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The asymmetric unit of the title compound, [Cd(C8H4O4)(C17H8ClN5)(H2O)]n, contains one CdII atom, two half ben­zene-1,4-dicarboxyl­ate (1,4-bdc) anions, one 11-chloro­py­rido[2',3':2,3]pyrimidino[5,6-f][1,10]phenanthroline (L) ligand and one coordination water mol­ecule. The 1,4-bdc ligands are on inversion centers at the centroids of the arene rings. The CdII atom is six-coordinated by two N atoms from one L ligand, three carboxyl­ate O atoms from two different 1,4-bdc ligands and one water O atom in a distorted octa­hedral coordination sphere. Each CdII center is bridged by the 1,4-bdc dianions to give a one-dimensional chain. [pi]-[pi] stacking inter­actions between L ligands of neighboring chains extend adjacent chains into a two-dimensional supra­molecular (6,3) network. Neighboring (6,3) networks are inter­penetrated in an unusual inclined mode, resulting in a three-dimensional framework. Additionally, the water-carboxyl­ate O-H...O hydrogen bonds observed in the network consolidate the inter­penetrating nets.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109045235/sq3222sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270109045235/sq3222Isup2.hkl
Contains datablock I

CCDC reference: 763587

Comment top

The current interest in polymeric coordination networks is growing rapidly not only because of their potential applications in host–guest chemistry, ion exchange, gas storage and nonlinear optics, but also because of the intriguing variety of topologies (Batten & Robson, 1998; Yang et al., 2008). Structural diversity in coordination polymers can occur as a result of various processes, including supramolecular isomerism, interpenetration or interweaving (Eddaoudi et al., 2001; Carlucci et al., 2003). Among these, entangled systems have attracted rapidly increasing interest not only because of their potential applications as functional solid materials, but also because of their intriguing architectures and topologies (Batten, 2001). Interpenetrating networks, as an important subject in the area of entanglement, have provided a long-standing fascination for chemists (Ockwig et al., 2005). These species can be regarded as infinite, ordered polycatenanes or polyrotaxanes, and are characterized by the presence of two or more independent networks that are inextricably entangled through the rings belonging to one framework. So far, a variety of appealing interpenetrated frameworks have been constructed and discussed in several excellent reviews (Batten & Robson, 1998; Batten, 2001; Carlucci et al., 2003). Among the known interpenetrating coordination polymers with (6,3) networks, parallel interpenetration is the most common arrangement (Carlucci et al., 2003). By contrast, inclined interpenetrating (6,3) networks are relatively scarce in coordination polymers, especially the ones constructed by ππ interactions (Carlucci et al., 2003).

Up to now, 1,10-phenanthroline (phen) and its derivatives have been widely used to build supramolecular architectures because of their excellent coordinating ability; the resulting large conjugated system can easily form ππ interactions (Wang et al., 2008; Qiao et al., 2008; Yang et al., 2007). However, to the best of our knowledge, coordination polymers based on its derivative 11-chloropyrido[2',3':2,3]pyrimidino[5,6-f][1,10]phenanthroline (L), have not been reported. In this study, we selected the benzene-1,4-dicarboxylate dianion (1,4-bdc) as an organic linker and L as a N-donor chelating ligand, generating a new inclined interpenetrating three-dimensional coordination polymer, [Cd(1,4-bdc)(L)(H2O)]n, (I).

