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Acta Cryst. (2008). C64, m20-m22
https://doi.org/10.1107/S0108270107058763
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Two pseudopolymorphs of LiCl trimers with semicubane structures

W. Domanska-Babul, K. Baranowska and J. Pikies
The title compounds, trichlorido(μ3-triethyl­phosphine oxide-κ3O:O:O)tris­(μ2-triethyl­phosphine oxide-κ2O:O)trilithium(I) toluene solvate, [Li3Cl3(C6H15OP)4]·C7H8, (I), and tri­chlori­do­(μ3-triethyl­phosphine oxide-κ3O:O:O)tris­(μ2-tri­ethylphos­phine oxide-κ2O:O)trilithium(I), [Li3Cl3(C6H15OP)4], (II), adopt separated semicubane structures in the solid state which are the first such structures to be reported for LiCl solvates. One triethyl­phosphine oxide ligand bonds via its O atom to the three Li atoms in a μ3 manner, while the other three triethyl­phosphine oxide ligands bridge three Li atoms in μ2 manners. The Cl atoms are in terminal instead of bridging positions, which is rather unusual for lithium chloride solvates.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107058763/gz3103sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107058763/gz3103Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107058763/gz3103IIsup3.hkl
Contains datablock II

CCDC references: 677080; 677081

Comment top

The most common feature of the aggregates of lithium chloride is a four-membered ring with Cl atoms in the bridging (µ2) positions (Bauer et al., 1960). Neutral Lewis bases are able to split the Cl bridges and replace the µ2-Cl atoms with other donor atoms, mainly O or N. A wide variety of aggregates of LiCl with Lewis bases have been found in the solid state. In monomeric [LiCl(3,5-Me2C5H3N)3], the Li atom is tetrahedrally coordinated (Raston et al., 1988), with an Li—Cl distance of 2.320 (9) Å. The more sterically demanding ligand 2-MeC5H4N leads to [Li2Cl2(2-MeC5H4N)4], a dimer with an intact Li2Cl2 ring. Tetrahydrofuran (THF) is not able to split the Li2Cl2 ring and yields [Li2Cl2]·2THF (Hahn & Rupprecht, 1991). HMPA [Please define] does not split the Li2Cl2 moiety either, and forms a cluster with a cubane skeleton, [LiCl·HMPA]4 (Barr et al., 1984a). The interaction of HMPA with hydrated LiCl leads to the formation of an ionic compound, [Li(H2O)2·HMPA]2Cl2, with an Li2O2 ring formed by the participation of the O atoms of HMPA (Barr et al., 1984b). Similarly, DMF and H2O split Li2Cl2, yielding [Li2Cl2]·2DMF·H2O, with an Li2O2 ring formed by O atoms from the DMF (Rao et al., 1984). The reaction of tetraisopropyl methylenediphosphonate with LiCl obtained in the reaction of BuLi with BuCl in THF leads to the formation of [LiCl{OP(OiPr)2CH2(iPrO)2PO}]2, with a planar Li2O2 ring (Henderson et al., 2003).

A search of the Cambridge Structural Dateabase (CSD; Version 5.28, May 2007 update; Allen, 2002) reveals 84 structures with an Li3O4 semicubane moiety, mainly incorporated in a cubane Li4O4 skeleton. Only three of them (Bock et al., 2000; Nassar et al., 2004) can be regarded as fused semicubane Li3O4 structures, being not incorporated in cubane Li4O4 or MLi3O4 structures (M = metal). Moreover, these compounds are lithium alkoxide derivatives but not lithium chloride solvates.

The X-ray analysis of the title compounds, [(LiCl)3(Et3PO)4].toluene, (I), and [(LiCl)3(Et3PO)4], (II), reveals very similar separated semicubane arrangements for both compounds. The molecular structures of (I) and (II) are presented in Figs. 1 and 2, respectively.

These structures can be viewed as cubanes with Cl atoms in the terminal positions, [Li4Cl4(OPEt3)4], with one LiCl molecule omitted. The absence of a bridging Li atom causes deformation in the cubane structure. It is noteworthy that similar cubane structures have not been known up to now for LiCl solvates.

The scheme shows the molecular arrangement of (I) along the P4—O4 bond. Atom O4 is a µ3-bridging atom of the Et3P═O group, with an average O4—Li distance of 2.039 (6) Å. The three four-membered rings O4Li2On (n = 1, 2 or 3) are nearly planar, with an average Li—On distance of 1.947 (6) Å in a µ2 arrangement. The average Pn═ On (n = 1, 2 or 3) distance is 1.504 (3) Å, slightly shorter than the P4—O4 distance of 1.518 (2) Å. Thus, the µ3 bridging causes a small but distinct elongation of the Li—O and P—O distances compared with the µ2 bridging. These distances are very close to the P—O distances reported for complexes incorporating HMPA and tetraisopropyl methylenediphosphonate as Lewis bases. The Li2O2 ring in [Li(H2O)2·HMPA]22+ is formed by the participation of Li+ ions and the O atoms of HMPA, and shows similar average bond lengths [P═O 1.496 (1) Å and Li—O 1.998 (3) Å; Barr et al., 1984b].

The average Li–Cl distance in (I) is 2.275 (6) Å, similar to the value of 2.293 (3) Å reported by Henderson for [LiCl{OP(OiPr)2CH2(iPrO)2PO}]2. This distance is shorter than the reported Li—Cl distances in Li2Cl2 rings [2.381 (9) Å; Raston et al., 1988] or for the Li4Cl4 cubane [2.357 (10)–2.441 (12) Å; Barr et al., 1984a]. It is also shorter than the sum of the covalent radii for Li (1.34 Å) and Cl (0.99 Å) (Purcell & Kotz, 1977) and is significantly shorter than the sum of the ionic radii of Li+ (0.60 Å) and Cl- (1.81 Å) (Purcell & Kotz, 1977). It is very close to the value of 2.23 (3) Å reported for the Li—Cl distance for an Li2Cl2 dimer in the gas phase (Bauer et al., 1960).

The direct comparison of [(iPrO)2PO]2CH2Et3PO with [(iPrO)2PO]2CH2 is not possible because of the chelating properties of the latter compound. The significant difference between HMPA (Barr et al., 1984b) or [(iPrO)2PO}2CH2] and Et3PO comes from the presence of additional electronegative atoms, N or O, on the P atoms in the first two compounds. Thus, Et3PO should possess better donor properties than HMPA or [(iPrO)2PO]2CH2. Additionally, due to the small Et groups around its P atoms, Et3PO exhibits a smaller steric effect than HMPA or (iPrO)2P(O)CH2P(O)(OiPr)2. These two factors probably enable this compound to replace the Li—Cl—Li bridges with Li—O—Li bridges and to push the Cl atoms in to the terminal positions, which HMPA is not capable of doing (Barr et al., 1984b).

The similarity of compounds (I) and (II) was examined as follows. The core of (I), O4/Li1/O1/Li2/O2/Li3/O3, was fixed in space and the relevant core of (II) was matched to it in three positions, firstly with O1/O2/O3 from (I) matched with O1/O2/O3 from (II), then with O1/O2/O3 from (I) matched with O2/O3/O1 from (II), and finally with O1/O2/O3 from (I) matched with O3/O1/O2 from (II). This is almost equivalent to rotation of (II) around the P4—O4 bond. The root mean square deviations of the core atoms were 0.0899, 0.0532 and 0.0359 Å, respectively. Fig. 3 illustrates the best overlap of molecules of (I) and (II) (the third case). Thus, the two cores are similar. However, the presence of toluene in (I) causes different conformations of the Et groups in the Et3P═O moieties.

Related literature top

For related literature, see: Allen (2002); Barr et al. (1984a, 1984b); Bauer et al. (1960); Bock et al. (2000); Fritz et al. (1987); Hahn & Rupprecht (1991); Henderson et al. (2003); Nassar et al. (2004); Purcell & Kotz (1977); Rao et al. (1984); Raston et al. (1988).

Experimental top

All experimental manipulations were performed under an argon atmosphere using standard Schlenk techniques. All solvents were carefully dried and deoxidized. In spite of the use of Schlenk techniques, (I) and (II) are probably the oxidation products of the reaction mixtures of tBu2P—P(SiMe3)Li (Fritz et al., 1987) with [(Et3P)2NiCl2].

Compound (I) was prepared as follows. tBu2P—P(SiMe3)Li (0.266 g, 0.665 mmol) in tetrahydrofuran (THF; 2 ml) was slowly added dropwise via syringe to a solution of [(Et3P)2NiCl2] (0.134 g, 0.366 mmol) in THF (2 ml) at 233 K. The THF was evaporated under vacuum. The residue was dissolved in toluene (3 ml), filtered and evaporated to 1 ml. After one month at ambient temperature, a small quantity of colourless crystals of (I) were deposited.

Compound (II) was prepared as follows. A solution of [(Et3P)2NiCl2] (0.147 g, 0.400 mmol) in THF (2 ml) was slowly added dropwise via syringe to tBu2P—P(SiMe3)Li (0.329 g, 0.795 mmol) in THF (3 ml) at ambient temperature. The THF was evaporated under vacuum. The residue was dissolved in THF (1 ml), filtered and left to stand at ambient temperature. After two weeks, a small quantity of colourless crystals of (II) were deposited near the neck of the Schlenk vessel.

