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In the title compound, [Cd(C8H4O4)(C10H8N2O2)(H2O)]n, (I), each CdII atom is seven-coordinated in a distorted monocapped trigonal prismatic coordination geometry, sur­rounded by four carboxyl­ate O atoms from two different benzene-1,4-dicarboxyl­ate (1,4-bdc) anions, two O atoms from two distinct 4,4'-bipyridine N,N'-dioxide (bpdo) ligands and one water O atom. The CdII atom and the water O atom are on a twofold rotation axis. The bpdo and 1,4-bdc ligands are on centers of inversion. Each crystallographically unique CdII center is bridged by the 1,4-bdc dianions and bpdo ligands to give a three-dimensional diamond framework containing large adamantanoid cages. Three identical such nets are inter­locked with each other, thus directly leading to the formation of a threefold inter­penetrated three-dimensional diamond architecture. To the best of our knowledge, (I) is the first example of a threefold inter­penetrating diamond net based on both bpdo and carboxyl­ate ligands. There are strong linear O-H...O hydrogen bonds between the water mol­ecules and carboxyl­ate O atoms within different diamond nets. Each diamond net is hydrogen bonded to its two neighbors through these hydrogen bonds, which further consolidates the threefold inter­penetrating diamond framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110023553/sq3245sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110023553/sq3245Isup2.hkl
Contains datablock I

CCDC reference: 790626

Comment top

The synthesis of metal–organic frameworks (MOFs) has attracted great attention, not only for their tremendous potential applications in nonlinear optics, catalysis, gas absorption, luminescence, magnetism, ion exchange and zeolite-like materials for molecular selection, but also for their intriguing variety of architectures and topologies (Abrahams et al., 1999; Noro et al., 2000; Spencer et al., 2006). The topologies of the MOFs 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. It is well known that careful selection of a suitable organic ligand with certain features is helpful for constructing MOFs with desirable properties (Wang et al., 2006). Recently, it has been demonstrated that 4,4'-bipyridine N,N'-dioxide (bpdo) and its derivatives show some unique features in the construction of MOFs (Hill et al., 2005; Manna et al., 2007) and have been shown to have extremely versatile coordination modes compared with 4,4'-bipyridine and its derivatives (Xu et al., 2005). So far, a number of MOFs based on bpdo ligands have been reported, including one-dimensional chain or ladder, two-dimensional layer, and unusual five-, six-, seven- and eight-connected frameworks (Hill et al., 2005). However, only a few MOFs based on both bpdo and carboxylate ligands have been documented (Manna et al., 2006, 2007; Fabelo et al., 2007). In the new material reported here, bpdo assembles with cadmium 1,4-benzenedicarboxylate (1,4-bdc) to furnish a 1:1 adduct, [Cd(bpdo)(1,4-bdc)(H2O)]n, (I), which exists as an unusual threefold interpenetrating diamond framework.

The asymmetric unit of (I) contains half a CdII atom, half a bpdo ligand, half a 1,4-bdc anion and half a coordination water molecule (Fig. 1). The CdII atom and the water O atom rest on a twofold rotation axis. The bpdo and 1,4-bdc ligands are on centers of inversion that occur at the midpoint of the C7—C7ii [symmetry code: (ii) -x, -y, -z] bond of bpdo and the centroid of the arene ring of 1,4-bdc. Each CdII atom is seven-coordinated in a distorted monocapped, trigonal prism[atic?] coordination geometry, surrounded by four carboxylate O atoms from two different 1,4-bdc anions (O2, O3, O2iii and O3iii) [symmetry code: (iii) 1-x, y, 1/2-z], two O atoms from two distinct bpdo ligands (O1 and O1iii) and one water O atom (OW1). The Cd—Ocarboxylate distances (Table 1) are comparable to those observed for [Cd4(1,4-bix)4(bpea)4].4H2O [1,4-bix = 1,4-bis(imidazol-1-ylmethyl)benzene; H2bpea = biphenylethene-4,4'-dicarboxylic acid] (Yang et al., 2008). Each crystallographically unique CdII center is bridged by the 1,4-bdc dianions and bpdo ligands to give a three-dimensional framework (Fig. 2). A better insight into the structure of (I) can be achieved by the application of a topological approach, that is, reducing multidimensional structures to simple node-and-linker nets (Batten & Robson, 1998). According to the simplification principle, the CdII center is defined as a four-connected node, while the 1,4-bdc and bpdo ligands serve as linkers. Therefore, on the basis of this concept of chemical topology, the overall structure is a diamond framework containing large adamantanoid cages (Fig. 2). As can be seen, each distorted rectangular ring has six CdII centers, leading to the formation of a hexagon which is the shortest circuit here. In the adamantanoid cage, the Cd···Cd distances bridged by bpdo and 1,4-bdc are 12.624 (5) and 11.245 (4) Å, respectively.

