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The title compound, {[Cd2(C9HNO8)(H2O)4]·H2O}n, consists of two crystallographically independent CdII cations, one tetra­basic pyridine-2,3,5,6-tetra­carboxyl­ate (pdtc) anion, four coordinated water mol­ecules and one solvent water mol­ecule. The CdII cations have distorted square-anti­prismatic (one pyridine N, six carboxyl­ate O and one water O atom) and octa­hedral (three carboxyl­ate O and three water O atoms) coordination environments. Each pdtc ligand employs its pyridine and carboxyl­ate groups to chelate and bridge seven CdII cations. The square-anti­prismatic coordinated CdII cations are linked by pdtc ligands into a lamellar framework structure, while the octa­hedral coordinated CdII cations are bridged by the [mu]2-carboxyl­ate O atoms and the pdtc ligands into a chain network that further joins neighbouring lamellae into a three-dimensional porous network. The cavities are filled with solvent water mol­ecules that are linked to the host through complex hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110008085/sq3239sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110008085/sq3239Isup2.hkl
Contains datablock I

CCDC reference: 774883

Comment top

In the past few years, crystal engineering of porous metal–organic coordination networks has attracted much attention because of their interesting structural patterns with both aesthetic appeal and special functionalities for potential applications (Czaja et al., 2009; Lee et al., 2009; Li et al., 2009; Ma et al., 2009; Murray et al., 2009; Tranchemontagne et al., 2009; Wang & Cohen, 2009). It has been shown that judicious choice of organic bridging ligands and metal nodes is the key step towards the construction of interesting topological frameworks.

Pyridine-2,3,5,6-tetracarboxylic acid (H4pdtc), which contains one pyridine and four carboxylate potential donor groups, should be an effective ligand for coordinating to transition metal cations to generate some interesting structural networks (Babu & Nangia, 2006). However, only two pdtc ligand coordinated compounds have been reported to date, a tetranuclear zinc(II) compound bridged by two pdtc anions, and a mononuclear nickel(II) compound chelated by pdtc (Yang et al., 2008). In the former case, because the additional coordination sites of the Zn cations are blocked by four chelating 1,10-phenanthroline molecules, the tetranuclear Zn unit cannot be further bridged by additional pdtc ligands to form a polymeric framework. In the latter case, as three water coordination sites of the Ni cation are not replaced by additional pdtc ligands, the pdtc ligand only chelates one Ni cation to form a mononuclear nickel(II) compound.

Because of the relatively large ionic radius of the CdII cation, its coordination numbers in O-donor complexes typically range from 6 to 8, which suggests that cadmium compounds should form some interesting three-dimensional frameworks (Wang et al., 2007). In fact, there are several examples of three-dimensional frameworks of CdII cations bridged by pyridine carboxylates, such as pyridine-3,4-dicarboxylate (Xia et al., 2004), pyridine-2,4-dicarboxylate (Bai et al., 2008), pyridine-2,3-dicarboxylate (Zhang et al., 2005; Han et al., 2006) and pyridine-2,4,6-tricarboxylate (Wang et al., 2007; Zou et al., 2008). Attracted by the interesting structural motifs of these pyridine carboxylate-bridged cadmium compounds, we anticipated that pdtc would be an effective bridging ligand to generate a novel structural network. We report here the first three-dimensional porous polymeric framework compound based on the pdtc ligand, the title compound, [Cd2(pdtc)(H2O)4].H2O, (I).

Compound (I) crystallizes in the triclinic P1 space group with two CdII cations, one fully deprotonated pdtc4- anion, four aqua ligands and one solvent water molecule in the asymmetric unit (Fig. 1). Each pdtc ligand employs its pyridine group and carboxylate groups to chelate and bridge seven CdII cations. Atom Cd1 is chelated by the pyridine group and two neighbouring carboxyl O atoms from the first pdtc ligand, two O atoms of a carboxylate group from a second pdtc ligand, one carboxyl O atom from a third pdtc ligand, a µ2 carboxyl O atom from a fourth pdtc ligand and one aqua ligand, in an octa-coordinated distorted square-antiprismatic coordination environment (Table 1).