Refinement top

All H atoms were refined as riding on their parent atoms, with methyl C—H = 0.98 Å, methylene C—H = 0.99 Å and aromatic C—H = 0.95 Å, and with Uiso(H) = 1.2Ueq(C) for aromatic and methylene C—H, 1.3Ueq(C) for CH2 groups and 1.5Ueq(C) for methyl groups.

Computing details top

For both compounds, data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. All H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The molecular structure of (II), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. All H atoms have been omitted for clarity.
[Figure 3] Fig. 3. The best overlap of (I), [(LiCl)3(Et3PO)4].toluene (dark grey), and (II), [(LiCl)3(Et3PO)4] (light grey).
(I) trichlorido(µ3-triethylphosphine oxide-κ3O:O:O)tris(µ2-triethylphosphine oxide-κ2O:O)trilithium(I) toluene solvate top
Crystal data top
[Li3Cl3(C6H15OP)4]·C7H8F(000) = 1624
Mr = 755.9Dx = 1.162 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 14410 reflections
a = 11.3414 (7) Åθ = 2.2–32.5°
b = 32.9899 (19) ŵ = 0.39 mm−1
c = 16.100 (1) ÅT = 120 K
β = 134.162 (3)°Prism, colourless
V = 4321.3 (5) Å30.3 × 0.2 × 0.1 mm
Z = 4
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		Rint = 0.06
Graphite monochromatorθmax = 25.1°, θmin = 2.2°
ω scans, 0.75 deg widthh = −13→13
29430 measured reflectionsk = −39→39
7657 independent reflectionsl = −16→19
5468 reflections with I > 2σ(I)
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.06Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0438P)2 + 6.5385P]
where P = (Fo2 + 2Fc2)/3
7657 reflections(Δ/σ)max = 0.001
419 parametersΔρmax = 0.93 e Å−3
0 restraintsΔρmin = −0.49 e Å−3
Crystal data top
[Li3Cl3(C6H15OP)4]·C7H8V = 4321.3 (5) Å3
Mr = 755.9Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.3414 (7) ŵ = 0.39 mm−1
b = 32.9899 (19) ÅT = 120 K
c = 16.100 (1) Å0.3 × 0.2 × 0.1 mm
β = 134.162 (3)°
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		5468 reflections with I > 2σ(I)
29430 measured reflectionsRint = 0.06
7657 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.060 restraints
wR(F2) = 0.127H-atom parameters constrained
S = 1.06Δρmax = 0.93 e Å−3
7657 reflectionsΔρmin = −0.49 e Å−3
419 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
Cl11.13713 (12)0.13798 (3)1.33835 (8)0.0377 (3)
Cl20.36644 (11)0.08998 (3)0.93977 (9)0.0312 (3)
Cl30.66269 (12)0.23318 (3)0.84637 (8)0.0333 (3)
P10.80135 (11)0.03679 (3)1.09962 (8)0.0215 (3)
P20.41313 (11)0.12871 (3)0.71391 (8)0.0223 (3)
P31.06489 (12)0.16585 (3)1.04556 (8)0.0258 (3)
P40.66900 (11)0.19583 (3)1.11529 (8)0.0198 (3)
O10.7896 (3)0.08209 (7)1.0831 (2)0.0258 (8)
O20.5439 (3)0.13307 (8)0.8435 (2)0.0261 (8)
O30.9336 (3)0.15388 (7)1.0421 (2)0.0250 (8)
O40.7093 (3)0.16540 (7)1.06735 (19)0.0191 (7)
C10.6931 (4)0.01074 (11)0.9650 (3)0.0265 (12)
C20.7621 (5)0.01953 (14)0.9127 (4)0.0407 (16)
C31.0123 (4)0.02053 (11)1.2015 (3)0.0301 (12)
C41.0372 (5)−0.02550 (12)1.2148 (4)0.0364 (12)
C50.7084 (4)0.01932 (11)1.1483 (3)0.0260 (12)
C60.7959 (7)0.03310 (16)1.2705 (4)0.0548 (19)
C70.2600 (5)0.16786 (12)0.6430 (3)0.0321 (12)
C80.1553 (5)0.16662 (14)0.6708 (4)0.0429 (16)
C90.3113 (4)0.08063 (11)0.6766 (3)0.0267 (12)
C100.1635 (5)0.07355 (12)0.5473 (3)0.0347 (12)
C110.4983 (4)0.13179 (12)0.6531 (3)0.0298 (11)
C120.6204 (5)0.09787 (13)0.6935 (4)0.0381 (12)
C131.1356 (5)0.21696 (12)1.0956 (3)0.0350 (12)
C141.2430 (6)0.22151 (13)1.2260 (4)0.0477 (16)
C151.2400 (5)0.13346 (12)1.1405 (3)0.0343 (12)
C161.2083 (6)0.09008 (13)1.0978 (4)0.0475 (16)
C170.9878 (5)0.16287 (14)0.9029 (3)0.0375 (14)
C181.1105 (6)0.17252 (16)0.8949 (4)0.0520 (17)
C190.6179 (5)0.17157 (12)1.1864 (3)0.0306 (12)
C200.7631 (7)0.15229 (16)1.3021 (4)0.060 (2)
C210.4952 (5)0.22563 (12)0.9980 (3)0.0296 (12)
C220.4501 (6)0.26074 (13)1.0331 (4)0.0417 (16)
C230.8399 (5)0.22876 (12)1.2176 (3)0.0312 (12)
C240.8808 (6)0.25423 (14)1.1612 (4)0.0509 (17)
C250.6169 (5)0.10110 (13)0.4618 (4)0.0384 (14)
C260.7534 (5)0.08232 (15)0.4942 (4)0.0428 (17)
C270.7574 (6)0.04091 (15)0.4847 (4)0.0449 (17)
C280.6255 (6)0.01766 (14)0.4424 (4)0.0462 (17)
C290.4896 (6)0.03553 (15)0.4095 (4)0.0444 (17)
C300.4849 (5)0.07693 (14)0.4190 (4)0.0425 (16)
C310.6131 (8)0.14606 (14)0.4739 (5)0.066 (2)
Li10.9152 (7)0.13172 (18)1.1452 (5)0.0246 (17)
Li20.5866 (7)0.11439 (17)0.9771 (5)0.0238 (17)
Li30.7107 (7)0.17445 (18)0.9417 (5)0.0257 (17)
H1A0.575950.018840.909010.0341*
H1B0.69856−0.018810.978120.0341*
H2A0.868690.006050.958760.0606*
H2B0.685810.009350.833030.0606*
H2C0.776070.048840.912700.0606*
H3A1.069250.032301.278160.0387*
H3B1.065360.031621.177080.0387*
H4A0.99665−0.037121.142750.0549*
H4B1.15452−0.031601.278430.0549*
H4C0.97650−0.037241.231740.0549*
H5A0.70562−0.010681.146060.0334*
H5B0.593370.029031.093630.0334*
H6A0.811960.062531.276650.0827*
H6B0.728910.025981.286000.0827*
H6C0.902950.019611.326980.0827*
H7A0.186780.165220.558230.0414*
H7B0.315050.194570.666410.0414*
H8A0.226950.168670.754750.0645*
H8B0.077760.189360.632550.0645*
H8C0.094210.141030.642980.0645*
H9A0.274230.078280.716740.0349*
H9B0.392350.058780.706350.0349*
H10A0.198090.075810.506140.0514*
H10B0.118770.046410.535360.0514*
H10C0.078870.093910.517470.0514*
H11A0.554520.158230.674330.0384*
H11B0.407630.130810.567640.0384*
H12A0.562010.071920.662260.0566*
H12B0.673250.103250.665880.0566*
H12C0.704170.096700.778290.0566*
H13A1.039260.235151.053340.0452*
H13B1.199380.225571.077670.0452*
H14A1.352870.210641.268620.0708*
H14B1.251670.250251.244990.0708*
H14C1.193220.206541.247720.0708*
H15A1.277030.133351.217240.0439*
H15B1.330360.144761.150760.0439*
H16A1.190430.089321.028890.0714*
H16B1.303400.073231.158720.0714*
H16C1.110510.079691.078320.0714*
H17A0.893840.181770.851600.0488*
H17B0.945230.135130.872740.0488*
H18A1.204400.154010.945020.0770*
H18B1.057590.169240.814640.0770*
H18C1.148760.200530.919770.0770*
H19A0.534660.150351.134570.0389*
