Tetrakis(μ₃-phenoxo-aceto­nitrile­lithium), a tetrameric lithium aryl­oxide with a cubane core

The title compound, (CH₃CNLiOC₆H₅)₄ or [Li₄(C₆H₅O)₄(C₂H₃N)₄], is tetrameric with a distorted Li₄O₄ cube core. The mol­ecule has crystallographic symmetry. Each Li atom has distorted tetrahedral coordination, with bonds to three triply bridging phenoxo ligands and a terminal aceto­nitrile ligand derived from the solvent in the synthesis.

Key indicators

• Single-crystal X-ray study
• T = 160 K
• Mean [sigma](C-C) = 0.002 Å
• R factor = 0.042
• wR factor = 0.102
• Data-to-parameter ratio = 18.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           28.60
         From the CIF: _reflns_number_total               1918
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         2049
         Completeness (_total/calc)             93.61%
          Alert C: < 95% complete


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: local programs; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Tetrakis(µ₃-phenoxo-acetonitrilelithium)

Crystal data

[Li4(C6H5O)4(C2H3N)4]	Dx = 1.172 Mg m^−3
Mr = 564.38	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 6123 reflections
a = 14.1961 (19) Å	θ = 1.9–28.6°
c = 15.869 (2) Å	µ = 0.08 mm^−1
V = 3198.0 (7) Å^3	T = 160 K
Z = 4	Block, colourless
F(000) = 1184	0.40 × 0.32 × 0.28 mm

Data collection

Bruker SMART 1K CCD diffractometer	1645 reflections with I > 2σ(I)
Radiation source: sealed tube	Rint = 0.040
Graphite monochromator	θmax = 28.6°, θmin = 1.9°
Detector resolution: 8.192 pixels mm^-1	h = −18→15
narrow–frame ω scans	k = −11→18
9983 measured reflections	l = −21→21
1918 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.042	H-atom parameters constrained
wR(F^2) = 0.102	w = 1/[σ^2(Fo^2) + (0.0353P)^2 + 1.6883P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
1918 reflections	Δρmax = 0.19 e Å^−3
102 parameters	Δρmin = −0.17 e Å^−3
0 restraints	Extinction correction: SHELXTL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0022 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Li	0.58904 (15)	0.22224 (15)	0.31667 (12)	0.0356 (4)
O	0.59693 (6)	0.21365 (6)	0.43747 (5)	0.0345 (2)
C1	0.66535 (8)	0.20709 (8)	0.49433 (7)	0.0282 (2)
C2	0.64533 (9)	0.19977 (9)	0.58077 (7)	0.0339 (3)
H2	0.5817	0.1957	0.5988	0.041*
C3	0.71677 (10)	0.19832 (9)	0.64006 (8)	0.0398 (3)
H3	0.7014	0.1940	0.6982	0.048*
C4	0.81030 (9)	0.20311 (9)	0.61590 (8)	0.0414 (3)
H4	0.8591	0.2031	0.6568	0.050*
C5	0.83114 (9)	0.20785 (9)	0.53098 (8)	0.0404 (3)
H5	0.8951	0.2102	0.5134	0.049*
C6	0.76035 (9)	0.20918 (9)	0.47109 (7)	0.0347 (3)
H6	0.7766	0.2116	0.4130	0.042*
N	0.67418 (8)	0.16167 (8)	0.23046 (7)	0.0438 (3)
C7	0.69479 (9)	0.11351 (9)	0.17676 (8)	0.0394 (3)
C8	0.71946 (14)	0.05151 (12)	0.10776 (11)	0.0649 (5)
H8A	0.7839	0.0283	0.1157	0.097*
H8B	0.7155	0.0862	0.0545	0.097*
H8C	0.6758	−0.0019	0.1064	0.097*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Li	0.0438 (11)	0.0387 (11)	0.0244 (9)	0.0017 (9)	0.0017 (8)	−0.0002 (8)
O	0.0351 (5)	0.0453 (5)	0.0232 (4)	0.0011 (4)	−0.0037 (3)	0.0035 (3)
C1	0.0334 (6)	0.0265 (5)	0.0247 (5)	−0.0002 (4)	−0.0024 (4)	0.0014 (4)
C2	0.0339 (6)	0.0412 (7)	0.0266 (6)	−0.0006 (5)	0.0002 (5)	0.0026 (5)
C3	0.0472 (7)	0.0457 (7)	0.0265 (6)	0.0004 (6)	−0.0065 (5)	0.0003 (5)
C4	0.0414 (7)	0.0419 (7)	0.0410 (7)	0.0010 (5)	−0.0142 (6)	−0.0036 (6)
C5	0.0312 (6)	0.0409 (7)	0.0492 (7)	−0.0007 (5)	−0.0013 (5)	−0.0029 (6)
C6	0.0371 (6)	0.0362 (6)	0.0309 (6)	−0.0006 (5)	0.0034 (5)	0.0014 (5)
N	0.0441 (6)	0.0479 (7)	0.0392 (6)	−0.0001 (5)	0.0093 (5)	0.0030 (5)
C7	0.0374 (7)	0.0391 (7)	0.0419 (7)	0.0005 (5)	0.0116 (5)	0.0070 (6)
C8	0.0854 (12)	0.0499 (9)	0.0595 (10)	0.0101 (8)	0.0285 (9)	−0.0053 (7)

