catena-Poly[[tricarbonyl-1κ³C-(1η⁵-cyclo-penta-dien-yl)lead(II)molyb-denum(0)](Mo-Pb)-μ₃-acetato-2':2:2''κ⁴O:O,O':O'].

In the title compound, [MoPb(C₅H₅)(CH₃COO)(CO)₃], the Pb(II) atom is coordinated pyramidally via the Mo(0) atom of a {Cp(CO)₃Mo} (Cp = cyclo-penta-dien-yl) fragment [Pb-Mo = 3.0589 (5) Å] and a chelating acetate (Ac) group. Additionally, the [{Cp(CO)₃Mo}PbAc] units are linked along [100] by Pb-O(acetate) inter-actions, giving a ladder-type polymeric structure composed of PbCO₂ and Pb₂O₂ four-membered rings. The {Cp(CO)₃Mo} units attached to the Pb(II) atom occupy terminal positions at opposite sides of the slightly puckered lead acetate chain. The angle between the Pb-Mo bond vector and the central chain plane is 67.8 (2)°.

Related literature

For organometallic compounds containing Pb—Mo bonds, see: Kubicki et al. (1984 ▶); Hitchcock et al. (1987 ▶); Pu et al. (2000 ▶); Campbell et al. (2002 ▶); Yong et al. (2005 ▶); Alonso et al. (2010 ▶). For lead(II) carboxyl­ates with ladder-type structures, see: Rajaram & Rao (1982 ▶); Dai et al. (2009 ▶).

Experimental

Crystal data

[MoPb(C5H5)(C2H3O2)(CO)3]

M = 511.29

Monoclinic,

a = 7.4813 (6) Å

b = 14.9431 (12) Å

c = 11.3323 (9) Å

β = 98.660 (9)°

V = 1252.44 (17) Å3

Z = 4

Mo Kα radiation

μ = 14.43 mm−1

T = 220 K

0.19 × 0.19 × 0.08 mm

Data collection

Stoe IPDS I diffractometer

Absorption correction: numerical (IPDS Program Package; Stoe & Cie, 1999 ▶) T min = 0.112, T max = 0.263

9600 measured reflections

2417 independent reflections

2130 reflections with I > 2σ(I)

R int = 0.066

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.056

S = 1.03

2417 reflections

154 parameters

H-atom parameters constrained

Δρmax = 1.29 e Å−3

Δρmin = −1.15 e Å−3

Data collection: IPDS Program Package (Stoe & Cie, 1999 ▶); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2009 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812024737/wm2639sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812024737/wm2639Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[MoPb(C5H5)(C2H3O2)(CO)3]	F(000) = 928
Mr = 511.29	Dx = 2.712 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8000 reflections
a = 7.4813 (6) Å	θ = 2.3–25.9°
b = 14.9431 (12) Å	µ = 14.43 mm−1
c = 11.3323 (9) Å	T = 220 K
β = 98.660 (9)°	Plate, orange
V = 1252.44 (17) Å3	0.19 × 0.19 × 0.08 mm
Z = 4

Stoe IPDS I diffractometer	2417 independent reflections
Radiation source: fine-focus sealed tube	2130 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.066
φ oscillation scans	θmax = 25.9°, θmin = 2.3°
Absorption correction: numerical (IPDS Program Package; Stoe & Cie, 1999)	h = −9→9
Tmin = 0.112, Tmax = 0.263	k = −18→18
9600 measured reflections	l = −13→13

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.0275P)2] where P = (Fo2 + 2Fc2)/3
2417 reflections	(Δ/σ)max = 0.001
154 parameters	Δρmax = 1.29 e Å−3
0 restraints	Δρmin = −1.15 e Å−3

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.