The asymmetric unit of (I) contains one CdII atom, two half 1,4-bdc anions, one L ligand and one coordination water molecule (Fig. 1). The two independent 1,4-bdc ligands are on inversion centers located at the centroids of the arene rings. Each CdII atom is six-coordinated by two N atoms from one L ligand, three carboxylate O atoms from two different 1,4-bdc ligands and one water O atom in a distored octahedral coordination sphere. The average Cd—O and Cd—N distances in (I) (Table 1) are comparable to those observed for [Cd(1,4-ndc)(L')]n (1,4-ndc = naphthalene-1,4-dicarboxylate and L' = pyrazino[2,3-f][1,10]phenanthroline) (Qiao et al., 2008). Each CdII center is bridged by the 1,4-bdc dianions to give a one-dimensional chain running approximately along the a axis (Fig. 2). Notably, the L ligands are arranged in a parallel fashion on both sides of the chain, leading to a structure suitable to form aromatic intercalation. The ππ stacking interactions between L ligands of neighboring chains [centroid–centroid distance 3.52 (3) and face-to-face distance 3.45 (4) Å] extend the adjacent chains into a two-dimensional supramolecular network (Fig. 3). If L and the ππ stacking interaction are considered as linkers, and the CdII atom is taken as a three-connected node, the two-dimensional supramolecular network can be classified as a three-connected (6,3) topology. Interestingly, the neighboring (6,3) networks are interpenetrated in an unusual inclined mode, resulting in a three-dimensional framework (Fig. 4). The manner of interpenetration is such that the smallest hexagonal circuit of each sheet has parts of two other sheets passing through it (Fig. 4). To the best of our knowledge, complex (I) is among only a few compounds having such inclined interpenetrating topology. Similar modes have so far only been reported in the structures of [Zn(bib)1.5(H2O)(SO4)].6H2O [bib = 1,1'-(1,4-butanediyl)bis(imidazole)] (Ma et al., 2000) and [Ag2(H2bpd)3.(cucurbituril)3](NO3)8.40H2O [bpd = N,N'-bis(4-pyridylmethyl)-1,4-diaminobutane] (Whang & Kim, 1997). Additionally, the O1W molecule, as the donor, forms hydrogen bonds with carboxylate O atoms (Table 2). The O–Hwater···Ocarboxylate hydrogen bonds observed in the network consolidate the interpenetrating nets of (I).

Notably, when the similar phen derivative L' was used to react with CdII atoms in the presence of 1,4-ndc, a structurally different three-dimensional α-polonium structure [Cd(1,4-ndc)(L')]n was obtained (Qiao et al., 2008). The topological difference between (I) and the reported material is mainly attributed to the structural difference of the dicarboxylates.

Related literature top

For related literature, see: Batten (2001); Batten & Robson (1998); Carlucci et al. (2003); Eddaoudi et al. (2001); Ockwig et al. (2005); Qiao et al. (2008); Wang et al. (2008); Yang et al. (2007, 2008).

Experimental top

A mixture of CdCl2.2.5H2O (0.5 mmol), 1,4-H2bdc (0.5 mmol) and L (0.5 mmol) was dissolved in 12 ml distilled water, followed by addition of triethylamine until the pH of the system was adjusted to about 5.6. 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 428 K for 5 d under autogenous pressure. Afterward, the reaction system was slowly cooled to room temperature. Pale-yellow 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: 46% 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 atoms were located in a difference Fourier map, and were refined freely.

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 view of the local coordination of the CdII cation in (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level (arbitrary spheres for the H atoms). [Symmetry codes: (i) 1 - x, 1 - y, -z; (ii) 2 - x, -y, -z.]
[Figure 2] Fig. 2. A view of the one-dimensional chain of (I).
[Figure 3] Fig. 3. A view of the two-dimensional (6,3) network structure of (I).
[Figure 4] Fig. 4. A view of the inclined interpenetrating (6,3) network structure of (I).
catena-Poly[[aqua(11-chloropyrido[2',3':2,3]pyrimidino[5,6- f][1,10]peneanthroline-κ2N4,N5)cadmium(II)]- µ-benzene-1,4-dicarboxylato-κ3O1,O1':O4] top
Crystal data top
[Cd(C17H8ClN5)(C8H4O4)(H2O)]F(000) = 1216
Mr = 612.26Dx = 1.774 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5256 reflections
a = 10.412 (3) Åθ = 3.0–28.7°
b = 14.466 (3) ŵ = 1.12 mm1
c = 15.411 (4) ÅT = 293 K
β = 98.956 (2)°Block, pale yellow
V = 2292.9 (10) Å30.32 × 0.27 × 0.22 mm
Z = 4
Data collection top
Bruker APEX
diffractometer
5256 independent reflections
Radiation source: fine-focus sealed tube3492 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ϕ and ω scansθmax = 28.7°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1314
Tmin = 0.752, Tmax = 0.891k = 1816
18357 measured reflectionsl = 2019
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 0.89 w = 1/[σ2(Fo2) + (0.0325P)2]
where P = (Fo2 + 2Fc2)/3
5256 reflections(Δ/σ)max = 0.001
342 parametersΔρmax = 1.42 e Å3
0 restraintsΔρmin = 0.65 e Å3
Crystal data top
[Cd(C17H8ClN5)(C8H4O4)(H2O)]V = 2292.9 (10) Å3
Mr = 612.26Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.412 (3) ŵ = 1.12 mm1
b = 14.466 (3) ÅT = 293 K
c = 15.411 (4) Å0.32 × 0.27 × 0.22 mm
β = 98.956 (2)°
Data collection top
Bruker APEX
diffractometer
5256 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3492 reflections with I > 2σ(I)
Tmin = 0.752, Tmax = 0.891Rint = 0.042
18357 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0320 restraints
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 0.89Δρmax = 1.42 e Å3
5256 reflectionsΔρmin = 0.65 e Å3
342 parameters
Special details top

