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In the title coordination compound, {[Cd(C8H10O4)(C10H14N4)]·0.5H2O}n, the 1,1'-(butane-1,4-di­yl)diimidazole ligand and the cyclo­hexane-1,4-dicarboxyl­ate dianion both function in a bridging mode to link adjacent cadmium(II) centers into a two-dimensional four-connected (4,4) network. The networks are parallel to the (001) plane. Two (4,4) networks are inter­penetrated in an unusual parallel mode. The compound is the first two-dimensional parallel inter­penetrating (4,4) network structure based on a flexible dicarboxyl­ate and a long bidentate N-donor ligand. The inter­penetrating nets are further consolidated by water-carboxyl­ate O-H...O hydro­gen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109002674/sk3286sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270109002674/sk3286Isup2.hkl
Contains datablock I

CCDC reference: 724196

Comment top

The design and synthesis of coordination polymers with infinite two- and three-dimensional networks have been an area of rapid growth in recent years because of the potential of these polymers in various applications, such as catalysis, electrical conductivity, host–guest chemistry and magnetism (Eddaoudi et al., 2001; Moulton et al., 2003). Generally, the topology of a coordination polymer can often be controlled and modified by selecting the coordination geometry preferred by the metal ion and the chemical structure of the organic ligand chosen (Carlucci et al., 2003; Hsu et al., 2008). It is well known that long ligands will lead to larger voids that may result in interpenetrated structures (Yang et al., 2008). Therefore, flexible dicarboxylate and long bidentate N-donor ligands with these characteristics are excellent candidates for the construction of interpenetrating networks (Batten, 2001). The cyclohexane-1,4-dicarboxylate dianion (chdc2-) is an example of a dianion with a flexible conformation (Yang et al., 2007). The H2chdc ligand has three possible conformations: a,a-trans-, e,e-trans-, and e,a-cis-H2chdc. Usually, the e,e-trans form is thermodynamically more stable than the e,a-cis form because of the presence of two equatorial substituents in the latter, and the a,a-trans form is the least stable owing to 1,3-diaxial hindrance. So far, the coordination polymers resulting from adduct formation with a rigid bidentate N-donor ligand, such as, for example, 2,5-bis(4-pyridyl)-1,3,4-oxadiazole, adopt layer structures, as observed for the copper (Du et al., 2005) adduct. On the other hand, flexible bidentate N-donor ligands in place of rigid spacers have been known to yield three-dimensional network structures, particularly if the spacer ligands are both flexible and long (Ockwig et al., 2005). In the present study, 1,1'-(butane-1,4-diyl)diimidazole (bis) assembles with cadmium cyclohexane-1,4-dicarboxylate (chdc2-) to furnish a 1:1 adduct, [Cd(bis)(cis-chdc)].0.5H2O, (I), which exists as an unusual twofold interpenetrating (4,4)-network.

Selected bond lengths and angles for (I) are given in Table 1. As shown in Fig. 1, the asymmetric unit of (I) contains one CdII atom, one cis-chdc2- anion, one bis ligand and half a free water molecule. Each CdII atom lies on a center of symmetry and is six-coordinated in a distorted octahedral environment surrounded by four carboxylate O atoms from two different chdc2- anions and two N atoms from two distinct bis ligands. The average Cd—O and Cd—N distances in (I) (Table 1) are comparable to those observed for [Cd4(1,4-bix)4(bpea)4].4H2O [1,4-bix is 1,4-bis(imidazol-1-ylmethyl)benzene and H2bpea is biphenylethene-4,4'-dicarboxylic acid; Yang et al., 2008]. As depicted in Fig. 2, each CdII center is bridged by the chdc2- dianions and bis ligands to give a two-dimensional four-connected (4,4)-network (Ma, Liu, Liu et al., 2000). The networks are parallel with the (001) plane. The two (4,4)-networks are further interpenetrated in an unusual parallel mode. It should be pointed out that the driving force for the formation of this unusual topology becomes apparent when the structure of (I) is examined in detail. The O1W molecule, as the donor, forms a hydrogen bond with carboxylate atom O3iii [symmetry code: (iii) x + 1, y, z; Table 2]. The O—Hwater···Ocarboxylate hydrogen bonds observed in the network consolidate the interpenetrating nets of (I).