	x	y	z	Uiso*/Ueq
C1	0.2861 (8)	0.5561 (4)	0.6488 (5)	0.0223 (12)
C2	0.3210 (12)	0.5900 (6)	0.7737 (6)	0.057 (2)
H3	0.4449	0.6109	0.7915	0.068*
H2	0.3018	0.5422	0.8282	0.068*
H1	0.2392	0.6391	0.7826	0.068*
C3	0.2737 (9)	0.7886 (4)	0.3061 (5)	0.0283 (13)
C4	0.4537 (8)	0.6461 (4)	0.3283 (5)	0.0223 (12)
C5	0.0974 (8)	0.6837 (4)	0.4177 (5)	0.0259 (13)
C6	−0.0802 (9)	0.6429 (5)	0.1399 (6)	0.0406 (17)
H4	−0.1923	0.6482	0.1672	0.049*
C7	0.0154 (10)	0.7132 (4)	0.0927 (5)	0.0385 (17)
H5	−0.0196	0.7736	0.0847	0.046*
C8	0.1749 (10)	0.6743 (5)	0.0599 (5)	0.0378 (16)
H6	0.2632	0.7048	0.0247	0.045*
C9	0.1782 (10)	0.5829 (5)	0.0891 (5)	0.0384 (16)
H7	0.2687	0.5415	0.0777	0.046*
C10	0.0208 (10)	0.5650 (4)	0.1386 (5)	0.0357 (16)
H8	−0.0113	0.5089	0.1666	0.043*
O1	0.4139 (5)	0.5565 (3)	0.5865 (3)	0.0244 (9)
O2	0.1338 (5)	0.5251 (3)	0.6061 (4)	0.0246 (9)
O3	0.3190 (8)	0.8626 (3)	0.3264 (4)	0.0491 (13)
O4	0.6102 (6)	0.6423 (3)	0.3575 (4)	0.0376 (11)
O5	0.0370 (7)	0.7031 (3)	0.5033 (4)	0.0465 (13)
Mo	0.19661 (6)	0.66595 (3)	0.26799 (4)	0.01695 (12)
Pb	0.22870 (3)	0.489761 (12)	0.406981 (17)	0.01569 (8)

	U11	U22	U33	U12	U13	U23
C1	0.020 (3)	0.028 (3)	0.019 (3)	−0.002 (2)	0.003 (2)	0.000 (2)
C2	0.055 (5)	0.084 (6)	0.034 (4)	−0.037 (5)	0.014 (4)	−0.021 (4)
C3	0.031 (4)	0.024 (3)	0.026 (3)	0.002 (3)	−0.007 (3)	0.006 (2)
C4	0.029 (4)	0.018 (3)	0.020 (3)	0.004 (2)	0.006 (3)	0.000 (2)
C5	0.033 (4)	0.018 (3)	0.029 (3)	0.006 (2)	0.011 (3)	0.002 (2)
C6	0.021 (4)	0.069 (5)	0.028 (3)	−0.007 (3)	−0.007 (3)	−0.003 (3)
C7	0.053 (5)	0.030 (3)	0.024 (3)	0.006 (3)	−0.020 (3)	−0.002 (3)
C8	0.035 (4)	0.063 (5)	0.015 (3)	−0.016 (3)	0.003 (3)	0.000 (3)
C9	0.051 (5)	0.040 (4)	0.022 (3)	0.003 (3)	−0.003 (3)	−0.010 (3)
C10	0.050 (5)	0.034 (4)	0.019 (3)	−0.018 (3)	−0.011 (3)	0.004 (2)
O1	0.019 (2)	0.032 (2)	0.023 (2)	−0.0025 (17)	0.0073 (18)	0.0014 (16)
O2	0.013 (2)	0.031 (2)	0.029 (2)	−0.0035 (17)	0.0006 (17)	−0.0033 (17)
O3	0.069 (4)	0.023 (2)	0.048 (3)	−0.013 (2)	−0.013 (3)	0.004 (2)
O4	0.018 (3)	0.040 (3)	0.054 (3)	−0.0005 (19)	0.003 (2)	0.001 (2)
O5	0.053 (3)	0.049 (3)	0.042 (3)	0.017 (2)	0.022 (3)	−0.001 (2)
Mo	0.0173 (2)	0.0174 (2)	0.0154 (2)	−0.00063 (18)	−0.00030 (18)	0.00218 (16)
Pb	0.01277 (13)	0.01757 (12)	0.01657 (11)	0.00013 (8)	0.00171 (8)	0.00066 (7)

