Poly­[bis­(benzotriazolato)­di-μ-oxo-dilead(II)]

The title compound, [Pb₂O₂(C₆H₄N₃)₂]_n, exhibits anti-corrosion properties. The coordination around each Pb atom is different, with coordination numbers of four and five. The compound forms a polymeric chain with pairs of oxo bridges between metal centers.

Key indicators

• Single-crystal X-ray study
• T = 290 K
• Mean [sigma](C-C) = 0.022 Å
• R factor = 0.056
• wR factor = 0.188
• Data-to-parameter ratio = 13.7

checkCIF/PLATON results

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Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ...         22

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   0 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993); software used to prepare material for publication: PLATON (Spek, 2003).

Poly[bis(benzotriazolato)di-µ-oxo-lead(II)]

Crystal data

[Pb2O2(C6H4N3)2]	F(000) = 2416
Mr = 682.64	Dx = 3.114 Mg m^−3
Monoclinic, C2/c	Melting point: 629 K
Hall symbol: -C 2yc	Mo Kα radiation, λ = 0.71073 Å
a = 35.035 (6) Å	Cell parameters from 625 reflections
b = 5.8335 (10) Å	θ = 1.4–25.2°
c = 16.049 (3) Å	µ = 23.11 mm^−1
β = 116.837 (2)°	T = 290 K
V = 2926.8 (9) Å^3	Thick plate, colorless
Z = 8	0.18 × 0.12 × 0.06 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2724 independent reflections
Radiation source: fine-focus sealed tube	2523 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
φ and ω scans	θmax = 25.5°, θmin = 1.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −42→42
Tmin = 0.033, Tmax = 0.250	k = −7→7
12665 measured reflections	l = −19→19

