Poly[diaqua-μ₃-nitrato-[μ₂-5-(2-pyrazin­yl)-5H-tetra­zolato]lead(II)]

In the crystal structure of the polymeric title compound, [Pb(C₅H₃N₆)(NO₃)(H₂O)₂]_n, pyrazinyltetra­zolate and nitrate ligands chelate a water-coordinated Pb atom, while the heterocyclic ligand is additionally linked to an adjacent Pb atom and the nitrate ligand is linked to two other neighboring Pb atoms. Bridging by the two ligands leads to the formation of a layer architecture with adjacent layers connected into a three-dimensional network by O–H...N hydrogen bonds. The Pb atom has a bicapped square-anti­prismatic coordination geometry.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](Wave) = 0.000 Å
• R factor = 0.027
• wR factor = 0.078
• Data-to-parameter ratio = 14.9

checkCIF/PLATON results

No syntax errors found



Alert level A
ABSTM02_ALERT_3_A  Crystal and compound unsuitable for non-numerical
               corrections. Product of mu and tmid > 3.0
             Value of mu given =    15.704 tmid =     0.200

Author Response: The crystal is only marginally larger.

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C5 H7 N7 O5 Pb1
            Atom count from _chemical_formula_moiety:

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

   1 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
   0 ALERT type 5 Informative message, check

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S1. Comment

The preceeding paper describes the structure of the copper derivative of 2-(1H-tetrazol-5-yl)pyrazine, which is the first report of a metal derivative (Liu et al., 2007).

Related literature

See Liu et al., 2007 for a report of the copper(II)pyrazinyltetrazolate derivative.

S2. Experimental

Lead nitrate (33 mg, 0.1 mmol) and 2-(1H-tetrazol-5-yl)pyrazine (30 mg, 0.2 mmol) were dissolved in 10 ml of 1:1 methanol/water solution. The solution was filtered and set aside for crystals to grow. Colorless crystals were isolated in 50% yield after two weeks.

S3. Refinement

H atoms were placed at calculated positions [C—H = 0.93, O–H = 0.82 Å; U(H) = 1.2U_eq(C,O)], as were included in the refinement in the riding model approximation. The hydrogen atoms of the water molecules were rotated to fit the electron density. The final difference Fourier map had a large peak at 1 Å and a deep hole at 1 Å from Pb1.

Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).

Figures

	Fig. 1. Thermal ellipsoid plot of a part of the layer structure of the title compound with ellipsoids are drawn at the 70% probability level.
	Fig. 2. A repesentation of the bicapped square-antiprismatic geometry of Pb1.

Poly[diaqua-µ₃-nitrato-[µ₂-5-(2-pyrazinyl)-5H-tetrazolato]lead(II)]

Crystal data

[Pb(C5H3N6)(NO3)(H2O)2]	F(000) = 1664
Mr = 452.37	Dx = 2.791 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4180 reflections
a = 25.2969 (6) Å	θ = 2.2–28.3°
b = 5.7523 (2) Å	µ = 15.70 mm^−1
c = 15.7938 (4) Å	T = 295 K
β = 110.484 (1)°	Block, colorless
V = 2152.9 (1) Å^3	0.22 × 0.20 × 0.16 mm
Z = 8

Data collection

Bruker APEX area-detector diffractometer	2475 independent reflections
Radiation source: fine-focus sealed tube	2011 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
φ and ω scans	θmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan SADABS (Sheldrick, 1996)	h = −31→32
Tmin = 0.056, Tmax = 0.188	k = −7→7
8341 measured reflections	l = −20→20

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)] = 0.027	H-atom parameters constrained
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0495P)^2 + 3.9882P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.001
2475 reflections	Δρmax = 2.05 e Å^−3
166 parameters	Δρmin = −1.44 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00140 (8)

