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Acta Cryst. (2007). E63, m2476    [ doi:10.1107/S1600536807037981 ]

Poly[bis([mu]3-benzene-1,4-dicarboxylato-[kappa]4O:O':O'',O''')bis(1-methylpyrrolidin-2-one-[kappa]O)dilead(II)\]

C. Du, S.-Y. Yang and R.-B. Huang

Abstract top

A new coordination polymer, [Pb2(C8H4O4)2(C5H9NO)2]n, has been prepared by the reaction of Pb(NO3)2 with benzene-1,4-dicarboxylic acid (H2bdc) in 1-methylpyrrolidin-2-one (nmp). There are two types of Pb ions in the crystal structure, one coordinated by five O atoms and the other by six O atoms, with severely distorted pyramidal and severely distorted octahedral coordination geometries, respectively.

Comment top

The three-dimensional coordination polymers have received much attention in recent years. However, most of the reported structures are transition metal compounds (Li et al., 1999; Rosi et al., 2005); compounds with main group metals such as Pb are seldom reported (Schuy & Ruschewitz, 2005; Zhou et al., 2006). Herein the crystal structure of a three-dimensional lead coordination polymer [Pb2(C8H4O4)2(C5H9NO)2]n, is reported.

In the title compound, [Pb2(C8H4O4)2(C5H9NO)2]n, the two Pb atoms in the structure exist in different coordination geometries (Fig. 1). The Pb1 ion is coordinated by five O atoms, four of which are from three carboxyl groups and one is from a nmp molecule, with 'stereo-chemically active' electron lone pair, and the coordination sphere is hemi-directed (Hancock et al., 1988). [Pb1—O2 2.381 (4) Å; Pb1—O5 2.410 (4) Å; Pb1—O6 2.461 (4) Å; Pb1—O3i 2.486 (4) Å; Pb1—O9 2.633 (5) Å]. The Pb2 ion is coordinated by six O atoms, five of which are from three carboxyl groups and one is from a nmp molecule. [Pb2—O7 2.434 (4) Å; Pb2—O8 2.456 (4) Å; Pb2—O4ii 2.494 (4) Å; Pb2—O1 2.552 (4) Å; Pb2—O10 2.657 (5) Å; Pb2—O3ii 2.660 (4) Å]. There are three coordination modes between Pb ions and carboxyl groups: (a) chelating/bridging bidentate, (b) chelating bidentate, (c) bidentate. The Pb ions are connected by carboxyl groups to form metal chains along a axis. Furthermore the bdc dianions connect each chain to four neighboring chains, resulting in a three-dimensional network with channels in which nmp molecules reside as coordinated ligands (Fig. 2).

Related literature top

For related literature, see: Hancock et al. (1988); Li et al. (1999); Rosi et al. (2005); Schuy & Ruschewitz (2005); Zhou et al. (2006).

Experimental top

The title compound was synthesized with lead nitrate (0.331 g, 1 mmol) and H2bdc (0.166 g, 1 mmol) in nmp (15 ml). The mixture was placed in a 25 ml conical flask, which was heated at 363 K for 3 days. The product was isolated in 55% yield. The elemental analysis for the title compound is almost in agreement with the theoretical values. (Found wt%: C, 32.88; H, 2.74; N, 2.99; calculated wt%: C, 33.19; H, 2.78; N, 2.98).