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.056	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.188	H-atom parameters constrained
S = 1.13	w = 1/[σ^2(Fo^2) + (0.1502P)^2] where P = (Fo^2 + 2Fc^2)/3
2724 reflections	(Δ/σ)max = 0.001
199 parameters	Δρmax = 2.96 e Å^−3
0 restraints	Δρmin = −4.15 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Pb1	0.220298 (14)	0.43726 (6)	0.29174 (3)	0.0324 (3)
Pb2	0.301065 (14)	0.82275 (7)	0.48911 (3)	0.0336 (3)
N1	0.1753 (4)	0.6682 (15)	0.1409 (7)	0.036 (2)
N2	0.1942 (4)	0.8436 (19)	0.1209 (8)	0.045 (3)
N3	0.1645 (4)	0.9558 (19)	0.0437 (8)	0.047 (3)
N4	0.3340 (3)	0.7195 (19)	0.6687 (7)	0.038 (2)
N5	0.3238 (4)	0.513 (2)	0.6939 (8)	0.047 (3)
N6	0.3570 (4)	0.4011 (18)	0.7530 (9)	0.045 (3)
O1	0.2537 (3)	0.7955 (12)	0.3201 (6)	0.0345 (18)
O2	0.2568 (3)	0.5265 (14)	0.4817 (5)	0.0343 (17)
C1	0.1274 (4)	0.850 (2)	0.0163 (9)	0.037 (3)
C2	0.1329 (4)	0.6650 (18)	0.0772 (8)	0.035 (3)
C3	0.1008 (5)	0.512 (3)	0.0639 (9)	0.045 (3)
C4	0.0627 (5)	0.552 (3)	−0.0072 (12)	0.058 (4)
C5	0.0565 (4)	0.744 (3)	−0.0693 (10)	0.054 (3)
C6	0.0870 (5)	0.890 (3)	−0.0595 (10)	0.052 (3)
C7	0.3922 (5)	0.527 (2)	0.7682 (9)	0.042 (3)
C8	0.3777 (4)	0.732 (2)	0.7148 (9)	0.040 (3)
C9	0.4064 (5)	0.900 (2)	0.7155 (11)	0.050 (3)
C10	0.4484 (5)	0.861 (3)	0.7694 (12)	0.058 (4)
C11	0.4627 (5)	0.655 (3)	0.8254 (13)	0.069 (5)
C12	0.4352 (5)	0.490 (3)	0.8218 (12)	0.057 (4)
H3	0.1055	0.3865	0.1030	0.054*
H4	0.0398	0.4557	−0.0172	0.069*
H5	0.0294	0.7649	−0.1189	0.065*
H6	0.0821	1.0125	−0.1003	0.062*
H9	0.3968	1.0332	0.6803	0.060*
H10	0.4684	0.9673	0.7705	0.070*
H11	0.4917	0.6368	0.8650	0.082*
H12	0.4451	0.3541	0.8548	0.069*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.0328 (4)	0.0305 (4)	0.0370 (4)	−0.00250 (14)	0.0185 (3)	0.00048 (13)
Pb2	0.0313 (4)	0.0369 (4)	0.0358 (4)	−0.00378 (15)	0.0179 (3)	−0.00160 (14)
N1	0.044 (7)	0.037 (5)	0.030 (5)	0.005 (4)	0.018 (5)	0.005 (3)
N2	0.039 (7)	0.053 (6)	0.044 (6)	0.000 (5)	0.020 (5)	0.014 (4)
N3	0.026 (6)	0.057 (7)	0.051 (7)	−0.001 (5)	0.012 (5)	0.016 (5)
N4	0.024 (6)	0.051 (6)	0.038 (5)	−0.003 (4)	0.012 (4)	0.008 (4)
N5	0.050 (8)	0.040 (5)	0.057 (6)	−0.015 (5)	0.031 (6)	−0.001 (5)
N6	0.035 (7)	0.038 (5)	0.059 (7)	0.005 (5)	0.020 (5)	0.013 (5)
O1	0.034 (5)	0.035 (4)	0.033 (4)	−0.006 (3)	0.013 (3)	0.002 (3)
O2	0.030 (5)	0.040 (4)	0.038 (4)	0.004 (3)	0.020 (4)	−0.002 (3)
C1	0.024 (7)	0.048 (6)	0.040 (6)	0.002 (5)	0.017 (5)	0.002 (5)
C2	0.042 (8)	0.035 (6)	0.032 (5)	−0.003 (5)	0.021 (5)	−0.004 (4)
C3	0.034 (7)	0.046 (6)	0.048 (7)	0.001 (6)	0.012 (6)	0.003 (6)
C4	0.018 (7)	0.069 (10)	0.072 (10)	−0.003 (6)	0.009 (7)	0.004 (7)
C5	0.023 (7)	0.067 (8)	0.054 (8)	−0.002 (7)	0.001 (6)	−0.007 (7)
C6	0.054 (10)	0.050 (7)	0.045 (7)	0.002 (7)	0.016 (7)	0.002 (6)
C7	0.042 (8)	0.038 (6)	0.042 (7)	−0.003 (5)	0.015 (6)	−0.001 (5)
C8	0.045 (8)	0.041 (6)	0.041 (6)	0.004 (6)	0.025 (6)	0.006 (5)
C9	0.050 (10)	0.039 (6)	0.067 (9)	−0.004 (6)	0.032 (8)	−0.001 (6)
C10	0.031 (9)	0.052 (7)	0.088 (11)	−0.014 (7)	0.024 (8)	−0.017 (8)
C11	0.018 (8)	0.072 (10)	0.092 (13)	0.001 (7)	0.003 (7)	−0.006 (9)
C12	0.027 (8)	0.054 (7)	0.081 (11)	0.015 (7)	0.016 (7)	0.019 (8)

Geometric parameters (Å, º)