The pdtc ligands link the Cd1 cations into an interesting lamellar framework structure in the ab plane (Fig. 2). Atom Cd2 has a hexa-coordinated octahedral geometry, chelated by two O atoms of one pdtc carboxylate group, one µ2 carboxyl O atom of another pdtc ligand and three aqua ligands (Table 1). There is one additional interaction, Cd2–O8v = 2.676 (4) Å [symmetry code: (v) x, y, z - 1], but this is outside the typical range of 2.1–2.4 Å for Cd—O coordination (Standard reference?). The µ2 carboxyl O atom bridges two Cd2 sites into a binuclear unit, which is further doubly bridged by pdtc ligands into a chain network along the c direction (Fig. 3). As the alternating pdtc ligands along c are attributed to different layers of pdtc linking up Cd1 sites, the Cd2 sites serve to join neighbouring lamellar Cd1–pdtc frameworks into a three-dimensional porous network structure (Fig. 4). The cavities are filled with solvent water molecules that interact with the host framework through hydrogen bonding. The hydrogen-bond distances between solvent water molecules and carboxyl O atoms range from 2.728 (6) to 2.730 (6) Å, and those between solvent water molecules and aqua ligands from 2.707 (6) to 2.765 (6) Å. Finally, there are also extensive hydrogen bonds between aqua ligands and carboxyl O atoms [2.686 (6)–2.975 (6) Å] and between aqua ligands themselves [2.870 (6)–2.946 (6) Å].

The framework structure of (I) is quite different from previously reported three-dimensional compounds bridged by pyridine dicarboxylates. For example, pyridine-3,4-dicarboxylate acts a tetradentate ligand to link four octahedrally distorted CdII cations into a three-dimensional architecture with small square channels without guest molecules (Xia et al., 2004). The pyridine-2,4-dicarboxylate ligand acts as a pentadentate ligand to link five octahedral CdII cations into a three-dimensional framework with large channels occupied by the pyridine groups of the ligands (Bai et al., 2008), while pyridine-2,3-dicarboxylate, adopting two different coordination modes, bridges CdII tetramers into a three-dimensional network without guest molecules (Han et al., 2006). The three-dimensional framework of pyridine-2,4,6-tricarboxylate-bridged CdII cations is similar to (I) in that there are two different types of CdII cations in distorted octahedral and pentagonal–bipyramidal coordination environments. Pyridine-2,4,6-tricarboxylate bridges the pentagonal–bipyramidal coordinated CdII cations into a two-dimensional layer structure, which is further extended into a three-dimensional network linked by the octahedrally coordinated CdII cations and carboxyl groups without guest molecules within the cavities thus formed (Wang et al., 2007).

Thermogravimetric analysis (TGA) of (I) indicates that a weight loss of 15.7% occurs between 303 and 433 K, corresponding to the loss of solvent water molecules and aqua ligands (expected 15.9%), without a distinct plateau in the curve. There is almost no further weight loss until 683 K, above which (I) began to lose the coordinated pdtc ligand and to decompose. After a sample of (I) was ground and heated at 368 K for 2 h, a powder X-ray diffraction (PXRD) profile of the resultant powder showed no sharp peaks in the PXRD pattern, and this material cannot be rehydrated and reverted to the original compound after being immersed in water, as confirmed by the PXRD pattern. These results indicate that both the solvent H2O and aqua ligands play important roles in the formation and stability of (I).

Experimental top

Heating a mixture of CdCl2.2.5H2O (4.6 mg, 0.02 mmol) and H4pdtc (2.6 mg, 0.01 mmol) in water (4.0 ml) at 368 K for 1 d afforded colourless crystals of (I), which were filtered off, washed with water, ethanol and [Diethyl?] ether, and dried at room temperature (yield 78% based on H4pdtc). IR (KBr pellet, ν, cm-1): 1616 s, 1560 s, 1453 m, 1371 s, 1334 m, 1269 w, 1159 m, 837 w.