It is well known that diamond networks tend to interpenetrate to fill the voids within a single net. Of particular interest, the most striking feature of (I) is that three identical three-dimensional single nets are interlocked with each other, thus directly leading to the formation of a threefold interpenetrated three-dimensional diamond architecture (Fig. 3). In addition, there are strong linear O—H···O hydrogen bonds between the water molecules and carboxylate O atoms within different diamond nets (Fig. 3). Each diamond net is hydrogen bonded to its two neighbors through these hydrogen bonds, which further consolidates the threefold interpenetrating diamond framework (Table 2). Although many diamond-related nets displaying various interpenetration modes ranging from twofold to 11-fold have been reported, threefold interpenetrating MOFs in the presence of mixed organic ligands with different lengths is relatively rare (Batten, 2001; O'Keeffe et al., 2008; Carlucci et al., 2003). So far, only a few threefold interpenetrating MOFs, including Co(D-cam)(TMDPy).2H2O (D-H2Cam = D-camphoric acid; TMDPy = 4,4'-trimethylenedipyridine) (Zhang et al., 2008), [Cu2(bpy)2(Hbpy)(H2O)](PW12O40) (bpy = 4,4'-bipyridine) (Yang et al., 2009), [Tb(bpdo)(CH3OH)(NO3)3] (Long et al., 2002) and Cu(3,4'-bpdc)(H2O).DMF.2H2O (3,4'-bpdc = 3,4'-biphenyldicarboxylic acid; DMF = dimethylformamide) (Feng et al., 2009), have been reported. The structure of (I) is entirely different from that of the related structure [Cu2(bpy)2(Hbpy)(H2O)](PW12O40), which shows an unprecedented threefold interpenetrating diamond-like network in polyoxometallate chemistry. The structure of (I) is also different from those of the polymers [Tb(bpdo)(CH3OH)(NO3)3] and [Cu(3,4'-bpdc)(H2O)].DMF.2H2O, whose threefold interpenetrating diamond nets only contain single organic ligands. In particular, [Tb(bpdo)(CH3OH)(NO3)3] adopts a zigzag chain structure, which forms threefold interpenetrating diamond frameworks through interchain hydrogen bonding between coordinated methanol and a nitrate group on an adjacent chain. Notably, although the reported compound Co(D-cam)(TMDPy).2H2O is constructed by mixed organic ligands, it exhibits a homochiral threefold interpenetrating diamond topology. Notably, there are only a few previously reported examples of MOFs based on bpdo–carboxylate mixed ligand systems (Manna et al., 2006, 2007; Fabelo et al., 2007). The related compounds [Co(H2O)6](H2bta).bpdo.4H2O and [{Co2(H2O)4(bpdo)}2(bta)].4H2O are discrete molecular complexes (H4bta = 1,2,4,5-benzenetetracarboxylic acid) (Fabelo et al., 2007). The structure of [Co(H2O)2)(bpdo)2(H2bta)]n is constituted by uniform chains of CoII ions bridged by the deprotonated H2bta2- species (Fabelo et al., 2007). The related compounds [Co(H2O)3(bpdo)(bta)1/2]n, {[Co(bpdo)(ox)]}n and [Mn(ox)(bpdo)]n display two-dimensional layer structures (ox = oxalate dianion) (Manna et al., 2006, 2007; Fabelo et al., 2007).