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

	x	y	z	Uiso*/Ueq
Pb1	0.64631 (1)	0.75580 (3)	0.70393 (1)	0.0202 (1)
O1	0.6691 (2)	0.2869 (6)	0.7253 (3)	0.035 (1)
O2	0.7463 (2)	0.4286 (7)	0.8195 (3)	0.050 (1)
O3	0.7162 (2)	0.0889 (7)	0.8421 (3)	0.050 (1)
O1w	0.5588 (1)	0.5188 (6)	0.6531 (2)	0.028 (1)
O2w	0.5674 (1)	0.9748 (6)	0.7340 (2)	0.030 (1)
N1	0.5892 (1)	0.9584 (6)	0.5529 (2)	0.019 (1)
N2	0.5576 (2)	1.1515 (7)	0.5335 (2)	0.023 (1)
N3	0.5363 (2)	1.1800 (7)	0.4459 (2)	0.024 (1)
N4	0.5536 (1)	1.0045 (6)	0.4050 (2)	0.022 (1)
N5	0.6433 (2)	0.3878 (7)	0.3736 (2)	0.026 (1)
N6	0.6472 (1)	0.5581 (6)	0.5411 (2)	0.020 (1)
N7	0.7111 (2)	0.2686 (6)	0.7966 (3)	0.026 (1)
C1	0.5856 (2)	0.8710 (8)	0.4729 (2)	0.017 (1)
C2	0.6164 (2)	0.6626 (9)	0.4636 (3)	0.018 (1)
C3	0.6142 (2)	0.5754 (8)	0.3806 (3)	0.026 (1)
C4	0.6739 (2)	0.2854 (8)	0.4513 (4)	0.024 (1)
C5	0.6757 (2)	0.3700 (8)	0.5335 (3)	0.023 (1)
H11	0.5608	0.4219	0.6163	0.033*
H12	0.5315	0.6036	0.6296	0.033*
H21	0.5407	0.9907	0.6865	0.036*
H22	0.5572	0.9013	0.7700	0.036*
H3	0.5916	0.6501	0.3282	0.032*
H4	0.6946	0.1530	0.4495	0.029*
H5	0.6977	0.2930	0.5858	0.027*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.0189 (2)	0.0236 (2)	0.0159 (2)	−0.0001 (1)	0.0034 (1)	0.0014 (1)
O1	0.028 (2)	0.042 (2)	0.027 (2)	0.009 (2)	0.001 (2)	0.006 (1)
O2	0.033 (2)	0.044 (3)	0.071 (3)	−0.013 (2)	0.015 (2)	−0.012 (2)
O3	0.059 (3)	0.038 (2)	0.044 (2)	0.002 (2)	0.005 (2)	0.019 (2)
O1w	0.025 (2)	0.024 (2)	0.028 (2)	0.002 (1)	0.000 (1)	−0.006 (1)
O2w	0.030 (2)	0.040 (2)	0.020 (2)	0.006 (2)	0.007 (1)	0.000 (1)
N1	0.021 (2)	0.016 (2)	0.018 (2)	0.002 (2)	0.003 (1)	−0.001 (1)
N2	0.025 (2)	0.022 (2)	0.022 (2)	−0.003 (2)	0.008 (2)	0.000 (2)
N3	0.020 (2)	0.022 (2)	0.025 (2)	−0.001 (2)	0.003 (2)	0.004 (2)
N4	0.026 (2)	0.019 (2)	0.017 (2)	0.005 (2)	0.003 (1)	0.001 (1)
N5	0.031 (2)	0.026 (2)	0.021 (2)	0.000 (2)	0.009 (2)	−0.002 (2)
N6	0.019 (2)	0.022 (2)	0.018 (2)	0.002 (2)	0.005 (1)	0.001 (1)
N7	0.024 (2)	0.028 (3)	0.028 (2)	0.002 (2)	0.011 (2)	0.002 (2)
C1	0.017 (2)	0.019 (2)	0.015 (2)	−0.001 (2)	0.005 (2)	0.001 (2)
C2	0.017 (2)	0.019 (2)	0.021 (2)	−0.001 (2)	0.010 (2)	0.005 (2)
C3	0.033 (2)	0.028 (3)	0.015 (2)	0.004 (2)	0.005 (2)	0.001 (2)
C4	0.020 (2)	0.021 (2)	0.032 (3)	0.002 (2)	0.010 (2)	−0.004 (2)
C5	0.023 (2)	0.020 (2)	0.022 (2)	0.003 (2)	0.005 (2)	0.003 (2)

Geometric parameters (Å, º)

