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The PbII cation in the title compound, [Pb2(C14H4N2O8)]n, is seven-coordinated by one N atom and six O atoms from four 4,4′-bipyridine-2,2′,6,6′-tetra­carboxyl­ate (BPTCA4−) ligands. The geometric centre of the BPTCA4− anion lies on an inversion centre. Each pyridine-2,6-dicarboxyl­ate moiety of the BPTCA4− ligand links four PbII cations via its pyridyl N atom and two carboxyl­ate groups to form two-dimensional sheets. The centrosymmetric BPTCA4− ligand then acts as a linker between the sheets, which results in a three-dimensional metal–organic framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109053736/eg3035sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270109053736/eg3035Isup2.hkl
Contains datablock I

CCDC reference: 774018

Comment top

A number of PbII–carboxylate complexes with layered or three-dimensional network structures have been reported in recent years (Ayyappan et al., 1999; Fredoueil et al., 2002; Drumel et al., 1995; Bentiss et al., 2004). This might be partly ascribed to the unique coordination chemistry of the PbII cation, due to its large radius, variable stereochemical activity and flexible coordination environment, which is different from those of the divalent transition metal ions (Zhang, Zhou et al., 2008). To construct the targeted PbII network, nitrogen-containing polytopic organic acids (Liang et al., 2007; Cheng et al., 2006; Zhao et al., 2003; Gao et al., 2006; Wang et al., 2007; Mahata & Natarajan, 2005) are usually selected as the linkers, due to their abundant coordination modes in bridging PbII cations into clusters or multi-dimensional frameworks (Ayyappan et al., 1999; Fredoueil et al., 2002). For further investigation of the coordination chemistry of PbII, 4,4'-bipyridine-2,2',6,6'-tetracarboxylic acid (H4BPTCA) was used as the linker in this work, due to its versatile binding modes and its interesting skeleton (Lin et al., 2006; Bai, Qi et al., 2008; Bai, Liu et al., 2008). Thus, we present here the synthesis and crystal structure of the title compound, [Pb2(C14H4N2O8)]n, (I).

Compound (I) was obtained in the form of light-yellow pyramid-shaped crystals, which are stable at ambient temperature. Single-crystal structure analysis reveals that it crystallizes in the monoclinic space group C2/c with the H4BPTCA ligand completely deprotonated, which is also indicated by IR spectroscopic data. As shown in Fig. 1, the PbII cation possesses a monocapped trigonal prism geometry completed by two O atoms and one N atom from one BPTCA4- ligand, two carboxylate O atoms from another BPTCA4- ligand, and another two carboxylate O atoms from two different BPTCA4- ligands. The Pb—O bond lengths are in the range 2.404 (6)–2.847 (7) Å and the Pb—N bond length is 2.459 (7) Å. The geometric centre of BPTCA4- anion lies on an inversion centre. Each pyridinedicarboxylate moiety of the BPTCA4- anion uses one syn–anti carboxylate group (O1—C1—O2) to connect adjacent PbII cations, forming one-dimensional chains along the b direction. The other carboxylate group of the pyridinedicarboxylate moiety uses atom O3 to coordinate to two PbII cations from two neighbouring chains to form a belt [Ribbon?] (Fig. 2) and atom O4 to coordinate to two PbII cations from two neighbouring belts [Ribbons?], leading to the construction of two-dimensional sheets parallel to the bc plane (Fig. 3). Neighbouring two-dimensional sheets are further connected via BPTCA4- ligands through two pyridinedicarboxylate moieties, resulting in the construction of a three-dimensional metal–organic framework (Fig. 4).

As described above, one carboxylate group of the pyridinedicarboxylate moiety of the BPTCA4- ligand adopts a syn–anti coordination mode, while the other presents a µ3,η4-bridging mode. Thus, each pyridinedicarboxylate moiety of the BPTCA4- ligand behaves as a µ4,η7 bridge and each BPTCA4- ligand acts as a µ8,η14 linker.