Related literature top

For related literature, see: Abrahams et al. (1999); Batten (2001); Batten & Robson (1998); Carlucci et al. (2003); Fabelo et al. (2007); Feng et al. (2009); Hill et al. (2005); Long et al. (2002); Manna et al. (2006, 2007); Noro et al. (2000); Spencer et al. (2006); Wang et al. (2006); Xu et al. (2005); Yang et al. (2008, 2009); Zhang et al. (2008).

Experimental top

A mixture of CdCl2.2.5H2O (0.5 mmol), 1,4-H2bdc (0.5 mmol) and bpdo (0.5 mmol) was dissolved in 10 ml N,N-dimethylformamide. 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 393 K for 1 d under autogenous pressure. Afterwards, the reaction system was slowly cooled to room temperature. 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: 38% based on CdII.

Refinement top

Carbon-bound H atoms were positioned geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H) fixed at 1.2Ueq(C). The water H atom was located in a difference Fourier map and refined freely.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART (Bruker, 1997); 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. A view of the local coordination of the CdII atom in (I), showing the atom-numbering scheme. Displacement ellipsoids are at the 30% probability level. Symmetry codes: (i) 1/2-x, 1/2-y, 1/2-z; (ii) -x, -y, -z; (iii) 1-x, y, 1/2-z.
[Figure 2] Fig. 2. A view of the diamond framework of (I) (the central CdII atom and its four neighbors are shown in pink).
[Figure 3] Fig. 3. A view of the threefold interpenetrating three-dimensional diamond net of (I) (the hydrogen-bonding interactions are shown as dashed lines).
Poly[aqua(µ2-benzene-1,4-dicarboxylato)(µ2-4,4'-bipyridine N,N'-dioxide)cadmium(II)] top
Crystal data top
[Cd(C8H4O4)(C10H8N2O2)(H2O)]F(000) = 960
Mr = 482.71Dx = 1.905 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1658 reflections
a = 14.1052 (15) Åθ = 2.2–26.0°
b = 16.8934 (18) ŵ = 1.35 mm1
c = 8.8967 (10) ÅT = 293 K
β = 127.451 (1)°Block, colorless
V = 1683.0 (3) Å30.22 × 0.18 × 0.15 mm
Z = 4
Data collection top
Bruker APEX
diffractometer
1658 independent reflections
Radiation source: fine-focus sealed tube1623 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.064
ϕ and ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1716
Tmin = 0.64, Tmax = 0.85k = 1420
4629 measured reflectionsl = 1010
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0426P)2 + 2.0359P]