Pb1—O1	2.754 (3)	N3—N4	1.351 (5)
Pb1—O1^i	3.105 (4)	N4—C1	1.337 (5)
Pb1—O2	3.169 (4)	N5—C3	1.333 (6)
Pb1—O2^ii	3.033 (4)	N5—C4	1.337 (6)
Pb1—O3^i	2.976 (4)	N6—C5	1.330 (5)
Pb1—O1w	2.483 (3)	N6—C2	1.341 (5)
Pb1—O2w	2.541 (3)	C1—C2	1.466 (7)
Pb1—N1	2.593 (3)	C2—C3	1.386 (6)
Pb1—N5^iii	2.830 (3)	C4—C5	1.373 (7)
Pb1—N6	2.819 (3)	O1w—H11	0.8200
O1—N7	1.253 (6)	O1w—H12	0.8200
O2—N7	1.243 (5)	O2w—H21	0.8200
O3—N7	1.240 (5)	O2w—H22	0.8200
N1—C1	1.334 (5)	C3—H3	0.9300
N1—N2	1.340 (5)	C4—H4	0.9300
N2—N3	1.307 (5)	C5—H5	0.9300
O1w—Pb1—O2w	70.3 (1)	N5^iii—Pb1—O2	64.0 (1)
O1w—Pb1—N1	78.6 (1)	O3^i—Pb1—O2	79.1 (1)
O2w—Pb1—N1	74.2 (1)	O2^ii—Pb1—O2	72.3 (1)
O1w—Pb1—O1	68.1 (1)	O1^i—Pb1—O2	116.2 (1)
O2w—Pb1—O1	127.4 (1)	N7—O1—Pb1	105.5 (3)
N1—Pb1—O1	125.3 (1)	N7—O2—Pb1	85.7 (3)
O1w—Pb1—N6	77.0 (1)	C1—N1—N2	105.0 (3)
O2w—Pb1—N6	128.9 (1)	C1—N1—Pb1	122.3 (3)
N1—Pb1—N6	61.4 (1)	N2—N1—Pb1	132.8 (2)
O1—Pb1—N6	69.4 (1)	N3—N2—N1	109.8 (4)
O1w—Pb1—N5^iii	80.2 (1)	N2—N3—N4	109.2 (4)
O2w—Pb1—N5^iii	71.6 (1)	C1—N4—N3	104.6 (3)
N1—Pb1—N5^iii	144.2 (1)	C3—N5—C4	116.1 (4)
O1—Pb1—N5^iii	70.9 (1)	C5—N6—C2	116.2 (3)
N6—Pb1—N5^iii	139.2 (1)	C5—N6—Pb1	126.0 (2)
O1w—Pb1—O3^i	145.5 (1)	C2—N6—Pb1	117.7 (3)
O2w—Pb1—O3^i	81.2 (1)	O3—N7—O2	122.0 (5)
N1—Pb1—O3^i	112.5 (1)	O3—N7—O1	118.3 (4)
O1—Pb1—O3^i	119.7 (1)	O2—N7—O1	119.7 (4)
N6—Pb1—O3^i	137.5 (1)	N1—C1—N4	111.4 (4)
N5^iii—Pb1—O3^i	72.5 (1)	N1—C1—C2	122.7 (3)
O1w—Pb1—O2^ii	151.2 (1)	N4—C1—C2	125.8 (3)
O2w—Pb1—O2^ii	131.0 (1)	N6—C2—C3	121.4 (4)
N1—Pb1—O2^ii	88.6 (1)	N6—C2—C1	115.8 (3)
O1—Pb1—O2^ii	100.2 (1)	C3—C2—C1	122.9 (4)
N6—Pb1—O2^ii	74.2 (1)	N5—C3—C2	122.0 (4)
N5^iii—Pb1—O2^ii	122.2 (1)	N5—C4—C5	121.9 (4)
O3^i—Pb1—O2^ii	63.3 (1)	N6—C5—C4	122.3 (4)
O1w—Pb1—O1^i	133.3 (1)	Pb1—O1w—H11	109.5
O2w—Pb1—O1^i	67.7 (1)	Pb1—O1w—H12	109.5
N1—Pb1—O1^i	71.4 (1)	H11—O1w—H12	109.5
O1—Pb1—O1^i	158.0 (2)	Pb1—O2w—H21	109.5
N6—Pb1—O1^i	115.8 (1)	Pb1—O2w—H22	109.5
N5^iii—Pb1—O1^i	104.5 (1)	H21—O2w—H22	109.5
O3^i—Pb1—O1^i	41.2 (1)	N5—C3—H3	119.0
O2^ii—Pb1—O1^i	63.3 (1)	C2—C3—H3	119.0
O1w—Pb1—O2	107.6 (1)	N5—C4—H4	119.0
O2w—Pb1—O2	135.1 (1)	C5—C4—H4	119.0
N1—Pb1—O2	150.7 (1)	N6—C5—H5	118.8
O1—Pb1—O2	42.0 (1)	C4—C5—H5	118.8
N6—Pb1—O2	91.5 (1)
