Di-μ-aqua-bis-(μ-pyridazine-4-carboxyl-ato-κN:N')bis-[triaqua-(pyridazine-4-carboxyl-ato-κO,O')lead(II)] dihydrate.

The structure of the title compound, [Pb(2)(C(5)H(3)N(2)O(2))(4)(H(2)O)(6)]·2H(2)O, is composed of dimeric mol-ecules in which two symmetry-related Pb(2+) ions are bridged by a pair of two pyridazine-4-carboxyl-ate ligand mol-ecules via both heterocyclic N atoms and two water O atoms. Each Pb(2+) ion is also coordinated by two carboxyl-ate O atoms and three water O atoms, leading to a highly irregular coordination polyhedron around Pb(2+). The dimers are inter-connected by hydrogen bonds between coordinated and uncoordinated water mol-ecules and the carboxyl-ate O atoms. O-H⋯N inter-actions are also present.

Related literature

For the crystal structure of pyridazine-4-carboxylic acid hydro­chloride, see: Starosta & Leciejewicz (2008 ▶). Centrosymmetric dimeric mol­ecules were reported in the structure of a calcium(II) complex with pyridazine-3-dicarboxyl­ate and water ligands (Starosta & Leciejewicz, 2007 ▶) and an uranyl complex with the same ligands (Leciejewicz & Starosta, (2009 ▶). Each dimer shows a different bridging mode.

Experimental

Crystal data

[Pb2(C5H3N2O2)4(H2O)6]·2H2O

M = 1086.92

Triclinic,

a = 7.0762 (14) Å

b = 9.2967 (19) Å

c = 12.830 (3) Å

α = 92.05 (3)°

β = 105.13 (3)°

γ = 102.85 (3)°

V = 790.4 (3) Å3

Z = 1

Mo Kα radiation

μ = 10.73 mm−1

T = 293 K

0.35 × 0.18 × 0.03 mm

Data collection

Kuma KM-4 four-circle diffractometer

Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 ▶) T min = 0.254, T max = 0.762

4862 measured reflections

4512 independent reflections

3958 reflections with I > 2σ(I)

R int = 0.016

3 standard reflections every 200 reflections intensity decay: 1.2%

Refinement

R[F 2 > 2σ(F 2)] = 0.045

wR(F 2) = 0.122

S = 1.06

4512 reflections

253 parameters

15 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 5.63 e Å−3

Δρmin = −3.77 e Å−3

Data collection: KM-4 Software (Kuma, 1996 ▶); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809039658/bv2128sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809039658/bv2128Isup2.hkl

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

[Pb2(C5H3N2O2)4(H2O)6]·2H2O	Z = 1
Mr = 1086.92	F(000) = 516
Triclinic, P1	Dx = 2.283 Mg m−3
a = 7.0762 (14) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.2967 (19) Å	Cell parameters from 25 reflections
c = 12.830 (3) Å	θ = 6–15°
α = 92.05 (3)°	µ = 10.73 mm−1
β = 105.13 (3)°	T = 293 K
γ = 102.85 (3)°	Plate, colourless
V = 790.4 (3) Å3	0.35 × 0.18 × 0.03 mm

Kuma KM-4 four-circle diffractometer	3958 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.016
graphite	θmax = 30.2°, θmin = 1.7°
Profile data from ω/2θ scans	h = 0→9
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = −13→12
Tmin = 0.254, Tmax = 0.762	l = −18→16
4862 measured reflections	3 standard reflections every 200 reflections
4512 independent reflections	intensity decay: 1.2%

