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The title compound, poly[aqua­([mu]2-1H-imidazole-4-carboxylato-[kappa]3N3,O:O')hemi([mu]2-oxalato-[kappa]4O1,O2:O1',O2')cadmium(II)], [Cd(C4H3N2O2)(C2O4)0.5(H2O)]n, exhibits a two-dimensional network. The CdII cation is coordinated to one N atom and two carboxyl­ate O atoms from two 1H-imidazole-4-carboxyl­ate (Himc) ligands, two carboxyl­ate O atoms from the bridging oxalate anion and one ligated water mol­ecule; these six donor atoms form a distorted octa­hedral configuration. The oxalate anion lies on a centre of inversion. The Himc ligands connect the CdII cations to form -Cd-Himc-Cd-Himc-Cd- zigzag chains, with a Cd...Cd separation of 5.8206 (6) Å along the b direction, which are further linked by tetra­dentate oxalate anions to generate a two-dimensional herringbone architecture in the ab plane. These layers are extended to form a three-dimensional supra­molecular framework via O-H...O and N-H...O hydrogen bonds and [pi]-[pi] stacking inter­actions. The solid-state photoluminscent behaviour of the title compound has been investigated at room temperature.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270112023153/sf3171sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270112023153/sf3171Isup2.hkl
Contains datablock I

CCDC reference: 893479

Comment top

Coordination polymers with multicarboxylate imidazole ligands are of great current interest due to their intriguing architectures and topologies, as well as their many promising applications as functional materials, including optics, magnetism and porosity (Alkordi et al., 2009; Gu et al., 2011; Liu et al., 2008). Many imidazole-based dicarboxylate ligands have been developed and widely applied in the construction of metal–organic frameworks (MOFs) over recent years (Li et al., 2010; Wang et al., 2011; Zheng et al., 2011). However, the coordination chemistry of the simple imidazole-based carboxylate ligand 1H-imidazole-4-carboxylic acid (H2imc) has been less well explored. Similar to imidazole-based dicarboxylate ligands, H2imc can be partially or fully deprotonated to generate Himc- or imc2- anions at different pH values, and it can bind to metal ions through the N atoms of the imidazole ring and the carboxylate O atoms. In addition, it may take part in the formation of noncovalent interactions, such as hydrogen bonds and ππ stacking interactions, thereby contributing greatly to the formation of a wide variety of supramolecular frameworks. To date, the few complexes with the H2imc ligand reported in the literature exhibit mononuclear (Gryz et al., 2006; Sun et al., 2010; Yin et al., 2009) or low-dimensional structures (Starosta & Leciejewicz, 2006; Sun & Yang, 2007). In our previous studies, we introduced different anions (such as acetate, NO3-, ClO4-, Cl-, Br-, I- and SO42-) to investigate their effect (Cai et al., 2012). Positive results indicated that the anions play crucial roles in the structure topologies and transformations. Herein, we selected oxalate for further study. The synthesis, structure and photoluminescence properties of the title new two-dimensional cadmium coordination polymer, (I), which was obtained by hydrothermal reaction of CdC2O4.3H2O with the H2imc ligand, are presented.

Compound (I) exhibits a two-dimensional herringbone-like network, consisting of one CdII ion, one Himc ligand, one half of an oxalate anion and one ligated water molecule, as shown in Fig. 1. The oxalate lies on a centre of inversion. In the structure, the six-coordinated CdII cation lies in a distorted octahedral environment, which is completed by one N atom [N1i; symmetry code: (i) -x + 1, y + 1/2, -z + 3/2] and two carboxylate O atoms (O1 and O2i) from two Himc ligands, two carboxylate O atoms from one bridging oxalate anion [O3ii and O4; symmetry code: (ii) -x, -y + 3, -z + 1], and the water O atom. The water molecule and atom O2i occupy the axial sites and the other donors are located in the equatorial plane. Selected bond lengths for (I) are listed in Table 1. The Cd—O and Cd—N bond lengths are in the normal ranges (Cai et al., 2012; Yin et al., 2009).