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
C10.5543 (3)0.0914 (2)0.17001 (19)0.0372 (8)
H10.52750.09130.10960.045*
C20.5807 (3)0.1754 (2)0.2120 (2)0.0416 (8)
H20.57460.23010.17990.050*
C30.6160 (3)0.1768 (2)0.30183 (19)0.0366 (8)
H30.63410.23240.33140.044*
C40.6243 (3)0.09378 (19)0.34742 (18)0.0267 (6)
C50.5995 (3)0.01158 (19)0.30052 (17)0.0251 (6)
C60.6111 (3)0.07791 (18)0.34585 (17)0.0237 (6)
C70.5996 (3)0.2361 (2)0.3366 (2)0.0366 (8)
H70.58660.28920.30230.044*
C80.6249 (3)0.2460 (2)0.4271 (2)0.0421 (9)
H80.62780.30420.45290.050*
C90.6456 (3)0.1677 (2)0.4778 (2)0.0372 (8)
H90.66390.17240.53860.045*
C100.6391 (3)0.08140 (19)0.43788 (17)0.0270 (7)
C110.6623 (3)0.00469 (19)0.48861 (18)0.0264 (7)
C120.6564 (3)0.0910 (2)0.44350 (17)0.0279 (7)
C130.7060 (3)0.1648 (2)0.57419 (18)0.0314 (7)
C140.7088 (3)0.0804 (2)0.61944 (18)0.0312 (7)
C150.7283 (3)0.2476 (2)0.6229 (2)0.0421 (8)
H150.73040.30470.59550.051*
C160.7464 (3)0.2396 (2)0.7117 (2)0.0417 (8)
C170.7497 (3)0.1526 (2)0.7525 (2)0.0465 (9)
H170.76620.15030.81360.056*
C180.5063 (3)0.30463 (19)0.0431 (2)0.0340 (7)
C190.5034 (3)0.40616 (19)0.02139 (19)0.0298 (7)
C200.5307 (3)0.4720 (2)0.0864 (2)0.0345 (7)
H200.55200.45350.14470.041*
C210.5266 (3)0.56480 (19)0.06603 (19)0.0344 (8)
H210.54400.60840.11070.041*
C220.7777 (3)0.06908 (19)0.0710 (2)0.0326 (7)
C230.8925 (3)0.03323 (19)0.0338 (2)0.0316 (7)
C241.0084 (3)0.0180 (2)0.0887 (2)0.0367 (8)
H241.01440.03020.14850.044*
C251.1159 (3)0.0151 (2)0.0557 (2)0.0366 (8)
H251.19350.02530.09320.044*
O10.6651 (2)0.05704 (14)0.02736 (13)0.0387 (5)
O20.7944 (2)0.10851 (14)0.14412 (14)0.0422 (6)
O1W0.3712 (2)0.10827 (19)0.06143 (16)0.0388 (6)
O30.4659 (3)0.24990 (14)0.01656 (15)0.0571 (7)
O40.5492 (2)0.28189 (13)0.12142 (13)0.0390 (6)
Cd10.57239 (2)0.132432 (13)0.143702 (13)0.02785 (7)
N10.5655 (2)0.01110 (16)0.21226 (15)0.0297 (6)
N20.5930 (2)0.15480 (15)0.29635 (15)0.0293 (6)
N30.6787 (3)0.17015 (16)0.48594 (15)0.0335 (6)
N40.6858 (2)0.00045 (16)0.57564 (15)0.0316 (6)
N50.7309 (3)0.07434 (19)0.70926 (16)0.0443 (7)
Cl10.76305 (11)0.33725 (6)0.77790 (6)0.0619 (3)
HW110.387 (3)0.149 (2)0.026 (2)0.048 (12)*
HW120.359 (3)0.059 (2)0.036 (2)0.041 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.058 (2)0.0299 (17)0.0229 (16)0.0005 (15)0.0034 (15)0.0023 (13)