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)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.122	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ2(Fo2) + (0.1029P)2] where P = (Fo2 + 2Fc2)/3
4512 reflections	(Δ/σ)max = 0.002
253 parameters	Δρmax = 5.63 e Å−3
15 restraints	Δρmin = −3.77 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
Pb1	0.11555 (3)	0.048890 (18)	0.675973 (14)	0.02300 (9)
O11	0.4666 (8)	0.6974 (5)	0.6607 (4)	0.0360 (10)
O4	−0.2317 (7)	0.0086 (5)	0.5150 (4)	0.0309 (9)
O21	0.2153 (8)	0.1496 (5)	0.8788 (4)	0.0387 (11)
O1	0.3206 (8)	−0.1283 (6)	0.7946 (4)	0.0395 (11)
H11	0.430 (8)	−0.075 (11)	0.838 (5)	0.047*
H12	0.347 (11)	−0.155 (10)	0.736 (4)	0.047*
N12	0.1246 (8)	0.2794 (5)	0.5304 (4)	0.0265 (9)
N11	0.0425 (8)	0.2525 (5)	0.4237 (4)	0.0280 (10)
O22	0.0922 (10)	0.3005 (6)	0.7692 (4)	0.0452 (13)
O12	0.4408 (7)	0.7751 (4)	0.4972 (4)	0.0331 (9)
C17	0.4044 (8)	0.6811 (6)	0.5601 (5)	0.0247 (10)
C14	0.2716 (7)	0.5309 (5)	0.5091 (4)	0.0208 (9)
C13	0.2351 (9)	0.4143 (6)	0.5710 (5)	0.0249 (10)
H13	0.2916	0.4317	0.6458	0.030*
C15	0.1807 (9)	0.5029 (6)	0.3995 (5)	0.0273 (11)
H15	0.1940	0.5769	0.3532	0.033*
C16	0.0682 (10)	0.3600 (7)	0.3606 (5)	0.0309 (12)
H16	0.0079	0.3389	0.2863	0.037*
C24	0.2220 (9)	0.3860 (6)	0.9548 (5)	0.0273 (11)
C27	0.1684 (10)	0.2701 (6)	0.8588 (5)	0.0297 (11)
O5	0.7080 (10)	0.0331 (7)	0.9439 (4)	0.0471 (13)
H51	0.753 (16)	0.123 (4)	0.975 (6)	0.057*
H52	0.682 (16)	−0.024 (7)	0.993 (5)	0.057*
N21	0.3150 (10)	0.6062 (7)	1.1197 (5)	0.0385 (13)
N22	0.2595 (11)	0.6394 (6)	1.0184 (6)	0.0391 (13)
C25	0.2804 (11)	0.3556 (7)	1.0582 (5)	0.0342 (13)
H23	0.2907	0.2606	1.0748	0.041*
C23	0.2131 (11)	0.5332 (7)	0.9376 (5)	0.0325 (12)
H25	0.1731	0.5571	0.8667	0.039*
C26	0.3247 (13)	0.4707 (9)	1.1396 (6)	0.0396 (15)
H26	0.3631	0.4503	1.2115	0.048*
O3	0.4919 (9)	0.1749 (7)	0.7070 (4)	0.0449 (12)
O2	−0.1694 (9)	−0.0786 (7)	0.7638 (5)	0.0490 (14)
H41	−0.277 (8)	0.082 (6)	0.533 (5)	0.07 (3)*
H42	−0.316 (12)	−0.072 (6)	0.521 (10)	0.07 (3)*
H31	0.529 (18)	0.231 (10)	0.661 (6)	0.07 (4)*
H32	0.557 (16)	0.215 (11)	0.771 (3)	0.08 (4)*
H21	−0.172 (17)	−0.018 (9)	0.815 (6)	0.05 (3)*
H22	−0.259 (10)	−0.160 (6)	0.740 (7)	0.04 (2)*