Refinement top

H atoms on C atoms were positioned geometrically and included in the structure-factor calculations as riding atoms, with C—H = 0.93 Å. The H atoms of the water molecules were clearly visible in difference maps, and these were placed in the difference-map positions and constrained to ride on their parent O atoms, with O—H = 0.82 Å. All H atoms were assigned fixed isotropic displacement parameters, with Uiso(H) = 1.2Ueq(parent atom), in the subsequent refinement.

Computing details top

Data collection: CrysAlis PRO (Oxford Diffraction, 2010); cell refinement: CrysAlis PRO (Oxford Diffraction, 2010); data reduction: CrysAlis PRO (Oxford Diffraction, 2010); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97 (Sheldrick, 2008); software used to prepare material for publication: PLATON (Spek, 2009).

Figures top
[Figure 1] Fig. 1. A perspective view of the locally expanded unit for (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 25% probability level and H atoms are shown as small spheres of arbitrary radii. [Symmetry codes: (i) x, y - 1, z; (ii) 1 - x, 1 - y, 2 - z; (iii) 2 - x, 1 - y, 2 - z; (iv) 2 - x, 1 - y, 1 - z; (v) x, y, z - 1.]
[Figure 2] Fig. 2. A view of the lamellar framework of Cd1 ions linked by pdtc ligands.
[Figure 3] Fig. 3. A view of the linear framework of Cd2 ions linked by pdtc ligands.
[Figure 4] Fig. 4. The packing of (I), viewed down the a axis. For clarity, H atoms have been omitted.
Poly[[tetraaqua(µ7-pyridine-2,3,5,6-tetracarboxylato)dicadmium(II)] monohydrate] top
Crystal data top
[Cd2(C9HNO8)(H2O)4]·H2OZ = 2
Mr = 565.99F(000) = 544
Triclinic, P1Dx = 2.680 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.3989 (5) ÅCell parameters from 4815 reflections
b = 8.5350 (3) Åθ = 3.5–25.7°
c = 11.4883 (5) ŵ = 3.11 mm1
α = 89.325 (4)°T = 293 K
β = 69.014 (5)°Prism, colourless
γ = 67.269 (4)°0.18 × 0.12 × 0.09 mm
V = 701.48 (6) Å3
Data collection top
Oxford Xcalibur, Atlas, Gemini Ultra
diffractometer
2650 independent reflections
Radiation source: Enhance (Mo) X-ray Source2181 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 10.3592 pixels mm-1θmax = 25.7°, θmin = 3.5°
ω scansh = 108
Absorption correction: analytical
(CrysAlis PRO; Oxford Diffraction, 2010)
k = 109
Tmin = 0.645, Tmax = 0.756l = 1310
4815 measured reflections
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.044H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0156P)2]
where P = (Fo2 + 2Fc2)/3
2650 reflections(Δ/σ)max < 0.001
226 parametersΔρmax = 0.68 e Å3
0 restraintsΔρmin = 0.87 e Å3
Crystal data top
[Cd2(C9HNO8)(H2O)4]·H2Oγ = 67.269 (4)°
Mr = 565.99V = 701.48 (6) Å3
Triclinic, P1Z = 2
a = 8.3989 (5) ÅMo Kα radiation
b = 8.5350 (3) ŵ = 3.11 mm1
c = 11.4883 (5) ÅT = 293 K
α = 89.325 (4)°0.18 × 0.12 × 0.09 mm
β = 69.014 (5)°
Data collection top
Oxford Xcalibur, Atlas, Gemini Ultra
diffractometer
2650 independent reflections
Absorption correction: analytical
(CrysAlis PRO; Oxford Diffraction, 2010)
2181 reflections with I > 2σ(I)
Tmin = 0.645, Tmax = 0.756Rint = 0.018
4815 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.044H-atom parameters constrained
S = 1.07Δρmax = 0.68 e Å3
2650 reflectionsΔρmin = 0.87 e Å3
226 parameters
Special details top