It is noteworthy that the structure of (I) is entirely different from that of the related structure [Mn(bis)(BF4)2] (Duncan et al., 1996). This reported complex is composed of two equivalent, mutually interpenetrating three-dimensional networks. The structure of (I) is also entirely different from that of the related polymer [Zn(bis)1.5(H2O)(SO4)].6H2O (Ma, Liu, Xing et al., 2000). In that structure, the networks are interpenetrated in an inclined mode by symmetry-related, identical networks to give an interlocked three-dimensional structure.

Over the past decade, interpenetrating structures have received much attention in coordination chemistry and materials chemistry because of their importantance in advanced materials (Batten & Robson, 1998). Consequently, many interpenetrating structures have been generated by self-assembly processes. To the best of our knowledge, the reported (4,4)-networks interpenetrated in parallel mode are usually constructed by only one type of ligand. Compound (I) is the first two-dimensional parallel interpenetrating (4,4)-network structure based on flexible dicarboxylate and long bidentate N-donor ligands.

Related literature top

For related literature, see: Batten & Robson (1998); Carlucci et al. (2003); Du et al. (2005); Duncan et al. (1996); Eddaoudi et al. (2001); Hsu et al. (2008); Ma et al. (2000); Moulton et al. (2003); Ockwig et al. (2005); Yang et al. (2007, 2008).

Experimental top

For the synthesis of bis, a mixture of imidazole (3.4 g, 50 mmol) and NaOH (2.0 g, 50 mmol) in dimethyl sulfoxide (10 ml) was stirred at 333 K for 1 h, then 1,4-dichlorobutane (3.2 g, 25 mmol) was added. The mixture was cooled to room temperature after stirring at 333 K for 2 h, then poured into 200 ml of water. A white solid formed immediately, which weighted 3.6 g after drying in air.

For the synthesis of (I), a mixture of CdCl2.2.5H2O (0.114 g, 0.5 mmol), H2chdc (0.086 g, 0.5 mmol) and bis (0.095, 0.5 mmol) was dissolved in 12 ml of distilled water, and then triethylamine was added until the pH value of the system was adjusted to about 5.5. The resulting solution was stirred for about 1 h at room temperature, sealed in a 23 ml Teflon-lined stainless steel autoclave and heated at 425 K for 3 d under autogenous pressure. The reaction system was subsequently cooled slowly to room temperature. Colorless block 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 57% based on CdII).

Refinement top

C-bound H atoms were positioned geometrically (C—H = 0.93 and 0.97 Å) and refined as riding, with Uiso(H) fixed at 1.2Ueq(C). The water H atoms were located in a difference Fourier map and were refined with O—H and H···H distance restraints of 0.82 (3) and 1.36 (3) Å, respectively; their displacement parameters were tied to those of the parent atoms by a factor of 1.5.

