Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805001716/lh6353sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805001716/lh6353Isup2.hkl |
CCDC reference: 263569
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.001 Å
- R factor = 0.017
- wR factor = 0.045
- Data-to-parameter ratio = 41.0
checkCIF/PLATON results
No syntax errors found
Alert level C CRYSC01_ALERT_1_C There is an ordering error in _exptl_crystal_colour. It should be (QUALIFIER) (INTENSITY) (BASE_COLOUR). PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.09 PLAT143_ALERT_4_C su on c - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.50 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 36.32 From the CIF: _reflns_number_total 3031 Count of symmetry unique reflns 1748 Completeness (_total/calc) 173.40% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1283 Fraction of Friedel pairs measured 0.734 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 and SAINT (Bruker, 2004); data reduction: SAINT and XPREP (Sheldrick, 2003); program(s) used to solve structure: XS (Sheldrick, 2001); program(s) used to refine structure: XL (Sheldrick, 2001); molecular graphics: XP (Sheldrick, 1998); software used to prepare material for publication: XCIF (Sheldrick, 2001).
[LiCl(C4H8O2)] | F(000) = 272 |
Mr = 130.49 | Dx = 1.380 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 7757 reflections |
a = 7.1227 (1) Å | θ = 3.2–38.3° |
b = 7.7284 (1) Å | µ = 0.51 mm−1 |
c = 11.4138 (1) Å | T = 100 K |
V = 628.30 (1) Å3 | Needle, clear colourless |
Z = 4 | 0.35 × 0.21 × 0.16 mm |
Bruker SMART APEX diffractometer | 3031 independent reflections |
Radiation source: fine-focus sealed tube, Siemens KFFMO2K-90 | 2941 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
Detector resolution: 8.33 pixels mm-1 | θmax = 36.3°, θmin = 3.2° |
ω scans | h = −11→11 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | k = −12→12 |
Tmin = 0.841, Tmax = 0.922 | l = −19→18 |
30357 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.017 | H-atom parameters constrained |
wR(F2) = 0.045 | w = 1/[σ2(Fo2) + (0.0324P)2 + 0.007P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
3031 reflections | Δρmax = 0.38 e Å−3 |
74 parameters | Δρmin = −0.12 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 1285 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.01 (2) |
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. Three-dimensional diamondoid network formed by lithium-chloride and lithium- dioxane interactions. H atoms were placed on at calculated positions and allowed to ride on parent atom. Hydrogen thermal parameters were set to 1.2 × the equivalent isotropic U of the parent atom. 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 | ||
Li1 | 0.86206 (14) | 0.12734 (14) | 0.03626 (8) | 0.01514 (16) | |
Cl1 | 0.685733 (16) | 0.365608 (15) | −0.022286 (11) | 0.01480 (3) | |