H19B0.567300.191861.198970.0389*
H20A0.835270.173591.359180.0896*
H20B0.723050.135571.328500.0896*
H20C0.824480.135291.293120.0896*
H21A0.398710.207480.945930.0379*
H21B0.517850.236690.953170.0379*
H22A0.543260.279451.083040.0636*
H22B0.354660.275120.963670.0636*
H22C0.423250.250221.075280.0636*
H23A0.937040.212341.280760.0400*
H23B0.814050.246951.252020.0400*
H24A0.794120.274411.109900.0769*
H24B0.986080.268041.221420.0769*
H24C0.888400.236591.116130.0769*
H260.845420.098240.523450.0518*
H270.851940.028520.507510.0537*
H280.62840−0.010870.435970.0556*
H290.397880.019370.379850.0536*
H300.389690.089010.395830.0510*
H31A0.511350.153420.452820.0989*
H31B0.707790.154070.554190.0989*
H31C0.617640.160050.422460.0989*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0268 (5)0.0525 (7)0.0228 (5)0.0030 (5)0.0132 (4)0.0032 (5)
Cl20.0278 (5)0.0270 (5)0.0421 (6)−0.0034 (4)0.0256 (5)0.0000 (4)
Cl30.0387 (6)0.0294 (5)0.0327 (5)0.0007 (4)0.0252 (5)0.0064 (4)
P10.0199 (5)0.0164 (5)0.0250 (5)−0.0011 (4)0.0145 (4)0.0007 (4)
P20.0213 (5)0.0216 (5)0.0194 (5)−0.0020 (4)0.0125 (4)−0.0017 (4)
P30.0254 (5)0.0284 (6)0.0277 (5)−0.0046 (4)0.0200 (5)−0.0023 (4)
P40.0231 (5)0.0178 (5)0.0208 (5)−0.0004 (4)0.0161 (4)−0.0010 (4)
O10.0233 (13)0.0165 (13)0.0333 (14)−0.0017 (11)0.0181 (12)0.0009 (11)
O20.0275 (14)0.0270 (14)0.0214 (13)−0.0068 (11)0.0161 (12)−0.0043 (11)
O30.0235 (13)0.0296 (14)0.0242 (13)−0.0010 (11)0.0175 (12)0.0018 (11)
O40.0219 (13)0.0159 (12)0.0218 (12)−0.0020 (10)0.0161 (11)−0.0021 (10)
C10.027 (2)0.019 (2)0.030 (2)−0.0014 (16)0.0186 (18)−0.0014 (16)
C20.049 (3)0.043 (3)0.039 (2)0.005 (2)0.034 (2)0.006 (2)
C30.024 (2)0.026 (2)0.036 (2)0.0000 (17)0.0193 (19)0.0027 (18)
C40.030 (2)0.030 (2)0.040 (2)0.0086 (18)0.021 (2)0.0074 (19)
C50.029 (2)0.024 (2)0.030 (2)−0.0008 (16)0.0224 (19)0.0009 (16)
C60.077 (4)0.060 (3)0.045 (3)−0.013 (3)0.049 (3)−0.011 (2)
C70.028 (2)0.024 (2)0.032 (2)0.0013 (17)0.0164 (19)−0.0033 (17)
C80.037 (2)0.036 (3)0.058 (3)−0.002 (2)0.034 (2)−0.012 (2)
C90.025 (2)0.027 (2)0.025 (2)−0.0047 (17)0.0163 (18)−0.0035 (17)
C100.029 (2)0.031 (2)0.029 (2)−0.0048 (18)0.0146 (19)−0.0075 (18)
C110.028 (2)0.038 (2)0.0190 (19)−0.0034 (18)0.0148 (17)−0.0004 (18)
C120.040 (2)0.038 (2)0.041 (2)0.003 (2)0.030 (2)0.001 (2)
C130.039 (2)0.027 (2)0.043 (2)−0.0064 (18)0.030 (2)−0.0008 (19)
C140.046 (3)0.030 (2)0.040 (3)−0.010 (2)0.020 (2)−0.008 (2)
C150.034 (2)0.033 (2)0.041 (2)0.0005 (19)0.028 (2)0.0027 (19)
C160.064 (3)0.031 (2)0.056 (3)0.008 (2)0.045 (3)0.007 (2)
C170.040 (2)0.041 (3)0.040 (2)0.002 (2)0.031 (2)0.004 (2)
C180.062 (3)0.062 (3)0.056 (3)0.020 (3)0.050 (3)0.023 (3)
C190.039 (2)0.027 (2)0.039 (2)−0.0032 (18)0.032 (2)−0.0032 (18)
C200.076 (4)0.065 (4)0.067 (3)0.027 (3)0.060 (3)0.036 (3)
C210.032 (2)0.029 (2)0.028 (2)0.0097 (18)0.0210 (19)0.0053 (17)
C220.053 (3)0.036 (2)0.043 (3)0.020 (2)0.036 (2)0.008 (2)
C230.033 (2)0.030 (2)0.029 (2)−0.0079 (18)0.0210 (19)−0.0131 (18)
C240.067 (3)0.040 (3)0.062 (3)−0.030 (2)0.051 (3)−0.023 (2)
C250.048 (3)0.036 (2)0.036 (2)0.002 (2)0.031 (2)0.004 (2)
C260.037 (3)0.050 (3)0.041 (3)−0.009 (2)0.027 (2)0.001 (2)
C270.043 (3)0.050 (3)0.048 (3)0.007 (2)0.034 (2)0.004 (2)
C280.054 (3)0.037 (3)0.047 (3)−0.001 (2)0.035 (3)−0.003 (2)
C290.039 (3)0.049 (3)0.042 (3)−0.008 (2)0.027 (2)−0.002 (2)
C300.039 (3)0.052 (3)0.036 (2)0.013 (2)0.026 (2)0.009 (2)
C310.092 (4)0.036 (3)0.071 (4)0.002 (3)0.057 (4)0.003 (3)
Li10.025 (3)0.023 (3)0.029 (3)0.002 (3)0.020 (3)0.004 (3)
Li20.025 (3)0.017 (3)0.028 (3)−0.007 (3)0.018 (3)−0.003 (3)
Li30.029 (3)0.022 (3)0.030 (3)−0.008 (3)0.022 (3)−0.005 (3)
Geometric parameters (Å, º) top
Cl1—Li12.268 (6)C8—H8B0.9800
Cl2—Li22.270 (9)C8—H8C0.9800
Cl3—Li32.289 (6)C9—H9A0.9900
P1—O11.508 (3)C9—H9B0.9900
P1—C11.799 (4)C10—H10A0.9800
P1—C31.798 (5)C10—H10B0.9800
P1—C51.791 (5)C10—H10C0.9800
P2—O21.504 (2)C11—H11A0.9900
P2—C71.796 (5)C11—H11B0.9900
P2—C91.801 (4)C12—H12A0.9800
P2—C111.794 (6)C12—H12B0.9800
P3—O31.504 (4)C12—H12C0.9800
P3—C131.799 (4)C13—H13A0.9900
P3—C151.787 (5)C13—H13B0.9900
P3—C171.803 (4)C14—H14A0.9800
P4—O41.518 (3)C14—H14B0.9800
P4—C191.792 (6)C14—H14C0.9800
P4—C211.798 (4)C15—H15A0.9900
P4—C231.789 (5)C15—H15B0.9900
O1—Li11.930 (7)C16—H16A0.9800
O1—Li21.968 (8)C16—H16B0.9800
O2—Li21.947 (8)C16—H16C0.9800
O2—Li31.943 (7)C17—H17A0.9900
O3—Li11.953 (9)C17—H17B0.9900
O3—Li31.942 (9)C18—H18A0.9800
O4—Li12.045 (9)C18—H18B0.9800
O4—Li22.016 (6)C18—H18C0.9800
O4—Li32.056 (9)C19—H19A0.9900
C1—C21.524 (9)C19—H19B0.9900
C3—C41.532 (5)C20—H20A0.9800
C5—C61.530 (6)C20—H20B0.9800
C7—C81.534 (10)C20—H20C0.9800
C9—C101.528 (5)C21—H21A0.9900
C11—C121.529 (7)C21—H21B0.9900
C13—C141.533 (6)C22—H22A0.9800
C15—C161.518 (6)C22—H22B0.9800
C17—C181.518 (10)C22—H22C0.9800
C19—C201.521 (6)C23—H23A0.9900
C21—C221.525 (8)C23—H23B0.9900
C23—C241.527 (9)C24—H24A0.9800
C1—H1A0.9900C24—H24B0.9800
C1—H1B0.9900C24—H24C0.9800
C2—H2A0.9800C25—C261.388 (9)
C2—H2B0.9800C25—C301.384 (9)
C2—H2C0.9800C25—C311.501 (6)
C3—H3A0.9900C26—C271.379 (7)
C3—H3B0.9900C27—C281.368 (10)
C4—H4A0.9800C28—C291.366 (10)
C4—H4B0.9800C29—C301.380 (7)
C4—H4C0.9800C26—H260.9500
C5—H5A0.9900C27—H270.9500
C5—H5B0.9900C28—H280.9500
C6—H6A0.9800C29—H290.9500
C6—H6B0.9800C30—H300.9500
C6—H6C0.9800C31—H31A0.9800
C7—H7A0.9900C31—H31B0.9800
C7—H7B0.9900C31—H31C0.9800
C8—H8A0.9800
O1—P1—C1111.03 (16)C11—C12—H12B109.00
O1—P1—C3110.77 (19)H12A—C12—H12B109.00
O1—P1—C5112.9 (2)H12A—C12—H12C109.00
C1—P1—C3108.3 (2)H12B—C12—H12C109.00
C1—P1—C5104.9 (2)P3—C13—H13B109.00
C3—P1—C5108.6 (2)C14—C13—H13A109.00
O2—P2—C7113.29 (18)C14—C13—H13B109.00
O2—P2—C9109.29 (17)P3—C13—H13A109.00
O2—P2—C11111.5 (2)H13A—C13—H13B108.00
C7—P2—C9108.1 (2)H14A—C14—H14C109.00
C7—P2—C11105.2 (2)C13—C14—H14B109.00
C9—P2—C11109.4 (2)H14B—C14—H14C110.00
O3—P3—C13112.6 (2)C13—C14—H14A109.00
O3—P3—C15110.9 (2)C13—C14—H14C109.00
O3—P3—C17110.5 (2)H14A—C14—H14B109.00