The structure of (I) is different from those of the related three-dimensional isostructural complexes [Mn2(BPTCA)(µ2-H2O)2]n (Bai, Qi et al., 2008) and [Cd2(BPTCA)(µ2-H2O)2]n (Bai, Liu et al., 2008), in which the infinite –M–O– (M = Mn or Cd) zigzag chains built from the bridging water molecules and MII ions are bridged by carboxylate groups to generate a two-dimensional network. These two-dimensional networks are further pillared by BPTCA4- ligands to form a three-dimensional porous inorganic–organic polymer. Each pyridinedicarboxylate moiety of the BPTCA4- ligand in the two compounds adopts a µ3-bridging mode to link three metal ions with two carboxylate groups, presenting different coordination modes: one adopts a syn–anti µ2η1:η1 bridging mode to link two metal ions, and the other acts as a µ2η2:η0 bridge. The structure of (I) is also entirely different from that of the related three-dimensional complex {[Zn2(BPTCA)].4H2O} (Lin et al., 2006) with a 4666 topology, which crystallizes in a chiral space group, P42212, with the chirality generated by the helical chains of hydrogen-bonded guest water molecules rather than by the coordination framework. Another two two-dimensional MnII complexes (Bai, Qi et al., 2008) and one two-dimensional CuII complex (Bai, Liu et al., 2008) were also reported to be constructed from the BPTCA4- ligand.

The geometries of PbII cations can be classified into hemidirectionality and holodirectionality. Hemidirectionality refers to a PbII cation which spreads the ligands within a single hemisphere to have its valence lone pair expanding within the other hemisphere (Gourlaouen et al., 2008; van Severen et al., 2009). In compound (I), the central PbII cation is seven-coordinated in a moncapped trigonal prism geometry by one N atom and six O atoms from four BPTCA4- ligands. The seven atoms are located on one side of the PbII cation, which shows hemidirectionality, leaving the other side for the stereochemically active lone pair. This is similar to previously reported examples of PbII hemidirectionality, such as [Pb(INO)2]2.7H2O (Zhao et al., 2007), [Pb(HIDC)]n (H3IDC is imidazole-4,5-dicarboxylic acid; Zhang, Song et al., 2008), [Pb(fum)]n (fum is fumarate; Zhang et al., 2009), [Pb23-ba)22-ba)2]n (ba is benzylacetylacetonate; Ahmadzadi et al., 2009), [Pb(suc)(H2bbp)]2 [H2suc is succinic acid and H2bbp is 2,6-bis(2-benzimidazolyl) pyridine; Meng et al., 2009], and [Pb(INA)2] (INA is isonicotinate, NC5H4-4-CO2-; Zhang, Zhou et al., 2008). The PbII cations in these compounds present different coordination numbers. The arrangement of the ligands around the PbII cations in these compounds suggest a vacant site in the coordination geometry around the metal ions, which is possibly occupied by a stereoactive lone electron pair on PbII. Therefore, the PbII cations in these compounds also adopt hemidirected geometry.

Experimental top

H4BPTCA (86 mg, 0.025 mmol) was dissolved in water (14 ml) and NaOH (66 mg, 0.165 mmol) was added to the solution. After stirring for 30 min, PbCO3 (108.1 mg, 0.028 mmol) was added to the mixture. The resulting solution was transferred to a 25 ml Teflon-lined stainless steel autoclave and heated at 373 K for 4 d. The autoclave was then allowed to cool down to room temperature over a period of 24 h. Light-yellow pyramid-shaped crystals of (I) were obtained, washed with deionized water and dried at ambient temperature (yield 40%). Spectroscopic analysis: IR (KBr, ν, cm-1): 3440 (s), 2341 (w), 2274 (w), 1630 (s), 1615 (s), 1593 (s), 1568 (s), 1429 (s), 1401 (s), 1380 (s), 1376 (s), 1333 (s), 1188 (m), 1071 (m), 996 (w), 902 (w), 809 (m), 799 (w), 736 (w), 658 (w).

