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The asymmetric unit of the title compound, [Pb2(C8H3IO4)2(CH4O)]n, contains two PbII atoms, two 5-iodo­isophthalate (5-IIP2−) ligands and one coordinated methanol mol­ecule. One Pb atom is eight-coordinated, surrounded by seven carboxyl­ate O atoms from five 5-IIP2− ligands and one O atom from the terminal methanol ligand. The other Pb atom is seven-coordinated in a hemidirected geometry, surrounded by seven carboxyl­ate O atoms from five 5-IIP2− ligands. Both Pb atoms are connected by carboxyl­ate groups to form a one-di­men­sional infinite rod along the a axis; neighbouring rods are further linked by the aromatic rings of 5-IIP2− to generate the final three-dimensional structure with channels in the a direction. An O—H...O hydrogen bond between the methanol ligand and one of the carboxyl­ate groups of a 5-IIP2− ligand stablizes the three-dimensional framework. Inter­estingly, a centrosymmetric rhombus-shaped I4 unit is formed by four 5-IIP2− ligands, with I...I distances of 3.8841 (8) and 3.9204 (8) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113010007/em3057sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113010007/em3057Isup2.hkl
Contains datablock I

CCDC reference: 950354

Comment top

Recently, the design and synthesis of metal–organic frameworks (MOFs) with unusual structures and properties have attracted considerable attention, not only for their fascinating molecular topologies, but also for their various applications such as catalysis, electrical conductivity, host–guest chemistry and magnetism (Abrahams et al., 1999; Eddaoudi et al., 2001; Farha et al., 2010; O'Keeffe et al., 2008). Until now, research into MOFs has mainly focused on incorporation of s-, d- and f-block metal ions as coordination centres, while less consideration has been given to the metals of the p block (Li et al., 2005; Eddaoudi et al., 2002; Xu et al., 2005). As a heavy p-block metal ion, PbII has a large ionic radius, variable coordination numbers from 2 to 10 and diverse coordination geometries, which provide unique opportunities for the formation of unusual network topologies with interesting properties (Li & Lu, 2000; Yang et al., 2007; Li et al., 2010). On the other hand, the selection of organic ligands also plays a significant role in constructing novel MOF nets and generating interesting properties. In this regard, organic carboxylate ligands have been extensively used to construct MOFs with various properties and topologies (Li et al., 2005; Eddaoudi et al., 2002). 5-Iodoisophthalic acid (5-H2IIP), as one type of bridging aromatic dicarboxylate ligand, has been less studied (Zang et al., 2011). The I atom in 5-H2IIP is a potential interaction site for forming C—I···N/O or C—I···I halogen bonds, which may help to construct MOFs with interesting nets and properties. We report here the synthesis and structure of poly[bis(µ-5-iodoisophthalato)(methanol)dilead(II)], (I), using Pb2+ and 5-H2IIP as the starting materials.

Selected bond lengths for (I) are given in Table 1. As shown in Fig. 1, the asymmetric unit of (I) contains two PbII atoms, two 5-IIP2- ions and one coordinated methanol molecule. Atom Pb1 is eight-coordinated, surrounded by seven carboxylate O atoms from five 5-IIP2- ligands and one O atom from the terminal methanol ligand. The coordination sphere of Pb1 is best described as a distorted tricapped trigonal prism with the ninth site occupied by its lone pair of electrons. The seven-coordinated Pb2 atom is surrounded by seven carboxylate O atoms from five 5-IIP2- ligands. The coordinated O atoms are located on one side of the Pb2 atom, which adopts a hemidirected structure categories, suggesting the presence of a stereochemically active lone electron pair around Pb2. The Pb—O distances range from 2.340 (6) to 3.110 (6) Å, comparable to those for the reported PbII polymers with aromatic carboxylic acids (Yang et al., 2007; Qiao et al., 2009). The two crystallographically independent 5-IIP2- ligands show the same coordination modes. Each 5-IIP2- ligand coordinates to five PbII atoms with a µ5-κ3;κ4 coordination mode. One carboxylate group links two PbII atoms in a chelating–bridging tridentate mode, while another connects three PbII atoms in an unusual chelating–bridging tetradentate mode.