Refinement top

H atoms were placed in calculated positions, C—H = 0.94 Å (aromatic), 0.98 Å (methylene), with Uiso(H) = 1.2Ueq(C) and 0.97 Å (methyl), with Uiso(H) = 1.5Ueq(C) and refined in riding mode.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, shown with 50% probability displacement ellipsoids. [Symmetry codes: (i) x, y + 1, z; (ii) x − 1, y + 1, z, (v) 2 − x, 1 − y, 1 − z, (vi) 1 − x, 2 − y, −z.]
[Figure 2] Fig. 2. Perspective view down the a axis showing the three-dimensional structrue of the title compound.
Poly[bis(µ3-benzene-1,4-dicarboxylato-κ4O:O':O'',O''')bis(1- methylpyrrolidin-2-one-κO)dilead(II)] top
Crystal data top
[Pb2(C8H4O4)2(C5H9NO)2]Z = 2
Mr = 940.87F000 = 880
Triclinic, P1Dx = 2.370 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 6.7327 (11) ÅCell parameters from 7207 reflections
b = 10.1503 (17) Åθ = 2.5–28.6º
c = 20.249 (3) ŵ = 12.82 mm−1
α = 78.521 (3)ºT = 223 (2) K
β = 83.357 (3)ºPlate, light-yellow
γ = 77.113 (3)º0.18 × 0.10 × 0.03 mm
V = 1318.3 (4) Å3
Data collection top
Bruker APEX area-detector
diffractometer		6153 independent reflections
Radiation source: fine-focus sealed tube5400 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.038
T = 223(2) Kθmax = 28.6º
φ and ω scansθmin = 1.0º
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		h = −8→8
Tmin = 0.206, Tmax = 0.700k = −13→13
15362 measured reflectionsl = −26→26
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.079  w = 1/[σ2(Fo2) + (0.0336P)2 + 2.0349P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
6153 reflectionsΔρmax = 2.38 e Å−3
361 parametersΔρmin = −1.53 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Pb2(C8H4O4)2(C5H9NO)2]γ = 77.113 (3)º
Mr = 940.87V = 1318.3 (4) Å3
Triclinic, P1Z = 2
a = 6.7327 (11) ÅMo Kα
b = 10.1503 (17) ŵ = 12.82 mm−1
c = 20.249 (3) ÅT = 223 (2) K
α = 78.521 (3)º0.18 × 0.10 × 0.03 mm
β = 83.357 (3)º
Data collection top
Bruker APEX area-detector
diffractometer		6153 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		5400 reflections with I > 2σ(I)
Tmin = 0.206, Tmax = 0.700Rint = 0.038
15362 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.033361 parameters
wR(F2) = 0.079H-atom parameters constrained
S = 1.04Δρmax = 2.38 e Å−3
6153 reflectionsΔρmin = −1.53 e Å−3
Special details top