C20.071 (2)0.0262 (17)0.0278 (17)0.0013 (16)0.0074 (16)0.0051 (13)
C30.058 (2)0.0230 (16)0.0274 (17)0.0026 (15)0.0040 (15)0.0012 (13)
C40.0335 (17)0.0233 (15)0.0244 (15)0.0018 (13)0.0075 (13)0.0015 (12)
C50.0295 (16)0.0250 (15)0.0211 (15)0.0011 (12)0.0048 (12)0.0020 (11)
C60.0277 (16)0.0221 (15)0.0214 (14)0.0010 (12)0.0037 (12)0.0021 (12)
C70.050 (2)0.0222 (16)0.0367 (19)0.0020 (15)0.0039 (16)0.0007 (13)
C80.065 (2)0.0229 (17)0.0351 (19)0.0002 (16)0.0006 (17)0.0055 (14)
C90.052 (2)0.0316 (17)0.0252 (16)0.0012 (15)0.0016 (15)0.0056 (14)
C100.0311 (17)0.0249 (16)0.0244 (15)0.0010 (13)0.0022 (12)0.0019 (12)
C110.0299 (17)0.0259 (15)0.0234 (16)0.0008 (13)0.0041 (13)0.0008 (12)
C120.0339 (17)0.0278 (16)0.0219 (15)0.0004 (13)0.0041 (13)0.0001 (12)
C130.0382 (18)0.0340 (17)0.0215 (15)0.0005 (14)0.0033 (13)0.0060 (13)
C140.0346 (18)0.0349 (18)0.0227 (16)0.0001 (14)0.0000 (13)0.0024 (13)
C150.059 (2)0.0316 (18)0.0348 (19)0.0003 (16)0.0042 (16)0.0065 (14)
C160.047 (2)0.047 (2)0.0298 (19)0.0026 (16)0.0023 (15)0.0194 (15)
C170.058 (2)0.055 (2)0.0248 (17)0.0025 (18)0.0009 (16)0.0062 (15)
C180.045 (2)0.0182 (15)0.041 (2)0.0036 (14)0.0115 (16)0.0052 (14)
C190.0346 (17)0.0175 (14)0.0379 (17)0.0051 (13)0.0079 (14)0.0044 (13)
C200.049 (2)0.0249 (16)0.0279 (16)0.0031 (14)0.0022 (15)0.0072 (13)
C210.050 (2)0.0207 (15)0.0320 (17)0.0007 (14)0.0045 (15)0.0027 (12)
C220.0395 (19)0.0184 (15)0.0422 (19)0.0014 (14)0.0135 (15)0.0015 (14)
C230.0319 (18)0.0229 (15)0.0417 (19)0.0027 (13)0.0115 (15)0.0053 (13)
C240.042 (2)0.0370 (19)0.0324 (18)0.0034 (15)0.0110 (15)0.0079 (14)
C250.0351 (19)0.0338 (18)0.0401 (19)0.0004 (14)0.0038 (15)0.0023 (14)
O10.0347 (13)0.0394 (13)0.0419 (13)0.0061 (10)0.0053 (10)0.0039 (10)
O20.0439 (13)0.0384 (13)0.0463 (13)0.0023 (10)0.0134 (11)0.0163 (11)
O1W0.0422 (14)0.0350 (15)0.0392 (14)0.0079 (11)0.0062 (11)0.0052 (12)
O30.115 (2)0.0206 (12)0.0348 (13)0.0077 (13)0.0075 (14)0.0014 (10)
O40.0595 (15)0.0214 (11)0.0339 (13)0.0057 (10)0.0006 (11)0.0065 (9)
Cd10.03799 (13)0.02110 (11)0.02452 (11)0.00384 (11)0.00504 (8)0.00282 (10)
N10.0456 (16)0.0241 (13)0.0192 (13)0.0002 (11)0.0046 (11)0.0000 (10)
N20.0392 (15)0.0211 (14)0.0280 (13)0.0016 (10)0.0062 (11)0.0019 (10)
N30.0479 (16)0.0277 (13)0.0240 (13)0.0026 (12)0.0031 (12)0.0044 (11)
N40.0376 (15)0.0335 (14)0.0224 (14)0.0016 (12)0.0004 (11)0.0015 (11)