Experimental. CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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
Cd10.76367 (5)0.19923 (5)1.11014 (4)0.02449 (13)
Cd20.85198 (6)0.56158 (5)0.40771 (4)0.02831 (14)
O10.7284 (6)0.1749 (5)0.9117 (4)0.0321 (10)
O20.7084 (6)0.2984 (5)0.7422 (4)0.0356 (10)
O30.8385 (5)0.5752 (5)0.6188 (3)0.0263 (9)
O40.5287 (5)0.6759 (5)0.7175 (3)0.0273 (9)
O50.9194 (5)0.8872 (5)1.0181 (4)0.0315 (9)
O60.6222 (5)0.9917 (5)1.1425 (4)0.0318 (10)
O70.8382 (6)0.6540 (5)1.2270 (4)0.0320 (10)
O80.8012 (6)0.4118 (5)1.2286 (4)0.0334 (10)
O90.9057 (6)0.0580 (5)1.2566 (4)0.0349 (10)
H9A1.01460.00621.21540.042*
H9B0.91340.12511.30240.042*
O100.8699 (6)0.8237 (5)0.4409 (4)0.0404 (11)
H10A0.86660.88370.38470.049*
H10B0.78350.90150.49590.049*
O110.5275 (6)0.6943 (6)0.4842 (4)0.0409 (11)
H11A0.49730.78330.45360.049*
H11B0.49500.72160.56010.049*
O120.8328 (6)0.3056 (5)0.4657 (4)0.0391 (11)
H12A0.88780.26220.51200.047*
H12B0.72260.32410.50410.047*
O130.6272 (6)1.0593 (5)0.6480 (4)0.0409 (11)
H13A0.54771.04400.70800.049*
H13B0.66391.11860.67760.049*
N10.7397 (6)0.4479 (6)1.0143 (4)0.0210 (10)
C10.7171 (7)0.2970 (7)0.8482 (5)0.0238 (12)
C20.7202 (7)0.4563 (7)0.9038 (5)0.0219 (12)
C30.7114 (7)0.5992 (7)0.8421 (5)0.0224 (12)
C40.6887 (8)0.6156 (7)0.7173 (5)0.0229 (12)
C50.7237 (7)0.7347 (7)0.8980 (5)0.0251 (13)
H5A0.71440.83290.86000.030*
C60.7500 (7)0.7236 (7)1.0111 (5)0.0224 (12)
C70.7663 (8)0.8755 (7)1.0643 (5)0.0244 (13)
C80.7591 (7)0.5767 (7)1.0663 (5)0.0230 (13)
C90.8002 (7)0.5451 (7)1.1830 (5)0.0246 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0271 (2)0.0227 (2)0.0239 (2)0.01080 (19)0.00933 (18)0.00413 (17)
Cd20.0290 (3)0.0312 (2)0.0259 (3)0.0119 (2)0.01241 (19)0.00600 (18)
O10.047 (3)0.026 (2)0.033 (2)0.019 (2)0.020 (2)0.0080 (18)
O20.054 (3)0.034 (2)0.026 (2)0.021 (2)0.020 (2)0.0053 (18)
O30.025 (2)0.030 (2)0.022 (2)0.0096 (18)0.0077 (17)0.0026 (17)
O40.024 (2)0.033 (2)0.023 (2)0.0086 (18)0.0099 (17)0.0026 (16)
O50.031 (2)0.033 (2)0.034 (2)0.0187 (19)0.0088 (18)0.0037 (18)
O60.030 (2)0.025 (2)0.033 (2)0.0074 (19)0.0077 (19)0.0033 (18)
O70.046 (3)0.031 (2)0.029 (2)0.019 (2)0.022 (2)0.0059 (17)