The most striking feature of (I) is that the Pb1 and Pb2 atoms are connected by carboxylate groups of 5-IIP2- to form a one-dimensional infinite rod along the a axis (Fig. 2). From Fig. 2 it can be seen that the Pb—O—C rod is constructed from [OPb2(COO)4] units, which contain two PbII atoms, one O atom from a terminal methanol ligand, and four carboxylate groups of 5-IIP2- linkers. This connectivity pattern is repeated infinitely to create a Pb—O—C rod-shaped secondary building unit (SBU) along the a axis. The rods are then linked by the aromatic rings of 5-IIP2-, which connect each rod to four neighbouring rods in the c and b directions, forming the final three-dimensional structure containing one-dimensional channels in the a direction. Fig. 4, viewed from the c direction, shows that the aromatic rings of 5-IIP2- link the rods to form a herringbone pattern. To the best of our knowledge, MOFs constructed by Pb—O—C rod-shaped SBUs like (I) are rare (Rosi et al. 2005; Lin et al. 2010).

Weak interactions in (I) stablize the three-dimensional framework. Fig. 5 shows the O9—H9···O6 hydrogen bond (Table 2) between the methanol molecule and a carboxylate group of a 5-IIP2- ligand. It is noteworthy that there is an interesting tetranuclear I4 unit, with I···I distances of 3.9204 (8) [I1··· I2v; symmetry code: (v) x+1, y, z] and 3.8841 (8) Å [I1 ··· I2vii; symmetry code: (vii) -x+1, -y+1, -z+2]. These distances are all shorter than the sum of van der Waals radii (3.96 Å; Bondi, 1964), indicating the existence of I···I interactions between the I atoms. To the best of our knowledge, this tetranuclear I4 unit has never been reported before in iodine-containing MOFs; this result will help us to construct novel iodine-containing MOFs with I···I interactions (Zang et al., 2011).

Related literature top

For related literature, see: Abrahams et al. (1999); Eddaoudi et al. (2001, 2002); Farha & Hupp (2010); Li & Lu (2000); Li et al. (2005, 2010); Lin et al. (2010); O'Keeffe et al. (2008); Qiao et al. (2009); Rosi et al. (2005); Xu et al. (2005); Yang et al. (2007); Zang et al. (2011).

Experimental top

A mixture of Pb(NO3)2 (0.1 mmol), 5-iodoisophthalic acid (0.1 mmol) and NaOH (0.2 mmol) was dissolved in H2O–MeOH (10 ml, 1:1 v/v). The resulting solution was stirred for about 0.5 h at room temperature, sealed in a 25 ml Teflon-lined stainless steel autoclave and heated at 423 K for 3 d under autogenous pressure. Afterwards, the reaction system was cooled slowly to room temperature. Colourless block-shaped crystals of (I) suitable for single-crystal X-ray diffraction analysis were collected from the final reaction system by filtration, washed several times with distilled water and dried in air at ambient temperature (yield 68%, based on PbII).

Refinement top

All C-bound H atoms were placed geometrically and treated as riding on their parent atoms, with C—H = 0.93 (arene) or 0.96 Å (methyl) and Uiso(H) = 1.2Ueq(C). The methanol hydroxy H atom was located in a difference Fourier map and included in the subsequent refinement using the constraints O—H = 0.85 Å and Uiso(H) = 1.5Ueq(O).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The atom-numbering scheme and the local coordination of the PbII atoms in (I). H atoms have been omitted for clarity. [Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+2, -y+1, -z+1; (iii) x-1, -y+1/2, z-1/2; (iv) x, -y+1/2, z-1/2; (v) x+1, y, z.]
[Figure 2] Fig. 2. The rod-shaped SBU of (I) along the a axis, constructed from PbII atoms and carboxylate groups.