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: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. A displacement ellipsoid plot at the 50% probability level; H atoms are drawn as spheres of arbitrary radii. [Symmetry codes: (i) -x + 3, y + 1/2, -z + 3/2; (ii) -x + 1, y - 1/2, -z + 3/2.]
[Figure 2] Fig. 2. A view of the two-dimensional (4,4)-network of (I) [the network is parallel to the (001) plane].
[Figure 3] Fig. 3. A view of the parallel interpenetrating (4,4)-networks of (I) [the networks are parallel to the (001) plane].
Poly[[[µ-1,1'-(butane-1,4-diyl)diimidazole-κ2N:N'](µ-cyclohexane-1,4-dicarboxylato-κ4O1,O1':O4,O4')cadmium(II)] hemihydrate] top
Crystal data top
[Cd(C8H10O4)(C10H14N4)]·0.5H2OF(000) = 980
Mr = 481.82Dx = 1.552 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3999 reflections
a = 9.468 (4) Åθ = 1.1–26.0°
b = 12.339 (5) ŵ = 1.09 mm1
c = 17.817 (8) ÅT = 293 K
β = 97.864 (6)°Block, colorless
V = 2061.8 (15) Å30.25 × 0.21 × 0.18 mm
Z = 4
Data collection top
Bruker APEX
diffractometer
3999 independent reflections
Radiation source: fine-focus sealed tube3391 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ϕ and ω scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1011
Tmin = 0.755, Tmax = 0.821k = 1514
11154 measured reflectionsl = 2116
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0423P)2 + 0.4711P]
where P = (Fo2 + 2Fc2)/3
3999 reflections(Δ/σ)max = 0.001
259 parametersΔρmax = 0.57 e Å3
4 restraintsΔρmin = 0.24 e Å3
Crystal data top
[Cd(C8H10O4)(C10H14N4)]·0.5H2OV = 2061.8 (15) Å3
Mr = 481.82Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.468 (4) ŵ = 1.09 mm1
b = 12.339 (5) ÅT = 293 K
c = 17.817 (8) Å0.25 × 0.21 × 0.18 mm
β = 97.864 (6)°
Data collection top
Bruker APEX
diffractometer
3999 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3391 reflections with I > 2σ(I)
Tmin = 0.755, Tmax = 0.821Rint = 0.026
11154 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0344 restraints
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.57 e Å3
3999 reflectionsΔρmin = 0.24 e Å3
259 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*/UeqOcc. (<1)
C11.1390 (3)0.0285 (3)0.80746 (18)0.0399 (7)
H11.14300.04090.75630.048*
C21.0739 (3)0.0297 (3)0.91085 (18)0.0457 (8)
H21.02420.06590.94480.055*
C31.1876 (4)0.0359 (3)0.93002 (18)0.0458 (8)
H31.22960.05310.97880.055*
C41.3434 (3)0.1493 (3)0.8550 (2)0.0428 (8)
H4A1.33420.17290.80260.051*
H4B1.33290.21260.88610.051*
C51.4916 (3)0.1011 (3)0.87738 (19)0.0400 (7)
H5A1.50300.07930.93020.048*
H5B1.50300.03750.84690.048*
C61.6052 (3)0.1858 (3)0.86523 (19)0.0425 (8)
H6A1.58650.25200.89150.051*
H6B1.59840.20230.81160.051*
C71.7524 (4)0.1480 (3)0.8931 (2)0.0519 (9)
H7A1.77030.08120.86730.062*
H7B1.75920.13220.94680.062*
C81.9233 (4)0.3027 (3)0.9316 (2)0.0529 (9)
H81.90380.31300.98080.064*
C91.9195 (3)0.2421 (3)0.81756 (19)0.0427 (8)
H91.89490.20150.77370.051*
C102.0164 (4)0.3586 (3)0.89630 (19)0.0495 (9)
H102.07370.41480.91780.059*
C110.7527 (3)0.2311 (3)0.87430 (18)0.0404 (8)
C120.6999 (4)0.2971 (3)0.93664 (18)0.0510 (9)
H120.75800.27560.98410.061*
C130.5454 (4)0.2685 (3)0.9449 (2)0.0655 (11)
H13A0.53470.19040.94430.079*
H13B0.52410.29470.99350.079*
C140.4403 (4)0.3172 (3)0.8824 (2)0.0562 (10)
H14A0.34390.29880.89060.067*
H14B0.45650.28720.83400.067*
C150.4566 (4)0.4401 (3)0.88090 (19)0.0468 (8)
H150.44470.46570.93170.056*