In (I), both the Himc anion and the oxalate act as µ2-bridges. The Himc ligands connect the CdII cations to form –Cd–Himc–Cd–Himc–Cd– zigzag chains with a Cd···Cd separation of 5.820 (5) Å along the b direction. These zigzag chains are further linked by tetradentate centrosymmetric oxalate anions to form a two-dimensional herringbone architecture in the ab plane (Fig. 2). Both surfaces of these layers are covered by protruding imidazole rings which interdigitate when adjacent layers come together. They form ππ stacking interactions and the centroid-to-centroid separations between two imidazole rings are 3.485 (5) and 3.544 (5) Å. In addition, there are multiple hydrogen bonds in the structure of (I) of two types. The first type is between the coordinated water molecule and the carboxylate O atoms of the oxalate anions [O···O = 2.815 (6) and 2.972 (5) Å] and the second between the N atom and one carboxylate O atom of the Himc anions [N···O = 2.760 (6) Å]. Thus, the connection of both ππ stacks and hydrogen bonds results in the formation of a three-dimensional supramolecular network (Fig. 3).

As illustrated in Fig. 4, the powder XRD pattern of (I) is in agreement with that simulated based on the single-crystal structure. The diffraction peaks in the experimental and simulated patterns correspond well in their positions, suggesting that the crystal samples are pure.

In our previous work, three CdII coordination polymers with Himc anions exhibited a one-dimensional zigzag chain, a two-dimensional layer and a three-dimensional diamondoid network, respectively (Cai et al., 2012). Although only a sulfate anion took part in the coordination of the last structure, positive results from many synthesis experiments revealed that the anions play crucial roles in the structure topologies of the resulting complexes. In this work, oxalate was selected to construct a new CdII coordination polymer, because it is a commonly used bridging ligand and adopts various coordination modes. In the structure of (I), the oxalate anion adopts a bis-chelating bridging mode connecting two CdII cations. Finally, a two-dimensional herringbone-like network is formed through alternating connections between Himc ligands and oxalate anions, and this is quite different from that in [Cd2(Himc)2(SO4)(H2O)] (Cai et al., 2012), which exhibit a two-dimensional structure with (3,4)-mixed connectivity. This difference can be explained as different coordination modes of the Himc ligand.

The solid-state photoluminescent behaviour of (I) was investigated at room temperature. As shown in Fig. 5, an intense broad emission band at 451 nm is observed after excitation at a wavelength of 369 nm. Compared with the free ligand H2imc (emission at 463 nm with λex = 376 nm), the blue-shifted emission for (I) may be attributed to intraligand transitions (Cai et al., 2012).

In summary, the hydrothermal reaction of CdC2O4 and H2imc results in the formation of a two-dimensional herringbone-like cadmium coordination polymer. Combined with our previous work, it is clear that the anion plays a significant role in the assembly of the metal–anionic ligand system. That is to say, the choice of anion could promote different topological structures. In addition, (I) in the solid state exhibits characteristic emission at room temperature.

Related literature top

For related literature, see: Alkordi et al. (2009); Bruker (2007); Cai et al. (2012); Gryz et al. (2006); Gu et al. (2011); Li et al. (2010); Liu et al. (2008); Sheldrick (2008); Starosta & Leciejewicz (2006); Sun & Yang (2007); Sun et al. (2010); Wang et al. (2011); Yin et al. (2009); Zheng et al. (2011).

Experimental top

CdC2O4.3H2O (25.5 mg, 0.10 mmol) and H2imc (22.4 mg, 0.20 mmol) were mixed into H2O–C2H5OH (6 ml, 1:1 v/v) and the pH was adjusted to about 6 using aqueous NaOH (0.20 mol l-1). The mixture was sealed in a 10 ml sample bottle reactor and heated at 373 K under autogenous pressure for 48 h. After the sample had been cooled slowly to room temperature at a rate of 2 K h-1, colourless block-shaped crystals of (I) were obtained in a yield of 68%. Analysis, calculated for C5H5CdN2O5: C 21.03, H 1.77, N 9.81%; found: C 20.97, H 1.82, N 9.88%. IR (KBr pellet, ν, cm-1): 3341 (s), 3152 (m), 2977 (w), 1643 (s), 1589 (s), 1561 (m), 1514 (w), 1398 (s), 1313 (s), 1241 (m), 1083 (w), 997 (m), 930 (w), 809 (s), 793 (m), 652 (m), 613 (w), 564 (w), 501 (w).

Refinement top

The crystal under investigation was found to be nonmerohedrally twinned. The orientation matrices for the two components were identified using the program CELL_NOW (Sheldrick, 2008), with the two components being related by a 180° rotation around the real/reciprocal axis (1 -0.002 -0.999; -0.829 -0.001 1). The two components were integrated using SAINT (Bruker, 2007), resulting in a total of 8238 reflections. 3619 reflections (1506 unique) involved component 1 only (mean I/σ = 13.2), 3602 reflections (1500 unique) involved component 2 only (mean I/σ = 10.2), and 1017 reflections (519 unique) involved both components (mean I/σ = 15.6). The exact twin matrix identified by the integration program was found to be (-0.09207 0.00002 -0.90797; 0.00011 -1 0; -1.09202 -0.00026 0.09207).