[Figure 3] Fig. 3. A view of the three-dimensional structure of (I), viewed paralled to a. The one-dimensional Pb—O—C rods based on PbII atoms and carboxylate groups are connected by bridging aromatic rings of 5-IIP2- to generate the three-dimensional structure. H atoms have been omitted for clarity.
[Figure 4] Fig. 4. A view of the three-dimensional structure of (I), viewed parallel to the c axis, showing the herringbone pattern.
[Figure 5] Fig. 5. A view of the tetranuclear I4 unit in (I),constructed from I atoms of 5-IIP2- by II interactions. O9—H9···O6 hydrogen bonds are shown. Nonhydroxy H atoms have been omitted for clarity. [Symmetry codes: (i) -x+1, -y+1, -z+1; (v) x+1, y, z; (vi) -x+2, -y+1, -z+2; (vii) -x+1, -y+1, -z+2; (viii) -x+2, y+1/2, -z+3/2.]
Poly[bis(µ-5-iodoisophthalato)(methanol)dilead(II)] top
Crystal data top
[Pb2(C8H3IO4)2(CH4O)]F(000) = 1816
Mr = 1026.43Dx = 3.216 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7918 reflections
a = 4.3137 (4) Åθ = 2.3–27.5°
b = 27.918 (2) ŵ = 18.82 mm1
c = 17.6437 (15) ÅT = 296 K
β = 93.897 (1)°Block, colourless
V = 2119.9 (3) Å30.35 × 0.23 × 0.21 mm
Z = 4
Data collection top
Bruker–Nonius KappaCCD
diffractometer
4855 independent reflections
Radiation source: fine-focus sealed tube4302 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scanθmax = 27.5°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 1997)
h = 55
Tmin = 0.058, Tmax = 0.110k = 3636
18249 measured reflectionsl = 2122
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)] = 0.032H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.070 w = 1/[σ2(Fo2) + (0.0209P)2 + 11.242P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
4855 reflectionsΔρmax = 2.23 e Å3
276 parametersΔρmin = 1.65 e Å3
8 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00024 (4)
Crystal data top
[Pb2(C8H3IO4)2(CH4O)]V = 2119.9 (3) Å3
Mr = 1026.43Z = 4
Monoclinic, P21/cMo Kα radiation
a = 4.3137 (4) ŵ = 18.82 mm1
b = 27.918 (2) ÅT = 296 K
c = 17.6437 (15) Å0.35 × 0.23 × 0.21 mm
β = 93.897 (1)°
Data collection top
Bruker–Nonius KappaCCD
diffractometer
4855 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 1997)
4302 reflections with I > 2σ(I)
Tmin = 0.058, Tmax = 0.110Rint = 0.040