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 (Å2) top
xyzUiso*/Ueq
Pb10.49390 (3)0.79973 (2)0.293309 (10)0.01922 (7)
Pb20.07338 (3)0.681658 (19)0.205959 (10)0.01888 (7)
O10.3686 (6)0.5548 (4)0.2779 (2)0.0249 (9)
O20.6821 (6)0.5951 (4)0.2572 (2)0.0245 (9)
O30.7606 (6)−0.1078 (4)0.2138 (2)0.0220 (8)
O41.0651 (6)−0.0907 (4)0.2364 (2)0.0294 (10)
O50.8092 (6)0.7332 (4)0.3482 (2)0.0248 (9)
O60.5560 (6)0.6398 (5)0.4009 (2)0.0306 (10)
O70.3786 (6)0.7598 (4)0.1514 (2)0.0282 (9)
O80.1058 (6)0.8232 (4)0.0934 (2)0.0294 (10)
O90.4368 (8)0.9887 (5)0.3696 (3)0.0462 (13)
O100.1395 (8)0.4857 (5)0.1317 (3)0.0397 (12)
C10.6404 (8)0.3726 (5)0.2533 (3)0.0211 (12)
C20.8410 (9)0.3127 (6)0.2657 (3)0.0257 (13)
H2A0.92550.36410.27860.031*
C30.9179 (9)0.1773 (6)0.2592 (3)0.0251 (13)
H3A1.05310.13540.26900.030*
C40.7941 (8)0.1038 (5)0.2381 (3)0.0191 (11)
C50.5969 (9)0.1660 (6)0.2233 (3)0.0237 (12)
H5A0.51550.11690.20720.028*
C60.5179 (9)0.2987 (6)0.2316 (3)0.0241 (12)
H6A0.38170.33940.22270.029*
C70.5572 (9)0.5174 (5)0.2632 (3)0.0206 (11)
C80.8810 (9)−0.0405 (6)0.2293 (3)0.0206 (11)
C90.8759 (9)0.5726 (6)0.4494 (3)0.0211 (11)
C101.0735 (9)0.5929 (6)0.4484 (3)0.0270 (13)
H10A1.12360.65550.41330.032*
C110.7381 (9)0.6534 (6)0.3962 (3)0.0231 (12)
C120.8054 (9)0.4786 (6)0.5013 (3)0.0238 (12)
H12A0.67220.46400.50180.029*
C130.2876 (9)0.8267 (6)0.1006 (3)0.0228 (12)
C140.3981 (8)0.9159 (5)0.0480 (3)0.0205 (11)
C150.5835 (8)0.9424 (6)0.0614 (3)0.0216 (12)
H15A0.63990.90260.10290.026*
C160.3171 (8)0.9733 (6)−0.0138 (3)0.0226 (12)
H16A0.19380.9544−0.02300.027*
C170.5294 (12)1.0507 (7)0.3975 (3)0.0365 (16)
C180.7348 (12)0.9995 (7)0.4256 (4)0.0421 (17)
H18A0.73330.91760.46050.050*
H18B0.83980.97590.38970.050*
C190.7776 (14)1.1124 (10)0.4549 (5)0.065 (3)
H19A0.90211.14090.43250.079*
H19B0.79541.08260.50330.079*
C200.5956 (13)1.2285 (8)0.4433 (4)0.0471 (19)
H20A0.53071.25250.48640.057*
H20B0.63631.30990.41520.057*
C210.2615 (12)1.2598 (8)0.3909 (4)0.0442 (18)
H21A0.19281.20760.36910.066*
H21B0.27991.34320.36000.066*
H21C0.17951.28340.43110.066*
C22−0.0052 (11)0.4676 (7)0.1046 (3)0.0350 (15)
C23−0.1965 (10)0.5733 (7)0.0896 (4)0.0381 (16)
H23A−0.26910.59970.13130.046*
H23B−0.16480.65560.05950.046*
C24−0.3207 (14)0.5057 (10)0.0563 (4)0.060 (2)
H24A−0.34160.55450.00990.072*
H24B−0.45450.50580.08110.072*