Pb1—O1	2.338 (7)	C4—C5	1.45 (2)
Pb1—O1^i	2.492 (8)	C4—H4	0.930
Pb1—N1	2.591 (9)	C6—C5	1.32 (2)
Pb1—N2^i	2.730 (12)	C6—H6	0.930
Pb2—O2	2.289 (9)	C5—H5	0.930
Pb2—O2^ii	2.442 (8)	O2—Pb2^ii	2.442 (8)
Pb2—O1	2.463 (8)	N4—C8	1.367 (18)
Pb2—N3^i	2.625 (11)	N4—N5	1.371 (15)
Pb2—N4	2.646 (10)	N6—N5	1.298 (18)
N1—N2	1.333 (14)	N6—C7	1.359 (19)
N1—C2	1.373 (17)	C7—C12	1.37 (2)
O1—Pb1^iii	2.492 (8)	C7—C8	1.422 (17)
C3—C4	1.33 (2)	C8—C9	1.40 (2)
C3—C2	1.374 (19)	C10—C9	1.35 (2)
C3—H3	0.930	C10—C11	1.45 (2)
N2—N3	1.372 (15)	C10—H10	0.930
N2—Pb1^iii	2.730 (12)	C9—H9	0.930
C1—N3	1.321 (17)	C12—C11	1.34 (2)
C1—C6	1.408 (19)	C12—H12	0.930
C1—C2	1.411 (16)	C11—H11	0.930
N3—Pb2^iii	2.625 (11)
O1—Pb1—O1^i	97.07 (18)	N1—C2—C1	105.6 (10)
O1—Pb1—N1	75.9 (3)	C3—C2—C1	122.9 (12)
O1^i—Pb1—N1	76.4 (3)	C3—C4—C5	120.4 (14)
O1—Pb1—N2^i	75.0 (3)	C3—C4—H4	119.8
O1^i—Pb1—N2^i	68.3 (3)	C5—C4—H4	119.8
N1—Pb1—N2^i	130.3 (4)	C5—C6—C1	116.0 (14)
O2—Pb2—O2^ii	71.3 (3)	C5—C6—H6	122.0
O2—Pb2—O1	77.9 (3)	C1—C6—H6	122.0
O2^ii—Pb2—O1	91.7 (3)	C6—C5—C4	123.8 (13)
O2—Pb2—N3^i	74.7 (3)	C6—C5—H5	118.1
O2^ii—Pb2—N3^i	146.0 (3)	C4—C5—H5	118.1
O1—Pb2—N3^i	82.4 (3)	Pb2—O2—Pb2^ii	108.7 (3)
O2—Pb2—N4	80.6 (3)	C8—N4—N5	105.4 (10)
O2^ii—Pb2—N4	82.2 (3)	C8—N4—Pb2	114.2 (8)
O1—Pb2—N4	158.5 (3)	N5—N4—Pb2	118.5 (8)
N3^i—Pb2—N4	91.1 (4)	N5—N6—C7	107.5 (11)
N2—N1—C2	108.6 (9)	N6—C7—C12	132.5 (12)
N2—N1—Pb1	117.7 (8)	N6—C7—C8	107.4 (12)
C2—N1—Pb1	133.3 (7)	C12—C7—C8	120.1 (13)
Pb1—O1—Pb2	107.5 (3)	N4—C8—C9	131.6 (12)
Pb1—O1—Pb1^iii	118.0 (3)	N4—C8—C7	106.9 (11)
Pb2—O1—Pb1^iii	119.3 (3)	C9—C8—C7	121.5 (13)
C4—C3—C2	117.1 (14)	N6—N5—N4	112.8 (12)
C4—C3—H3	121.4	C9—C10—C11	120.6 (14)
C2—C3—H3	121.4	C9—C10—H10	119.7
N1—N2—N3	109.1 (11)	C11—C10—H10	119.7
N1—N2—Pb1^iii	125.3 (8)	C10—C9—C8	117.3 (14)
N3—N2—Pb1^iii	125.3 (8)	C10—C9—H9	121.3
N3—C1—C6	131.6 (13)	C8—C9—H9	121.3
N3—C1—C2	108.7 (11)	C11—C12—C7	118.4 (13)
C6—C1—C2	119.7 (12)	C11—C12—H12	120.8
C1—N3—N2	108.0 (11)	C7—C12—H12	120.8
C1—N3—Pb2^iii	141.8 (9)	C12—C11—C10	121.9 (14)
N2—N3—Pb2^iii	109.9 (8)	C12—C11—H11	119.1
