82387 (4) | 0.39249 (8) | 0.09187 (4) | 0.01597 (15) | |
C1 | 0.66103 (17) | 0.2386 (4) | 0.1016 (2) | 0.0247 (4) | |
Li1 | 1.1010 (3) | 0.1123 (6) | 0.0906 (3) | 0.0212 (6) | |
F1 | 0.57236 (12) | 0.4162 (3) | 0.13686 (15) | 0.0466 (4) | |
F2 | 0.62774 (11) | 0.1362 (3) | −0.02208 (13) | 0.0376 (3) | |
F3 | 0.66341 (12) | 0.0468 (3) | 0.19553 (13) | 0.0404 (4) | |
O1 | 0.85216 (14) | 0.4918 (3) | 0.22993 (14) | 0.0306 (3) | |
O2 | 0.90882 (11) | 0.1728 (3) | 0.05312 (13) | 0.0208 (3) | |
O3 | 0.80845 (13) | 0.5895 (3) | −0.01570 (14) | 0.0252 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S1 | 0.0160 (2) | 0.0157 (2) | 0.0162 (2) | −0.00001 (15) | 0.00001 (15) | −0.00175 (17) |
C1 | 0.0188 (8) | 0.0307 (11) | 0.0247 (10) | 0.0004 (8) | 0.0046 (7) | 0.0032 (8) |
Li1 | 0.0241 (14) | 0.0213 (16) | 0.0184 (14) | −0.0011 (12) | −0.0013 (11) | 0.0020 (13) |
F1 | 0.0242 (6) | 0.0514 (9) | 0.0644 (10) | 0.0118 (6) | 0.0148 (6) | −0.0015 (7) |
F2 | 0.0294 (6) | 0.0488 (8) | 0.0347 (7) | −0.0179 (6) | −0.0045 (5) | −0.0039 (6) |
F3 | 0.0386 (7) | 0.0426 (8) | 0.0401 (8) | −0.0087 (6) | 0.0110 (5) | 0.0176 (6) |
O1 | 0.0358 (7) | 0.0349 (8) | 0.0211 (7) | 0.0033 (6) | −0.0037 (5) | −0.0114 (6) |
O2 | 0.0175 (6) | 0.0188 (7) | 0.0262 (7) | 0.0019 (5) | 0.0011 (5) | −0.0056 (5) |
O3 | 0.0265 (7) | 0.0207 (7) | 0.0285 (7) | −0.0042 (5) | −0.0016 (5) | 0.0065 (6) |
Geometric parameters (Å, º) top
S1—O1 | 1.4351 (13) | Li1—O3ii | 1.901 (3) |
S1—O3 | 1.4351 (13) | Li1—O2iii | 1.988 (3) |
S1—O2 | 1.4500 (13) | Li1—O2 | 1.995 (3) |
S1—C1 | 1.8212 (18) | Li1—Li1iii | 2.895 (6) |
C1—F1 | 1.311 (2) | O1—Li1iv | 1.873 (3) |
C1—F3 | 1.318 (2) | O2—Li1iii | 1.988 (3) |
C1—F2 | 1.328 (2) | O3—Li1ii | 1.901 (3) |
Li1—O1i | 1.873 (3) | | |
| | | |
O1—S1—O3 | 115.70 (9) | O3ii—Li1—O2iii | 109.57 (16) |
O1—S1—O2 | 112.67 (8) | O1i—Li1—O2 | 116.93 (17) |
O3—S1—O2 | 114.08 (8) | O3ii—Li1—O2 | 106.35 (15) |
O1—S1—C1 | 106.05 (9) | O2iii—Li1—O2 | 86.74 (12) |
O3—S1—C1 | 103.72 (8) | O1i—Li1—Li1iii | 126.23 (19) |
O2—S1—C1 | 102.93 (8) | O3ii—Li1—Li1iii | 115.09 (18) |
F1—C1—F3 | 109.63 (15) | O2iii—Li1—Li1iii | 43.46 (9) |
F1—C1—F2 | 108.87 (15) | O2—Li1—Li1iii | 43.28 (9) |
F3—C1—F2 | 108.73 (17) | S1—O1—Li1iv | 176.61 (13) |
F1—C1—S1 | 109.93 (14) | S1—O2—Li1iii | 134.49 (11) |
F3—C1—S1 | 109.55 (12) | S1—O2—Li1 | 130.38 (12) |
F2—C1—S1 | 110.11 (12) | Li1iii—O2—Li1 | 93.26 (12) |
O1i—Li1—O3ii | 118.68 (16) | S1—O3—Li1ii | 139.93 (12) |
O1i—Li1—O2iii | 113.97 (16) | | |
| | | |
O1—S1—C1—F1 | 61.21 (15) | O1—S1—O2—Li1 | −38.74 (18) |
O3—S1—C1—F1 | −61.12 (15) | O3—S1—O2—Li1 | 95.81 (16) |
O2—S1—C1—F1 | 179.73 (13) | C1—S1—O2—Li1 | −152.52 (16) |
O1—S1—C1—F3 | −59.32 (16) | O1i—Li1—O2—S1 | 78.8 (2) |
O3—S1—C1—F3 | 178.35 (13) | O3ii—Li1—O2—S1 | −56.5 (2) |
O2—S1—C1—F3 | 59.20 (15) | O2iii—Li1—O2—S1 | −165.91 (14) |
O1—S1—C1—F2 | −178.86 (13) | Li1iii—Li1—O2—S1 | −165.91 (14) |
O3—S1—C1—F2 | 58.81 (15) | O1i—Li1—O2—Li1iii | −115.3 (2) |
O2—S1—C1—F2 | −60.33 (15) | O3ii—Li1—O2—Li1iii | 109.45 (18) |
O1—S1—O2—Li1iii | 161.18 (16) | O1—S1—O3—Li1ii | 52.0 (2) |
O3—S1—O2—Li1iii | −64.27 (18) | O2—S1—O3—Li1ii | −81.1 (2) |
C1—S1—O2—Li1iii | 47.40 (18) | C1—S1—O3—Li1ii | 167.7 (2) |
Symmetry codes: (i) −x+2, y−1/2, −z+1/2; (ii) −x+2, −y+1, −z; (iii) −x+2, −y, −z; (iv) −x+2, y+1/2, −z+1/2. |
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