C25−0.2025 (14)0.3580 (10)0.0561 (4)0.057 (2)
H25A−0.27620.29160.08440.068*
H25B−0.17800.33790.01010.068*
C260.1454 (15)0.2341 (8)0.0906 (5)0.062 (3)
H26A0.26050.25240.10940.093*
H26B0.18860.20870.04660.093*
H26C0.09500.15950.12050.093*
N10.4575 (9)1.1788 (6)0.4093 (3)0.0355 (13)
N2−0.0156 (11)0.3562 (6)0.0834 (3)0.0448 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.01844 (12)0.01974 (11)0.01939 (12)−0.00224 (8)−0.00335 (8)−0.00412 (8)
Pb20.01798 (12)0.01763 (11)0.02114 (12)−0.00417 (8)−0.00126 (8)−0.00327 (8)
O10.019 (2)0.024 (2)0.028 (2)0.0010 (16)−0.0018 (17)−0.0013 (17)
O20.023 (2)0.0189 (19)0.032 (2)−0.0030 (16)−0.0017 (17)−0.0068 (17)
O30.024 (2)0.0224 (19)0.023 (2)−0.0090 (17)−0.0032 (16)−0.0054 (16)
O40.024 (2)0.022 (2)0.043 (3)−0.0011 (18)−0.0036 (19)−0.0104 (19)
O50.025 (2)0.028 (2)0.018 (2)−0.0050 (17)−0.0075 (16)0.0043 (17)
O60.023 (2)0.045 (3)0.022 (2)−0.010 (2)−0.0072 (17)0.0041 (19)
O70.025 (2)0.033 (2)0.021 (2)−0.0061 (18)−0.0024 (17)0.0083 (18)
O80.025 (2)0.038 (2)0.025 (2)−0.0110 (19)−0.0041 (17)0.0025 (19)
O90.056 (3)0.043 (3)0.050 (3)−0.018 (3)−0.002 (3)−0.025 (3)
O100.042 (3)0.047 (3)0.035 (3)−0.006 (2)−0.010 (2)−0.019 (2)
C10.020 (3)0.019 (3)0.022 (3)0.000 (2)0.000 (2)−0.005 (2)
C20.023 (3)0.024 (3)0.032 (3)−0.007 (2)−0.004 (2)−0.006 (3)
C30.020 (3)0.026 (3)0.029 (3)−0.001 (2)0.001 (2)−0.008 (2)
C40.022 (3)0.019 (3)0.015 (3)−0.004 (2)−0.003 (2)0.000 (2)
C50.025 (3)0.025 (3)0.025 (3)−0.010 (2)−0.005 (2)−0.004 (2)
C60.026 (3)0.023 (3)0.023 (3)−0.003 (2)−0.006 (2)−0.004 (2)
C70.024 (3)0.019 (3)0.017 (3)−0.002 (2)−0.003 (2)−0.001 (2)
C80.022 (3)0.022 (3)0.016 (3)−0.003 (2)0.001 (2)−0.003 (2)
C90.021 (3)0.025 (3)0.017 (3)−0.005 (2)−0.002 (2)−0.005 (2)
C100.029 (3)0.031 (3)0.021 (3)−0.011 (3)−0.003 (2)0.003 (2)
C110.026 (3)0.029 (3)0.016 (3)−0.007 (2)−0.002 (2)−0.008 (2)
C120.019 (3)0.031 (3)0.022 (3)−0.008 (2)−0.006 (2)0.000 (2)
C130.024 (3)0.021 (3)0.021 (3)−0.001 (2)0.002 (2)−0.003 (2)
C140.020 (3)0.019 (3)0.020 (3)−0.001 (2)0.001 (2)−0.001 (2)
C150.019 (3)0.027 (3)0.016 (3)−0.001 (2)−0.004 (2)0.000 (2)
C160.016 (3)0.028 (3)0.024 (3)−0.002 (2)−0.005 (2)−0.008 (2)
C170.056 (5)0.036 (4)0.021 (3)−0.019 (3)0.005 (3)−0.006 (3)
C180.052 (5)0.040 (4)0.032 (4)−0.005 (3)0.004 (3)−0.010 (3)
C190.049 (5)0.086 (7)0.076 (7)−0.024 (5)−0.003 (5)−0.036 (6)