C13—P3—C15107.1 (2)P3—C15—H15B109.00
C13—P3—C17106.9 (2)P3—C15—H15A109.00
C15—P3—C17108.7 (2)C16—C15—H15B109.00
O4—P4—C19112.05 (19)H15A—C15—H15B108.00
O4—P4—C21109.01 (18)C16—C15—H15A109.00
O4—P4—C23110.7 (2)C15—C16—H16C109.00
C19—P4—C21108.0 (3)H16A—C16—H16B110.00
C19—P4—C23107.9 (2)C15—C16—H16A110.00
C21—P4—C23109.07 (19)C15—C16—H16B109.00
P1—O1—Li1143.8 (3)H16B—C16—H16C109.00
P1—O1—Li2126.6 (3)H16A—C16—H16C109.00
Li1—O1—Li289.2 (3)P3—C17—H17A108.00
P2—O2—Li2138.5 (3)H17A—C17—H17B107.00
P2—O2—Li3131.0 (3)C18—C17—H17B108.00
Li2—O2—Li388.4 (3)P3—C17—H17B108.00
P3—O3—Li1139.1 (3)C18—C17—H17A108.00
P3—O3—Li3128.4 (3)C17—C18—H18A110.00
Li1—O3—Li389.4 (4)H18B—C18—H18C109.00
P4—O4—Li1131.9 (2)C17—C18—H18C110.00
P4—O4—Li2128.1 (4)H18A—C18—H18B109.00
P4—O4—Li3128.0 (2)C17—C18—H18B109.00
Li1—O4—Li284.7 (3)H18A—C18—H18C109.00
Li1—O4—Li383.9 (3)P4—C19—H19A109.00
Li2—O4—Li383.5 (3)P4—C19—H19B109.00
P1—C1—C2113.1 (3)C20—C19—H19A109.00
P1—C3—C4114.9 (3)C20—C19—H19B109.00
P1—C5—C6114.5 (4)H19A—C19—H19B108.00
P2—C7—C8113.4 (3)H20B—C20—H20C109.00
P2—C9—C10115.4 (3)H20A—C20—H20C109.00
P2—C11—C12113.5 (3)H20A—C20—H20B109.00
P3—C13—C14112.7 (3)C19—C20—H20A109.00
P3—C15—C16113.9 (3)C19—C20—H20B109.00
P3—C17—C18115.9 (3)C19—C20—H20C109.00
P4—C19—C20114.4 (5)P4—C21—H21B108.00
P4—C21—C22115.6 (3)P4—C21—H21A108.00
P4—C23—C24111.7 (3)C22—C21—H21A108.00
H1A—C1—H1B108.00C22—C21—H21B108.00
P1—C1—H1B109.00H21A—C21—H21B108.00
C2—C1—H1A109.00C21—C22—H22A110.00
P1—C1—H1A109.00C21—C22—H22B110.00
C2—C1—H1B109.00C21—C22—H22C110.00
C1—C2—H2A109.00H22A—C22—H22B109.00
C1—C2—H2B109.00H22A—C22—H22C109.00
C1—C2—H2C109.00H22B—C22—H22C109.00
H2A—C2—H2B110.00P4—C23—H23A109.00
H2A—C2—H2C109.00P4—C23—H23B109.00
H2B—C2—H2C109.00C24—C23—H23A109.00
C4—C3—H3B109.00C24—C23—H23B109.00
H3A—C3—H3B108.00H23A—C23—H23B108.00
C4—C3—H3A109.00C23—C24—H24A109.00
P1—C3—H3A109.00H24B—C24—H24C109.00
P1—C3—H3B109.00C23—C24—H24C109.00
H4B—C4—H4C109.00H24A—C24—H24B109.00
C3—C4—H4C110.00C23—C24—H24B109.00
C3—C4—H4A109.00H24A—C24—H24C109.00
C3—C4—H4B109.00C26—C25—C30117.8 (4)
H4A—C4—H4B109.00C26—C25—C31121.2 (6)
H4A—C4—H4C109.00C30—C25—C31121.0 (6)
P1—C5—H5A109.00C25—C26—C27121.0 (6)
C6—C5—H5A109.00C26—C27—C28120.1 (7)
C6—C5—H5B109.00C27—C28—C29119.9 (5)
P1—C5—H5B109.00C28—C29—C30120.3 (6)
H5A—C5—H5B108.00C25—C30—C29120.9 (6)
C5—C6—H6C109.00C25—C26—H26119.00
H6A—C6—H6B110.00C27—C26—H26120.00
C5—C6—H6A109.00C26—C27—H27120.00
C5—C6—H6B109.00C28—C27—H27120.00
H6A—C6—H6C109.00C27—C28—H28120.00
H6B—C6—H6C110.00C29—C28—H28120.00
H7A—C7—H7B108.00C30—C29—H29120.00
C8—C7—H7A109.00C28—C29—H29120.00
C8—C7—H7B109.00C29—C30—H30120.00
P2—C7—H7A109.00C25—C30—H30120.00
P2—C7—H7B109.00H31B—C31—H31C109.00
H8B—C8—H8C109.00C25—C31—H31C109.00
C7—C8—H8B110.00C25—C31—H31A109.00
C7—C8—H8C110.00C25—C31—H31B109.00
C7—C8—H8A110.00H31A—C31—H31B110.00
H8A—C8—H8C109.00H31A—C31—H31C109.00
H8A—C8—H8B109.00Cl1—Li1—O3117.2 (4)
C10—C9—H9B108.00Cl1—Li1—O1120.1 (3)
C10—C9—H9A108.00O1—Li1—O3110.8 (3)
P2—C9—H9B108.00O1—Li1—O491.6 (4)
P2—C9—H9A108.00Cl1—Li1—O4119.6 (3)
H9A—C9—H9B107.00O3—Li1—O491.6 (3)
H10B—C10—H10C109.00Cl2—Li2—O2116.0 (3)
C9—C10—H10A109.00Cl2—Li2—O4124.5 (4)
C9—C10—H10B109.00Cl2—Li2—O1116.4 (3)
C9—C10—H10C109.00O1—Li2—O491.4 (3)
H10A—C10—H10B109.00O2—Li2—O492.7 (3)
H10A—C10—H10C109.00O1—Li2—O2111.7 (5)
C12—C11—H11A109.00O2—Li3—O491.6 (4)
P2—C11—H11A109.00O3—Li3—O491.6 (3)
P2—C11—H11B109.00Cl3—Li3—O2114.0 (3)
C12—C11—H11B109.00Cl3—Li3—O3114.7 (4)
H11A—C11—H11B108.00Cl3—Li3—O4128.4 (3)
C11—C12—H12C109.00O2—Li3—O3113.4 (3)
C11—C12—H12A109.00
C1—P1—O1—Li1−133.3 (6)Li2—O1—Li1—O3−78.8 (4)
C1—P1—O1—Li257.4 (4)Li2—O1—Li1—O413.5 (3)
C3—P1—O1—Li1−12.9 (6)P1—O1—Li2—Cl229.9 (5)
C3—P1—O1—Li2177.8 (4)P1—O1—Li2—O2−106.5 (4)
C5—P1—O1—Li1109.2 (6)P1—O1—Li2—O4160.0 (3)
C5—P1—O1—Li2−60.2 (4)Li1—O1—Li2—Cl2−143.8 (4)
O1—P1—C1—C261.4 (4)Li1—O1—Li2—O279.8 (4)
C3—P1—C1—C2−60.4 (3)Li1—O1—Li2—O4−13.7 (4)
C5—P1—C1—C2−176.3 (3)P2—O2—Li2—Cl2−17.2 (6)
O1—P1—C3—C4−173.7 (3)P2—O2—Li2—O1119.3 (4)
C1—P1—C3—C4−51.8 (4)P2—O2—Li2—O4−148.1 (3)
C5—P1—C3—C461.7 (4)Li3—O2—Li2—Cl2146.0 (4)
O1—P1—C5—C6−66.8 (4)Li3—O2—Li2—O1−77.4 (4)
C1—P1—C5—C6172.2 (3)Li3—O2—Li2—O415.1 (4)
C3—P1—C5—C656.5 (4)P2—O2—Li3—Cl316.7 (7)
C7—P2—O2—Li291.9 (5)P2—O2—Li3—O3−117.0 (4)
C7—P2—O2—Li3−65.7 (5)P2—O2—Li3—O4150.5 (3)
C9—P2—O2—Li2−28.7 (5)Li2—O2—Li3—Cl3−148.7 (5)
C9—P2—O2—Li3173.8 (4)Li2—O2—Li3—O377.6 (5)
C11—P2—O2—Li2−149.7 (4)Li2—O2—Li3—O4−14.8 (3)
C11—P2—O2—Li352.7 (5)P3—O3—Li1—Cl120.5 (6)
O2—P2—C7—C8−65.9 (4)P3—O3—Li1—O1−122.5 (4)
C9—P2—C7—C855.3 (3)P3—O3—Li1—O4145.2 (3)
C11—P2—C7—C8172.1 (3)Li3—O3—Li1—Cl1−139.1 (4)
O2—P2—C9—C10174.2 (4)Li3—O3—Li1—O178.0 (4)
C7—P2—C9—C1050.5 (5)Li3—O3—Li1—O4−14.3 (3)
C11—P2—C9—C10−63.5 (4)P3—O3—Li3—Cl3−14.6 (5)
O2—P2—C11—C1262.7 (3)P3—O3—Li3—O2118.8 (4)
C7—P2—C11—C12−174.1 (3)P3—O3—Li3—O4−148.8 (2)
C9—P2—C11—C12−58.3 (3)Li1—O3—Li3—Cl3148.4 (3)
C13—P3—O3—Li1−86.0 (4)Li1—O3—Li3—O2−78.2 (4)
C13—P3—O3—Li367.5 (3)Li1—O3—Li3—O414.2 (3)
C15—P3—O3—Li134.0 (4)P4—O4—Li1—Cl1−1.0 (6)
C15—P3—O3—Li3−172.5 (3)P4—O4—Li1—O1125.4 (3)
C17—P3—O3—Li1154.5 (4)P4—O4—Li1—O3−123.8 (3)
C17—P3—O3—Li3−51.9 (3)Li2—O4—Li1—Cl1−139.6 (4)
O3—P3—C13—C1472.9 (5)Li2—O4—Li1—O1−13.3 (3)
C15—P3—C13—C14−49.2 (6)Li2—O4—Li1—O397.6 (3)
C17—P3—C13—C14−165.6 (5)Li3—O4—Li1—Cl1136.4 (4)
O3—P3—C15—C1667.7 (5)Li3—O4—Li1—O1−97.2 (3)
C13—P3—C15—C16−169.1 (4)Li3—O4—Li1—O313.6 (3)
C17—P3—C15—C16−54.0 (5)P4—O4—Li2—Cl2−4.5 (5)
O3—P3—C17—C18−177.6 (3)P4—O4—Li2—O1−128.3 (3)
C13—P3—C17—C1859.7 (4)P4—O4—Li2—O2119.9 (3)
C15—P3—C17—C18−55.7 (4)Li1—O4—Li2—Cl2136.7 (4)
C19—P4—O4—Li1−77.8 (4)Li1—O4—Li2—O113.0 (3)
C19—P4—O4—Li245.4 (3)Li1—O4—Li2—O2−98.8 (4)
C19—P4—O4—Li3160.9 (4)Li3—O4—Li2—Cl2−138.8 (4)
C21—P4—O4—Li1162.7 (4)Li3—O4—Li2—O197.4 (4)
C21—P4—O4—Li2−74.2 (3)Li3—O4—Li2—O2−14.4 (4)
C21—P4—O4—Li341.4 (4)P4—O4—Li3—Cl32.8 (7)
C23—P4—O4—Li142.7 (4)P4—O4—Li3—O2−120.0 (3)