18249 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0328 restraints
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0209P)2 + 11.242P]
where P = (Fo2 + 2Fc2)/3
4855 reflectionsΔρmax = 2.23 e Å3
276 parametersΔρmin = 1.65 e Å3
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 > 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
Pb10.42997 (6)0.359536 (9)0.468120 (15)0.02579 (8)
Pb21.06483 (6)0.340255 (9)0.698110 (15)0.02848 (8)
I11.11882 (13)0.474418 (18)0.88313 (3)0.03791 (13)
I20.25214 (13)0.402666 (19)1.07356 (3)0.04389 (14)
O11.0482 (11)0.59910 (18)0.5617 (3)0.0345 (12)
O21.4538 (11)0.59467 (18)0.6435 (3)0.0347 (12)
O30.4803 (13)0.43503 (18)0.5367 (3)0.0391 (13)
O40.6139 (12)0.38246 (17)0.6271 (3)0.0336 (11)
O50.6761 (13)0.34714 (18)0.7933 (3)0.0364 (12)
O61.0108 (14)0.2875 (2)0.8149 (3)0.0421 (13)
O70.9856 (14)0.19388 (19)1.0519 (3)0.0429 (14)
O80.7680 (18)0.2246 (2)1.1505 (3)0.0581 (19)
C11.1927 (15)0.5803 (2)0.6190 (4)0.0251 (14)
C21.0581 (15)0.5371 (2)0.6565 (4)0.0251 (14)
C31.1319 (16)0.5290 (2)0.7334 (4)0.0288 (15)
H31.26040.55000.76160.035*
C41.0113 (16)0.4891 (2)0.7671 (4)0.0249 (14)
C50.8355 (15)0.4564 (2)0.7250 (4)0.0235 (13)
H50.75850.42940.74830.028*
C60.7722 (15)0.4635 (2)0.6472 (4)0.0243 (14)
C70.8748 (15)0.5052 (2)0.6133 (4)0.0241 (13)
H70.82080.51150.56230.029*
C80.6111 (15)0.4248 (2)0.6003 (4)0.0254 (14)
C90.7997 (18)0.3147 (2)0.8365 (4)0.0306 (15)
C100.7015 (16)0.3101 (2)0.9156 (4)0.0260 (14)
C110.5359 (17)0.3470 (2)0.9481 (4)0.0299 (15)
H110.47060.37340.91900.036*
C120.4692 (18)0.3442 (2)1.0239 (4)0.0300 (15)
C130.5569 (18)0.3048 (2)1.0674 (4)0.0312 (16)
H130.50810.30301.11780.037*
C140.7198 (18)0.2678 (2)1.0347 (4)0.0296 (15)
C150.7920 (17)0.2714 (2)0.9596 (4)0.0268 (14)
H150.90450.24690.93850.032*
C160.8333 (19)0.2262 (2)1.0812 (4)0.0345 (16)
O90.223 (3)0.3057 (3)0.3413 (5)0.101 (3)
H90.18 (3)0.2765 (16)0.348 (8)0.121*
C170.128 (6)0.3237 (6)0.2691 (10)0.163 (9)
H17A0.09380.32090.26100.244*
H17B0.22560.30580.23100.244*
H17C0.18630.35680.26610.244*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.02857 (14)0.02363 (14)0.02498 (15)0.00394 (10)0.00031 (10)0.00612 (10)
Pb20.03729 (15)0.02935 (15)0.01864 (14)0.00444 (10)0.00073 (10)0.00021 (10)
I10.0543 (3)0.0378 (3)0.0208 (3)0.0037 (2)0.0030 (2)0.00380 (19)