O80.046 (3)0.033 (2)0.028 (2)0.019 (2)0.0186 (19)0.0117 (18)
O90.038 (2)0.031 (2)0.034 (3)0.012 (2)0.014 (2)0.0011 (19)
O100.052 (3)0.034 (2)0.029 (2)0.016 (2)0.009 (2)0.0044 (19)
O110.037 (3)0.051 (3)0.030 (2)0.013 (2)0.014 (2)0.007 (2)
O120.046 (3)0.044 (3)0.037 (3)0.023 (2)0.022 (2)0.010 (2)
O130.046 (3)0.045 (3)0.034 (3)0.026 (2)0.009 (2)0.002 (2)
N10.020 (2)0.021 (2)0.020 (2)0.006 (2)0.0075 (19)0.0021 (18)
C10.022 (3)0.022 (3)0.027 (3)0.007 (2)0.011 (2)0.001 (2)
C20.017 (3)0.024 (3)0.022 (3)0.007 (2)0.006 (2)0.001 (2)
C30.022 (3)0.023 (3)0.019 (3)0.008 (2)0.007 (2)0.001 (2)
C40.030 (3)0.020 (3)0.021 (3)0.011 (3)0.011 (3)0.005 (2)
C50.027 (3)0.024 (3)0.025 (3)0.012 (3)0.009 (2)0.008 (2)
C60.025 (3)0.021 (3)0.021 (3)0.009 (2)0.009 (2)0.005 (2)
C70.031 (3)0.028 (3)0.020 (3)0.014 (3)0.015 (3)0.010 (2)
C80.015 (3)0.025 (3)0.024 (3)0.003 (2)0.006 (2)0.001 (2)
C90.025 (3)0.027 (3)0.020 (3)0.009 (3)0.008 (2)0.004 (2)
Geometric parameters (Å, º) top
Cd1—O5i2.345 (4)O7—C91.256 (7)
Cd1—N12.352 (5)O7—Cd2vii2.238 (4)
Cd1—O4ii2.373 (4)O8—C91.245 (7)
Cd1—O12.423 (4)O9—H9A0.8184
Cd1—O6iii2.446 (4)O9—H9B0.8182
Cd1—O92.447 (4)O10—H10A0.8210
Cd1—O82.460 (4)O10—H10B0.8221
Cd1—O5iii2.511 (4)O11—H11A0.8206
Cd2—O7iv2.238 (4)O11—H11B0.8205
Cd2—O3v2.304 (4)O12—H12A0.8198
Cd2—O112.325 (4)O12—H12B0.8196
Cd2—O122.325 (4)O13—H13A0.8212
Cd2—O102.344 (4)O13—H13B0.8156
Cd2—O32.389 (4)N1—C21.335 (7)
O1—C11.258 (7)N1—C81.347 (7)
O2—C11.246 (7)C1—C21.522 (8)
O3—C41.279 (6)C2—C31.393 (8)
O3—Cd2v2.304 (4)C3—C51.384 (8)
O4—C41.238 (6)C3—C41.511 (7)
O4—Cd1ii2.373 (4)C5—C61.390 (8)
O5—C71.247 (6)C5—H5A0.9300
O5—Cd1i2.345 (4)C6—C81.386 (8)
O5—Cd1vi2.511 (4)C6—C71.513 (8)
O6—C71.253 (7)C8—C91.497 (8)
O6—Cd1vi2.446 (4)
O5i—Cd1—N181.77 (14)C7—O5—Cd1vi90.3 (3)
O5i—Cd1—O4ii162.11 (13)Cd1i—O5—Cd1vi112.46 (15)
N1—Cd1—O4ii96.79 (14)C7—O6—Cd1vi93.2 (3)
O5i—Cd1—O183.95 (14)C9—O7—Cd2vii101.7 (3)
N1—Cd1—O168.07 (14)C9—O8—Cd1117.7 (3)
O4ii—Cd1—O1112.19 (13)Cd1—O9—H9A108.1
O5i—Cd1—O6iii120.12 (13)Cd1—O9—H9B112.7
N1—Cd1—O6iii138.26 (15)H9A—O9—H9B103.8
O4ii—Cd1—O6iii72.44 (13)Cd2—O10—H10A116.1
O1—Cd1—O6iii78.83 (13)Cd2—O10—H10B120.7
O5i—Cd1—O980.08 (14)H10A—O10—H10B93.2
N1—Cd1—O9135.63 (15)Cd2—O11—H11A108.3