The data were corrected for absorption using TWINABS (SHELXL97; Sheldrick, 2008), and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the HKLF 5 routine with all reflections of component 1 (including the overlapping reflections), resulting in a BASF value of 0.365 (2). The reflections involving component 2 only were omitted from the data set, as this component was somewhat weaker than component 1 and gave a slightly inferior Rint value.

The Rint value given is for all reflections and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS).

The H atoms of water molecule were located in the difference Fourier maps and the other H atoms were placed in calculated positions. They were refined as riding atoms, with C—H = 0.93 Å (imidazole C—H) and N—H = 0.86 Å, and with Uiso(H) = 1.2Ueq(C), 1.2Ueq(N) or 1.5 Ueq(O).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: APEX2 (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) -x + 1, y + 1/2, -z + 3/2; (ii) -x, -y + 3, -z + 1.]
[Figure 2] Fig. 2. A packing diagram for (I), showing the two-dimensional herringbone-like network in the ab plane.
[Figure 3] Fig. 3. A packing diagram for (I), showing the three-dimensional supramolecular network driven by hydrogen bonds (dashed lines) and ππ stacking interactions.
[Figure 4] Fig. 4. (a) The simulated X-ray powder diffraction pattern and (b) the experimental powder X-ray diffraction pattern of (I).
[Figure 5] Fig. 5. The solid-state photoluminescence of (I) at room temperature (λex = 369 nm).
poly[aqua(µ2-1H-imidazole-4-carboxylato- κ3N3,O:O')hemi(µ2-oxalato- κ4O1,O2:O1',O2')cadmium(II)] top
Crystal data top
[Cd(C4H3N2O2)(C2O4)0.5(H2O)]F(000) = 548
Mr = 285.51Dx = 2.476 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1557 reflections
a = 10.0259 (12) Åθ = 2.6–27.9°
b = 6.9271 (8) ŵ = 2.84 mm1
c = 13.9278 (12) ÅT = 296 K
β = 127.630 (5)°Block, colourless
V = 766.07 (14) Å30.32 × 0.25 × 0.18 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer
1393 independent reflections
Radiation source: fine-focus sealed tube1298 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ϕ and ω scansθmax = 25.3°, θmin = 2.6°
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2008)
h = 1211
Tmin = 0.395, Tmax = 0.746k = 80
5542 measured reflectionsl = 1610
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-atom parameters constrained
wR(F2) = 0.089 w = 1/[σ2(Fo2) + (0.0409P)2 + 1.2027P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
1393 reflectionsΔρmax = 0.96 e Å3
120 parametersΔρmin = 1.06 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0102 (15)
Crystal data top
[Cd(C4H3N2O2)(C2O4)0.5(H2O)]V = 766.07 (14) Å3
Mr = 285.51Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.0259 (12) ŵ = 2.84 mm1
b = 6.9271 (8) ÅT = 296 K
c = 13.9278 (12) Å0.32 × 0.25 × 0.18 mm
β = 127.630 (5)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
1393 independent reflections
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2008)
1298 reflections with I > 2σ(I)
Tmin = 0.395, Tmax = 0.746Rint = 0.047
5542 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0320 restraints
wR(F2) = 0.089H-atom parameters constrained
S = 1.10Δρmax = 0.96 e Å3
1393 reflectionsΔρmin = 1.06 e Å3
120 parameters
Special details top

Experimental. The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program CELL_NOW, with the two components being related by a 180° rotation around the real/reciprocal axis (1.000 -0.002 -0.999; -0.829 -0.001 1.000). The two components were integrated using SAINT, resulting in a total of 8270 reflections. 3624 reflections (1506 unique) involved component 1 only (mean I/σ = 13.2), 3624 reflections (1500 unique) involved component 2 only (mean I/σ = 10.2), and 1022 reflections (519 unique) involved both components (mean I/σ = 15.6). The exact twin matrix identified by the integration program was found to be (-0.09207 0.00002 -0.90797; 0.00011 -1.00000 -0.00000; -1.09202 -0.00026 0.09207).

The data were corrected for absorption using TWINABS, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the HKLF 5 routine with all reflections of component 1 (including the overlapping ones), resulting in a BASF value of 0.36437.