I20.0554 (3)0.0370 (3)0.0395 (3)0.0128 (2)0.0052 (2)0.0053 (2)
O10.026 (2)0.039 (3)0.037 (3)0.003 (2)0.000 (2)0.019 (2)
O20.029 (3)0.039 (3)0.035 (3)0.009 (2)0.002 (2)0.012 (2)
O30.059 (3)0.031 (3)0.025 (3)0.000 (2)0.014 (2)0.002 (2)
O40.053 (3)0.020 (2)0.026 (3)0.007 (2)0.006 (2)0.0034 (19)
O50.056 (3)0.030 (3)0.023 (3)0.002 (2)0.001 (2)0.013 (2)
O60.067 (4)0.039 (3)0.021 (3)0.012 (3)0.012 (3)0.005 (2)
O70.063 (4)0.035 (3)0.032 (3)0.015 (3)0.014 (3)0.010 (2)
O80.125 (6)0.039 (3)0.011 (3)0.031 (3)0.005 (3)0.003 (2)
C10.028 (3)0.019 (3)0.029 (4)0.000 (3)0.007 (3)0.002 (3)
C20.029 (3)0.019 (3)0.027 (4)0.003 (3)0.005 (3)0.007 (3)
C30.037 (4)0.025 (3)0.025 (4)0.002 (3)0.002 (3)0.001 (3)
C40.038 (4)0.022 (3)0.016 (3)0.004 (3)0.003 (3)0.005 (2)
C50.032 (3)0.020 (3)0.019 (3)0.001 (3)0.004 (3)0.006 (2)
C60.028 (3)0.017 (3)0.028 (4)0.002 (2)0.004 (3)0.001 (3)
C70.030 (3)0.023 (3)0.019 (3)0.005 (3)0.003 (3)0.004 (3)
C80.027 (3)0.022 (3)0.027 (4)0.001 (3)0.002 (3)0.001 (3)
C90.047 (4)0.022 (3)0.022 (4)0.008 (3)0.007 (3)0.002 (3)
C100.042 (4)0.019 (3)0.016 (3)0.003 (3)0.003 (3)0.001 (2)
C110.042 (4)0.022 (3)0.025 (4)0.001 (3)0.003 (3)0.004 (3)
C120.043 (4)0.023 (3)0.023 (4)0.004 (3)0.003 (3)0.000 (3)
C130.053 (5)0.027 (4)0.014 (3)0.002 (3)0.005 (3)0.002 (3)
C140.049 (4)0.022 (3)0.016 (3)0.002 (3)0.001 (3)0.001 (3)
C150.044 (4)0.021 (3)0.016 (3)0.004 (3)0.003 (3)0.001 (2)
C160.058 (5)0.020 (3)0.025 (4)0.000 (3)0.002 (3)0.003 (3)
O90.198 (10)0.052 (5)0.055 (5)0.054 (6)0.015 (6)0.005 (4)
C170.31 (3)0.081 (11)0.097 (11)0.031 (15)0.017 (15)0.005 (9)
Geometric parameters (Å, º) top
Pb1—O1i2.391 (5)C1—Pb1ii2.860 (6)
Pb1—O2ii2.428 (5)C2—C71.384 (10)
Pb1—O32.433 (5)C2—C31.391 (10)
Pb1—O1ii2.615 (5)C3—C41.381 (9)
Pb1—O92.790 (8)C3—H30.9300
Pb1—O7iii2.910 (5)C4—C51.374 (9)
Pb1—O42.933 (5)C5—C61.394 (9)
Pb1—O7iv3.110 (6)C5—H50.9300
Pb2—O8iv2.340 (6)C6—C71.395 (9)
Pb2—O52.461 (5)C6—C81.504 (9)
Pb2—O42.532 (5)C7—H70.9300
Pb2—O62.556 (5)C9—C101.490 (9)
Pb2—O7iv2.750 (5)C10—C151.373 (9)
Pb2—O4v2.995 (5)C10—C111.398 (10)
Pb2—O5v3.035 (6)C11—C121.389 (10)
I1—C42.107 (6)C11—H110.9300
I2—C122.102 (7)C12—C131.378 (10)
O1—C11.266 (8)C13—C141.397 (9)
O2—C11.245 (8)C13—H130.9300
O2—Pb1ii2.428 (5)C14—C151.385 (9)
O3—C81.255 (8)C14—C161.486 (10)