O4ii—Cd1—O988.89 (13)Cd2—O11—H11B104.7
O1—Cd1—O9147.89 (13)H11A—O11—H11B107.4
O6iii—Cd1—O985.37 (14)Cd2—O12—H12A114.3
O5i—Cd1—O886.42 (13)Cd2—O12—H12B108.7
N1—Cd1—O867.71 (14)H12A—O12—H12B106.9
O4ii—Cd1—O876.64 (13)H13A—O13—H13B106.1
O1—Cd1—O8135.62 (13)C2—N1—C8119.9 (5)
O6iii—Cd1—O8141.20 (13)C2—N1—Cd1119.9 (3)
O9—Cd1—O871.03 (13)C8—N1—Cd1120.0 (4)
O5i—Cd1—O5iii67.54 (15)O2—C1—O1126.1 (5)
N1—Cd1—O5iii131.36 (14)O2—C1—C2116.6 (5)
O4ii—Cd1—O5iii123.59 (13)O1—C1—C2117.3 (5)
O1—Cd1—O5iii71.84 (13)N1—C2—C3121.6 (5)
O6iii—Cd1—O5iii52.58 (12)N1—C2—C1115.4 (5)
O9—Cd1—O5iii76.33 (13)C3—C2—C1122.9 (5)
O8—Cd1—O5iii141.20 (13)C5—C3—C2118.5 (5)
O7iv—Cd2—O3v108.53 (14)C5—C3—C4117.7 (5)
O7iv—Cd2—O1184.78 (15)C2—C3—C4123.8 (5)
O3v—Cd2—O11166.47 (14)O4—C4—O3124.7 (5)
O7iv—Cd2—O12123.72 (14)O4—C4—C3118.6 (5)
O3v—Cd2—O1285.24 (14)O3—C4—C3116.5 (5)
O11—Cd2—O1289.31 (16)C3—C5—C6119.9 (5)
O7iv—Cd2—O1082.08 (15)C3—C5—H5A120.1
O3v—Cd2—O1088.22 (14)C6—C5—H5A120.0
O11—Cd2—O1091.34 (15)C8—C6—C5118.4 (5)
O12—Cd2—O10154.12 (15)C8—C6—C7125.1 (5)
O7iv—Cd2—O3158.25 (13)C5—C6—C7116.5 (5)
O3v—Cd2—O377.03 (14)O5—C7—O6122.9 (5)
O11—Cd2—O389.69 (14)O5—C7—C6117.8 (5)
O12—Cd2—O377.11 (14)O6—C7—C6118.9 (5)
O10—Cd2—O377.03 (14)N1—C8—C6121.7 (5)
C1—O1—Cd1119.3 (3)N1—C8—C9115.2 (5)
C4—O3—Cd2v130.9 (4)C6—C8—C9123.1 (5)
C4—O3—Cd2124.4 (3)O8—C9—O7123.7 (5)
Cd2v—O3—Cd2102.97 (14)O8—C9—C8119.2 (5)
C4—O4—Cd1ii129.4 (3)O7—C9—C8117.1 (5)
C7—O5—Cd1i156.7 (4)
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y+1, z+2; (iii) x, y1, z; (iv) x, y, z1; (v) x+2, y+1, z+1; (vi) x, y+1, z; (vii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9B···O12vii0.822.172.946 (6)158.6
O9—H9A···O1viii0.822.062.872 (5)169.9
O10—H10A···O9ix0.822.112.912 (6)164.3
O10—H10B···O130.821.912.707 (6)164.3
O11—H11A···O13x0.822.002.765 (6)154.1
O11—H11B···O40.821.942.686 (6)150.6
O12—H12A···O10v0.822.142.892 (6)151.7
O12—H12A···O20.822.482.975 (6)119.7
O12—H12B···O11xi0.822.122.870 (6)151.5
O13—H13A···O6xii0.821.912.728 (6)174.0
O13—H13B···O2vi0.821.932.730 (6)167.9
Symmetry codes: (v) x+2, y+1, z+1; (vi) x, y+1, z; (vii) x, y, z+1; (viii) x+2, y, z+2; (ix) x, y+1, z1; (x) x+1, y+2, z+1; (xi) x+1, y+1, z+1; (xii) x+1, y+2, z+2.