	U11	U22	U33	U12	U13	U23
Pb1	0.02442 (13)	0.01967 (12)	0.02294 (13)	0.00112 (8)	0.00730 (9)	−0.00286 (7)
O11	0.040 (2)	0.026 (2)	0.032 (2)	−0.0024 (18)	0.0027 (19)	−0.0031 (17)
O4	0.029 (2)	0.0177 (18)	0.044 (3)	0.0019 (15)	0.0105 (19)	0.0037 (16)
O21	0.049 (3)	0.029 (2)	0.035 (2)	0.010 (2)	0.008 (2)	−0.0061 (18)
O1	0.041 (3)	0.039 (3)	0.039 (3)	0.012 (2)	0.010 (2)	−0.003 (2)
N12	0.031 (2)	0.0161 (19)	0.032 (2)	0.0016 (17)	0.012 (2)	0.0006 (17)
N11	0.032 (2)	0.0169 (19)	0.032 (2)	0.0005 (17)	0.009 (2)	−0.0032 (17)
O22	0.069 (4)	0.039 (3)	0.025 (2)	0.016 (3)	0.007 (2)	−0.0038 (19)
O12	0.036 (2)	0.0166 (17)	0.046 (3)	−0.0025 (16)	0.016 (2)	0.0023 (16)
C17	0.022 (2)	0.015 (2)	0.036 (3)	0.0028 (17)	0.009 (2)	−0.0044 (18)
C14	0.019 (2)	0.0133 (19)	0.031 (3)	0.0033 (16)	0.0100 (19)	−0.0011 (17)
C13	0.025 (2)	0.020 (2)	0.028 (3)	0.0035 (19)	0.006 (2)	0.0020 (19)
C15	0.030 (3)	0.019 (2)	0.033 (3)	0.003 (2)	0.010 (2)	0.006 (2)
C16	0.032 (3)	0.024 (3)	0.030 (3)	0.000 (2)	0.003 (2)	−0.002 (2)
C24	0.032 (3)	0.023 (2)	0.026 (3)	0.005 (2)	0.007 (2)	−0.0055 (19)
C27	0.038 (3)	0.024 (2)	0.027 (3)	0.004 (2)	0.011 (2)	−0.006 (2)
O5	0.064 (4)	0.042 (3)	0.039 (3)	0.016 (3)	0.017 (3)	0.001 (2)
N21	0.040 (3)	0.037 (3)	0.034 (3)	0.004 (2)	0.009 (2)	−0.013 (2)
N22	0.048 (3)	0.025 (2)	0.042 (3)	0.009 (2)	0.010 (3)	−0.005 (2)
C25	0.048 (4)	0.031 (3)	0.025 (3)	0.013 (3)	0.012 (3)	0.001 (2)
C23	0.044 (3)	0.028 (3)	0.027 (3)	0.013 (2)	0.009 (2)	0.003 (2)
C26	0.052 (4)	0.042 (4)	0.024 (3)	0.010 (3)	0.009 (3)	−0.006 (2)
O3	0.043 (3)	0.051 (3)	0.025 (2)	−0.016 (2)	0.008 (2)	−0.007 (2)
O2	0.045 (3)	0.053 (3)	0.042 (3)	−0.012 (2)	0.023 (2)	−0.011 (2)