O4—C81.272 (8)C15—H150.9300
O5—C91.278 (8)O9—C171.405 (18)
O6—C91.263 (9)O9—H90.84 (2)
O7—C161.249 (9)C17—H17A0.9600
O8—C161.275 (9)C17—H17B0.9600
C1—C21.510 (9)C17—H17C0.9600
O1i—Pb1—O2ii77.88 (16)O2—C1—O1121.8 (6)
O1i—Pb1—O374.78 (18)O2—C1—C2118.2 (6)
O2ii—Pb1—O386.03 (18)O1—C1—C2119.9 (6)
O1i—Pb1—O1ii118.95 (19)O2—C1—Pb1ii57.4 (3)
O2ii—Pb1—O1ii51.42 (16)O1—C1—Pb1ii66.0 (3)
O3—Pb1—O1ii70.64 (19)C2—C1—Pb1ii162.7 (4)
O1i—Pb1—O981.9 (3)C7—C2—C3121.1 (6)
O2ii—Pb1—O972.9 (2)C7—C2—C1119.6 (6)
O3—Pb1—O9151.4 (2)C3—C2—C1119.2 (6)
O1ii—Pb1—O9108.0 (2)C4—C3—C2119.0 (7)
O1i—Pb1—O7iii76.76 (17)C4—C3—H3120.5
O2ii—Pb1—O7iii149.43 (17)C2—C3—H3120.5
O3—Pb1—O7iii103.36 (17)C5—C4—C3120.8 (6)
O1ii—Pb1—O7iii159.11 (17)C5—C4—I1118.3 (5)
O9—Pb1—O7iii86.9 (2)C3—C4—I1120.7 (5)
O1i—Pb1—O4106.16 (17)C4—C5—C6120.1 (6)
O2ii—Pb1—O4127.09 (15)C4—C5—H5119.9
O3—Pb1—O447.63 (15)C6—C5—H5119.9
O1ii—Pb1—O485.15 (16)C5—C6—C7119.7 (6)
O9—Pb1—O4159.23 (19)C5—C6—C8119.4 (6)
O7iii—Pb1—O476.76 (15)C7—C6—C8120.8 (6)
O1i—Pb1—O7iv164.08 (16)C2—C7—C6119.0 (6)
O2ii—Pb1—O7iv116.27 (15)C2—C7—H7120.5
O3—Pb1—O7iv98.01 (16)C6—C7—H7120.5
O1ii—Pb1—O7iv70.19 (14)O3—C8—O4122.5 (6)
O9—Pb1—O7iv108.5 (3)O3—C8—C6119.4 (6)
O7iii—Pb1—O7iv91.49 (16)O4—C8—C6118.1 (6)
O4—Pb1—O7iv60.04 (14)O6—C9—O5121.7 (7)
O8iv—Pb2—O585.6 (2)O6—C9—C10119.2 (6)
O8iv—Pb2—O478.4 (2)O5—C9—C10119.0 (7)
O5—Pb2—O476.43 (17)C15—C10—C11118.8 (6)
O8iv—Pb2—O676.47 (19)C15—C10—C9120.5 (6)
O5—Pb2—O652.46 (16)C11—C10—C9120.5 (6)
O4—Pb2—O6123.91 (18)C12—C11—C10119.9 (6)
O8iv—Pb2—O7iv50.60 (17)C12—C11—H11120.0
O5—Pb2—O7iv128.37 (18)C10—C11—H11120.0
O4—Pb2—O7iv69.80 (17)C13—C12—C11120.9 (6)
O6—Pb2—O7iv123.00 (17)C13—C12—I2120.0 (5)
O8iv—Pb2—O4v125.67 (18)C11—C12—I2119.0 (5)
O5—Pb2—O4v148.20 (16)C12—C13—C14119.2 (6)
O4—Pb2—O4v102.28 (15)C12—C13—H13120.4
O6—Pb2—O4v132.98 (17)C14—C13—H13120.4
O7iv—Pb2—O4v78.18 (15)C15—C14—C13119.6 (6)
O8iv—Pb2—O5v132.9 (2)C15—C14—C16119.8 (6)
O5—Pb2—O5v102.93 (17)C13—C14—C16120.5 (6)
O4—Pb2—O5v148.63 (14)C10—C15—C14121.6 (6)
O6—Pb2—O5v73.35 (17)C10—C15—H15119.2
O7iv—Pb2—O5v126.11 (16)C14—C15—H15119.2
O4v—Pb2—O5v61.62 (13)O7—C16—O8122.0 (7)
C1—O1—Pb1i138.3 (4)O7—C16—C14119.9 (7)
C1—O1—Pb1ii87.7 (4)O8—C16—C14118.1 (7)
Pb1i—O1—Pb1ii118.95 (19)C17—O9—Pb1126.3 (8)