Refinement top

H atoms were generated geometrically, with C—H = 0.93 Å, and refined as riding, with Uiso(H) = 1.2Ueq(C). In the final difference Fourier map the positions of the highest peak (1.46 e Å-3) and deepest hole (-1.89 e Å-3) are at (0.2100, 0.2182, 0.8709) and (0.2723, 0.1024, 0.0412), which are 0.90 and 1.37 Å from Pb1, respectively.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SHELXTL (Sheldrick, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of compound (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) -x + 1/2, y + 1/2, -z + 1/2; (ii) x, y - 1, z; (iii) x, -y, z - 1/2; (iv) x, y + 1, z; (v) -x + 1/2, y - 1/2 , -z + 1/2; (vi) x, -y, z + 1/2; (vii) -x + 1, -y + 1, -z + 1; (viii) -x + 1, -y, -z + 1; (ix) x + 1/2, -y + 1/2, z + 1/2; (x) -x + 1, y + 1, -z + 3/2; (xi) -x + 1, -y + 2, -z + 1; (xii) x + 1/2, -y + 3/2, z + 1/2; (xiii) -x + 1, y + 1, -z + 1/2]
[Figure 2] Fig. 2. A view of the one-dimensional chain running along the b direction.
[Figure 3] Fig. 3. A view of the two-dimensional sheet parallel to the bc plane.
[Figure 4] Fig. 4. A view of the three-dimensional metal–organic framework of (I). [Figure seems to be distorted (spheres look oval) - please revise]
Poly[µ8-4,4'-bipyridine-2,2',6,6'-tetracarboxylato-dilead(II)] top
Crystal data top
[Pb2(C14H4N2O8)]F(000) = 1320
Mr = 742.58Dx = 3.387 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2595 reflections
a = 19.696 (2) Åθ = 4.1–28.2°
b = 5.3916 (8) ŵ = 23.15 mm1
c = 14.2090 (16) ÅT = 298 K
β = 105.203 (2)°Pyramid, light-yellow
V = 1456.1 (3) Å30.18 × 0.11 × 0.07 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
1285 independent reflections
Radiation source: fine-focus sealed tube1116 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
ϕ and ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 2323
Tmin = 0.103, Tmax = 0.294k = 64
3640 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.087H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0608P)2]
where P = (Fo2 + 2Fc2)/3
1285 reflections(Δ/σ)max < 0.001
118 parametersΔρmax = 1.46 e Å3
0 restraintsΔρmin = 1.89 e Å3
Crystal data top
[Pb2(C14H4N2O8)]V = 1456.1 (3) Å3
Mr = 742.58Z = 4
Monoclinic, C2/cMo Kα radiation
a = 19.696 (2) ŵ = 23.15 mm1
b = 5.3916 (8) ÅT = 298 K
c = 14.2090 (16) Å0.18 × 0.11 × 0.07 mm
β = 105.203 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
1285 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
1116 reflections with I > 2σ(I)
Tmin = 0.103, Tmax = 0.294Rint = 0.058
3640 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.087H-atom parameters constrained
S = 1.01Δρmax = 1.46 e Å3
1285 reflectionsΔρmin = 1.89 e Å3
118 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 (Å2) top
xyzUiso*/Ueq
Pb10.294943 (16)0.11722 (5)0.14086 (2)0.02183 (18)
N10.3686 (3)0.2881 (13)0.2943 (5)0.0188 (14)
O10.3440 (3)0.5164 (12)0.1216 (4)0.0315 (15)
O20.4088 (3)0.8424 (10)0.1896 (5)0.0257 (14)
O30.2874 (3)0.0997 (9)0.3020 (4)0.0266 (15)
O40.3297 (4)0.1324 (10)0.4622 (5)0.0334 (16)
C10.3863 (5)0.6250 (14)0.1912 (6)0.024 (2)
C20.4069 (4)0.4921 (14)0.2894 (6)0.0170 (17)
C30.4585 (5)0.5794 (14)0.3673 (6)0.0214 (18)
H30.48430.71940.36040.026*
C40.4716 (4)0.4579 (16)0.4557 (6)0.0211 (17)
C50.4286 (5)0.2534 (15)0.4624 (6)0.0208 (18)
H50.43360.17250.52170.025*
C60.3791 (4)0.1746 (15)0.3807 (6)0.0213 (18)
C70.3293 (5)0.0381 (16)0.3837 (7)0.0240 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0186 (3)0.0256 (2)0.0190 (2)0.00259 (12)0.00094 (16)0.00006 (11)
N10.009 (4)0.027 (3)0.017 (3)0.002 (3)0.003 (3)0.001 (3)
O10.035 (4)0.039 (4)0.013 (3)0.009 (3)0.007 (3)0.000 (3)
O20.023 (4)0.027 (3)0.028 (3)0.000 (2)0.008 (3)0.006 (3)
O30.019 (4)0.039 (4)0.018 (3)0.010 (2)0.001 (3)0.001 (2)
O40.036 (4)0.038 (4)0.023 (3)0.015 (3)0.003 (3)0.005 (3)
C10.024 (5)0.030 (5)0.017 (4)0.002 (3)0.004 (4)0.002 (3)
C20.014 (4)0.019 (4)0.018 (4)0.000 (3)0.003 (3)0.003 (3)