C1—O2	1.258 (7)	C7—Mo	2.339 (6)
C1—O1	1.272 (7)	C7—H5	0.9400
C1—C2	1.488 (9)	C8—C9	1.405 (10)
C2—H3	0.9700	C8—Mo	2.342 (6)
C2—H2	0.9700	C8—H6	0.9400
C2—H1	0.9700	C9—C10	1.404 (10)
C3—O3	1.168 (7)	C9—Mo	2.363 (6)
C3—Mo	1.951 (6)	C9—H7	0.9400
C4—O4	1.169 (7)	C10—Mo	2.361 (6)
C4—Mo	1.965 (6)	C10—H8	0.9400
C5—O5	1.166 (7)	O1—Pb	2.491 (4)
C5—Mo	1.970 (5)	O1—Pbi	2.752 (4)
C6—C10	1.390 (10)	O2—Pb	2.522 (4)
C6—C7	1.420 (10)	O2—Pbii	2.703 (4)
C6—Mo	2.368 (7)	Mo—Pb	3.0589 (5)
C6—H4	0.9400	Pb—O2ii	2.703 (4)
C7—C8	1.426 (10)	Pb—O1i	2.752 (4)
O2—C1—O1	120.1 (5)	Pb—O2—Pbii	110.43 (15)
O2—C1—C2	120.7 (5)	C3—Mo—C4	79.8 (2)
O1—C1—C2	119.2 (6)	C3—Mo—C5	79.6 (2)
C1—C2—H3	109.5	C4—Mo—C5	101.3 (2)
C1—C2—H2	109.5	C3—Mo—C7	91.1 (2)
H3—C2—H2	109.5	C4—Mo—C7	138.9 (2)
C1—C2—H1	109.5	C5—Mo—C7	116.5 (3)
H3—C2—H1	109.5	C3—Mo—C8	98.4 (2)
H2—C2—H1	109.5	C4—Mo—C8	105.9 (2)
O3—C3—Mo	178.6 (5)	C5—Mo—C8	151.9 (3)
O4—C4—Mo	172.8 (5)	C7—Mo—C8	35.5 (2)
O5—C5—Mo	173.3 (5)	C3—Mo—C10	148.9 (2)
C10—C6—C7	108.1 (6)	C4—Mo—C10	123.0 (2)
C10—C6—Mo	72.6 (4)	C5—Mo—C10	112.0 (3)
C7—C6—Mo	71.3 (4)	C7—Mo—C10	57.9 (2)
C10—C6—H4	125.9	C8—Mo—C10	57.4 (2)
C7—C6—H4	125.9	C3—Mo—C9	131.3 (2)
Mo—C6—H4	121.8	C4—Mo—C9	98.4 (2)
C6—C7—C8	106.6 (6)	C5—Mo—C9	146.0 (3)
C6—C7—Mo	73.6 (4)	C7—Mo—C9	58.6 (2)
C8—C7—Mo	72.4 (4)	C8—Mo—C9	34.8 (2)
C6—C7—H5	126.7	C10—Mo—C9	34.6 (2)
C8—C7—H5	126.7	C3—Mo—C6	118.3 (3)
Mo—C7—H5	119.3	C4—Mo—C6	155.7 (2)
C9—C8—C7	108.7 (6)	C5—Mo—C6	98.0 (3)
C9—C8—Mo	73.4 (3)	C7—Mo—C6	35.1 (2)
C7—C8—Mo	72.1 (3)	C8—Mo—C6	57.9 (2)
C9—C8—H6	125.6	C10—Mo—C6	34.2 (3)
C7—C8—H6	125.6	C9—Mo—C6	57.7 (3)
Mo—C8—H6	120.5	C3—Mo—Pb	134.20 (17)
C10—C9—C8	107.0 (6)	C4—Mo—Pb	72.17 (16)
C10—C9—Mo	72.6 (4)	C5—Mo—Pb	71.52 (16)
C8—C9—Mo	71.8 (3)	C7—Mo—Pb	133.44 (17)
C10—C9—H7	126.5	C8—Mo—Pb	123.54 (18)
C8—C9—H7	126.5	C10—Mo—Pb	76.28 (15)
Mo—C9—H7	120.9	C9—Mo—Pb	88.82 (17)