C200.063 (5)0.052 (4)0.039 (4)−0.027 (4)0.002 (4)−0.023 (4)
C210.053 (5)0.048 (4)0.036 (4)−0.017 (4)0.008 (3)−0.015 (3)
C220.046 (4)0.038 (4)0.023 (3)−0.015 (3)0.006 (3)−0.007 (3)
C230.033 (4)0.047 (4)0.030 (4)−0.001 (3)−0.003 (3)−0.004 (3)
C240.059 (6)0.090 (7)0.040 (5)−0.023 (5)−0.009 (4)−0.024 (5)
C250.073 (6)0.086 (7)0.030 (4)−0.050 (5)0.005 (4)−0.021 (4)
C260.089 (7)0.036 (4)0.050 (5)0.004 (4)0.005 (5)−0.008 (4)
N10.045 (4)0.036 (3)0.032 (3)−0.019 (3)0.003 (3)−0.014 (3)
N20.067 (4)0.040 (3)0.031 (3)−0.016 (3)0.000 (3)−0.010 (3)
Geometric parameters (Å, °) top
Pb1—O22.381 (4)C10—C12v1.365 (8)
Pb1—O52.410 (4)C10—H10A0.9400
Pb1—O62.461 (4)C12—C10v1.365 (8)
Pb1—O3i2.486 (4)C12—H12A0.9400
Pb1—O92.633 (5)C13—C141.496 (8)
Pb1—C112.779 (6)C14—C161.388 (8)
Pb2—O72.434 (4)C14—C151.400 (8)
Pb2—O82.456 (4)C15—C16vi1.374 (8)
Pb2—O4ii2.494 (4)C15—H15A0.9400
Pb2—O12.552 (4)C16—C15vi1.374 (8)
Pb2—O102.657 (5)C16—H16A0.9400
Pb2—O3ii2.660 (4)C17—N11.341 (8)
Pb2—C132.791 (6)C17—C181.500 (10)
O1—C71.260 (7)C18—C191.485 (11)
O2—C71.256 (7)C18—H18A0.9800
O3—C81.271 (7)C18—H18B0.9800
O3—Pb1iii2.486 (4)C19—C201.503 (12)
O3—Pb2iv2.660 (4)C19—H19A0.9800
O4—C81.243 (7)C19—H19B0.9800
O4—Pb2iv2.494 (4)C20—N11.445 (9)
O5—C111.257 (7)C20—H20A0.9800
O6—C111.255 (7)C20—H20B0.9800
O7—C131.256 (7)C21—N11.437 (10)
O8—C131.259 (7)C21—H21A0.9700
O9—C171.224 (8)C21—H21B0.9700
O10—C221.236 (8)C21—H21C0.9700
C1—C21.381 (8)C22—N21.306 (9)
C1—C61.388 (8)C22—C231.499 (9)
C1—C71.496 (7)C23—C241.482 (10)
C2—C31.384 (8)C23—H23A0.9800
C2—H2A0.9400C23—H23B0.9800
C3—C41.386 (8)C24—C251.533 (13)
C3—H3A0.9400C24—H24A0.9800
C4—C51.377 (8)C24—H24B0.9800
C4—C81.488 (7)C25—N21.427 (10)
C5—C61.369 (8)C25—H25A0.9800
C5—H5A0.9400C25—H25B0.9800
C6—H6A0.9400C26—N21.448 (10)
C9—C101.388 (8)C26—H26A0.9700
C9—C121.388 (8)C26—H26B0.9700
C9—C111.495 (8)C26—H26C0.9700
O2—Pb1—O572.48 (14)O6—C11—Pb162.3 (3)
O2—Pb1—O677.41 (15)O5—C11—Pb160.0 (3)
O5—Pb1—O653.70 (13)C9—C11—Pb1177.6 (4)
O2—Pb1—O3i79.52 (13)C10v—C12—C9121.0 (5)
O5—Pb1—O3i72.31 (13)C10v—C12—H12A119.5
O6—Pb1—O3i125.39 (13)C9—C12—H12A119.5
O2—Pb1—O9152.10 (16)O7—C13—O8122.0 (5)
O5—Pb1—O979.82 (16)O7—C13—C14118.7 (5)
O6—Pb1—O983.63 (16)O8—C13—C14119.3 (5)
O3i—Pb1—O995.47 (15)O7—C13—Pb260.6 (3)
O2—Pb1—C1172.56 (15)O8—C13—Pb261.6 (3)