The Rint value given is for all reflections and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions [TWINABS (Sheldrick, 2007)].

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
Cd10.21993 (5)1.19201 (5)0.67889 (3)0.0306 (2)
O10.2679 (5)0.9359 (6)0.6062 (4)0.0439 (10)
O1W0.0460 (6)0.9916 (7)0.6959 (4)0.0565 (13)
H1W0.01090.92140.63300.085*
H2W0.00070.98040.73080.085*
O20.5273 (5)0.8519 (6)0.7661 (3)0.0388 (9)
O30.0584 (5)1.5365 (6)0.3544 (3)0.0457 (11)
O40.0871 (5)1.2964 (5)0.4834 (3)0.0356 (9)
N10.6074 (6)0.7293 (6)0.6212 (4)0.0295 (10)
N20.4569 (7)0.7345 (7)0.4244 (4)0.0412 (12)
H20.42990.72030.35320.049*
C10.4116 (7)0.8666 (7)0.6536 (5)0.0295 (11)
C20.4506 (7)0.8010 (6)0.5725 (5)0.0266 (11)
C30.3547 (8)0.8032 (7)0.4492 (5)0.0358 (13)
H30.24330.84310.39420.043*
C40.6049 (8)0.6929 (7)0.5275 (6)0.0362 (13)
H40.69580.64390.53310.043*
C50.0078 (6)1.4519 (8)0.4531 (4)0.0314 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0281 (3)0.0337 (3)0.0269 (3)0.00464 (15)0.0152 (2)0.00168 (15)
O10.035 (2)0.049 (2)0.049 (2)0.0032 (19)0.0262 (19)0.015 (2)
O1W0.057 (3)0.066 (3)0.061 (3)0.026 (2)0.044 (3)0.026 (2)
O20.046 (2)0.050 (2)0.031 (2)0.0083 (19)0.029 (2)0.0018 (17)
O30.058 (3)0.048 (2)0.035 (2)0.026 (2)0.030 (2)0.0099 (18)
O40.036 (2)0.037 (2)0.033 (2)0.0107 (16)0.0204 (18)0.0021 (16)
N10.031 (2)0.027 (2)0.037 (2)0.0032 (19)0.024 (2)0.0019 (19)
N20.067 (4)0.036 (3)0.030 (3)0.007 (2)0.034 (3)0.004 (2)
C10.036 (3)0.023 (2)0.036 (3)0.001 (2)0.025 (3)0.004 (2)
C20.029 (3)0.024 (3)0.028 (3)0.002 (2)0.018 (2)0.0022 (19)
C30.039 (3)0.033 (3)0.028 (3)0.003 (2)0.017 (3)0.000 (2)
C40.051 (4)0.030 (3)0.052 (4)0.002 (2)0.043 (3)0.001 (2)
C50.026 (2)0.035 (3)0.030 (3)0.006 (2)0.015 (2)0.002 (2)
Geometric parameters (Å, º) top
Cd1—N1i2.220 (5)O4—C51.249 (6)
Cd1—O12.235 (4)N1—C41.315 (7)
Cd1—O42.298 (4)N1—C21.370 (7)
Cd1—O3ii2.336 (4)N1—Cd1iii2.220 (5)
Cd1—O1W2.351 (4)N2—C41.321 (8)
Cd1—O2i2.422 (4)N2—C31.352 (8)
O1—C11.258 (6)N2—H20.8600
O1W—H1W0.8475C1—C21.474 (7)
O1W—H2W0.8483C2—C31.363 (8)
O2—C11.261 (7)C3—H30.9300
O2—Cd1iii2.422 (4)C4—H40.9300
O3—C51.248 (6)C5—C5ii1.559 (9)
O3—Cd1ii2.336 (4)
N1i—Cd1—O1116.20 (16)C4—N1—C2104.9 (5)
N1i—Cd1—O4153.27 (15)C4—N1—Cd1iii138.6 (4)
O1—Cd1—O480.94 (14)C2—N1—Cd1iii116.3 (3)
N1i—Cd1—O3ii94.05 (15)C4—N2—C3108.8 (5)
O1—Cd1—O3ii149.72 (14)C4—N2—H2125.6
O4—Cd1—O3ii71.41 (12)C3—N2—H2125.6
N1i—Cd1—O1W90.06 (15)O1—C1—O2125.0 (5)
O1—Cd1—O1W87.40 (16)O1—C1—C2118.0 (5)
O4—Cd1—O1W112.09 (16)O2—C1—C2117.0 (5)
O3ii—Cd1—O1W91.65 (17)C3—C2—N1109.9 (5)
N1i—Cd1—O2i71.69 (14)C3—C2—C1130.5 (5)
O1—Cd1—O2i91.91 (15)N1—C2—C1119.6 (5)
O4—Cd1—O2i88.19 (13)N2—C3—C2104.9 (5)
O3ii—Cd1—O2i99.17 (15)N2—C3—H3127.6
O1W—Cd1—O2i159.28 (15)C2—C3—H3127.6
C1—O1—Cd1124.0 (3)N1—C4—N2111.4 (5)
Cd1—O1W—H1W107.9N1—C4—H4124.3
Cd1—O1W—H2W143.3N2—C4—H4124.3
H1W—O1W—H2W106.4O3—C5—O4125.3 (5)
C1—O2—Cd1iii114.9 (3)O3—C5—C5ii117.7 (6)
C5—O3—Cd1ii115.8 (3)O4—C5—C5ii117.0 (6)
C5—O4—Cd1117.5 (3)
N1i—Cd1—O1—C132.5 (5)C4—N1—C2—C1177.1 (4)
O4—Cd1—O1—C1125.9 (4)Cd1iii—N1—C2—C16.1 (6)
O3ii—Cd1—O1—C1149.9 (4)O1—C1—C2—C30.6 (8)
O1W—Cd1—O1—C1121.2 (4)O2—C1—C2—C3178.2 (5)
O2i—Cd1—O1—C138.0 (4)O1—C1—C2—N1178.4 (5)
N1i—Cd1—O4—C553.1 (5)O2—C1—C2—N10.4 (7)
O1—Cd1—O4—C5174.3 (4)C4—N2—C3—C20.4 (6)
O3ii—Cd1—O4—C56.8 (4)N1—C2—C3—N20.9 (6)
O1W—Cd1—O4—C590.9 (4)C1—C2—C3—N2177.0 (5)
O2i—Cd1—O4—C593.5 (4)C2—N1—C4—N20.9 (6)
Cd1—O1—C1—O238.7 (8)Cd1iii—N1—C4—N2174.8 (4)
Cd1—O1—C1—C2139.9 (4)C3—N2—C4—N10.3 (6)
Cd1iii—O2—C1—O1176.3 (4)Cd1ii—O3—C5—O4174.0 (4)
Cd1iii—O2—C1—C25.1 (6)Cd1ii—O3—C5—C5ii6.5 (8)
C4—N1—C2—C31.1 (6)Cd1—O4—C5—O3173.4 (4)
Cd1iii—N1—C2—C3175.7 (3)Cd1—O4—C5—C5ii6.0 (7)
Symmetry codes: (i) x+1, y+1/2, z+3/2; (ii) x, y+3, z+1; (iii) x+1, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O4iv0.851.992.815 (6)163
O1W—H2W···O3v0.852.142.972 (5)167
N2—H2···O2vi0.862.032.760 (6)142
Symmetry codes: (iv) x, y+2, z+1; (v) x, y+5/2, z+1/2; (vi) x, y+3/2, z1/2.