where P = (Fo2 + 2Fc2)/3
1658 reflections(Δ/σ)max < 0.001
132 parametersΔρmax = 1.07 e Å3
0 restraintsΔρmin = 0.83 e Å3
Crystal data top
[Cd(C8H4O4)(C10H8N2O2)(H2O)]V = 1683.0 (3) Å3
Mr = 482.71Z = 4
Monoclinic, C2/cMo Kα radiation
a = 14.1052 (15) ŵ = 1.35 mm1
b = 16.8934 (18) ÅT = 293 K
c = 8.8967 (10) Å0.22 × 0.18 × 0.15 mm
β = 127.451 (1)°
Data collection top
Bruker APEX
diffractometer
1658 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
1623 reflections with I > 2σ(I)
Tmin = 0.64, Tmax = 0.85Rint = 0.064
4629 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0270 restraints
wR(F2) = 0.073H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 1.07 e Å3
1658 reflectionsΔρmin = 0.83 e Å3
132 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 > 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
Cd10.50000.121775 (12)0.25000.01900 (12)
C10.3978 (2)0.18005 (16)0.4098 (3)0.0234 (5)
C20.3230 (2)0.21612 (15)0.4602 (3)0.0222 (5)
C30.3294 (2)0.19039 (16)0.6140 (3)0.0253 (5)
H30.38270.15040.69120.030*
C40.2426 (2)0.27640 (15)0.3458 (4)0.0263 (5)
H40.23760.29430.24230.032*
C50.1481 (3)0.12819 (17)0.0186 (4)0.0351 (7)
H50.15470.18270.02480.042*
C60.0601 (3)0.09790 (19)0.0114 (4)0.0333 (6)
H60.00840.13240.01220.040*
C70.0473 (2)0.01719 (18)0.0029 (4)0.0337 (6)
C80.1276 (3)0.0311 (2)0.0051 (6)0.0573 (11)
H80.12210.08580.00130.069*
C90.2140 (3)0.0007 (2)0.0128 (6)0.0509 (9)
H90.26570.03240.01530.061*
N10.22446 (19)0.07991 (16)0.0167 (3)0.0333 (6)
O10.30712 (19)0.10944 (14)0.0268 (3)0.0391 (5)
O20.4223 (2)0.22237 (12)0.3220 (3)0.0371 (5)
O30.42876 (19)0.10875 (11)0.4489 (3)0.0266 (4)
O1W0.50000.01188 (16)0.25000.0286 (6)
H1W0.514 (3)0.042 (2)0.333 (5)0.038 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01784 (17)0.01890 (17)0.02478 (17)0.0000.01530 (13)0.000
C10.0221 (12)0.0289 (14)0.0234 (11)0.0016 (10)0.0161 (10)0.0009 (10)
C20.0227 (12)0.0223 (12)0.0266 (11)0.0010 (9)0.0176 (10)0.0001 (9)
C30.0276 (13)0.0241 (12)0.0263 (12)0.0079 (10)0.0175 (11)0.0070 (9)
C40.0319 (14)0.0270 (13)0.0266 (11)0.0071 (11)0.0211 (11)0.0068 (10)
C50.0331 (17)0.0380 (17)0.0298 (14)0.0069 (12)0.0168 (13)0.0043 (10)
C60.0322 (15)0.0350 (15)0.0316 (13)0.0043 (13)0.0188 (12)0.0013 (12)
C70.0181 (12)0.0369 (15)0.0314 (13)0.0011 (11)0.0074 (10)0.0115 (11)
C80.0265 (15)0.0362 (18)0.097 (3)0.0083 (13)0.0313 (18)0.0257 (19)
C90.0226 (15)0.0416 (18)0.078 (2)0.0071 (13)0.0252 (16)0.0180 (16)
N10.0160 (11)0.0467 (15)0.0248 (10)0.0034 (10)0.0059 (9)0.0129 (10)
O10.0199 (10)0.0576 (14)0.0315 (10)0.0032 (9)0.0113 (9)0.0189 (9)
O20.0497 (12)0.0322 (11)0.0560 (12)0.0098 (9)0.0461 (11)0.0109 (9)
O30.0307 (11)0.0267 (9)0.0299 (9)0.0079 (8)0.0223 (9)0.0035 (7)
O1W0.0365 (15)0.0211 (13)0.0236 (12)0.0000.0159 (12)0.000
Geometric parameters (Å, º) top
Cd1—O1W2.258 (3)C4—H40.9300
Cd1—O22.314 (2)C5—N11.342 (4)
Cd1—O2i2.314 (2)C5—C61.381 (5)
Cd1—O1i2.316 (2)C5—H50.9300
Cd1—O12.316 (2)C6—C71.383 (4)
Cd1—O3i2.520 (2)C6—H60.9300
Cd1—O32.520 (2)C7—C81.406 (5)
C1—O21.253 (3)C7—C7iii1.484 (6)
C1—O31.256 (3)C8—C91.371 (5)
C1—C21.503 (3)C8—H80.9300
C2—C31.386 (3)C9—N11.348 (4)
C2—C41.398 (4)C9—H90.9300
C3—C4ii1.385 (4)N1—O11.321 (3)
C3—H30.9300O1W—H1W0.81 (3)
C4—C3ii1.385 (4)
O1W—Cd1—O2137.26 (5)C4—C2—C1118.9 (2)
O1W—Cd1—O2i137.26 (5)C4ii—C3—C2120.7 (2)
O2—Cd1—O2i85.48 (10)C4ii—C3—H3119.7
O1W—Cd1—O1i84.84 (6)C2—C3—H3119.7
O2—Cd1—O1i102.69 (8)C3ii—C4—C2120.3 (2)
O2i—Cd1—O1i84.98 (9)C3ii—C4—H4119.8
O1W—Cd1—O184.84 (6)C2—C4—H4119.8
O2—Cd1—O184.98 (9)N1—C5—C6120.8 (3)
O2i—Cd1—O1102.69 (8)N1—C5—H5119.6
O1i—Cd1—O1169.67 (12)C6—C5—H5119.6
O1W—Cd1—O3i84.99 (4)C5—C6—C7121.2 (3)
O2—Cd1—O3i135.79 (7)C5—C6—H6119.4
O2i—Cd1—O3i53.95 (6)C7—C6—H6119.4
O1i—Cd1—O3i91.53 (8)C6—C7—C8116.0 (3)
O1—Cd1—O3i87.57 (8)C6—C7—C7iii122.5 (4)
O1W—Cd1—O384.99 (4)C8—C7—C7iii121.5 (4)
O2—Cd1—O353.95 (6)C9—C8—C7121.4 (3)
O2i—Cd1—O3135.79 (7)C9—C8—H8119.3
O1i—Cd1—O387.57 (8)C7—C8—H8119.3
O1—Cd1—O391.53 (8)N1—C9—C8120.3 (3)
O3i—Cd1—O3169.98 (9)N1—C9—H9119.8
O2—C1—O3122.5 (2)C8—C9—H9119.8
O2—C1—C2117.7 (2)O1—N1—C5120.3 (3)
O3—C1—C2119.7 (2)O1—N1—C9119.4 (3)
O2—C1—Cd156.74 (13)C5—N1—C9120.2 (3)
O3—C1—Cd166.17 (14)N1—O1—Cd1118.44 (15)
C2—C1—Cd1169.34 (17)C1—O2—Cd196.34 (16)
C3—C2—C4119.0 (2)C1—O3—Cd186.71 (15)
C3—C2—C1122.1 (2)Cd1—O1W—H1W128 (2)
O1W—Cd1—C1—O2169.19 (15)C6—C7—C8—C90.8 (5)
O2i—Cd1—C1—O216.1 (2)C7iii—C7—C8—C9179.2 (4)
O1i—Cd1—C1—O2103.54 (17)C7—C8—C9—N10.6 (6)
O1—Cd1—C1—O286.15 (17)C6—C5—N1—O1178.8 (3)
O3i—Cd1—C1—O216.1 (3)C6—C5—N1—C91.8 (4)
O3—Cd1—C1—O2173.2 (3)C8—C9—N1—O1179.0 (3)
C1i—Cd1—C1—O210.81 (15)C8—C9—N1—C51.9 (5)
O1W—Cd1—C1—O317.57 (16)C5—N1—O1—Cd1100.1 (2)
O2—Cd1—C1—O3173.2 (3)C9—N1—O1—Cd182.8 (3)
O2i—Cd1—C1—O3157.19 (15)O1W—Cd1—O1—N167.5 (2)
O1i—Cd1—C1—O369.70 (16)O2—Cd1—O1—N170.9 (2)
O1—Cd1—C1—O3100.61 (15)O2i—Cd1—O1—N1155.1 (2)
O3i—Cd1—C1—O3170.69 (12)O1i—Cd1—O1—N167.5 (2)
C1i—Cd1—C1—O3162.43 (16)O3i—Cd1—O1—N1152.7 (2)
O1W—Cd1—C1—C2108.1 (10)O3—Cd1—O1—N117.3 (2)
O2—Cd1—C1—C261.0 (10)C1i—Cd1—O1—N1178.1 (2)
O2i—Cd1—C1—C277.1 (10)C1—Cd1—O1—N143.9 (2)
O1i—Cd1—C1—C2164.6 (10)O3—C1—O2—Cd17.3 (3)
O1—Cd1—C1—C225.1 (10)C2—C1—O2—Cd1169.47 (18)
O3i—Cd1—C1—C245.0 (11)O1W—Cd1—O2—C115.0 (2)
O3—Cd1—C1—C2125.7 (10)O2i—Cd1—O2—C1165.0 (2)
C1i—Cd1—C1—C271.9 (10)O1i—Cd1—O2—C181.23 (18)
O2—C1—C2—C3153.5 (3)O1—Cd1—O2—C191.77 (17)
O3—C1—C2—C329.6 (4)O3i—Cd1—O2—C1173.06 (14)
Cd1—C1—C2—C3150.8 (9)O3—Cd1—O2—C13.81 (15)
O2—C1—C2—C427.9 (4)C1i—Cd1—O2—C1172.26 (11)
O3—C1—C2—C4149.0 (3)O2—C1—O3—Cd16.7 (3)
Cd1—C1—C2—C427.8 (11)C2—C1—O3—Cd1170.0 (2)
C4—C2—C3—C4ii0.1 (4)O1W—Cd1—O3—C1163.56 (15)
C1—C2—C3—C4ii178.5 (2)O2—Cd1—O3—C13.78 (14)
C3—C2—C4—C3ii0.1 (4)O2i—Cd1—O3—C131.16 (19)
C1—C2—C4—C3ii178.6 (2)O1i—Cd1—O3—C1111.42 (16)
N1—C5—C6—C70.3 (4)O1—Cd1—O3—C178.88 (16)
C5—C6—C7—C80.9 (4)O3i—Cd1—O3—C1163.56 (15)
C5—C6—C7—C7iii179.4 (3)C1i—Cd1—O3—C141.5 (4)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x+1/2, y+1/2, z+1; (iii) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3iv0.81 (3)1.95 (3)2.755 (2)172 (4)
Symmetry code: (iv) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[Cd(C8H4O4)(C10H8N2O2)(H2O)]
Mr482.71
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)14.1052 (15), 16.8934 (18), 8.8967 (10)
β (°) 127.451 (1)
V3)1683.0 (3)
Z4
Radiation typeMo Kα
µ (mm1)1.35
Crystal size (mm)0.22 × 0.18 × 0.15
Data collection
DiffractometerBruker APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.64, 0.85
No. of measured, independent and
observed [I > 2σ(I)] reflections
4629, 1658, 1623
Rint0.064
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.073, 1.07
No. of reflections1658
No. of parameters132
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.07, 0.83

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

Selected geometric parameters (Å, º) top
Cd1—O1W2.258 (3)Cd1—O12.316 (2)
Cd1—O22.314 (2)Cd1—O32.520 (2)
O1W—Cd1—O2137.26 (5)O1W—Cd1—O384.99 (4)
O2—Cd1—O2i85.48 (10)O2—Cd1—O353.95 (6)
O1W—Cd1—O184.84 (6)O2i—Cd1—O3135.79 (7)
O2—Cd1—O184.98 (9)O1i—Cd1—O387.57 (8)
O2i—Cd1—O1102.69 (8)O1—Cd1—O391.53 (8)
O1i—Cd1—O1169.67 (12)O3i—Cd1—O3169.98 (9)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3ii0.81 (3)1.95 (3)2.755 (2)172 (4)
Symmetry code: (ii) x+1, y, z+1.
 

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