O5—Pb1—C1126.86 (15)C14—C13—Pb2174.3 (4)
O6—Pb1—C1126.85 (15)C16—C14—C15119.8 (5)
O3i—Pb1—C1198.80 (15)C16—C14—C13120.4 (5)
O9—Pb1—C1181.26 (17)C15—C14—C13119.8 (5)
O7—Pb2—O853.45 (13)C16vi—C15—C14119.9 (5)
O7—Pb2—O4ii72.48 (14)C16vi—C15—H15A120.1
O8—Pb2—O4ii79.12 (15)C14—C15—H15A120.1
O7—Pb2—O172.97 (13)C15vi—C16—C14120.3 (5)
O8—Pb2—O1125.62 (13)C15vi—C16—H16A119.8
O4ii—Pb2—O194.54 (13)C14—C16—H16A119.8
O7—Pb2—O1090.42 (15)O9—C17—N1124.3 (7)
O8—Pb2—O1080.92 (15)O9—C17—C18127.7 (7)
O4ii—Pb2—O10159.02 (16)N1—C17—C18108.0 (6)
O1—Pb2—O1091.84 (14)C19—C18—C17106.8 (6)
O7—Pb2—O3ii111.17 (13)C19—C18—H18A110.4
O8—Pb2—O3ii78.39 (13)C17—C18—H18A110.4
O4ii—Pb2—O3ii50.44 (12)C19—C18—H18B110.4
O1—Pb2—O3ii136.11 (13)C17—C18—H18B110.4
O10—Pb2—O3ii130.70 (13)H18A—C18—H18B108.6
O7—Pb2—C1326.71 (15)C18—C19—C20106.0 (7)
O8—Pb2—C1326.80 (15)C18—C19—H19A110.5
O4ii—Pb2—C1372.88 (16)C20—C19—H19A110.5
O1—Pb2—C1399.48 (15)C18—C19—H19B110.5
O10—Pb2—C1386.36 (16)C20—C19—H19B110.5
O3ii—Pb2—C1394.22 (14)H19A—C19—H19B108.7
C7—O1—Pb2132.2 (4)N1—C20—C19105.6 (6)
C7—O2—Pb1105.6 (3)N1—C20—H20A110.6
C8—O3—Pb1iii124.5 (4)C19—C20—H20A110.6
C8—O3—Pb2iv89.4 (3)N1—C20—H20B110.6
Pb1iii—O3—Pb2iv106.20 (13)C19—C20—H20B110.6
C8—O4—Pb2iv97.9 (3)H20A—C20—H20B108.7
C11—O5—Pb193.2 (3)N1—C21—H21A109.5
C11—O6—Pb190.9 (3)N1—C21—H21B109.5
C13—O7—Pb292.7 (3)H21A—C21—H21B109.5
C13—O8—Pb291.6 (3)N1—C21—H21C109.5
C17—O9—Pb1142.2 (5)H21A—C21—H21C109.5
C22—O10—Pb2118.8 (4)H21B—C21—H21C109.5
C2—C1—C6120.0 (5)O10—C22—N2126.1 (7)
C2—C1—C7119.5 (5)O10—C22—C23124.7 (6)
C6—C1—C7120.5 (5)N2—C22—C23109.2 (6)
C1—C2—C3120.1 (5)C24—C23—C22104.9 (7)
C1—C2—H2A119.9C24—C23—H23A110.8
C3—C2—H2A119.9C22—C23—H23A110.8
C2—C3—C4119.5 (5)C24—C23—H23B110.8
C2—C3—H3A120.3C22—C23—H23B110.8
C4—C3—H3A120.3H23A—C23—H23B108.8
C5—C4—C3120.0 (5)C23—C24—C25107.0 (7)
C5—C4—C8121.2 (5)C23—C24—H24A110.3
C3—C4—C8118.8 (5)C25—C24—H24A110.3
C6—C5—C4120.9 (5)C23—C24—H24B110.3
C6—C5—H5A119.6C25—C24—H24B110.3
C4—C5—H5A119.6H24A—C24—H24B108.6
C5—C6—C1119.5 (5)N2—C25—C24102.9 (6)
C5—C6—H6A120.3N2—C25—H25A111.2
C1—C6—H6A120.3C24—C25—H25A111.2
O2—C7—O1123.4 (5)N2—C25—H25B111.2
O2—C7—C1117.4 (5)C24—C25—H25B111.2
O1—C7—C1119.2 (5)H25A—C25—H25B109.1
O4—C8—O3122.3 (5)N2—C26—H26A109.5
O4—C8—C4120.4 (5)N2—C26—H26B109.5
O3—C8—C4117.4 (5)H26A—C26—H26B109.5