C30.016 (5)0.026 (4)0.022 (4)0.002 (3)0.005 (4)0.002 (3)
C40.011 (4)0.031 (4)0.020 (4)0.002 (4)0.002 (4)0.000 (4)
C50.020 (5)0.025 (4)0.015 (4)0.004 (3)0.001 (4)0.004 (3)
C60.016 (5)0.022 (4)0.026 (4)0.004 (3)0.007 (4)0.008 (4)
C70.019 (5)0.026 (4)0.029 (5)0.003 (4)0.009 (4)0.004 (4)
Geometric parameters (Å, º) top
Pb1—O12.404 (6)O3—Pb1v2.512 (6)
Pb1—N12.459 (7)O4—C71.225 (10)
Pb1—O3i2.512 (6)O4—Pb1vi2.798 (7)
Pb1—O32.610 (6)O4—Pb1v2.847 (7)
Pb1—O2ii2.625 (6)C1—C21.526 (11)
Pb1—O4iii2.798 (7)C2—C31.374 (12)
Pb1—O4i2.847 (7)C3—C41.380 (12)
N1—C61.338 (11)C3—H30.9300
N1—C21.346 (10)C4—C51.409 (12)
O1—C11.258 (11)C4—C4vii1.517 (16)
O2—C11.256 (9)C5—C61.372 (12)
O2—Pb1iv2.625 (6)C5—H50.9300
O3—C71.279 (11)C6—C71.517 (11)
O1—Pb1—N166.7 (2)C7—O3—Pb1120.5 (5)
O1—Pb1—O3i78.8 (2)Pb1v—O3—Pb1138.2 (3)
N1—Pb1—O3i76.5 (2)C7—O4—Pb1vi150.5 (6)
O1—Pb1—O3128.19 (18)C7—O4—Pb1v86.0 (5)
N1—Pb1—O363.0 (2)Pb1vi—O4—Pb1v95.6 (2)
O3i—Pb1—O378.39 (12)O2—C1—O1125.7 (8)
O1—Pb1—O2ii101.2 (2)O2—C1—C2116.4 (8)
N1—Pb1—O2ii73.3 (2)O1—C1—C2117.6 (7)
O3i—Pb1—O2ii146.9 (2)N1—C2—C3123.0 (7)
O3—Pb1—O2ii75.94 (19)N1—C2—C1114.4 (7)
O1—Pb1—O4iii70.67 (18)C3—C2—C1122.6 (7)
N1—Pb1—O4iii124.5 (2)C2—C3—C4119.5 (7)
O3i—Pb1—O4iii127.40 (18)C2—C3—H3120.2
O3—Pb1—O4iii153.23 (16)C4—C3—H3120.2
O2ii—Pb1—O4iii81.98 (18)C3—C4—C5117.4 (8)
O1—Pb1—O4i80.5 (2)C3—C4—C4vii122.3 (9)
N1—Pb1—O4i120.5 (2)C5—C4—C4vii120.3 (9)
O3i—Pb1—O4i48.36 (19)C6—C5—C4119.4 (7)
O3—Pb1—O4i115.1 (2)C6—C5—H5120.3
O2ii—Pb1—O4i164.78 (19)C4—C5—H5120.3
O4iii—Pb1—O4i84.4 (2)N1—C6—C5122.6 (7)
C6—N1—C2117.8 (7)N1—C6—C7115.2 (7)
C6—N1—Pb1123.8 (5)C5—C6—C7122.1 (8)
C2—N1—Pb1117.9 (5)O4—C7—O3124.5 (8)
C1—O1—Pb1122.0 (5)O4—C7—C6119.3 (8)
C1—O2—Pb1iv104.5 (6)O3—C7—C6116.1 (7)
C7—O3—Pb1v100.5 (5)
O1—Pb1—N1—C6178.4 (7)Pb1—O1—C1—C21.0 (11)
O3i—Pb1—N1—C694.9 (6)C6—N1—C2—C33.7 (12)
O3—Pb1—N1—C611.2 (6)Pb1—N1—C2—C3168.7 (6)
O2ii—Pb1—N1—C671.2 (6)C6—N1—C2—C1174.0 (7)
O4iii—Pb1—N1—C6138.7 (6)Pb1—N1—C2—C113.6 (9)
O4i—Pb1—N1—C6115.9 (6)O2—C1—C2—N1164.4 (8)
O1—Pb1—N1—C29.7 (5)O1—C1—C2—N19.9 (11)
O3i—Pb1—N1—C293.2 (6)O2—C1—C2—C313.3 (12)
O3—Pb1—N1—C2176.9 (6)O1—C1—C2—C3172.4 (8)
O2ii—Pb1—N1—C2100.7 (6)N1—C2—C3—C41.2 (13)
O4iii—Pb1—N1—C233.2 (7)C1—C2—C3—C4176.3 (7)
O4i—Pb1—N1—C272.2 (6)C2—C3—C4—C52.6 (12)
N1—Pb1—O1—C14.3 (7)C2—C3—C4—C4vii179.2 (9)
O3i—Pb1—O1—C184.2 (7)C3—C4—C5—C64.0 (12)
O3—Pb1—O1—C118.9 (8)C4vii—C4—C5—C6177.8 (9)
O2ii—Pb1—O1—C162.0 (7)C2—N1—C6—C52.2 (12)
O4iii—Pb1—O1—C1139.2 (7)Pb1—N1—C6—C5169.7 (6)
O4i—Pb1—O1—C1133.4 (7)C2—N1—C6—C7174.1 (7)
O1—Pb1—O3—C722.4 (7)Pb1—N1—C6—C714.0 (10)
N1—Pb1—O3—C77.3 (6)C4—C5—C6—N11.6 (13)
O3i—Pb1—O3—C787.9 (6)C4—C5—C6—C7177.7 (8)
O2ii—Pb1—O3—C770.9 (6)Pb1vi—O4—C7—O3102.0 (13)
O4iii—Pb1—O3—C7106.3 (7)Pb1v—O4—C7—O37.7 (9)
O4i—Pb1—O3—C7120.2 (6)Pb1vi—O4—C7—C675.2 (14)
O1—Pb1—O3—Pb1v145.7 (3)Pb1v—O4—C7—C6169.5 (7)
N1—Pb1—O3—Pb1v160.8 (4)Pb1v—O3—C7—O48.8 (10)
O3i—Pb1—O3—Pb1v80.2 (5)Pb1—O3—C7—O4179.2 (7)
O2ii—Pb1—O3—Pb1v121.0 (4)Pb1v—O3—C7—C6168.4 (6)
O4iii—Pb1—O3—Pb1v85.6 (6)Pb1—O3—C7—C63.6 (10)
O4i—Pb1—O3—Pb1v47.9 (4)N1—C6—C7—O4171.2 (8)
Pb1iv—O2—C1—O156.4 (10)C5—C6—C7—O45.1 (13)
Pb1iv—O2—C1—C2117.3 (7)N1—C6—C7—O36.1 (11)
Pb1—O1—C1—O2172.7 (7)C5—C6—C7—O3177.5 (8)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x, y1, z; (iii) x, y, z1/2; (iv) x, y+1, z; (v) x+1/2, y1/2, z+1/2; (vi) x, y, z+1/2; (vii) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Pb2(C14H4N2O8)]
Mr742.58
Crystal system, space groupMonoclinic, C2/c
Temperature (K)298
a, b, c (Å)19.696 (2), 5.3916 (8), 14.2090 (16)
β (°) 105.203 (2)
V3)1456.1 (3)
Z4
Radiation typeMo Kα
µ (mm1)23.15
Crystal size (mm)0.18 × 0.11 × 0.07
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.103, 0.294
No. of measured, independent and
observed [I > 2σ(I)] reflections
3640, 1285, 1116
Rint0.058
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.087, 1.01
No. of reflections1285
No. of parameters118
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.46, 1.89