C160.3455 (3)0.4993 (3)0.82619 (19)0.0433 (8)
C170.6080 (4)0.4689 (3)0.8693 (2)0.0538 (9)
H17A0.61910.54700.87090.065*
H17B0.62510.44420.81960.065*
C180.7180 (4)0.4180 (3)0.9294 (2)0.0616 (11)
H18A0.81260.43280.91680.074*
H18B0.71080.45170.97790.074*
N11.0436 (3)0.0345 (2)0.83359 (14)0.0391 (6)
N21.2285 (3)0.0718 (2)0.86376 (14)0.0361 (6)
N31.8632 (3)0.2279 (2)0.88104 (15)0.0410 (6)
N42.0147 (3)0.3208 (2)0.82413 (15)0.0402 (6)
O10.8117 (2)0.27688 (18)0.82333 (13)0.0481 (6)
O20.7399 (3)0.13002 (19)0.87639 (16)0.0589 (7)
O1W1.0816 (5)0.3499 (5)0.8937 (2)0.0533 (13)0.50
HW111.119 (7)0.375 (6)0.858 (3)0.080*0.50
HW121.003 (4)0.324 (6)0.875 (3)0.080*0.50
O30.2411 (3)0.4501 (2)0.79178 (14)0.0594 (7)
O40.3583 (3)0.5981 (2)0.81789 (19)0.0782 (10)
Cd10.85413 (2)0.114714 (17)0.763790 (12)0.03428 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0358 (17)0.051 (2)0.0328 (17)0.0069 (14)0.0028 (14)0.0048 (14)
C20.0441 (19)0.055 (2)0.0389 (19)0.0157 (16)0.0077 (15)0.0038 (15)
C30.049 (2)0.053 (2)0.0341 (18)0.0135 (16)0.0009 (15)0.0019 (15)
C40.0351 (18)0.0407 (18)0.051 (2)0.0112 (14)0.0015 (15)0.0062 (15)
C50.0313 (17)0.0393 (18)0.049 (2)0.0052 (13)0.0043 (14)0.0042 (14)
C60.0355 (18)0.0431 (19)0.049 (2)0.0064 (14)0.0059 (15)0.0049 (15)
C70.0382 (19)0.046 (2)0.073 (3)0.0082 (15)0.0099 (17)0.0148 (18)
C80.053 (2)0.066 (2)0.041 (2)0.0147 (18)0.0103 (16)0.0046 (17)
C90.0413 (18)0.0432 (19)0.0434 (19)0.0099 (15)0.0057 (15)0.0089 (15)
C100.048 (2)0.056 (2)0.043 (2)0.0179 (17)0.0012 (16)0.0069 (16)
C110.0317 (17)0.0426 (19)0.0449 (19)0.0128 (14)0.0024 (14)0.0015 (15)
C120.054 (2)0.064 (2)0.0330 (18)0.0278 (18)0.0022 (15)0.0006 (16)
C130.069 (3)0.072 (3)0.060 (2)0.035 (2)0.029 (2)0.025 (2)
C140.038 (2)0.056 (2)0.077 (3)0.0133 (17)0.0176 (18)0.0234 (19)
C150.049 (2)0.049 (2)0.0415 (19)0.0180 (16)0.0002 (15)0.0063 (15)
C160.0372 (18)0.043 (2)0.049 (2)0.0104 (15)0.0020 (15)0.0051 (15)
C170.043 (2)0.039 (2)0.075 (3)0.0078 (15)0.0067 (18)0.0062 (17)
C180.054 (2)0.061 (2)0.064 (2)0.0221 (19)0.0124 (19)0.0210 (19)
N10.0317 (14)0.0458 (16)0.0390 (15)0.0079 (12)0.0018 (11)0.0025 (12)
N20.0288 (13)0.0394 (14)0.0394 (15)0.0079 (11)0.0023 (11)0.0030 (12)
N30.0305 (14)0.0430 (16)0.0503 (17)0.0058 (11)0.0082 (12)0.0053 (12)
N40.0331 (14)0.0445 (16)0.0424 (16)0.0068 (12)0.0032 (11)0.0005 (12)
O10.0574 (15)0.0419 (13)0.0465 (14)0.0014 (11)0.0126 (11)0.0010 (10)
O20.0667 (18)0.0427 (15)0.0729 (18)0.0092 (12)0.0299 (14)0.0045 (12)
O1W0.030 (2)0.093 (4)0.037 (3)0.011 (3)0.008 (2)0.012 (3)
O30.0550 (16)0.0496 (16)0.0669 (17)0.0052 (12)0.0149 (13)0.0098 (12)
O40.0578 (17)0.0391 (16)0.124 (3)0.0078 (12)0.0364 (17)0.0052 (15)
Cd10.02753 (14)0.03359 (14)0.04128 (15)0.00105 (9)0.00314 (9)0.00081 (9)
Geometric parameters (Å, º) top
C1—N11.323 (4)C11—C121.516 (4)
C1—N21.334 (4)C11—Cd12.716 (3)
C1—H10.9300C12—C181.509 (5)
C2—C31.353 (4)C12—C131.531 (5)
C2—N11.369 (4)C12—H120.9800
C2—H20.9300C13—C141.513 (5)
C3—N21.366 (4)C13—H13A0.9700
C3—H30.9300C13—H13B0.9700
C4—N21.473 (4)C14—C151.525 (5)
C4—C51.526 (4)C14—H14A0.9700
C4—H4A0.9700C14—H14B0.9700
C4—H4B0.9700C15—C171.518 (5)
C5—C61.536 (4)C15—C161.520 (4)
C5—H5A0.9700C15—H150.9800
C5—H5B0.9700C16—O41.236 (4)
C6—C71.488 (5)C16—O31.248 (4)
C6—H6A0.9700C16—Cd1i2.709 (3)
C6—H6B0.9700C17—C181.523 (5)
C7—N31.477 (4)C17—H17A0.9700
C7—H7A0.9700C17—H17B0.9700
C7—H7B0.9700C18—H18A0.9700
C8—C101.341 (5)C18—H18B0.9700