C10—C9—C12119.3 (5)N2—C26—H26C109.5
C10—C9—C11120.5 (5)H26A—C26—H26C109.5
C12—C9—C11120.1 (5)H26B—C26—H26C109.5
C12v—C10—C9119.6 (6)C17—N1—C21123.9 (6)
C12v—C10—H10A120.2C17—N1—C20113.6 (6)
C9—C10—H10A120.2C21—N1—C20122.5 (6)
O6—C11—O5122.3 (5)C22—N2—C25115.8 (7)
O6—C11—C9119.2 (5)C22—N2—C26122.9 (7)
O5—C11—C9118.6 (5)C25—N2—C26121.2 (7)
O7—Pb2—O1—C7−29.7 (5)C3—C4—C8—O3176.0 (5)
O8—Pb2—O1—C7−20.0 (5)C12—C9—C10—C12v−0.7 (10)
O4ii—Pb2—O1—C7−99.9 (5)C11—C9—C10—C12v177.8 (5)
O10—Pb2—O1—C760.1 (5)Pb1—O6—C11—O52.2 (6)
O3ii—Pb2—O1—C7−132.8 (4)Pb1—O6—C11—C9−177.9 (5)
C13—Pb2—O1—C7−26.5 (5)Pb1—O5—C11—O6−2.2 (6)
O5—Pb1—O2—C7132.5 (4)Pb1—O5—C11—C9177.9 (4)
O6—Pb1—O2—C776.9 (4)C10—C9—C11—O6−175.2 (6)
O3i—Pb1—O2—C7−153.0 (4)C12—C9—C11—O63.2 (8)
O9—Pb1—O2—C7125.2 (4)C10—C9—C11—O54.7 (8)
C11—Pb1—O2—C7104.3 (4)C12—C9—C11—O5−176.8 (5)
O2—Pb1—O5—C11−85.8 (3)O2—Pb1—C11—O6−96.6 (4)
O6—Pb1—O5—C111.2 (3)O5—Pb1—C11—O6177.9 (6)
O3i—Pb1—O5—C11−170.1 (4)O3i—Pb1—C11—O6−172.6 (3)
O9—Pb1—O5—C1190.7 (4)O9—Pb1—C11—O693.2 (4)
O2—Pb1—O6—C1176.2 (3)O2—Pb1—C11—O585.5 (3)
O5—Pb1—O6—C11−1.2 (3)O6—Pb1—C11—O5−177.9 (6)
O3i—Pb1—O6—C119.0 (4)O3i—Pb1—C11—O59.5 (3)
O9—Pb1—O6—C11−83.2 (4)O9—Pb1—C11—O5−84.7 (3)
O8—Pb2—O7—C132.7 (3)C10—C9—C12—C10v0.7 (10)
O4ii—Pb2—O7—C13−86.6 (3)C11—C9—C12—C10v−177.8 (6)
O1—Pb2—O7—C13172.8 (4)Pb2—O7—C13—O8−5.0 (6)
O10—Pb2—O7—C1381.0 (3)Pb2—O7—C13—C14173.6 (4)
O3ii—Pb2—O7—C13−53.6 (4)Pb2—O8—C13—O74.9 (6)
O7—Pb2—O8—C13−2.7 (3)Pb2—O8—C13—C14−173.6 (5)
O4ii—Pb2—O8—C1373.5 (3)O8—Pb2—C13—O7−175.2 (6)
O1—Pb2—O8—C13−14.3 (4)O4ii—Pb2—C13—O784.9 (3)
O10—Pb2—O8—C13−100.0 (4)O1—Pb2—C13—O7−6.9 (4)
O3ii—Pb2—O8—C13125.0 (4)O10—Pb2—C13—O7−98.2 (3)
O2—Pb1—O9—C1733.1 (10)O3ii—Pb2—C13—O7131.2 (3)
O5—Pb1—O9—C1726.1 (8)O7—Pb2—C13—O8175.2 (6)
O6—Pb1—O9—C1780.3 (8)O4ii—Pb2—C13—O8−99.9 (4)
O3i—Pb1—O9—C17−44.8 (8)O1—Pb2—C13—O8168.3 (3)
C11—Pb1—O9—C1753.3 (8)O10—Pb2—C13—O877.0 (3)
O7—Pb2—O10—C22−134.2 (5)O3ii—Pb2—C13—O8−53.6 (3)
O8—Pb2—O10—C22−81.4 (5)O7—C13—C14—C16169.3 (5)
O4ii—Pb2—O10—C22−99.5 (6)O8—C13—C14—C16−12.2 (8)
O1—Pb2—O10—C22152.8 (5)O7—C13—C14—C15−11.3 (8)
O3ii—Pb2—O10—C22−15.4 (6)O8—C13—C14—C15167.3 (5)
C13—Pb2—O10—C22−107.8 (5)C16—C14—C15—C16vi1.0 (9)
C6—C1—C2—C3−2.6 (9)C13—C14—C15—C16vi−178.5 (5)
C7—C1—C2—C3177.5 (5)C15—C14—C16—C15vi−1.0 (9)
C1—C2—C3—C42.0 (9)C13—C14—C16—C15vi178.5 (5)