C23—P4—O4—Li2165.9 (3)P4—O4—Li3—O3126.6 (3)
C23—P4—O4—Li3−78.6 (4)Li1—O4—Li3—Cl3−137.4 (5)
O4—P4—C19—C2071.9 (3)Li1—O4—Li3—O299.8 (3)
C21—P4—C19—C20−168.0 (3)Li1—O4—Li3—O3−13.7 (3)
C23—P4—C19—C20−50.2 (4)Li2—O4—Li3—Cl3137.2 (5)
O4—P4—C21—C22−173.7 (4)Li2—O4—Li3—O214.4 (3)
C19—P4—C21—C2264.3 (5)Li2—O4—Li3—O3−99.0 (3)
C23—P4—C21—C22−52.8 (5)C30—C25—C26—C27−0.4 (7)
O4—P4—C23—C2463.2 (4)C31—C25—C26—C27178.9 (5)
C19—P4—C23—C24−173.9 (4)C26—C25—C30—C290.3 (8)
C21—P4—C23—C24−56.8 (5)C31—C25—C30—C29−179.1 (5)
P1—O1—Li1—Cl1−32.0 (9)C25—C26—C27—C280.3 (8)
P1—O1—Li1—O3109.7 (5)C26—C27—C28—C290.0 (8)
P1—O1—Li1—O4−158.0 (4)C27—C28—C29—C30−0.2 (8)
Li2—O1—Li1—Cl1139.5 (5)C28—C29—C30—C250.0 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5A···Cl2i0.99002.80003.749 (4)160.00
C5—H5B···Cl20.99002.81003.688 (4)148.00
C11—H11B···Cl1ii0.99002.70003.685 (4)170.00
C30—H30···Cl1ii0.95002.82003.763 (7)170.00
Symmetry codes: (i) −x+1, −y, −z+2; (ii) x−1, y, z−1.
(II) trichlorido(µ3-triethylphosphine oxide-κ3O:O:O)tris(µ2-triethylphosphine oxide-κ2O:O)trilithium(I) top
Crystal data top
[Li3Cl3(C6H15OP)4]F(000) = 1424
Mr = 663.77Dx = 1.168 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25086 reflections
a = 12.0507 (4) Åθ = 2.2–32.4°
b = 12.1447 (3) ŵ = 0.44 mm−1
c = 25.8698 (7) ÅT = 120 K
β = 94.564 (2)°Prism, colourless
V = 3774.09 (19) Å30.44 × 0.39 × 0.26 mm
Z = 4
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		6073 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.011
Detector resolution: 8.1883 pixels mm-1θmax = 25.1°, θmin = 2.2°
ω scans, 0.6 deg widthh = −14→13
19943 measured reflectionsk = −14→14
6648 independent reflectionsl = −28→30
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0547P)2 + 1.7432P]
where P = (Fo2 + 2Fc2)/3
6648 reflections(Δ/σ)max = 0.002
355 parametersΔρmax = 0.52 e Å−3
0 restraintsΔρmin = −0.30 e Å−3
Crystal data top
[Li3Cl3(C6H15OP)4]V = 3774.09 (19) Å3
Mr = 663.77Z = 4
Monoclinic, P21/cMo Kα radiation
a = 12.0507 (4) ŵ = 0.44 mm−1
b = 12.1447 (3) ÅT = 120 K
c = 25.8698 (7) Å0.44 × 0.39 × 0.26 mm
β = 94.564 (2)°
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		6073 reflections with I > 2σ(I)
19943 measured reflectionsRint = 0.011
6648 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.092H-atom parameters constrained
S = 1.13Δρmax = 0.52 e Å−3
6648 reflectionsΔρmin = −0.30 e Å−3
355 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
Cl10.46893 (3)0.79903 (3)0.24776 (2)0.0251 (1)
Cl20.27246 (3)0.50901 (3)0.04806 (2)0.0221 (1)
Cl30.00069 (4)0.94288 (4)0.13007 (2)0.0290 (1)
P10.53722 (3)0.65668 (3)0.10305 (2)0.0176 (1)
P20.13554 (3)0.81383 (3)0.00557 (2)0.0163 (1)
P30.34084 (3)1.04647 (3)0.16477 (2)0.0160 (1)
P40.18511 (3)0.63762 (3)0.20395 (2)0.0155 (1)
O10.43210 (9)0.71904 (9)0.11271 (4)0.0206 (3)
O20.19051 (9)0.78643 (9)0.05841 (4)0.0196 (3)
O30.30027 (9)0.93334 (9)0.14814 (4)0.0188 (3)
O40.22513 (9)0.71109 (9)0.16174 (4)0.0163 (3)
C10.54541 (15)0.63129 (15)0.03532 (7)0.0242 (5)
C20.53995 (19)0.73545 (19)0.00238 (8)0.0402 (7)
C30.65719 (14)0.73655 (16)0.12687 (8)0.0284 (5)
C40.77053 (16)0.70392 (19)0.10906 (10)0.0398 (7)
C50.53669 (15)0.52512 (15)0.13495 (8)0.0269 (5)
C60.63267 (18)0.44550 (17)0.12808 (10)0.0429 (7)
C7−0.00840 (14)0.77375 (15)−0.00100 (7)0.0249 (5)
C8−0.02364 (18)0.64922 (17)0.00261 (10)0.0409 (7)
C90.20506 (16)0.74565 (15)−0.04442 (6)0.0260 (5)
C100.1533 (2)0.76764 (18)−0.09942 (7)0.0382 (7)
C110.14065 (15)0.95926 (14)−0.00587 (7)0.0223 (5)
C120.25881 (18)1.00286 (17)−0.00781 (9)0.0378 (7)
C130.31123 (15)1.07984 (15)0.22989 (7)0.0240 (5)
C140.18908 (17)1.10612 (19)0.23619 (9)0.0398 (7)
C150.48965 (14)1.05627 (14)0.16481 (7)0.0229 (5)
C160.53313 (18)1.03958 (18)0.11144 (8)0.0371 (7)
C170.27859 (17)1.15024 (14)0.12222 (7)0.0274 (5)
C180.3148 (2)1.26800 (15)0.13621 (8)0.0397 (7)
C190.28054 (14)0.52599 (14)0.21784 (7)0.0208 (5)
C200.24594 (16)0.44252 (15)0.25809 (8)0.0302 (6)
C210.04952 (14)0.58149 (15)0.18517 (7)0.0246 (5)
C220.04763 (16)0.49732 (17)0.14117 (8)0.0336 (6)
C230.17392 (15)0.71109 (15)0.26363 (7)0.0245 (5)
C240.0927 (2)0.80687 (18)0.25912 (8)0.0454 (8)
Li10.3718 (2)0.7951 (2)0.16896 (11)0.0202 (8)
Li20.2800 (2)0.6729 (2)0.09008 (11)0.0201 (8)
Li30.1659 (2)0.8540 (2)0.12467 (11)0.0201 (8)
H1A0.483490.582000.022910.0314*
H1B0.616040.592470.030410.0314*
H2A0.605630.781020.011690.0603*
H2B0.538180.71543−0.034370.0603*
H2C0.472540.776880.008640.0603*
H3A0.662350.733510.165220.0369*
H3B0.643130.814250.116800.0369*
H4A0.766230.701310.071090.0597*
H4B0.826460.758290.121580.0597*
H4C0.791600.631250.123080.0597*
H5A0.466610.487180.122940.0349*
H5B0.534100.538780.172560.0349*
H6A0.702450.477910.143060.0644*
H6B0.618930.375980.145720.0644*
H6C0.638160.431570.091060.0644*
H7A−0.042550.79982−0.034870.0324*
H7B−0.047840.809810.026570.0324*
H8A0.009830.622950.036120.0613*
H8B−0.103240.63156−0.000530.0613*
H8C0.012720.61324−0.025450.0613*
H9A0.204290.66532−0.037940.0338*
H9B0.283790.76972−0.042170.0338*
H10A0.152980.84704−0.106180.0572*
H10B0.197130.73020−0.124490.0572*
H10C0.076790.73976−0.102790.0572*
H11A0.104550.997980.022000.0290*
H11B0.097680.97613−0.039140.0290*
H12A0.290870.97414−0.038740.0568*
H12B0.257271.08349−0.009190.0568*
H12C0.304300.978970.023260.0568*
H13A0.356991.144120.241710.0312*
H13B0.333931.017050.252740.0312*
H14A0.141961.048360.219580.0596*
H14B0.176941.109700.273160.0596*
H14C0.169981.177170.219860.0596*
H15A0.523991.000370.188930.0297*
H15B0.513511.129690.178100.0297*
H16A0.509411.101350.088810.0556*
H16B0.614621.035970.115030.0556*
H16C0.503230.970740.096270.0556*
H17A0.196651.145320.122590.0356*
H17B0.297591.134390.086440.0356*
H18A0.395911.273830.136230.0595*
H18B0.279541.319210.110630.0595*
H18C0.292131.286370.170720.0595*
H19A0.353730.557210.230280.0270*
H19B0.290410.486240.185120.0270*
H20A0.174480.409290.245920.0453*