O1w—Pb1—O1—N7	−144.1 (3)	N1—Pb1—N6—C5	178.1 (4)
O2w—Pb1—O1—N7	−104.0 (3)	O1—Pb1—N6—C5	−26.7 (3)
N1—Pb1—O1—N7	159.0 (3)	N5^iii—Pb1—N6—C5	−40.4 (4)
N6—Pb1—O1—N7	132.2 (3)	O3^i—Pb1—N6—C5	85.2 (4)
N5^iii—Pb1—O1—N7	−57.3 (3)	O2^ii—Pb1—N6—C5	80.9 (3)
O3^i—Pb1—O1—N7	−1.6 (4)	O1^i—Pb1—N6—C5	130.0 (3)
O2^ii—Pb1—O1—N7	63.4 (3)	O2—Pb1—N6—C5	9.8 (3)
O1^i—Pb1—O1—N7	24.0 (7)	O1w—Pb1—N6—C2	82.6 (3)
O2—Pb1—O1—N7	14.8 (3)	O2w—Pb1—N6—C2	31.8 (3)
O1w—Pb1—O2—N7	6.0 (3)	N1—Pb1—N6—C2	−1.4 (3)
O2w—Pb1—O2—N7	85.4 (3)	O1—Pb1—N6—C2	153.8 (3)
N1—Pb1—O2—N7	−92.1 (3)	N5^iii—Pb1—N6—C2	140.1 (3)
O1—Pb1—O2—N7	−14.4 (3)	O3^i—Pb1—N6—C2	−94.2 (3)
N6—Pb1—O2—N7	−70.8 (3)	O2^ii—Pb1—N6—C2	−98.5 (3)
N5^iii—Pb1—O2—N7	75.3 (3)	O1^i—Pb1—N6—C2	−49.5 (3)
O3^i—Pb1—O2—N7	151.0 (3)	O2—Pb1—N6—C2	−169.7 (3)
O2^ii—Pb1—O2—N7	−143.7 (3)	Pb1—O2—N7—O3	−155.2 (5)
O1^i—Pb1—O2—N7	169.4 (3)	Pb1—O2—N7—O1	25.0 (4)
O1w—Pb1—N1—C1	−78.5 (3)	Pb1—O1—N7—O3	150.0 (4)
O2w—Pb1—N1—C1	−151.0 (3)	Pb1—O1—N7—O2	−30.2 (5)
O1—Pb1—N1—C1	−26.0 (4)	N2—N1—C1—N4	0.8 (4)
N6—Pb1—N1—C1	2.7 (3)	Pb1—N1—C1—N4	179.5 (3)
N5^iii—Pb1—N1—C1	−133.2 (3)	N2—N1—C1—C2	177.2 (4)
O3^i—Pb1—N1—C1	135.8 (3)	Pb1—N1—C1—C2	−4.2 (6)
O2^ii—Pb1—N1—C1	75.5 (3)	N3—N4—C1—N1	−0.8 (5)
O1^i—Pb1—N1—C1	137.7 (3)	N3—N4—C1—C2	−177.1 (4)
O2—Pb1—N1—C1	27.2 (4)	C5—N6—C2—C3	1.1 (6)
O1w—Pb1—N1—N2	99.7 (4)	Pb1—N6—C2—C3	−179.4 (3)
O2w—Pb1—N1—N2	27.2 (3)	C5—N6—C2—C1	−179.4 (4)
O1—Pb1—N1—N2	152.2 (3)	Pb1—N6—C2—C1	0.1 (5)
N6—Pb1—N1—N2	−179.0 (4)	N1—C1—C2—N6	2.6 (6)
N5^iii—Pb1—N1—N2	45.0 (4)	N4—C1—C2—N6	178.4 (4)
O3^i—Pb1—N1—N2	−46.0 (4)	N1—C1—C2—C3	−177.9 (4)
O2^ii—Pb1—N1—N2	−106.3 (4)	N4—C1—C2—C3	−2.1 (7)
O1^i—Pb1—N1—N2	−44.0 (3)	C4—N5—C3—C2	1.4 (7)
O2—Pb1—N1—N2	−154.5 (3)	N6—C2—C3—N5	−1.7 (7)
C1—N1—N2—N3	−0.5 (4)	C1—C2—C3—N5	178.8 (4)
Pb1—N1—N2—N3	−178.9 (3)	C3—N5—C4—C5	−0.6 (7)
N1—N2—N3—N4	0.0 (5)	C2—N6—C5—C4	−0.3 (6)
N2—N3—N4—C1	0.5 (4)	Pb1—N6—C5—C4	−179.8 (3)
O1w—Pb1—N6—C5	−97.9 (3)	N5—C4—C5—N6	0.1 (7)
O2w—Pb1—N6—C5	−148.7 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···N2^iv	0.82	2.02	2.827 (5)	171
O1w—H12···N3^v	0.82	2.12	2.932 (5)	173
O2w—H21···N4^v	0.82	2.32	3.081 (4)	156
O2w—H22···N4^vi	0.82	2.23	2.846 (4)	132

Symmetry codes: (iv) x, y−1, z; (v) −x+1, −y+2, −z+1; (vi) x, −y+2, z+1/2.