C8—N31.359 (4)O1W—HW110.838 (10)
C8—H80.9300O1W—HW120.837 (8)
C9—N41.320 (4)Cd1—N12.265 (2)
C9—N31.326 (4)Cd1—N4ii2.272 (3)
C9—H90.9300Cd1—O12.325 (2)
C10—N41.365 (4)Cd1—O22.414 (3)
C10—H100.9300Cd1—O4iii2.325 (3)
C11—O21.255 (4)Cd1—O3iii2.382 (3)
C11—O11.262 (4)
N1—C1—N2111.4 (3)C13—C14—H14A109.6
N1—C1—H1124.3C15—C14—H14A109.6
N2—C1—H1124.3C13—C14—H14B109.6
C3—C2—N1109.3 (3)C15—C14—H14B109.6
C3—C2—H2125.4H14A—C14—H14B108.1
N1—C2—H2125.4C17—C15—C16112.6 (3)
C2—C3—N2106.6 (3)C17—C15—C14109.6 (3)
C2—C3—H3126.7C16—C15—C14115.3 (3)
N2—C3—H3126.7C17—C15—H15106.3
N2—C4—C5112.7 (3)C16—C15—H15106.3
N2—C4—H4A109.1C14—C15—H15106.3
C5—C4—H4A109.1O4—C16—O3120.4 (3)
N2—C4—H4B109.1O4—C16—C15118.7 (3)
C5—C4—H4B109.1O3—C16—C15120.9 (3)
H4A—C4—H4B107.8O4—C16—Cd1i58.86 (18)
C4—C5—C6109.6 (3)O3—C16—Cd1i61.54 (17)
C4—C5—H5A109.8C15—C16—Cd1i176.1 (2)
C6—C5—H5A109.8C15—C17—C18112.1 (3)
C4—C5—H5B109.8C15—C17—H17A109.2
C6—C5—H5B109.8C18—C17—H17A109.2
H5A—C5—H5B108.2C15—C17—H17B109.2
C7—C6—C5112.4 (3)C18—C17—H17B109.2
C7—C6—H6A109.1H17A—C17—H17B107.9
C5—C6—H6A109.1C12—C18—C17113.1 (3)
C7—C6—H6B109.1C12—C18—H18A109.0
C5—C6—H6B109.1C17—C18—H18A109.0
H6A—C6—H6B107.9C12—C18—H18B109.0
N3—C7—C6113.2 (3)C17—C18—H18B109.0
N3—C7—H7A108.9H18A—C18—H18B107.8
C6—C7—H7A108.9C1—N1—C2105.6 (3)
N3—C7—H7B108.9C1—N1—Cd1126.2 (2)
C6—C7—H7B108.9C2—N1—Cd1127.8 (2)
H7A—C7—H7B107.8C1—N2—C3107.1 (3)
C10—C8—N3106.3 (3)C1—N2—C4125.7 (3)
C10—C8—H8126.8C3—N2—C4127.1 (3)
N3—C8—H8126.8C9—N3—C8107.1 (3)
N4—C9—N3111.8 (3)C9—N3—C7126.1 (3)
N4—C9—H9124.1C8—N3—C7126.8 (3)
N3—C9—H9124.1C9—N4—C10104.7 (3)
C8—C10—N4110.0 (3)C9—N4—Cd1iv128.9 (2)
C8—C10—H10125.0C10—N4—Cd1iv126.3 (2)
N4—C10—H10125.0C11—O1—Cd193.70 (19)
O2—C11—O1121.3 (3)C11—O2—Cd189.8 (2)
O2—C11—C12118.0 (3)HW11—O1W—HW12107 (3)
O1—C11—C12120.6 (3)C16—O3—Cd1i91.0 (2)
O2—C11—Cd162.68 (18)C16—O4—Cd1i94.1 (2)
O1—C11—Cd158.67 (17)N1—Cd1—N4ii93.72 (10)
C12—C11—Cd1178.5 (2)N1—Cd1—O4iii149.02 (9)
C18—C12—C11114.5 (3)N4ii—Cd1—O4iii96.15 (11)
C18—C12—C13110.9 (3)N1—Cd1—O1107.38 (9)
C11—C12—C13111.2 (3)N4ii—Cd1—O199.10 (9)
C18—C12—H12106.5O4iii—Cd1—O199.95 (9)
C11—C12—H12106.5N1—Cd1—O3iii94.69 (9)
C13—C12—H12106.5N4ii—Cd1—O3iii102.91 (10)
C14—C13—C12112.3 (3)O4iii—Cd1—O3iii54.48 (9)
C14—C13—H13A109.2O1—Cd1—O3iii147.59 (9)
C12—C13—H13A109.2N1—Cd1—O289.38 (9)
C14—C13—H13B109.2N4ii—Cd1—O2153.55 (9)
C12—C13—H13B109.2O4iii—Cd1—O294.55 (12)
H13A—C13—H13B107.9O1—Cd1—O255.14 (8)
C13—C14—C15110.4 (3)O3iii—Cd1—O2103.00 (9)
Symmetry codes: (i) x+1, y+1/2, z+3/2; (ii) x+3, y+1/2, z+3/2; (iii) x+1, y1/2, z+3/2; (iv) x+3, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O3v0.84 (1)1.98 (2)2.803 (5)166 (6)
O1W—HW12···O10.84 (1)2.00 (1)2.835 (5)173 (6)
Symmetry code: (v) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Cd(C8H10O4)(C10H14N4)]·0.5H2O
Mr481.82
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)9.468 (4), 12.339 (5), 17.817 (8)
β (°) 97.864 (6)
V3)2061.8 (15)
Z4
Radiation typeMo Kα
µ (mm1)1.09
Crystal size (mm)0.25 × 0.21 × 0.18
Data collection
DiffractometerBruker APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.755, 0.821
No. of measured, independent and
observed [I > 2σ(I)] reflections
11154, 3999, 3391
Rint0.026
(sin θ/λ)max1)0.616
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.081, 1.04
No. of reflections3999
No. of parameters259
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.57, 0.24