Experimental details

Crystal data
Chemical formula[Cd2(C9HNO8)(H2O)4]·H2O
Mr565.99
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)8.3989 (5), 8.5350 (3), 11.4883 (5)
α, β, γ (°)89.325 (4), 69.014 (5), 67.269 (4)
V3)701.48 (6)
Z2
Radiation typeMo Kα
µ (mm1)3.11
Crystal size (mm)0.18 × 0.12 × 0.09
Data collection
DiffractometerOxford Xcalibur, Atlas, Gemini Ultra
diffractometer
Absorption correctionAnalytical
(CrysAlis PRO; Oxford Diffraction, 2010)
Tmin, Tmax0.645, 0.756
No. of measured, independent and
observed [I > 2σ(I)] reflections
4815, 2650, 2181
Rint0.018
(sin θ/λ)max1)0.609
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.044, 1.07
No. of reflections2650
No. of parameters226
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.68, 0.87

Computer programs: CrysAlis PRO (Oxford Diffraction, 2010), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009).

Selected geometric parameters (Å, º) top
Cd1—O5i2.345 (4)Cd1—O5iii2.511 (4)
Cd1—N12.352 (5)Cd2—O7iv2.238 (4)
Cd1—O4ii2.373 (4)Cd2—O3v2.304 (4)
Cd1—O12.423 (4)Cd2—O112.325 (4)
Cd1—O6iii2.446 (4)Cd2—O122.325 (4)
Cd1—O92.447 (4)Cd2—O102.344 (4)
Cd1—O82.460 (4)Cd2—O32.389 (4)
O5i—Cd1—N181.77 (14)O6iii—Cd1—O5iii52.58 (12)
N1—Cd1—O168.07 (14)O9—Cd1—O5iii76.33 (13)
O4ii—Cd1—O6iii72.44 (13)O7iv—Cd2—O1184.78 (15)
O1—Cd1—O6iii78.83 (13)O3v—Cd2—O1285.24 (14)
N1—Cd1—O867.71 (14)O7iv—Cd2—O1082.08 (15)
O4ii—Cd1—O876.64 (13)O3v—Cd2—O377.03 (14)
O9—Cd1—O871.03 (13)O12—Cd2—O377.11 (14)
O5i—Cd1—O5iii67.54 (15)O10—Cd2—O377.03 (14)
O1—Cd1—O5iii71.84 (13)
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y+1, z+2; (iii) x, y1, z; (iv) x, y, z1; (v) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9B···O12vi0.822.172.946 (6)158.6
O9—H9A···O1vii0.822.062.872 (5)169.9
O10—H10A···O9viii0.822.112.912 (6)164.3
O10—H10B···O130.821.912.707 (6)164.3
O11—H11A···O13ix0.822.002.765 (6)154.1
O11—H11B···O40.821.942.686 (6)150.6
O12—H12A···O10v0.822.142.892 (6)151.7
O12—H12A···O20.822.482.975 (6)119.7
O12—H12B···O11x0.822.122.870 (6)151.5
O13—H13A···O6xi0.821.912.728 (6)174.0
O13—H13B···O2xii0.821.932.730 (6)167.9
Symmetry codes: (v) x+2, y+1, z+1; (vi) x, y, z+1; (vii) x+2, y, z+2; (viii) x, y+1, z1; (ix) x+1, y+2, z+1; (x) x+1, y+1, z+1; (xi) x+1, y+2, z+2; (xii) x, y+1, z.
 

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