N50.0646 (19)0.0433 (17)0.0235 (14)0.0016 (15)0.0018 (13)0.0019 (12)
Cl10.0960 (8)0.0495 (5)0.0376 (5)0.0022 (5)0.0023 (5)0.0183 (4)
Geometric parameters (Å, º) top
C1—N11.328 (4)C16—C171.405 (5)
C1—C21.383 (4)C16—Cl11.735 (3)
C1—H10.9300C17—N51.313 (4)
C2—C31.376 (4)C17—H170.9300
C2—H20.9300C18—O31.237 (4)
C3—C41.387 (4)C18—O41.263 (3)
C3—H30.9300C18—C191.506 (4)
C4—C51.395 (4)C19—C201.379 (4)
C4—C121.467 (4)C19—C21i1.399 (4)
C5—N11.351 (3)C20—C211.378 (4)
C5—C61.467 (4)C20—H200.9300
C6—N21.345 (3)C21—C19i1.399 (4)
C6—C101.404 (4)C21—H210.9300
C7—N21.326 (4)C22—O21.251 (3)
C7—C81.387 (4)C22—O11.269 (4)
C7—H70.9300C22—C231.497 (4)
C8—C91.374 (4)C23—C241.379 (4)
C8—H80.9300C23—C25ii1.393 (4)
C9—C101.388 (4)C24—C251.386 (4)
C9—H90.9300C24—H240.9300
C10—C111.470 (4)C25—C23ii1.393 (4)
C11—N41.327 (4)C25—H250.9300
C11—C121.426 (4)O1W—HW110.84 (4)
C12—N31.321 (4)O1W—HW120.81 (3)
C13—N31.348 (4)Cd1—O12.424 (2)
C13—C141.405 (4)Cd1—O22.337 (2)
C13—C151.413 (4)Cd1—O42.197 (2)
C14—N41.353 (4)Cd1—O1W2.301 (2)
C14—N51.370 (4)Cd1—N12.336 (2)
C15—C161.357 (4)Cd1—N22.351 (2)
C15—H150.9300
N1—C1—C2122.9 (3)C20—C19—C21i118.8 (3)
N1—C1—H1118.6C20—C19—C18121.1 (3)
C2—C1—H1118.6C21i—C19—C18120.0 (3)
C3—C2—C1119.1 (3)C21—C20—C19120.8 (3)
C3—C2—H2120.4C21—C20—H20119.6
C1—C2—H2120.4C19—C20—H20119.6
C2—C3—C4118.8 (3)C20—C21—C19i120.4 (3)
C2—C3—H3120.6C20—C21—H21119.8
C4—C3—H3120.6C19i—C21—H21119.8
C3—C4—C5118.9 (2)O2—C22—O1121.8 (3)
C3—C4—C12121.4 (3)O2—C22—C23119.7 (3)
C5—C4—C12119.6 (3)O1—C22—C23118.5 (3)
N1—C5—C4121.6 (3)O2—C22—Cd158.93 (16)
N1—C5—C6117.6 (2)O1—C22—Cd162.91 (16)
C4—C5—C6120.7 (2)C23—C22—Cd1178.2 (2)
N2—C6—C10122.1 (3)C24—C23—C25ii119.4 (3)
N2—C6—C5117.8 (2)C24—C23—C22119.7 (3)
C10—C6—C5120.1 (2)C25ii—C23—C22120.9 (3)
N2—C7—C8123.3 (3)C23—C24—C25120.6 (3)
N2—C7—H7118.3C23—C24—H24119.7
C8—C7—H7118.3C25—C24—H24119.7
C9—C8—C7118.4 (3)C24—C25—C23ii120.0 (3)
C9—C8—H8120.8C24—C25—H25120.0
C7—C8—H8120.8C23ii—C25—H25120.0
C8—C9—C10119.8 (3)C22—O1—Cd189.30 (18)
C8—C9—H9120.1C22—O2—Cd193.77 (18)
C10—C9—H9120.1Cd1—O1W—HW1189 (2)
C9—C10—C6117.9 (3)Cd1—O1W—HW12117 (2)
C9—C10—C11122.2 (2)HW11—O1W—HW12110 (3)
C6—C10—C11119.9 (3)C18—O4—Cd1114.80 (18)
N4—C11—C12121.9 (3)O4—Cd1—O1W89.70 (9)
N4—C11—C10118.6 (2)O4—Cd1—N1159.27 (8)
C12—C11—C10119.4 (2)O1W—Cd1—N191.42 (9)
N3—C12—C11121.8 (2)O4—Cd1—O2103.35 (8)
N3—C12—C4118.1 (3)O1W—Cd1—O2142.64 (8)
C11—C12—C4120.1 (3)N1—Cd1—O288.12 (8)
N3—C13—C14122.4 (3)O4—Cd1—N290.67 (8)
N3—C13—C15118.6 (3)O1W—Cd1—N2120.38 (9)
C14—C13—C15119.0 (3)N1—Cd1—N270.99 (8)
N4—C14—N5116.0 (3)O2—Cd1—N294.68 (8)
N4—C14—C13121.0 (2)O4—Cd1—O1111.97 (8)
N5—C14—C13123.0 (3)O1W—Cd1—O187.56 (8)
C16—C15—C13116.7 (3)N1—Cd1—O188.76 (8)
C16—C15—H15121.7O2—Cd1—O155.08 (7)
C13—C15—H15121.7N2—Cd1—O1144.81 (7)
C15—C16—C17121.2 (3)C1—N1—C5118.6 (2)
C15—C16—Cl1120.6 (3)C1—N1—Cd1124.24 (19)
C17—C16—Cl1118.2 (2)C5—N1—Cd1115.99 (18)
N5—C17—C16123.6 (3)C7—N2—C6118.4 (3)
N5—C17—H17118.2C7—N2—Cd1125.4 (2)
C16—C17—H17118.2C6—N2—Cd1115.88 (18)
O3—C18—O4124.9 (3)C12—N3—C13116.3 (3)
O3—C18—C19117.8 (3)C11—N4—C14116.5 (2)
O4—C18—C19117.3 (3)C17—N5—C14116.5 (3)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O30.84 (4)1.84 (4)2.643 (4)160 (3)
O1W—HW12···O1iii0.81 (3)1.94 (3)2.752 (3)178 (3)
Symmetry code: (iii) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Cd(C17H8ClN5)(C8H4O4)(H2O)]
Mr612.26
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)10.412 (3), 14.466 (3), 15.411 (4)
β (°) 98.956 (2)
V3)2292.9 (10)
Z4
Radiation typeMo Kα
µ (mm1)1.12
Crystal size (mm)0.32 × 0.27 × 0.22
Data collection
DiffractometerBruker APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.752, 0.891
No. of measured, independent and
observed [I > 2σ(I)] reflections
18357, 5256, 3492
Rint0.042
(sin θ/λ)max1)0.675
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.066, 0.89
No. of reflections5256
No. of parameters342
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.42, 0.65

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—O12.424 (2)Cd1—O1W2.301 (2)
Cd1—O22.337 (2)Cd1—N12.336 (2)
Cd1—O42.197 (2)Cd1—N22.351 (2)
O4—Cd1—O1W89.70 (9)N1—Cd1—N270.99 (8)
O4—Cd1—N1159.27 (8)O2—Cd1—N294.68 (8)
O1W—Cd1—N191.42 (9)O4—Cd1—O1111.97 (8)
O4—Cd1—O2103.35 (8)O1W—Cd1—O187.56 (8)
O1W—Cd1—O2142.64 (8)N1—Cd1—O188.76 (8)
N1—Cd1—O288.12 (8)O2—Cd1—O155.08 (7)
O4—Cd1—N290.67 (8)N2—Cd1—O1144.81 (7)
O1W—Cd1—N2120.38 (9)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O30.84 (4)1.84 (4)2.643 (4)160 (3)
O1W—HW12···O1i0.81 (3)1.94 (3)2.752 (3)178 (3)
Symmetry code: (i) x+1, y, z.
 

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