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2004).

Selected geometric parameters (Å, º) top
Pb1—O12.404 (6)Pb1—O2ii2.625 (6)
Pb1—N12.459 (7)Pb1—O4iii2.798 (7)
Pb1—O3i2.512 (6)Pb1—O4i2.847 (7)
Pb1—O32.610 (6)
O1—Pb1—N166.7 (2)N1—Pb1—O4iii124.5 (2)
O1—Pb1—O3i78.8 (2)O3i—Pb1—O4iii127.40 (18)
N1—Pb1—O3i76.5 (2)O3—Pb1—O4iii153.23 (16)
O1—Pb1—O3128.19 (18)O2ii—Pb1—O4iii81.98 (18)
N1—Pb1—O363.0 (2)O1—Pb1—O4i80.5 (2)
O3i—Pb1—O378.39 (12)N1—Pb1—O4i120.5 (2)
O1—Pb1—O2ii101.2 (2)O3i—Pb1—O4i48.36 (19)
N1—Pb1—O2ii73.3 (2)O3—Pb1—O4i115.1 (2)
O3i—Pb1—O2ii146.9 (2)O2ii—Pb1—O4i164.78 (19)
O3—Pb1—O2ii75.94 (19)O4iii—Pb1—O4i84.4 (2)
O1—Pb1—O4iii70.67 (18)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x, y1, z; (iii) x, y, z1/2.
 

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