Experimental details

Crystal data
Chemical formula[Cd(C4H3N2O2)(C2O4)0.5(H2O)]
Mr285.51
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)10.0259 (12), 6.9271 (8), 13.9278 (12)
β (°) 127.630 (5)
V3)766.07 (14)
Z4
Radiation typeMo Kα
µ (mm1)2.84
Crystal size (mm)0.32 × 0.25 × 0.18
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(TWINABS; Sheldrick, 2008)
Tmin, Tmax0.395, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
5542, 1393, 1298
Rint0.047
(sin θ/λ)max1)0.600
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.089, 1.10
No. of reflections1393
No. of parameters120
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.96, 1.06

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Cd1—N1i2.220 (5)Cd1—O3ii2.336 (4)
Cd1—O12.235 (4)Cd1—O1W2.351 (4)
Cd1—O42.298 (4)Cd1—O2i2.422 (4)
Symmetry codes: (i) x+1, y+1/2, z+3/2; (ii) x, y+3, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O4iii0.851.992.815 (6)162.9
O1W—H2W···O3iv0.852.142.972 (5)167.3
N2—H2···O2v0.862.032.760 (6)142.2
Symmetry codes: (iii) x, y+2, z+1; (iv) x, y+5/2, z+1/2; (v) x, y+3/2, z1/2.
 

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