H20B0.302730.384860.262880.0453*
H20C0.238530.480080.291160.0453*
H21A−0.001360.642730.174370.0319*
H21B0.020450.546030.215800.0319*
H22A0.085800.430020.153660.0503*
H22B−0.029680.480000.129350.0503*
H22C0.085570.528000.112290.0503*
H23A0.248400.739340.276000.0318*
H23B0.150110.659040.290050.0318*
H24A0.016650.778640.252670.0681*
H24B0.098670.849240.291460.0681*
H24C0.110310.854520.230320.0681*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0265 (2)0.0238 (2)0.0235 (2)0.0013 (2)−0.0064 (2)0.0028 (2)
Cl20.0225 (2)0.0172 (2)0.0268 (2)−0.0006 (2)0.0025 (2)−0.0041 (2)
Cl30.0238 (2)0.0370 (3)0.0257 (2)0.0102 (2)−0.0010 (2)−0.0008 (2)
P10.0151 (2)0.0181 (2)0.0197 (2)0.0013 (2)0.0026 (2)−0.0031 (2)
P20.0196 (2)0.0156 (2)0.0133 (2)0.0024 (2)−0.0007 (2)−0.0007 (2)
P30.0191 (2)0.0130 (2)0.0158 (2)0.0004 (2)0.0012 (2)−0.0012 (2)
P40.0164 (2)0.0160 (2)0.0144 (2)0.0013 (2)0.0025 (2)0.0006 (2)
O10.0175 (6)0.0218 (6)0.0226 (6)0.0025 (4)0.0022 (5)−0.0066 (5)
O20.0242 (6)0.0192 (6)0.0148 (6)0.0051 (5)−0.0017 (4)−0.0013 (4)
O30.0208 (6)0.0141 (5)0.0210 (6)0.0008 (4)−0.0015 (4)−0.0024 (4)
O40.0191 (5)0.0157 (5)0.0142 (5)0.0008 (4)0.0020 (4)0.0006 (4)
C10.0242 (9)0.0279 (9)0.0214 (9)−0.0041 (7)0.0074 (7)−0.0062 (7)
C20.0453 (12)0.0484 (13)0.0267 (10)−0.0126 (10)0.0018 (9)0.0092 (9)
C30.0198 (8)0.0289 (10)0.0358 (10)−0.0035 (7)−0.0014 (7)−0.0085 (8)
C40.0189 (9)0.0440 (12)0.0565 (14)−0.0035 (8)0.0028 (9)−0.0010 (10)
C50.0228 (9)0.0267 (9)0.0314 (10)0.0032 (7)0.0037 (7)0.0070 (8)
C60.0381 (12)0.0271 (10)0.0645 (15)0.0120 (9)0.0096 (10)0.0118 (10)
C70.0219 (8)0.0244 (9)0.0275 (9)−0.0014 (7)−0.0037 (7)−0.0009 (7)
C80.0379 (12)0.0253 (10)0.0583 (14)−0.0095 (9)−0.0030 (10)−0.0037 (9)
C90.0359 (10)0.0268 (9)0.0154 (8)0.0095 (8)0.0026 (7)−0.0024 (7)
C100.0619 (14)0.0368 (11)0.0154 (9)0.0182 (10)0.0003 (9)−0.0030 (8)
C110.0296 (9)0.0175 (8)0.0197 (9)0.0007 (7)0.0013 (7)0.0013 (7)
C120.0424 (12)0.0341 (11)0.0390 (12)−0.0138 (9)0.0156 (9)−0.0054 (9)
C130.0284 (9)0.0245 (9)0.0197 (9)−0.0059 (7)0.0062 (7)−0.0061 (7)
C140.0314 (10)0.0468 (12)0.0434 (12)−0.0086 (9)0.0176 (9)−0.0195 (10)
C150.0206 (8)0.0216 (9)0.0269 (9)−0.0023 (7)0.0053 (7)−0.0021 (7)
C160.0364 (11)0.0424 (12)0.0349 (11)0.0044 (9)0.0183 (9)0.0012 (9)
C170.0392 (10)0.0179 (9)0.0242 (9)0.0056 (7)−0.0037 (8)0.0011 (7)
C180.0656 (14)0.0159 (9)0.0365 (11)0.0046 (9)−0.0027 (10)0.0035 (8)
C190.0204 (8)0.0190 (8)0.0232 (9)0.0035 (6)0.0026 (7)0.0027 (7)
C200.0343 (10)0.0243 (9)0.0324 (10)0.0053 (8)0.0047 (8)0.0114 (8)
C210.0167 (8)0.0306 (9)0.0267 (9)−0.0022 (7)0.0040 (7)0.0036 (8)
C220.0281 (10)0.0442 (12)0.0285 (10)−0.0152 (9)0.0028 (8)−0.0049 (9)
C230.0315 (9)0.0273 (9)0.0152 (8)0.0049 (7)0.0052 (7)−0.0012 (7)
C240.0768 (17)0.0349 (11)0.0253 (11)0.0254 (11)0.0084 (10)−0.0041 (9)
Li10.0223 (14)0.0165 (13)0.0218 (14)0.0014 (11)0.0015 (11)−0.0022 (11)
Li20.0206 (13)0.0186 (13)0.0212 (14)0.0025 (11)0.0017 (11)−0.0022 (11)
Li30.0232 (14)0.0187 (13)0.0180 (14)0.0018 (11)−0.0012 (11)−0.0007 (11)
Geometric parameters (Å, º) top
Cl1—Li12.269 (3)C5—H5A0.9900
Cl2—Li22.266 (3)C5—H5B0.9900
Cl3—Li32.279 (2)C6—H6A0.9800
P1—O11.5136 (11)C6—H6B0.9800
P1—C11.7895 (19)C6—H6C0.9800
P1—C31.8080 (19)C7—H7A0.9900
P1—C51.7985 (19)C7—H7B0.9900
P2—O21.5080 (12)C8—H8A0.9800
P2—C71.7966 (17)C8—H8B0.9800
P2—C91.7979 (18)C8—H8C0.9800
P2—C111.7927 (17)C9—H9A0.9900
P3—O31.5094 (12)C9—H9B0.9900
P3—C131.7959 (19)C10—H10A0.9800
P3—C151.7971 (17)C10—H10B0.9800
P3—C171.7976 (18)C10—H10C0.9800
P4—O41.5182 (12)C11—H11A0.9900
P4—C191.7955 (17)C11—H11B0.9900
P4—C211.8012 (18)C12—H12A0.9800
P4—C231.7975 (19)C12—H12B0.9800
O1—Li11.915 (3)C12—H12C0.9800
O1—Li21.961 (3)C13—H13A0.9900
O2—Li21.896 (3)C13—H13B0.9900
O2—Li31.944 (3)C14—H14A0.9800
O3—Li11.944 (3)C14—H14B0.9800
O3—Li31.940 (3)C14—H14C0.9800
O4—Li12.037 (3)C15—H15A0.9900
O4—Li22.070 (3)C15—H15B0.9900
O4—Li32.082 (3)C16—H16A0.9800
C1—C21.524 (3)C16—H16B0.9800
C3—C41.528 (3)C16—H16C0.9800
C5—C61.529 (3)C17—H17A0.9900
C7—C81.527 (3)C17—H17B0.9900
C9—C101.531 (2)C18—H18A0.9800
C11—C121.524 (3)C18—H18B0.9800
C13—C141.528 (3)C18—H18C0.9800
C15—C161.529 (3)C19—H19A0.9900
C17—C181.530 (3)C19—H19B0.9900
C19—C201.535 (3)C20—H20A0.9800
C21—C221.529 (3)C20—H20B0.9800
C23—C241.519 (3)C20—H20C0.9800
C1—H1A0.9900C21—H21A0.9900
C1—H1B0.9900C21—H21B0.9900
C2—H2A0.9800C22—H22A0.9800
C2—H2B0.9800C22—H22B0.9800
C2—H2C0.9800C22—H22C0.9800
C3—H3A0.9900C23—H23A0.9900
C3—H3B0.9900C23—H23B0.9900
C4—H4A0.9800C24—H24A0.9800
C4—H4B0.9800C24—H24B0.9800
C4—H4C0.9800C24—H24C0.9800
O1—P1—C1111.10 (7)C9—C10—H10A109.00
O1—P1—C3109.41 (8)C9—C10—H10B109.00
O1—P1—C5109.58 (8)C9—C10—H10C109.00
C1—P1—C3108.74 (9)H10A—C10—H10B109.00
C1—P1—C5107.38 (9)H10A—C10—H10C110.00
C3—P1—C5110.62 (9)C12—C11—H11A109.00
O2—P2—C7112.16 (8)P2—C11—H11A109.00
O2—P2—C9110.74 (7)P2—C11—H11B109.00
O2—P2—C11110.41 (8)C12—C11—H11B109.00
C7—P2—C9107.99 (9)H11A—C11—H11B108.00
C7—P2—C11107.27 (8)C11—C12—H12C109.00
C9—P2—C11108.11 (8)C11—C12—H12A109.00
O3—P3—C13112.88 (7)C11—C12—H12B109.00
O3—P3—C15111.16 (7)H12A—C12—H12B109.00
O3—P3—C17110.71 (8)H12A—C12—H12C109.00
C13—P3—C15104.91 (8)H12B—C12—H12C109.00
C13—P3—C17108.17 (8)P3—C13—H13B109.00
C15—P3—C17108.77 (9)C14—C13—H13A109.00
O4—P4—C19110.65 (7)C14—C13—H13B109.00
O4—P4—C21111.20 (8)P3—C13—H13A109.00
O4—P4—C23112.08 (7)H13A—C13—H13B108.00
C19—P4—C21108.73 (8)H14A—C14—H14C109.00
C19—P4—C23107.07 (9)C13—C14—H14B109.00
C21—P4—C23106.92 (8)H14B—C14—H14C109.00
P1—O1—Li1137.73 (10)C13—C14—H14A109.00
P1—O1—Li2125.62 (10)C13—C14—H14C109.00
Li1—O1—Li287.85 (12)H14A—C14—H14B109.00
P2—O2—Li2138.24 (11)P3—C15—H15B109.00
P2—O2—Li3128.26 (10)P3—C15—H15A109.00
Li2—O2—Li392.72 (12)C16—C15—H15B109.00
P3—O3—Li1125.51 (10)H15A—C15—H15B108.00
P3—O3—Li3141.70 (10)C16—C15—H15A109.00
Li1—O3—Li389.91 (11)C15—C16—H16C109.00
P4—O4—Li1123.47 (10)H16A—C16—H16B109.00
P4—O4—Li2130.91 (10)C15—C16—H16A109.00