C1—O2—Pb1ii97.0 (4)C17—O9—H9116 (10)
C8—O3—Pb1105.5 (4)Pb1—O9—H9117 (10)
C8—O4—Pb2127.1 (4)O9—C17—H17A109.5
C8—O4—Pb181.5 (4)O9—C17—H17B109.5
Pb2—O4—Pb1121.37 (19)H17A—C17—H17B109.5
C9—O5—Pb294.3 (4)O9—C17—H17C109.5
C9—O6—Pb290.3 (4)H17A—C17—H17C109.5
C16—O7—Pb2vi84.1 (4)H17B—C17—H17C109.5
C16—O8—Pb2vi102.7 (5)
O1i—Pb1—O3—C8139.4 (5)C7—C2—C3—C42.0 (10)
O2ii—Pb1—O3—C8142.1 (5)C1—C2—C3—C4179.2 (6)
O1ii—Pb1—O3—C891.8 (5)C2—C3—C4—C53.7 (10)
O9—Pb1—O3—C8175.9 (6)C2—C3—C4—I1179.3 (5)
O7iii—Pb1—O3—C867.3 (5)C3—C4—C5—C61.0 (10)
O4—Pb1—O3—C89.7 (4)I1—C4—C5—C6176.8 (5)
O7iv—Pb1—O3—C826.1 (5)C4—C5—C6—C73.3 (9)
O8iv—Pb2—O4—C8156.3 (6)C4—C5—C6—C8173.0 (6)
O5—Pb2—O4—C8115.4 (6)C3—C2—C7—C62.2 (10)
O6—Pb2—O4—C8138.9 (5)C1—C2—C7—C6174.9 (6)
O7iv—Pb2—O4—C8104.3 (6)C5—C6—C7—C24.8 (9)
O4v—Pb2—O4—C831.9 (6)C8—C6—C7—C2171.4 (6)
O5v—Pb2—O4—C822.8 (7)Pb1—O3—C8—O419.9 (8)
O8iv—Pb2—O4—Pb152.2 (2)Pb1—O3—C8—C6159.9 (5)
O5—Pb2—O4—Pb1140.4 (2)Pb2—O4—C8—O3139.1 (6)
O6—Pb2—O4—Pb1117.0 (2)Pb1—O4—C8—O315.9 (6)
O7iv—Pb2—O4—Pb10.10 (18)Pb2—O4—C8—C640.7 (8)
O4v—Pb2—O4—Pb172.2 (2)Pb1—O4—C8—C6163.9 (6)
O5v—Pb2—O4—Pb1127.0 (2)C5—C6—C8—O3161.0 (6)
O1i—Pb1—O4—C860.0 (4)C7—C6—C8—O322.7 (9)
O2ii—Pb1—O4—C826.9 (5)C5—C6—C8—O419.2 (9)
O3—Pb1—O4—C89.3 (4)C7—C6—C8—O4157.1 (6)
O1ii—Pb1—O4—C858.8 (4)Pb2—O6—C9—O510.9 (7)
O9—Pb1—O4—C8170.6 (8)Pb2—O6—C9—C10166.4 (6)
O7iii—Pb1—O4—C8131.7 (4)Pb2—O5—C9—O611.3 (7)
O7iv—Pb1—O4—C8128.7 (4)Pb2—O5—C9—C10165.9 (5)
O1i—Pb1—O4—Pb2171.44 (19)O6—C9—C10—C1512.8 (10)
O2ii—Pb1—O4—Pb2101.7 (2)O5—C9—C10—C15169.9 (7)
O3—Pb1—O4—Pb2137.9 (3)O6—C9—C10—C11162.3 (7)
O1ii—Pb1—O4—Pb269.8 (2)O5—C9—C10—C1115.0 (10)
O9—Pb1—O4—Pb260.8 (8)C15—C10—C11—C120.7 (11)
O7iii—Pb1—O4—Pb299.7 (2)C9—C10—C11—C12174.4 (7)
O7iv—Pb1—O4—Pb20.10 (17)C10—C11—C12—C131.7 (11)
O8iv—Pb2—O5—C982.3 (4)C10—C11—C12—I2175.1 (5)
O4—Pb2—O5—C9161.4 (4)C11—C12—C13—C141.2 (12)
O6—Pb2—O5—C96.0 (4)I2—C12—C13—C14175.6 (6)
O7iv—Pb2—O5—C9111.5 (4)C12—C13—C14—C150.4 (11)
O4v—Pb2—O5—C9107.1 (4)C12—C13—C14—C16176.5 (7)
O5v—Pb2—O5—C950.8 (5)C11—C10—C15—C140.8 (11)
O8iv—Pb2—O6—C9101.0 (5)C9—C10—C15—C14176.0 (7)
O5—Pb2—O6—C96.0 (4)C13—C14—C15—C101.4 (11)
O4—Pb2—O6—C935.2 (5)C16—C14—C15—C10177.5 (7)
O7iv—Pb2—O6—C9121.8 (4)Pb2vi—O7—C16—O87.6 (8)
O4v—Pb2—O6—C9132.5 (4)Pb2vi—O7—C16—C14173.1 (7)