Pb1—O3	2.578 (6)	C13—H13	0.9300
Pb1—O21	2.593 (5)	C15—C16	1.386 (8)
Pb1—O2	2.638 (6)	C15—H15	0.9300
Pb1—O22	2.647 (5)	C16—H16	0.9300
Pb1—O1	2.688 (6)	C24—C25	1.343 (9)
Pb1—O4	2.707 (5)	C24—C23	1.406 (8)
O11—C17	1.242 (8)	C24—C27	1.517 (8)
O4—H41	0.86 (2)	O5—H51	0.86 (2)
O4—H42	0.87 (2)	O5—H52	0.87 (2)
O21—C27	1.254 (8)	N21—C26	1.308 (10)
O1—H11	0.86 (2)	N21—N22	1.324 (10)
O1—H12	0.86 (2)	N22—C23	1.328 (8)
N12—C13	1.327 (7)	C25—C26	1.390 (9)
N12—N11	1.331 (7)	C25—H23	0.9300
N11—C16	1.320 (8)	C23—H25	0.9300
O22—C27	1.208 (8)	C26—H26	0.9300
O12—C17	1.241 (7)	O3—H31	0.86 (2)
C17—C14	1.514 (7)	O3—H32	0.86 (2)
C14—C15	1.373 (8)	O2—H21	0.86 (2)
C14—C13	1.385 (7)	O2—H22	0.86 (2)
O3—Pb1—O21	79.05 (17)	N12—C13—H13	118.0
O3—Pb1—O2	146.72 (18)	C14—C13—H13	118.0
O21—Pb1—O2	70.88 (18)	C14—C15—C16	117.4 (5)
O3—Pb1—O22	85.5 (2)	C14—C15—H15	121.3
O21—Pb1—O22	49.16 (16)	C16—C15—H15	121.3
O2—Pb1—O22	85.5 (2)	N11—C16—C15	123.2 (6)
O3—Pb1—O1	74.2 (2)	N11—C16—H16	118.4
O21—Pb1—O1	71.28 (16)	C15—C16—H16	118.4
O2—Pb1—O1	82.8 (2)	C25—C24—C23	117.0 (5)
O22—Pb1—O1	119.77 (16)	C25—C24—C27	123.0 (6)
O3—Pb1—O4	137.65 (16)	C23—C24—C27	120.1 (6)
O21—Pb1—O4	132.46 (16)	O22—C27—O21	124.6 (6)
O2—Pb1—O4	75.25 (18)	O22—C27—C24	119.1 (6)
O22—Pb1—O4	96.49 (16)	O21—C27—C24	116.3 (6)
O1—Pb1—O4	135.76 (15)	H51—O5—H52	107 (3)
Pb1—O4—H41	100.9 (17)	C26—N21—N22	120.3 (6)
Pb1—O4—H42	110 (8)	N21—N22—C23	119.1 (6)
H41—O4—H42	107 (3)	C24—C25—C26	117.9 (6)
C27—O21—Pb1	93.8 (4)	C24—C25—H23	121.1
Pb1—O1—H11	110 (8)	C26—C25—H23	121.1
Pb1—O1—H12	87 (7)	N22—C23—C24	122.7 (6)
H11—O1—H12	109 (3)	N22—C23—H25	118.7
C13—N12—N11	118.9 (5)	C24—C23—H25	118.7
C16—N11—N12	119.9 (5)	N21—C26—C25	123.0 (7)
C27—O22—Pb1	92.3 (4)	N21—C26—H26	118.5
O12—C17—O11	126.7 (5)	C25—C26—H26	118.5
O12—C17—C14	116.7 (5)	Pb1—O3—H31	120 (8)
O11—C17—C14	116.6 (5)	Pb1—O3—H32	117 (8)
C15—C14—C13	116.5 (5)	H31—O3—H32	109 (4)
C15—C14—C17	122.0 (5)	Pb1—O2—H21	108 (7)
C13—C14—C17	121.5 (5)	Pb1—O2—H22	127 (6)
N12—C13—C14	124.0 (5)	H21—O2—H22	124 (10)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H41···O12i	0.86 (2)	1.93 (2)	2.736 (6)	154 (4)
O4—H42···O12ii	0.87 (2)	1.92 (4)	2.754 (6)	161 (11)
O1—H11···O5	0.86 (2)	2.08 (3)	2.943 (9)	174 (10)
O1—H12···O11iii	0.86 (2)	2.09 (6)	2.849 (7)	146 (9)
O5—H51···N22iv	0.86 (2)	2.23 (5)	3.013 (8)	151 (9)
O5—H52···O21v	0.87 (2)	2.12 (6)	2.897 (8)	149 (10)
O3—H31···O12vi	0.86 (2)	2.09 (7)	2.819 (7)	142 (10)
O3—H32···N21iv	0.86 (2)	2.01 (6)	2.794 (7)	151 (10)
O2—H21···O5vii	0.86 (2)	2.13 (5)	2.906 (8)	150 (9)
O2—H22···O11ii	0.86 (2)	2.07 (4)	2.891 (7)	159 (9)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H41⋯O12i	0.86 (2)	1.93 (2)	2.736 (6)	154 (4)
O4—H42⋯O12ii	0.87 (2)	1.92 (4)	2.754 (6)	161 (11)
O1—H11⋯O5	0.86 (2)	2.08 (3)	2.943 (9)	174 (10)
O1—H12⋯O11iii	0.86 (2)	2.09 (6)	2.849 (7)	146 (9)
O5—H51⋯N22iv	0.86 (2)	2.23 (5)	3.013 (8)	151 (9)
O5—H52⋯O21v	0.87 (2)	2.12 (6)	2.897 (8)	149 (10)
O3—H31⋯O12vi	0.86 (2)	2.09 (7)	2.819 (7)	142 (10)
O3—H32⋯N21iv	0.86 (2)	2.01 (6)	2.794 (7)	151 (10)
O2—H21⋯O5vii	0.86 (2)	2.13 (5)	2.906 (8)	150 (9)
O2—H22⋯O11ii	0.86 (2)	2.07 (4)	2.891 (7)	159 (9)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .