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Solvothermal reaction between Cd(NO3)2, 1,4-phenyl­ene­diacetate (1,4-PDA) and 1,3-bis­(pyridin-4-yl)­propane (bpp) afforded the title complex, [Cd(C10H8O4)(C13H14N2)]n. Adjacent carboxylate-bridged CdII ions are related by an inversion centre. The 1,4-PDA ligands adopt a cis conformation and connect the CdII ions to form a one-dimensional chain extending along the c axis. These chains are in turn linked into a two-dimensional network through bpp bridges. The bpp ligands adopt an anti-gauche conformation. From a topo­logi­cal point of view, each bpp ligand and each pair of 1,4-PDA ligands can be considered as linkers, while the dinuclear CdII unit can be regarded as a 6-connecting node. Thus, the structure can be simplified to a two-dimensional 6-connected network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270111055454/qs3010sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270111055454/qs3010Isup2.hkl
Contains datablock I

CCDC reference: 867003

Comment top

The design and construction of coordination polymers based on transition metals and organic spacers are currently attracting considerable attention (Moulton & Zaworotko, 2001; Kitagawa et al., 2004). Flexible ligands such as 1,4-phenylenediacetate (1,4-PDA) and 1,3-bis(pyridin-4-yl)propane (bpp) are usually the typical building elements in coordination networks, since they can adopt varied coordination modes and geometries. For 1,4-PDA, the two carboxyl groups can exhibit various coordination modes. Furthermore, this flexible ligand can adopt either cis or trans conformations (Blake et al., 2010; Lan et al., 2011; Sposato et al., 2010; Yang et al., 2010). The bpp ligand is more flexible than 1,4-PDA due to its –CH2–CH2–CH2– moieties, and it can adopt antianti, antigauche or gauchegauche conformations (Carlucci et al., 2000; Hulvey et al., 2010; Mao et al., 1999). To understand further the coordination chemistry of flexible dicarboxylate and dipyridyl ligands, we employed these two ligands to react with CdII ions under solvothermal conditions and obtained the title two-dimensional coordination polymer, [Cd(C10H8O4)(C13H14N2)]n, (I).

As shown in Fig. 1, each CdII ion of (I) has pentagonal–bipyramidal coordination, with five O atoms from three 1,4-PDA ligands occupying the basal sites and two N atoms from two bpp ligands located on the axial positions. The Cd—O bond lengths range from 2.313 (3) to 2.488 (3) Å, and the Cd—N distances are 2.340 (3) and 2.315 (3) Å. Two equivalent CdII ions related by a twofold axis with an interatomic distance of 3.7959 (9) Å are bridged by 1,4-PDA ligands to form a [Cd2(1,4-PDA)2] unit. Adjacent [Cd2(1,4-PDA)2] units are linked via Cd—O bonds to afford a one-dimensional [Cd2(1,4-PDA)2]n chain (Fig. 2). These chains are further interconnected through bridging bpp ligands to generate a rare two-dimensional 6-connected net. The size of each triangular grid in the two-dimensional net is 10.31 × 12.29 × 12.29 Å (Fig. 3). Different from that of the reported complex {[Cu4(1,4-PDA)3(OH)2(bpp)2]2H2O}n (Reference?) constructed from trans-1,4-PDA and anti–anti bpp ligands, the conformations of the 1,4-PDA and bpp ligands in (I) are cis–gauche and anti–gauche, respectively.

The aromatic rings of the organic ligands of (I) are not close. The closest ring–ring contact is between the N1/C1–C5 and N2/C9–C13 rings, at a distance of 3.944 (3) Å.

Considering previously reported coordination polymers constructed from rigid dicarboxylate and dipyridyl ligands, we found that the structures of these complexes are usually two-dimensional (4,4) nets or three-dimensional frameworks. The structural motif of (I) is not only different from the reported rectangular sheets generated by metal ions and mixed ligands (Yang et al., 2010), but also from the reported coordination polymers which are composed of three-dimensional networks (Tao et al., 2000). The reason may be related to the flexibility of the 1,4-PDA ligand, which means the infinite [Cd2(1,4-PDA)2]n units can not form a two-dimensional net. Furthermore, the flexibility of the bpp ligand also plays an important role in determining the final structure. In contrast with rigid dipyridyl ligands such as 4,4'-bipyridine (Liu et al., 2009; Yang et al., 2010), four flexible bpp ligands in (I) form bridges between four [Cd2(1,4-PDA)2] units and a central [Cd2(1,4-PDA)2] unit. These bridges complete links to two [Cd2(1,4-PDA)2] units in the [Cd2(1,4-PDA)2]n chain on one side of the central unit and a further two [Cd2(1,4-PDA)2] units in the chain on the other side of the central unit. Together with the intrachain links, these connections make each [Cd2(1,4-PDA)2] unit a 6-connecting node.

each pair of flexible bpp ligands in (I) can bridge four [Cd2(1,4-PDA)2] units to a central [Cd2(1,4-PDA)2] unit, which makes the [Cd2(1,4-PDA)2] unit a 6-connecting node.

In summary, a new two-dimensional coordination polymer, (I), constructed from flexible dicarboxylate and dipyridyl ligands has been presented. The structure is different from those constructed from mixed rigid ligands or a mixture of both rigid and flexible ligands. Thus, the flexibility of organic ligands plays an important role in constructing coordination networks. This work emphasizes the coordinative flexibility and versatility of mixed ligands and their synthetic utility in coordination chemistry. We are currently extending this study by preparing new ligands of this type with other substituted functional groups. We anticipate this approach to be useful for constructing novel coordination complexes.

Related literature top

For related literature, see: Blake et al. (2010); Carlucci et al. (2000); Hulvey et al. (2010); Kitagawa et al. (2004); Lan et al. (2011); Liu et al. (2009); Mao et al. (1999); Moulton & Zaworotko (2001); Sposato et al. (2010); Tao et al. (2000); Yang et al. (2010).

Experimental top

Into a 25 ml Teflon-lined stainless steel autoclave were loaded Cd(NO3)2.4H2O (154 mg, 0.5 mmol), 1,4-phenylenediacetic acid (97 mg, 0.5 mmol), 1,3-bis(pyridin-4-yl)propane (99 mg, 0.5 mmol), H2O (8 ml) and EtOH (8 ml). The autoclave was sealed and heated in an oven to 433 K for 3 d, and then cooled to ambient temperature at a rate of 5 K h-1 to form colourless crystals of (I), which were washed with ethanol and dried in air (yield 188 mg, 75% based on Cd). Analysis, calculated for C23H22CdN2O4: C 54.94, H 4.41, N 5.57%; found: C 54.62, H 4.18, N 5.75%. Spectroscopic analysis: IR (KBr, ν, cm-1): 1606 (s), 1590 (s), 1541 (s), 1506 (m), 1494 (m), 1401 (s), 1376 (s), 1226 (m), 1168 (m), 1069 (m), 1013 (s), 853 (s), 829 (s), 771 (s), 683 (m), 548 (s).

Refinement top

All H atoms were placed in geometrically idealized positions, with C—H = 0.95 Å for phenyl and pyridyl groups or 0.98 Å for methylene groups, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C) for phenyl and pyridyl groups or 1.5Ueq(C) for methylene groups.

Computing details top

Data collection: CrystalClear (Rigaku, 2001); cell refinement: CrystalClear (Rigaku, 2001); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Figures top
[Figure 1] Fig. 1. The coordination environment of the CdII ion in (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) x, y, z - 1; (ii) -x + 1, -y + 1, -z; (iii) -x + 1, y - 1/2, -z - 1/2.]
[Figure 2] Fig. 2. A view of the one-dimensional [Cd(1,4-PDA)]n chain extending along the c axis. The black balls represent the inversion centres. The a axis is directed out of the paper towards the viewer.
[Figure 3] Fig. 3. A view of the two-dimensional network of (I), extending along the bc axis. The black balls and thickest lines represent the topological net. The a axis is directed out of the paper towards the viewer.
Poly[[µ2-1,3-bis(pyridin-4-yl)propane](µ3-1,4-phenylenediacetato)cadmium] top
Crystal data top
[Cd(C10H8O4)(C13H14N2)]F(000) = 1016
Mr = 502.84Dx = 1.618 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8184 reflections
a = 10.022 (2) Åθ = 3.5–27.5°
b = 22.316 (5) ŵ = 1.09 mm1
c = 10.316 (2) ÅT = 223 K
β = 116.51 (3)°Block, colourless
V = 2064.6 (9) Å30.30 × 0.30 × 0.10 mm
Z = 4
Data collection top
Rigaku Mercury CCD area-detector
diffractometer
4699 independent reflections
Radiation source: fine-focus sealed tube3702 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω scansθmax = 27.5°, θmin = 3.5°
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
h = 1113
Tmin = 0.736, Tmax = 0.899k = 2823
11710 measured reflectionsl = 139
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)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0414P)2 + 0.6308P]
where P = (Fo2 + 2Fc2)/3
4699 reflections(Δ/σ)max = 0.001
271 parametersΔρmax = 0.60 e Å3
0 restraintsΔρmin = 0.53 e Å3
Crystal data top
[Cd(C10H8O4)(C13H14N2)]V = 2064.6 (9) Å3
Mr = 502.84Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.022 (2) ŵ = 1.09 mm1
b = 22.316 (5) ÅT = 223 K
c = 10.316 (2) Å0.30 × 0.30 × 0.10 mm
β = 116.51 (3)°
Data collection top
Rigaku Mercury CCD area-detector
diffractometer
4699 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
3702 reflections with I > 2σ(I)
Tmin = 0.736, Tmax = 0.899Rint = 0.035
11710 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.099H-atom parameters constrained
S = 1.10Δρmax = 0.60 e Å3
4699 reflectionsΔρmin = 0.53 e Å3
271 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
Cd10.50810 (3)0.437184 (11)0.37266 (3)0.03559 (11)
N10.6340 (3)0.50732 (14)0.1898 (3)0.0380 (7)
N20.6275 (4)0.86966 (14)0.0545 (3)0.0410 (7)
O10.7236 (3)0.36904 (14)0.2451 (3)0.0556 (8)
O20.5297 (3)0.36719 (13)0.1990 (3)0.0486 (7)
O30.6325 (3)0.47537 (13)0.5028 (3)0.0479 (7)
O40.7351 (3)0.52707 (11)0.3915 (3)0.0434 (6)
C10.7734 (4)0.52475 (19)0.1540 (5)0.0467 (10)
H10.82580.50560.19850.056*
C20.8441 (5)0.56950 (19)0.0551 (5)0.0495 (10)
H20.94370.57910.03160.059*
C30.7711 (4)0.60046 (19)0.0101 (5)0.0469 (10)
C40.6267 (5)0.5805 (2)0.0240 (5)0.0562 (12)
H40.57310.59820.02110.067*
C50.5627 (5)0.5351 (2)0.1231 (4)0.0507 (11)
H50.46500.52310.14510.061*
C60.8407 (5)0.6546 (2)0.1070 (5)0.0588 (12)
H6A0.94880.65330.14000.071*
H6B0.80330.69090.04850.071*
C70.8123 (5)0.65966 (17)0.2364 (5)0.0486 (10)
H7A0.86220.62660.30320.058*
H7B0.70500.65630.20620.058*
C80.8689 (5)0.71924 (18)0.3148 (5)0.0521 (11)
H8A0.86070.71840.40600.062*
H8B0.97470.72340.33890.062*
C90.7869 (4)0.77270 (17)0.2294 (4)0.0424 (9)
C100.8506 (4)0.81248 (19)0.1719 (5)0.0498 (10)
H100.95090.80750.19100.060*
C110.7697 (4)0.85949 (19)0.0868 (5)0.0477 (10)
H110.81740.88580.04950.057*
C120.5672 (5)0.8322 (2)0.1147 (6)0.0710 (15)
H120.46780.83880.09670.085*
C130.6410 (5)0.7848 (2)0.2008 (6)0.0690 (15)
H130.59250.76030.24070.083*
C140.7670 (4)0.34242 (16)0.0973 (4)0.0370 (8)
C150.8127 (4)0.40199 (16)0.1199 (4)0.0384 (8)
H150.82340.42290.04590.046*
C160.8428 (4)0.43119 (16)0.2476 (4)0.0359 (8)
H160.87410.47140.25970.043*
C170.8271 (4)0.40150 (16)0.3597 (4)0.0345 (8)
C180.7820 (4)0.34232 (16)0.3375 (4)0.0386 (8)
H180.77160.32140.41160.046*
C190.7516 (4)0.31305 (17)0.2090 (4)0.0418 (9)
H190.72030.27290.19700.050*
C200.7417 (5)0.31138 (18)0.0420 (4)0.0456 (10)
H20A0.68400.27470.05270.055*
H20B0.83810.30000.03740.055*
C210.6588 (4)0.35144 (16)0.1734 (4)0.0388 (9)
C220.8510 (4)0.43454 (16)0.4975 (4)0.0371 (8)
H22A0.84590.40610.56750.045*
H22B0.95020.45300.54090.045*
C230.7333 (4)0.48234 (16)0.4634 (4)0.0351 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03852 (17)0.03556 (16)0.03327 (16)0.00254 (12)0.01652 (12)0.00252 (11)
N10.0406 (17)0.0404 (17)0.0354 (17)0.0019 (15)0.0191 (14)0.0034 (13)
N20.0416 (17)0.0412 (18)0.0407 (18)0.0010 (15)0.0189 (15)0.0033 (14)
O10.0570 (18)0.0632 (19)0.0559 (19)0.0120 (16)0.0334 (16)0.0153 (15)
O20.0479 (16)0.0511 (17)0.0479 (17)0.0077 (14)0.0222 (13)0.0108 (13)
O30.0472 (15)0.0573 (18)0.0500 (17)0.0096 (14)0.0314 (14)0.0125 (13)
O40.0520 (16)0.0380 (14)0.0466 (16)0.0066 (13)0.0276 (13)0.0078 (12)
C10.042 (2)0.052 (2)0.051 (3)0.008 (2)0.0249 (19)0.0014 (19)
C20.036 (2)0.060 (3)0.055 (3)0.006 (2)0.0225 (19)0.011 (2)
C30.042 (2)0.053 (2)0.048 (2)0.005 (2)0.0229 (19)0.0078 (19)
C40.043 (2)0.077 (3)0.054 (3)0.001 (2)0.026 (2)0.019 (2)
C50.041 (2)0.072 (3)0.042 (2)0.013 (2)0.0215 (19)0.010 (2)
C60.060 (3)0.058 (3)0.059 (3)0.014 (2)0.027 (2)0.010 (2)
C70.054 (2)0.040 (2)0.050 (2)0.0007 (19)0.022 (2)0.0033 (18)
C80.063 (3)0.041 (2)0.046 (2)0.001 (2)0.018 (2)0.0027 (18)
C90.046 (2)0.042 (2)0.035 (2)0.0035 (19)0.0143 (17)0.0070 (16)
C100.034 (2)0.051 (2)0.057 (3)0.0060 (19)0.0138 (19)0.001 (2)
C110.037 (2)0.053 (2)0.052 (3)0.007 (2)0.0188 (19)0.006 (2)
C120.049 (3)0.085 (4)0.085 (4)0.016 (3)0.036 (3)0.033 (3)
C130.058 (3)0.072 (3)0.084 (4)0.003 (3)0.038 (3)0.035 (3)
C140.0395 (19)0.0347 (19)0.035 (2)0.0082 (17)0.0152 (16)0.0016 (15)
C150.043 (2)0.039 (2)0.036 (2)0.0055 (18)0.0208 (17)0.0077 (16)
C160.0377 (19)0.0337 (19)0.039 (2)0.0032 (16)0.0195 (16)0.0031 (16)
C170.0318 (18)0.0357 (19)0.0350 (19)0.0065 (16)0.0140 (15)0.0046 (15)
C180.044 (2)0.0339 (19)0.042 (2)0.0024 (17)0.0225 (18)0.0075 (16)
C190.046 (2)0.0298 (18)0.049 (2)0.0010 (18)0.0212 (18)0.0047 (17)
C200.056 (2)0.036 (2)0.041 (2)0.012 (2)0.0184 (19)0.0048 (17)
C210.048 (2)0.0299 (18)0.036 (2)0.0040 (18)0.0162 (18)0.0001 (15)
C220.0392 (19)0.038 (2)0.0324 (19)0.0052 (17)0.0144 (15)0.0056 (15)
C230.0358 (19)0.039 (2)0.0274 (18)0.0024 (16)0.0109 (15)0.0045 (15)
Geometric parameters (Å, º) top
Cd1—O22.313 (3)C7—C81.528 (5)
Cd1—O3i2.315 (3)C7—H7A0.9800
Cd1—N2ii2.315 (3)C7—H7B0.9800
Cd1—N12.340 (3)C8—C91.493 (6)
Cd1—O3iii2.430 (3)C8—H8A0.9800
Cd1—O12.484 (3)C8—H8B0.9800
Cd1—O4iii2.488 (3)C9—C101.372 (6)
Cd1—C212.719 (4)C9—C131.383 (6)
N1—C11.334 (5)C10—C111.376 (6)
N1—C51.345 (5)C10—H100.9400
N2—C111.331 (5)C11—H110.9400
N2—C121.336 (6)C12—C131.367 (6)
N2—Cd1iv2.315 (3)C12—H120.9400
O1—C211.246 (5)C13—H130.9400
O2—C211.250 (5)C14—C151.391 (5)
O3—C231.256 (4)C14—C191.392 (5)
O3—Cd1v2.315 (3)C14—C201.512 (5)
O3—Cd1iii2.430 (3)C15—C161.377 (5)
O4—C231.249 (4)C15—H150.9400
O4—Cd1iii2.488 (3)C16—C171.401 (5)
C1—C21.376 (6)C16—H160.9400
C1—H10.9400C17—C181.381 (5)
C2—C31.380 (6)C17—C221.522 (5)
C2—H20.9400C18—C191.384 (5)
C3—C41.401 (6)C18—H180.9400
C3—C61.524 (6)C19—H190.9400
C4—C51.377 (6)C20—C211.524 (5)
C4—H40.9400C20—H20A0.9800
C5—H50.9400C20—H20B0.9800
C6—C71.489 (6)C22—C231.511 (5)
C6—H6A0.9800C22—H22A0.9800
C6—H6B0.9800C22—H22B0.9800
O2—Cd1—O3i142.27 (10)C6—C7—H7B109.3
O2—Cd1—N2ii90.36 (11)C8—C7—H7B109.3
O3i—Cd1—N2ii93.24 (11)H7A—C7—H7B108.0
O2—Cd1—N189.83 (11)C9—C8—C7114.0 (3)
O3i—Cd1—N188.34 (11)C9—C8—H8A108.8
N2ii—Cd1—N1177.18 (11)C7—C8—H8A108.8
O2—Cd1—O3iii143.22 (10)C9—C8—H8B108.8
O3i—Cd1—O3iii73.79 (10)C7—C8—H8B108.8
N2ii—Cd1—O3iii95.11 (11)H8A—C8—H8B107.6
N1—Cd1—O3iii83.07 (11)C10—C9—C13115.6 (4)
O2—Cd1—O154.39 (10)C10—C9—C8122.2 (4)
O3i—Cd1—O187.88 (10)C13—C9—C8122.2 (4)
N2ii—Cd1—O195.04 (11)C9—C10—C11120.9 (4)
N1—Cd1—O187.36 (11)C9—C10—H10119.6
O3iii—Cd1—O1159.49 (9)C11—C10—H10119.6
O2—Cd1—O4iii91.54 (9)N2—C11—C10123.4 (4)
O3i—Cd1—O4iii126.15 (9)N2—C11—H11118.3
N2ii—Cd1—O4iii86.86 (10)C10—C11—H11118.3
N1—Cd1—O4iii90.31 (10)N2—C12—C13124.1 (4)
O3iii—Cd1—O4iii52.66 (9)N2—C12—H12118.0
O1—Cd1—O4iii145.82 (9)C13—C12—H12118.0
O2—Cd1—C2127.26 (11)C12—C13—C9120.3 (4)
O3i—Cd1—C21115.05 (11)C12—C13—H13119.9
N2ii—Cd1—C2194.68 (11)C9—C13—H13119.9
N1—Cd1—C2186.76 (11)C15—C14—C19117.5 (3)
O3iii—Cd1—C21166.38 (11)C15—C14—C20120.0 (4)
O1—Cd1—C2127.22 (10)C19—C14—C20122.5 (3)
O4iii—Cd1—C21118.60 (11)C16—C15—C14121.8 (3)
C1—N1—C5117.0 (3)C16—C15—H15119.1
C1—N1—Cd1122.6 (3)C14—C15—H15119.1
C5—N1—Cd1120.1 (3)C15—C16—C17120.6 (3)
C11—N2—C12115.7 (4)C15—C16—H16119.7
C11—N2—Cd1iv119.3 (3)C17—C16—H16119.7
C12—N2—Cd1iv124.1 (3)C18—C17—C16117.7 (3)
C21—O1—Cd187.0 (2)C18—C17—C22121.4 (3)
C21—O2—Cd194.8 (2)C16—C17—C22120.8 (3)
C23—O3—Cd1v159.3 (3)C17—C18—C19121.7 (4)
C23—O3—Cd1iii94.2 (2)C17—C18—H18119.2
Cd1v—O3—Cd1iii106.21 (10)C19—C18—H18119.2
C23—O4—Cd1iii91.7 (2)C18—C19—C14120.8 (4)
N1—C1—C2123.1 (4)C18—C19—H19119.6
N1—C1—H1118.5C14—C19—H19119.6
C2—C1—H1118.5C14—C20—C21111.7 (3)
C1—C2—C3121.0 (4)C14—C20—H20A109.3
C1—C2—H2119.5C21—C20—H20A109.3
C3—C2—H2119.5C14—C20—H20B109.3
C2—C3—C4115.6 (4)C21—C20—H20B109.3
C2—C3—C6122.0 (4)H20A—C20—H20B107.9
C4—C3—C6122.4 (4)O1—C21—O2123.4 (3)
C5—C4—C3120.5 (4)O1—C21—C20119.4 (4)
C5—C4—H4119.8O2—C21—C20117.1 (4)
C3—C4—H4119.8O1—C21—Cd165.8 (2)
N1—C5—C4122.7 (4)O2—C21—Cd157.93 (19)
N1—C5—H5118.6C20—C21—Cd1169.6 (3)
C4—C5—H5118.6C23—C22—C17110.1 (3)
C7—C6—C3115.7 (4)C23—C22—H22A109.6
C7—C6—H6A108.4C17—C22—H22A109.6
C3—C6—H6A108.4C23—C22—H22B109.6
C7—C6—H6B108.4C17—C22—H22B109.6
C3—C6—H6B108.4H22A—C22—H22B108.2
H6A—C6—H6B107.4O4—C23—O3121.2 (3)
C6—C7—C8111.5 (4)O4—C23—C22119.1 (3)
C6—C7—H7A109.3O3—C23—C22119.6 (3)
C8—C7—H7A109.3
Symmetry codes: (i) x, y, z1; (ii) x+1, y1/2, z1/2; (iii) x+1, y+1, z; (iv) x+1, y+1/2, z1/2; (v) x, y, z+1.

Experimental details

Crystal data
Chemical formula[Cd(C10H8O4)(C13H14N2)]
Mr502.84
Crystal system, space groupMonoclinic, P21/c
Temperature (K)223
a, b, c (Å)10.022 (2), 22.316 (5), 10.316 (2)
β (°) 116.51 (3)
V3)2064.6 (9)
Z4
Radiation typeMo Kα
µ (mm1)1.09
Crystal size (mm)0.30 × 0.30 × 0.10
Data collection
DiffractometerRigaku Mercury CCD area-detector
diffractometer
Absorption correctionMulti-scan
(REQAB; Jacobson, 1998)
Tmin, Tmax0.736, 0.899
No. of measured, independent and
observed [I > 2σ(I)] reflections
11710, 4699, 3702
Rint0.035
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.099, 1.10
No. of reflections4699
No. of parameters271
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.60, 0.53

Computer programs: CrystalClear (Rigaku, 2001), CrystalStructure (Rigaku/MSC, 2004), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

 

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