C2—C3—C4—C50.6 (9)Pb1—O9—C17—N1150.4 (6)
C2—C3—C4—C8178.1 (5)Pb1—O9—C17—C18−31.4 (12)
C3—C4—C5—C6−2.6 (9)O9—C17—C18—C19−179.1 (8)
C8—C4—C5—C6179.9 (5)N1—C17—C18—C19−0.6 (8)
C4—C5—C6—C12.0 (9)C17—C18—C19—C200.0 (9)
C2—C1—C6—C50.6 (9)C18—C19—C20—N10.6 (9)
C7—C1—C6—C5−179.6 (5)Pb2—O10—C22—N2−159.4 (6)
Pb1—O2—C7—O17.5 (7)Pb2—O10—C22—C2322.1 (9)
Pb1—O2—C7—C1−171.6 (4)O10—C22—C23—C24178.9 (7)
Pb2—O1—C7—O283.5 (7)N2—C22—C23—C240.1 (8)
Pb2—O1—C7—C1−97.5 (6)C22—C23—C24—C253.0 (9)
C2—C1—C7—O226.5 (8)C23—C24—C25—N2−4.8 (9)
C6—C1—C7—O2−153.3 (6)O9—C17—N1—C210.0 (11)
C2—C1—C7—O1−152.6 (6)C18—C17—N1—C21−178.5 (6)
C6—C1—C7—O127.6 (8)O9—C17—N1—C20179.6 (7)
Pb2iv—O4—C8—O32.6 (6)C18—C17—N1—C201.1 (8)
Pb2iv—O4—C8—C4−176.6 (4)C19—C20—N1—C17−1.1 (9)
Pb1iii—O3—C8—O4106.9 (6)C19—C20—N1—C21178.5 (7)
Pb2iv—O3—C8—O4−2.4 (6)O10—C22—N2—C25177.7 (7)
Pb1iii—O3—C8—C4−73.9 (6)C23—C22—N2—C25−3.6 (9)
Pb2iv—O3—C8—C4176.8 (4)O10—C22—N2—C261.5 (12)
C5—C4—C8—O4172.7 (6)C23—C22—N2—C26−179.8 (7)
C3—C4—C8—O4−4.8 (8)C24—C25—N2—C225.3 (9)
C5—C4—C8—O3−6.5 (8)C24—C25—N2—C26−178.4 (7)
Symmetry codes: (i) x, y+1, z; (ii) x−1, y+1, z; (iii) x, y−1, z; (iv) x+1, y−1, z; (v) −x+2, −y+1, −z+1; (vi) −x+1, −y+2, −z.
Table 1
Selected geometric parameters (Å, °) top
Pb1—O22.381 (4)Pb2—O4ii2.494 (4)
Pb1—O52.410 (4)Pb2—O12.552 (4)
Pb1—O62.461 (4)Pb2—O102.657 (5)
Pb1—O3i2.486 (4)Pb2—O3ii2.660 (4)
Pb1—O92.633 (5)O3—Pb1iii2.486 (4)
Pb2—O72.434 (4)O3—Pb2iv2.660 (4)
Pb2—O82.456 (4)O4—Pb2iv2.494 (4)
O2—Pb1—O572.48 (14)O7—Pb2—O172.97 (13)
O2—Pb1—O677.41 (15)O8—Pb2—O1125.62 (13)
O5—Pb1—O653.70 (13)O4ii—Pb2—O194.54 (13)
O2—Pb1—O3i79.52 (13)O7—Pb2—O1090.42 (15)
O5—Pb1—O3i72.31 (13)O8—Pb2—O1080.92 (15)
O6—Pb1—O3i125.39 (13)O4ii—Pb2—O10159.02 (16)
O2—Pb1—O9152.10 (16)O1—Pb2—O1091.84 (14)
O5—Pb1—O979.82 (16)O7—Pb2—O3ii111.17 (13)
O6—Pb1—O983.63 (16)O8—Pb2—O3ii78.39 (13)
O3i—Pb1—O995.47 (15)O4ii—Pb2—O3ii50.44 (12)
O7—Pb2—O853.45 (13)O1—Pb2—O3ii136.11 (13)
O7—Pb2—O4ii72.48 (14)O10—Pb2—O3ii130.70 (13)
O8—Pb2—O4ii79.12 (15)
Symmetry codes: (i) x, y+1, z; (ii) x−1, y+1, z; (iii) x, y−1, z; (iv) x+1, y−1, z.
Acknowledgements top

The authors thank the National Natural Science Foundation of China (grant No. 20471049) and Xiamen University for supporting this work.

references
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