N1—C2—C3	131.3 (11)	C10—C11—H11	119.1
O1—Pb1—N1—N2	23.8 (8)	N3—C1—C2—C3	−175.7 (12)
O1^i—Pb1—N1—N2	−77.2 (8)	C6—C1—C2—C3	3.1 (19)
N2^i—Pb1—N1—N2	−31.9 (9)	C2—C3—C4—C5	2 (2)
O1—Pb1—N1—C2	−148.7 (11)	N3—C1—C6—C5	177.1 (15)
O1^i—Pb1—N1—C2	110.3 (10)	C2—C1—C6—C5	−1 (2)
N2^i—Pb1—N1—C2	155.5 (9)	C1—C6—C5—C4	0 (2)
O1^i—Pb1—O1—Pb2	−121.5 (4)	C3—C4—C5—C6	−1 (3)
N1—Pb1—O1—Pb2	164.5 (4)	O2^ii—Pb2—O2—Pb2^ii	0.0
N2^i—Pb1—O1—Pb2	−56.3 (4)	O1—Pb2—O2—Pb2^ii	−96.0 (4)
O1^i—Pb1—O1—Pb1^iii	17.0 (3)	N3^i—Pb2—O2—Pb2^ii	178.6 (4)
N1—Pb1—O1—Pb1^iii	−57.0 (4)	N4—Pb2—O2—Pb2^ii	84.9 (3)
N2^i—Pb1—O1—Pb1^iii	82.2 (4)	O2—Pb2—N4—C8	141.1 (9)
O2—Pb2—O1—Pb1	−17.3 (3)	O2^ii—Pb2—N4—C8	−146.7 (9)
O2^ii—Pb2—O1—Pb1	−87.8 (3)	O1—Pb2—N4—C8	138.6 (9)
N3^i—Pb2—O1—Pb1	58.6 (4)	N3^i—Pb2—N4—C8	66.8 (9)
N4—Pb2—O1—Pb1	−14.9 (11)	O2—Pb2—N4—N5	16.0 (9)
O2—Pb2—O1—Pb1^iii	−155.2 (4)	O2^ii—Pb2—N4—N5	88.2 (10)
O2^ii—Pb2—O1—Pb1^iii	134.3 (4)	O1—Pb2—N4—N5	13.5 (15)
N3^i—Pb2—O1—Pb1^iii	−79.3 (4)	N3^i—Pb2—N4—N5	−58.3 (9)
N4—Pb2—O1—Pb1^iii	−152.7 (7)	N5—N6—C7—C12	−178.3 (16)
C2—N1—N2—N3	−0.5 (14)	N5—N6—C7—C8	1.4 (15)
Pb1—N1—N2—N3	−174.8 (8)	N5—N4—C8—C9	179.0 (14)
C2—N1—N2—Pb1^iii	−174.6 (8)	Pb2—N4—C8—C9	47.2 (17)
Pb1—N1—N2—Pb1^iii	11.1 (12)	N5—N4—C8—C7	−0.7 (13)
C6—C1—N3—N2	−178.3 (14)	Pb2—N4—C8—C7	−132.6 (8)
C2—C1—N3—N2	0.2 (15)	N6—C7—C8—N4	−0.4 (14)
C6—C1—N3—Pb2^iii	9 (3)	C12—C7—C8—N4	179.4 (13)
C2—C1—N3—Pb2^iii	−172.3 (11)	N6—C7—C8—C9	179.9 (12)
N1—N2—N3—C1	0.1 (15)	C12—C7—C8—C9	0 (2)
Pb1^iii—N2—N3—C1	174.3 (9)	C7—N6—N5—N4	−2.0 (16)
N1—N2—N3—Pb2^iii	175.2 (7)	C8—N4—N5—N6	1.7 (15)
Pb1^iii—N2—N3—Pb2^iii	−10.7 (13)	Pb2—N4—N5—N6	131.0 (10)
N2—N1—C2—C3	175.2 (13)	C11—C10—C9—C8	−1 (2)
Pb1—N1—C2—C3	−12 (2)	N4—C8—C9—C10	180.0 (14)
N2—N1—C2—C1	0.6 (13)	C7—C8—C9—C10	0 (2)
Pb1—N1—C2—C1	173.6 (8)	N6—C7—C12—C11	−177.4 (17)
C4—C3—C2—N1	−177.4 (15)	C8—C7—C12—C11	3 (2)
C4—C3—C2—C1	−4 (2)	C7—C12—C11—C10	−5 (3)
N3—C1—C2—N1	−0.5 (14)	C9—C10—C11—C12	4 (3)
C6—C1—C2—N1	178.3 (12)

Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1/2, −y+3/2, −z+1; (iii) −x+1/2, y+1/2, −z+1/2.