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008)), publCIF (Westrip, 2009).

Selected geometric parameters (Å, º) top
Cd1—N12.265 (2)Cd1—O22.414 (3)
Cd1—N4i2.272 (3)Cd1—O4ii2.325 (3)
Cd1—O12.325 (2)Cd1—O3ii2.382 (3)
N1—Cd1—N4i93.72 (10)O4ii—Cd1—O3ii54.48 (9)
N1—Cd1—O4ii149.02 (9)O1—Cd1—O3ii147.59 (9)
N4i—Cd1—O4ii96.15 (11)N1—Cd1—O289.38 (9)
N1—Cd1—O1107.38 (9)N4i—Cd1—O2153.55 (9)
N4i—Cd1—O199.10 (9)O4ii—Cd1—O294.55 (12)
O4ii—Cd1—O199.95 (9)O1—Cd1—O255.14 (8)
N1—Cd1—O3ii94.69 (9)O3ii—Cd1—O2103.00 (9)
N4i—Cd1—O3ii102.91 (10)
Symmetry codes: (i) x+3, y+1/2, z+3/2; (ii) x+1, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O3iii0.838 (10)1.982 (18)2.803 (5)166 (6)
O1W—HW12···O10.837 (8)2.001 (9)2.835 (5)173 (6)
Symmetry code: (iii) x+1, y, z.
 

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