C6—C10—C9	109.5 (6)	C6—Mo—Pb	100.61 (19)
C6—C10—Mo	73.2 (4)	O1—Pb—O2	51.85 (12)
C9—C10—Mo	72.8 (4)	O1—Pb—O2ii	120.53 (12)
C6—C10—H8	125.2	O2—Pb—O2ii	69.57 (15)
C9—C10—H8	125.2	O1—Pb—O1i	70.11 (13)
Mo—C10—H8	120.5	O2—Pb—O1i	115.60 (12)
C1—O1—Pb	94.6 (3)	O2ii—Pb—O1i	160.67 (12)
C1—O1—Pbi	142.5 (4)	O1—Pb—Mo	93.83 (9)
Pb—O1—Pbi	109.89 (13)	O2—Pb—Mo	105.64 (9)
C1—O2—Pb	93.5 (3)	O2ii—Pb—Mo	92.42 (9)
C1—O2—Pbii	153.5 (4)	O1i—Pb—Mo	103.33 (8)
C10—C6—C7—C8	1.6 (7)	C10—C9—Mo—C7	−77.8 (4)
Mo—C6—C7—C8	65.4 (4)	C8—C9—Mo—C7	37.5 (4)
C10—C6—C7—Mo	−63.8 (5)	C10—C9—Mo—C8	−115.2 (6)
C6—C7—C8—C9	−1.3 (7)	C8—C9—Mo—C10	115.2 (6)
Mo—C7—C8—C9	64.8 (4)	C10—C9—Mo—C6	−36.2 (4)
C6—C7—C8—Mo	−66.2 (4)	C8—C9—Mo—C6	79.0 (5)
C7—C8—C9—C10	0.6 (7)	C10—C9—Mo—Pb	67.2 (4)
Mo—C8—C9—C10	64.6 (4)	C8—C9—Mo—Pb	−177.6 (4)
C7—C8—C9—Mo	−64.0 (4)	C10—C6—Mo—C3	159.8 (4)
C7—C6—C10—C9	−1.3 (7)	C7—C6—Mo—C3	43.1 (5)
Mo—C6—C10—C9	−64.2 (5)	C10—C6—Mo—C4	24.9 (8)
C7—C6—C10—Mo	62.9 (4)	C7—C6—Mo—C4	−91.8 (7)
C8—C9—C10—C6	0.4 (7)	C10—C6—Mo—C5	−117.7 (4)
Mo—C9—C10—C6	64.5 (5)	C7—C6—Mo—C5	125.6 (4)
C8—C9—C10—Mo	−64.0 (4)	C10—C6—Mo—C7	116.7 (6)
O2—C1—O1—Pb	1.3 (6)	C10—C6—Mo—C8	78.0 (4)
C2—C1—O1—Pb	179.4 (6)	C7—C6—Mo—C8	−38.7 (4)
O2—C1—O1—Pbi	−130.3 (5)	C7—C6—Mo—C10	−116.7 (6)
C2—C1—O1—Pbi	47.8 (9)	C10—C6—Mo—C9	36.6 (4)
O1—C1—O2—Pb	−1.3 (6)	C7—C6—Mo—C9	−80.1 (4)
C2—C1—O2—Pb	−179.3 (6)	C10—C6—Mo—Pb	−45.1 (4)
O1—C1—O2—Pbii	−156.3 (5)	C7—C6—Mo—Pb	−161.8 (4)
C2—C1—O2—Pbii	25.6 (13)	C1—O1—Pb—O2	−0.7 (3)
C6—C7—Mo—C3	−143.0 (4)	Pbi—O1—Pb—O2	150.3 (2)
C8—C7—Mo—C3	103.0 (4)	C1—O1—Pb—O2ii	11.1 (4)
C6—C7—Mo—C4	141.2 (4)	Pbi—O1—Pb—O2ii	162.11 (12)
C8—C7—Mo—C4	27.3 (6)	C1—O1—Pb—O1i	−151.0 (4)
C6—C7—Mo—C5	−64.1 (5)	Pbi—O1—Pb—O1i	0.0
C8—C7—Mo—C5	−178.0 (4)	C1—O1—Pb—Mo	106.2 (3)
C6—C7—Mo—C8	113.9 (6)	Pbi—O1—Pb—Mo	−102.80 (11)
C6—C7—Mo—C10	36.3 (4)	C1—O2—Pb—O1	0.7 (3)