O1 | 0.80639 (6) | 0.09282 (5) | 0.20256 (3) | 0.01520 (7) | |
O2 | 0.72100 (5) | 0.07984 (5) | 0.44527 (3) | 0.01363 (7) | |
C1 | 0.93006 (8) | 0.00899 (7) | 0.28467 (5) | 0.01644 (9) | |
H1A | 1.0614 | 0.0192 | 0.2571 | 0.020* | |
H1B | 0.8984 | −0.1155 | 0.2897 | 0.020* | |
C2 | 0.91189 (7) | 0.09083 (7) | 0.40439 (4) | 0.01515 (8) | |
H2A | 0.9960 | 0.0309 | 0.4603 | 0.018* | |
H2B | 0.9506 | 0.2137 | 0.4003 | 0.018* | |
C3 | 0.60039 (7) | 0.16809 (7) | 0.36373 (4) | 0.01485 (8) | |
H3A | 0.6368 | 0.2915 | 0.3588 | 0.018* | |
H3B | 0.4688 | 0.1620 | 0.3913 | 0.018* | |
C4 | 0.61601 (7) | 0.08537 (8) | 0.24411 (5) | 0.01611 (9) | |
H4A | 0.5749 | −0.0368 | 0.2486 | 0.019* | |
H4B | 0.5327 | 0.1464 | 0.1884 | 0.019* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Li1 | 0.0160 (4) | 0.0177 (4) | 0.0118 (4) | 0.0001 (3) | 0.0003 (3) | −0.0011 (3) |
Cl1 | 0.01154 (5) | 0.01466 (5) | 0.01820 (5) | 0.00052 (4) | −0.00224 (4) | 0.00037 (4) |
O1 | 0.01494 (15) | 0.02127 (16) | 0.00938 (13) | 0.00168 (14) | 0.00048 (12) | 0.00138 (12) |
O2 | 0.01435 (16) | 0.01624 (15) | 0.01031 (13) | 0.00198 (12) | 0.00079 (11) | 0.00285 (12) |
C1 | 0.0157 (2) | 0.0201 (2) | 0.01351 (18) | 0.00490 (18) | 0.00200 (15) | 0.00266 (16) |
C2 | 0.01311 (19) | 0.0200 (2) | 0.01233 (17) | −0.00085 (16) | −0.00196 (15) | 0.00277 (16) |
C3 | 0.0150 (2) | 0.0175 (2) | 0.01207 (17) | 0.00399 (16) | 0.00072 (15) | 0.00307 (15) |
C4 | 0.01371 (19) | 0.0224 (2) | 0.01217 (18) | −0.00213 (17) | −0.00183 (15) | 0.00026 (17) |
Li1—O1 | 1.9574 (10) | C1—C2 | 1.5112 (8) |
Li1—O2i | 1.9981 (11) | C1—H1A | 0.9900 |
Li1—Cl1ii | 2.3115 (10) | C1—H1B | 0.9900 |
Li1—Cl1 | 2.3270 (11) | C2—H2A | 0.9900 |
Cl1—Li1iii | 2.3116 (10) | C2—H2B | 0.9900 |
O1—C4 | 1.4377 (7) | C3—C4 | 1.5117 (8) |
O1—C1 | 1.4401 (7) | C3—H3A | 0.9900 |
O2—C3 | 1.4385 (6) | C3—H3B | 0.9900 |
O2—C2 | 1.4400 (6) | C4—H4A | 0.9900 |
O2—Li1iv | 1.9981 (11) | C4—H4B | 0.9900 |
O1—Li1—O2i | 109.56 (5) | O2—C2—C1 | 110.43 (4) |
O1—Li1—Cl1ii | 105.79 (4) | O2—C2—H2A | 109.6 |
O2i—Li1—Cl1ii | 106.16 (4) | C1—C2—H2A | 109.6 |
O1—Li1—Cl1 | 106.08 (4) | O2—C2—H2B | 109.6 |
O2i—Li1—Cl1 | 108.97 (4) | C1—C2—H2B | 109.6 |
Cl1ii—Li1—Cl1 | 119.99 (4) | H2A—C2—H2B | 108.1 |
Li1iii—Cl1—Li1 | 125.22 (3) | O2—C3—C4 | 109.87 (4) |
C4—O1—C1 | 110.14 (4) | O2—C3—H3A | 109.7 |
C4—O1—Li1 | 121.09 (4) | C4—C3—H3A | 109.7 |
C1—O1—Li1 | 124.64 (4) | O2—C3—H3B | 109.7 |
C3—O2—C2 | 109.04 (4) | C4—C3—H3B | 109.7 |
C3—O2—Li1iv | 122.64 (4) | H3A—C3—H3B | 108.2 |
C2—O2—Li1iv | 119.69 (4) | O1—C4—C3 | 110.51 (4) |
O1—C1—C2 | 110.35 (4) | O1—C4—H4A | 109.5 |
O1—C1—H1A | 109.6 | C3—C4—H4A | 109.5 |
C2—C1—H1A | 109.6 | O1—C4—H4B | 109.5 |
O1—C1—H1B | 109.6 | C3—C4—H4B | 109.5 |
C2—C1—H1B | 109.6 | H4A—C4—H4B | 108.1 |
H1A—C1—H1B | 108.1 |
Symmetry codes: (i) −x+3/2, −y, z−1/2; (ii) x+1/2, −y+1/2, −z; (iii) x−1/2, −y+1/2, −z; (iv) −x+3/2, −y, z+1/2. |