P4—O4—Li3134.79 (10)C15—C16—H16B109.00
Li1—O4—Li281.82 (11)H16B—C16—H16C109.00
Li1—O4—Li383.56 (11)H16A—C16—H16C109.00
Li2—O4—Li384.06 (11)P3—C17—H17A109.00
P1—C1—C2113.66 (13)H17A—C17—H17B108.00
P1—C3—C4117.89 (15)C18—C17—H17B109.00
P1—C5—C6118.57 (14)P3—C17—H17B109.00
P2—C7—C8112.48 (13)C18—C17—H17A109.00
P2—C9—C10114.17 (14)C17—C18—H18A109.00
P2—C11—C12113.10 (13)H18B—C18—H18C109.00
P3—C13—C14114.35 (14)C17—C18—H18C109.00
P3—C15—C16113.85 (13)H18A—C18—H18B109.00
P3—C17—C18114.40 (14)C17—C18—H18B109.00
P4—C19—C20115.49 (12)H18A—C18—H18C109.00
P4—C21—C22114.42 (12)P4—C19—H19A108.00
P4—C23—C24113.96 (13)P4—C19—H19B108.00
H1A—C1—H1B108.00C20—C19—H19A108.00
P1—C1—H1B109.00C20—C19—H19B108.00
C2—C1—H1A109.00H19A—C19—H19B107.00
P1—C1—H1A109.00H20B—C20—H20C109.00
C2—C1—H1B109.00H20A—C20—H20C109.00
C1—C2—H2A109.00H20A—C20—H20B109.00
C1—C2—H2B109.00C19—C20—H20A109.00
C1—C2—H2C109.00C19—C20—H20B109.00
H2A—C2—H2B109.00C19—C20—H20C109.00
H2A—C2—H2C109.00P4—C21—H21B109.00
H2B—C2—H2C109.00P4—C21—H21A109.00
C4—C3—H3B108.00C22—C21—H21A109.00
H3A—C3—H3B107.00C22—C21—H21B109.00
C4—C3—H3A108.00H21A—C21—H21B108.00
P1—C3—H3A108.00C21—C22—H22A109.00
P1—C3—H3B108.00C21—C22—H22B109.00
H4B—C4—H4C109.00C21—C22—H22C109.00
C3—C4—H4C109.00H22A—C22—H22B109.00
C3—C4—H4A109.00H22A—C22—H22C109.00
C3—C4—H4B109.00H22B—C22—H22C109.00
H4A—C4—H4B109.00P4—C23—H23A109.00
H4A—C4—H4C109.00P4—C23—H23B109.00
P1—C5—H5A108.00C24—C23—H23A109.00
C6—C5—H5A108.00C24—C23—H23B109.00
C6—C5—H5B108.00H23A—C23—H23B108.00
P1—C5—H5B108.00C23—C24—H24A109.00
H5A—C5—H5B107.00H24B—C24—H24C109.00
C5—C6—H6C109.00C23—C24—H24C109.00
H6A—C6—H6B109.00H24A—C24—H24B109.00
C5—C6—H6A109.00C23—C24—H24B109.00
C5—C6—H6B109.00H24A—C24—H24C109.00
H6A—C6—H6C109.00Cl1—Li1—O3114.61 (12)
H6B—C6—H6C109.00Cl1—Li1—O4118.35 (13)
H7A—C7—H7B108.00Cl1—Li1—O1119.54 (12)
C8—C7—H7A109.00O1—Li1—O3113.13 (15)
C8—C7—H7B109.00O1—Li1—O493.88 (12)
P2—C7—H7A109.00O3—Li1—O492.57 (11)
P2—C7—H7B109.00Cl2—Li2—O4128.53 (12)
H8B—C8—H8C109.00O1—Li2—O2114.03 (13)
C7—C8—H8B109.00O1—Li2—O491.50 (12)
C7—C8—H8C109.00Cl2—Li2—O1113.27 (12)
C7—C8—H8A109.00Cl2—Li2—O2115.58 (13)
H8A—C8—H8C109.00O2—Li2—O490.73 (11)
H8A—C8—H8B109.00O2—Li3—O489.05 (11)
C10—C9—H9B109.00O3—Li3—O491.31 (11)
C10—C9—H9A109.00Cl3—Li3—O2116.70 (13)
P2—C9—H9B109.00Cl3—Li3—O3117.20 (12)
P2—C9—H9A109.00Cl3—Li3—O4129.49 (13)
H9A—C9—H9B108.00O2—Li3—O3107.67 (13)
H10B—C10—H10C109.00
C1—P1—O1—Li1−168.35 (15)P1—O1—Li1—Cl1−2.4 (2)
C1—P1—O1—Li255.64 (14)P1—O1—Li1—O3137.26 (12)
C3—P1—O1—Li1−48.28 (17)P1—O1—Li1—O4−128.28 (12)
C3—P1—O1—Li2175.70 (13)Li2—O1—Li1—Cl1143.16 (14)
C5—P1—O1—Li173.16 (16)Li2—O1—Li1—O3−77.14 (14)
C5—P1—O1—Li2−62.86 (14)Li2—O1—Li1—O417.32 (12)
O1—P1—C1—C256.88 (16)P1—O1—Li2—Cl21.53 (19)
C3—P1—C1—C2−63.58 (16)P1—O1—Li2—O2−133.40 (12)
C5—P1—C1—C2176.69 (14)P1—O1—Li2—O4135.13 (9)
O1—P1—C3—C4−164.67 (15)Li1—O1—Li2—Cl2−150.60 (14)
C1—P1—C3—C4−43.17 (18)Li1—O1—Li2—O274.47 (16)
C5—P1—C3—C474.51 (18)Li1—O1—Li2—O4−17.00 (11)
O1—P1—C5—C6176.93 (15)P2—O2—Li2—Cl2−21.0 (2)
C1—P1—C5—C656.15 (18)P2—O2—Li2—O1112.89 (16)
C3—P1—C5—C6−62.36 (18)P2—O2—Li2—O4−155.14 (11)
C7—P2—O2—Li296.91 (16)Li3—O2—Li2—Cl2148.72 (13)
C7—P2—O2—Li3−69.93 (14)Li3—O2—Li2—O1−77.43 (15)
C9—P2—O2—Li2−23.81 (17)Li3—O2—Li2—O414.54 (11)
C9—P2—O2—Li3169.36 (13)P2—O2—Li3—Cl322.08 (19)
C11—P2—O2—Li2−143.52 (15)P2—O2—Li3—O3−112.12 (13)
C11—P2—O2—Li349.65 (14)P2—O2—Li3—O4156.81 (9)
O2—P2—C7—C8−64.24 (16)Li2—O2—Li3—Cl3−149.18 (13)
C9—P2—C7—C858.05 (16)Li2—O2—Li3—O376.61 (14)
C11—P2—C7—C8174.37 (15)Li2—O2—Li3—O4−14.46 (11)
O2—P2—C9—C10179.10 (13)P3—O3—Li1—Cl128.67 (18)
C7—P2—C9—C1055.94 (16)P3—O3—Li1—O1−113.09 (13)
C11—P2—C9—C10−59.83 (16)P3—O3—Li1—O4151.58 (9)
O2—P2—C11—C1264.26 (15)Li3—O3—Li1—Cl1−135.68 (13)
C7—P2—C11—C12−173.26 (14)Li3—O3—Li1—O182.56 (15)
C9—P2—C11—C12−57.03 (16)Li3—O3—Li1—O4−12.77 (12)
C13—P3—O3—Li1−76.59 (14)P3—O3—Li3—Cl3−10.1 (3)
C13—P3—O3—Li377.61 (18)P3—O3—Li3—O2123.81 (14)
C15—P3—O3—Li140.98 (14)P3—O3—Li3—O4−146.77 (12)
C15—P3—O3—Li3−164.83 (17)Li1—O3—Li3—Cl3149.11 (15)
C17—P3—O3—Li1161.99 (13)Li1—O3—Li3—O2−76.95 (14)
C17—P3—O3—Li3−43.82 (19)Li1—O3—Li3—O412.48 (12)
O3—P3—C13—C14−73.91 (15)P4—O4—Li1—Cl1−9.01 (18)
C15—P3—C13—C14164.91 (14)P4—O4—Li1—O1117.73 (11)
C17—P3—C13—C1448.95 (16)P4—O4—Li1—O3−128.87 (10)
O3—P3—C15—C1662.22 (15)Li2—O4—Li1—Cl1−143.29 (14)
C13—P3—C15—C16−175.48 (13)Li2—O4—Li1—O1−16.55 (11)
C17—P3—C15—C16−59.93 (15)Li2—O4—Li1—O396.85 (12)
O3—P3—C17—C18179.88 (13)Li3—O4—Li1—Cl1131.82 (14)
C13—P3—C17—C1855.72 (17)Li3—O4—Li1—O1−101.44 (12)
C15—P3—C17—C18−57.70 (17)Li3—O4—Li1—O311.96 (12)
C19—P4—O4—Li1−61.54 (13)P4—O4—Li2—Cl210.1 (2)
C19—P4—O4—Li248.77 (14)P4—O4—Li2—O1−111.67 (12)
C19—P4—O4—Li3−179.37 (14)P4—O4—Li2—O2134.27 (10)
C21—P4—O4—Li1177.51 (11)Li1—O4—Li2—Cl2137.85 (16)
C21—P4—O4—Li2−72.18 (14)Li1—O4—Li2—O116.12 (10)
C21—P4—O4—Li359.68 (15)Li1—O4—Li2—O2−97.94 (11)
C23—P4—O4—Li157.89 (13)Li3—O4—Li2—Cl2−137.83 (16)
C23—P4—O4—Li2168.20 (13)Li3—O4—Li2—O1100.44 (11)
C23—P4—O4—Li3−59.94 (15)Li3—O4—Li2—O2−13.63 (10)
O4—P4—C19—C20−177.04 (12)P4—O4—Li3—Cl3−7.6 (2)
C21—P4—C19—C20−54.64 (15)P4—O4—Li3—O2−132.26 (11)
C23—P4—C19—C2060.55 (15)P4—O4—Li3—O3120.09 (12)
O4—P4—C21—C2268.92 (15)Li1—O4—Li3—Cl3−139.67 (17)
C19—P4—C21—C22−53.15 (16)Li1—O4—Li3—O295.68 (11)
C23—P4—C21—C22−168.43 (13)Li1—O4—Li3—O3−11.98 (11)
O4—P4—C23—C2460.39 (16)Li2—O4—Li3—Cl3137.94 (17)
C19—P4—C23—C24−178.10 (14)Li2—O4—Li3—O213.28 (10)
C21—P4—C23—C24−61.71 (16)Li2—O4—Li3—O3−94.37 (11)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···Cl20.99002.82003.6477 (19)142.00
C1—H1B···Cl2i0.99002.81003.6231 (19)140.00
C11—H11B···Cl3ii0.99002.73003.7103 (19)170.00
C13—H13A···Cl1iii0.99002.81003.7677 (19)162.00
C15—H15B···Cl1iii0.99002.81003.7252 (18)154.00
C18—H18B···Cl2iv0.98002.81003.721 (2)154.00
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+2, −z; (iii) −x+1, y+1/2, −z+1/2; (iv) x, y+1, z.