C8—C7—Mo—C10	−77.6 (4)	Pbii—O2—Pb—O1	169.1 (2)
C6—C7—Mo—C9	77.2 (4)	C1—O2—Pb—O2ii	−168.4 (4)
C8—C7—Mo—C9	−36.7 (4)	Pbii—O2—Pb—O2ii	0.0
C8—C7—Mo—C6	−113.9 (6)	C1—O2—Pb—O1i	31.9 (4)
C6—C7—Mo—Pb	24.9 (5)	Pbii—O2—Pb—O1i	−159.73 (13)
C8—C7—Mo—Pb	−89.0 (4)	C1—O2—Pb—Mo	−81.7 (3)
C9—C8—Mo—C3	163.5 (4)	Pbii—O2—Pb—Mo	86.71 (13)
C7—C8—Mo—C3	−79.9 (4)	C3—Mo—Pb—O1	−4.2 (3)
C9—C8—Mo—C4	81.7 (4)	C4—Mo—Pb—O1	50.95 (18)
C7—C8—Mo—C4	−161.7 (4)	C5—Mo—Pb—O1	−58.0 (2)
C9—C8—Mo—C5	−112.8 (6)	C7—Mo—Pb—O1	−167.3 (3)
C7—C8—Mo—C5	3.7 (7)	C8—Mo—Pb—O1	148.6 (2)
C9—C8—Mo—C7	−116.6 (6)	C10—Mo—Pb—O1	−177.2 (2)
C9—C8—Mo—C10	−37.5 (4)	C9—Mo—Pb—O1	150.2 (2)
C7—C8—Mo—C10	79.0 (4)	C6—Mo—Pb—O1	−153.0 (2)
C7—C8—Mo—C9	116.6 (6)	C3—Mo—Pb—O2	47.2 (3)
C9—C8—Mo—C6	−78.2 (5)	C4—Mo—Pb—O2	102.33 (19)
C7—C8—Mo—C6	38.3 (4)	C5—Mo—Pb—O2	−6.7 (2)
C9—C8—Mo—Pb	2.9 (5)	C7—Mo—Pb—O2	−115.9 (3)
C7—C8—Mo—Pb	119.4 (4)	C8—Mo—Pb—O2	−160.1 (2)
C6—C10—Mo—C3	−36.1 (7)	C10—Mo—Pb—O2	−125.9 (2)
C9—C10—Mo—C3	81.2 (7)	C9—Mo—Pb—O2	−158.4 (2)
C6—C10—Mo—C4	−168.1 (4)	C6—Mo—Pb—O2	−101.7 (2)
C9—C10—Mo—C4	−50.7 (5)	C3—Mo—Pb—O2ii	116.6 (3)
C6—C10—Mo—C5	71.0 (4)	C4—Mo—Pb—O2ii	171.78 (18)
C9—C10—Mo—C5	−171.7 (4)	C5—Mo—Pb—O2ii	62.8 (2)
C6—C10—Mo—C7	−37.3 (4)	C7—Mo—Pb—O2ii	−46.5 (3)
C9—C10—Mo—C7	80.0 (4)	C8—Mo—Pb—O2ii	−90.6 (2)
C6—C10—Mo—C8	−79.6 (4)	C10—Mo—Pb—O2ii	−56.4 (2)
C9—C10—Mo—C8	37.7 (4)	C9—Mo—Pb—O2ii	−89.0 (2)
C6—C10—Mo—C9	−117.3 (6)	C6—Mo—Pb—O2ii	−32.22 (19)
C9—C10—Mo—C6	117.3 (6)	C3—Mo—Pb—O1i	−74.7 (3)
C6—C10—Mo—Pb	134.2 (4)	C4—Mo—Pb—O1i	−19.50 (18)
C9—C10—Mo—Pb	−108.5 (4)	C5—Mo—Pb—O1i	−128.5 (2)
C10—C9—Mo—C3	−137.2 (4)	C7—Mo—Pb—O1i	122.2 (3)
C8—C9—Mo—C3	−22.0 (6)	C8—Mo—Pb—O1i	78.1 (2)
C10—C9—Mo—C4	138.9 (4)	C10—Mo—Pb—O1i	112.3 (2)
C8—C9—Mo—C4	−105.8 (4)	C9—Mo—Pb—O1i	79.7 (2)
C10—C9—Mo—C5	13.8 (7)	C6—Mo—Pb—O1i	136.50 (19)
C8—C9—Mo—C5	129.1 (5)