O5v—Pb2—O6—C9115.6 (4)Pb2vi—O8—C16—O79.1 (10)
Pb1ii—O2—C1—O115.5 (7)Pb2vi—O8—C16—C14171.5 (6)
Pb1ii—O2—C1—C2160.5 (5)C15—C14—C16—O72.1 (12)
Pb1i—O1—C1—O2118.9 (7)C13—C14—C16—O7178.2 (7)
Pb1ii—O1—C1—O214.3 (7)C15—C14—C16—O8178.5 (7)
Pb1i—O1—C1—C265.1 (9)C13—C14—C16—O82.5 (12)
Pb1ii—O1—C1—C2161.7 (5)O1i—Pb1—O9—C1752.6 (15)
Pb1i—O1—C1—Pb1ii133.2 (6)O2ii—Pb1—O9—C1727.1 (15)
O2—C1—C2—C7145.9 (7)O3—Pb1—O9—C1717.1 (18)
O1—C1—C2—C730.2 (9)O1ii—Pb1—O9—C1765.3 (16)
Pb1ii—C1—C2—C775.3 (18)O7iii—Pb1—O9—C17129.7 (16)
O2—C1—C2—C331.3 (9)O4—Pb1—O9—C17167.4 (14)
O1—C1—C2—C3152.5 (7)O7iv—Pb1—O9—C17139.8 (15)
Pb1ii—C1—C2—C3101.9 (16)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+1; (iii) x1, y+1/2, z1/2; (iv) x, y+1/2, z1/2; (v) x+1, y, z; (vi) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9···O6iii0.84 (2)2.01 (7)2.789 (9)153 (14)
Symmetry code: (iii) x1, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Pb2(C8H3IO4)2(CH4O)]
Mr1026.43
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)4.3137 (4), 27.918 (2), 17.6437 (15)
β (°) 93.897 (1)
V3)2119.9 (3)
Z4
Radiation typeMo Kα
µ (mm1)18.82
Crystal size (mm)0.35 × 0.23 × 0.21
Data collection
DiffractometerBruker–Nonius KappaCCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Bruker, 1997)
Tmin, Tmax0.058, 0.110
No. of measured, independent and
observed [I > 2σ(I)] reflections
18249, 4855, 4302
Rint0.040
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.070, 1.08
No. of reflections4855
No. of parameters276
No. of restraints8
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.0209P)2 + 11.242P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.23, 1.65

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Selected bond lengths (Å) top
Pb1—O1i2.391 (5)Pb2—O8iv2.340 (6)
Pb1—O2ii2.428 (5)Pb2—O52.461 (5)
Pb1—O32.433 (5)Pb2—O42.532 (5)
Pb1—O1ii2.615 (5)Pb2—O62.556 (5)
Pb1—O92.790 (8)Pb2—O7iv2.750 (5)
Pb1—O7iii2.910 (5)Pb2—O4v2.995 (5)
Pb1—O42.933 (5)Pb2—O5v3.035 (6)
Pb1—O7iv3.110 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+1; (iii) x1, y+1/2, z1/2; (iv) x, y+1/2, z1/2; (v) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9···O6iii0.84 (2)2.01 (7)2.789 (9)153 (14)
Symmetry code: (iii) x1, y+1/2, z1/2.
 

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