Experimental details

(I)(II)
Crystal data
Chemical formula[Li3Cl3(C6H15OP)4]·C7H8[Li3Cl3(C6H15OP)4]
Mr755.9663.77
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)120120
a, b, c (Å)11.3414 (7), 32.9899 (19), 16.100 (1)12.0507 (4), 12.1447 (3), 25.8698 (7)
β (°) 134.162 (3) 94.564 (2)
V (Å3)4321.3 (5)3774.09 (19)
Z44
Radiation typeMo KαMo Kα
µ (mm−1)0.390.44
Crystal size (mm)0.3 × 0.2 × 0.10.44 × 0.39 × 0.26
Data collection
DiffractometerOxford Diffraction KM4 CCD
diffractometer		Oxford Diffraction KM4 CCD
diffractometer
Absorption correction––
No. of measured, independent and
observed [I > 2σ(I)] reflections		29430, 7657, 5468 19943, 6648, 6073
Rint0.060.011
(sin θ/λ)max (Å−1)0.5960.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.06, 0.127, 1.06 0.034, 0.092, 1.13
No. of reflections76576648
No. of parameters419355
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.93, −0.490.52, −0.30

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) for (I) top
Cl1—Li12.268 (6)O1—Li11.930 (7)
P1—O11.508 (3)O4—Li12.045 (9)
P1—O1—Li1143.8 (3)P4—O4—Li2128.1 (4)
P1—O1—Li2126.6 (3)P4—O4—Li3128.0 (2)
Li1—O1—Li289.2 (3)Li1—O4—Li284.7 (3)
P4—O4—Li1131.9 (2)O1—Li2—O491.4 (3)
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
C5—H5A···Cl2i0.99002.80003.749 (4)160.00
C5—H5B···Cl20.99002.81003.688 (4)148.00
C11—H11B···Cl1ii0.99002.70003.685 (4)170.00
C30—H30···Cl1ii0.95002.82003.763 (7)170.00
Symmetry codes: (i) −x+1, −y, −z+2; (ii) x−1, y, z−1.
Selected geometric parameters (Å, º) for (II) top
Cl1—Li12.269 (3)O1—Li11.915 (3)
P1—O11.5136 (11)O4—Li12.037 (3)
P4—O41.5182 (12)
P1—O1—Li1137.73 (10)P4—O4—Li2130.91 (10)
P1—O1—Li2125.62 (10)P4—O4—Li3134.79 (10)
Li1—O1—Li287.85 (12)Li1—O4—Li281.82 (11)
P4—O4—Li1123.47 (10)O1—Li2—O491.50 (12)
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···Cl20.99002.82003.6477 (19)142.00
C1—H1B···Cl2i0.99002.81003.6231 (19)140.00
C11—H11B···Cl3ii0.99002.73003.7103 (19)170.00
C13—H13A···Cl1iii0.99002.81003.7677 (19)162.00
C15—H15B···Cl1iii0.99002.81003.7252 (18)154.00
C18—H18B···Cl2iv0.98002.81003.721 (2)154.00
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+2, −z; (iii) −x+1, y+1/2, −z+1/2; (iv) x, y+1, z.
 

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