Geometric parameters (Å, º)

Li—O	1.924 (2)	C3—C4	1.3836 (19)
Li—O^i	1.923 (2)	C4—H4	0.950
Li—O^ii	2.034 (2)	C4—C5	1.3814 (19)
Li—N	2.018 (2)	C5—H5	0.950
O—Li^ii	1.923 (2)	C5—C6	1.3833 (17)
O—Li^i	2.034 (2)	C6—H6	0.950
O—C1	1.3290 (13)	N—C7	1.1310 (17)
C1—C2	1.4047 (16)	C7—C8	1.448 (2)
C1—C6	1.3985 (17)	C8—H8A	0.980
C2—H2	0.950	C8—H8B	0.980
C2—C3	1.3834 (17)	C8—H8C	0.980
C3—H3	0.950
O—Li—O^i	96.60 (9)	C2—C3—C4	120.95 (12)
O^i—Li—O^ii	95.91 (10)	H3—C3—C4	119.5
O—Li—O^ii	93.01 (9)	C3—C4—H4	120.7
O—Li—N	127.85 (12)	C3—C4—C5	118.57 (11)
O^i—Li—N	127.02 (11)	H4—C4—C5	120.7
O^ii—Li—N	107.25 (10)	C4—C5—H5	119.5
Li—O—Li^ii	86.39 (9)	C4—C5—C6	121.02 (12)
Li^ii—O—Li^i	83.97 (10)	H5—C5—C6	119.5
Li—O—Li^i	83.35 (9)	C1—C6—C5	121.27 (11)
Li—O—C1	136.34 (10)	C1—C6—H6	119.4
Li^ii—O—C1	131.97 (9)	C5—C6—H6	119.4
Li^i—O—C1	115.85 (9)	Li—N—C7	157.42 (13)
O—C1—C2	121.36 (10)	N—C7—C8	179.01 (16)
O—C1—C6	121.61 (10)	C7—C8—H8A	109.5
C2—C1—C6	117.01 (10)	C7—C8—H8B	109.5
C1—C2—H2	119.4	C7—C8—H8C	109.5
C1—C2—C3	121.13 (12)	H8A—C8—H8B	109.5
H2—C2—C3	119.4	H8A—C8—H8C	109.5
C2—C3—H3	119.5	H8B—C8—H8C	109.5

Symmetry codes: (i) −y+3/4, x−1/4, −z+3/4; (ii) y+1/4, −x+3/4, −z+3/4.