Tetra­methyl­lead(IV) at 150 K

Tetra­methyl­lead, [Pb(CH₃)₄], crystallizes in the cubic space group Pa, with the Pb atom and one C atom on a crystallographic threefold axis. The average Pb-C distance is 2.211 (11) Å. The crystal structure is isostructural with that of the Sn analogue, and adopts the SnI₄-type structure.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](Pb-C) = 0.008 Å
• R factor = 0.033
• wR factor = 0.105
• Data-to-parameter ratio = 33.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level A:



ABSTM_02  Alert A Crystal and compound unsuitable for non-numerical
          corrections. Product of mu and tmid > 3.0
           Value of mu given =    24.070 tmid =     0.400

Author response: See _publ_section_exptl_prep

 Alert Level B:



CRYSS_02  Alert B The value of _exptl_crystal_size_max is > 1.0
 Maximum crystal size given =   3.000

Author response: See _publ_section_exptl_prep

 1 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 0 Alert Level C = Please check

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: CRYSTALS (Watkin et al., 2001); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: CRYSTALS.

Tetramethyl lead

Crystal data

[Pb(CH3)4]	Melting point: 243 K
Mr = 267.34	Mo Kα radiation, λ = 0.71073 Å
Cubic, Pa3	Cell parameters from 3546 reflections
Hall symbol: -P 2ac 2ab 3	θ = 3–28.5°
a = 11.1725 (6) Å	µ = 24.07 mm^−1
V = 1394.60 (13) Å^3	T = 150 K
Z = 8	Cylinder, colourless
F(000) = 944.00	3.00 × 0.40 × 0.40 × 0.20 (radius) mm
Dx = 2.546 Mg m^−3

Data collection

Bruker SMART APEX CCD diffractometer	375 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.062
ω scans	θmax = 28.6°, θmin = 3.2°
Absorption correction: multi-scan [SADABS (Sheldrick, 2002) based on the method of Blessing (1995)]	h = −13→14
Tmin = 0.111, Tmax = 1.000	k = −14→14
7703 measured reflections	l = −7→14
586 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters not refined
R[F^2 > 2σ(F^2)] = 0.033	Method = Tukey and Prince (Carruthers & Watkin, 1979) W = [weight][1-(deltaF/6σF)^2] where [weight] is given by a five-term Chebychev polynomial with coefficients: 96.4 162. 107. 51.2 13.7
wR(F^2) = 0.105	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 1.55 e Å^−3
577 reflections	Δρmin = −1.84 e Å^−3
17 parameters	Extinction correction: Larson (1970), equation 22
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 139.0 (122)

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

	x	y	z	Uiso*/Ueq
Pb1	0.872030 (14)	0.372030 (14)	0.127970 (14)	0.0145
C1	0.7586 (8)	0.2586 (8)	0.2414 (8)	0.0258
C2	0.9865 (8)	0.2561 (6)	0.0148 (5)	0.0224
H11	0.7071	0.3109	0.2921	0.0315*
H21	1.0390	0.3065	−0.0370	0.0254*
H22	1.0382	0.2043	0.0675	0.0254*
H23	0.9353	0.2035	−0.0363	0.0254*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.0145 (3)	0.0145 (3)	0.0145 (3)	−0.00001 (6)	0.00001 (6)	0.00001 (6)
C1	0.026 (2)	0.026 (2)	0.026 (2)	−0.002 (3)	0.002 (3)	0.002 (3)
C2	0.027 (3)	0.018 (3)	0.021 (2)	0.003 (2)	0.005 (3)	−0.007 (2)

Geometric parameters (Å, º)

Pb1—C1	2.194 (15)	C2—H22	1.008
Pb1—C2	2.216 (7)	C2—H23	0.999
C2—H21	0.998	C1—H11	0.997
C2—Pb1—C1	108.96 (16)	Pb1—C2—H23	109.858
C2—Pb1—C2^i	109.98 (16)	H21—C2—H23	109.669
Pb1—C2—H21	109.906	H22—C2—H23	108.937
Pb1—C2—H22	109.458	Pb1—C1—H11	108.908
H21—C2—H22	108.993	H11—C1—H11^i	110.029

Symmetry code: (i) y+1/2, −z+1/2, −x+1.