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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 1| January 2008| Pages m260-m261
https://doi.org/10.1107/S1600536807067396

Poly[di­aqua­bis­(2,2′-bi­pyridine)tris­­(μ4-2,2′-bi­pyridine-4,4′-di­carboxyl­ato)dineodymium(III)]

Chia-Jung Tsaia and Yen-Hsiang Liua*

aDepartment of Chemistry, Fu Jen Catholic University, Taipei 24205, Taiwan
*Correspondence e-mail: chem2022@mails.fju.edu.tw

(Received 4 December 2007; accepted 17 December 2007; online 21 December 2007)

In the crystal structure of the title mixed-ligand coordination polymer, [Nd2(C12H6N2O4)3(C10H8N2)2(H2O)2]n, the NdIII ion is in an octa­hedral coordination environment formed by one water mol­ecule, one chelating 2,2′-bipyridine ligand, and five monodentate carboxyl­ate groups. The local coordination polyhedron around the NdIII ion is a bicapped trigonal prism. Two NdIII centers are bridged by four carboxyl­ate groups to form an Nd2 dimeric unit; these are further connected by 2,2′-bipyridine-4,4′-dicarboxyl­ate linkers, resulting in a layered coordination network.

Related literature

Only lanthanide-2,2′-bipyridine-4,4′-dicarboxyl­ate-based coordination polymers with three-dimensional porous framework structures have been previously reported (Wu et al., 2006[Wu, J.-Y., Yeh, T.-T., Wen, Y.-S., Twu, J. & Lu, K.-L. (2006). Cryst. Growth Des. 6, 467-473.]).

[Scheme 1]

Experimental

Crystal data

  • [Nd2(C12H6N2O4)3(C10H8N2)2(H2O)2]

  • Mr = 681.72

  • Triclinic, [P \overline 1]

  • a = 8.9914 (2) Å

  • b = 12.5409 (3) Å

  • c = 12.7455 (3) Å

  • α = 67.809 (2)°

  • β = 88.645 (2)°

  • γ = 75.437 (1)°

  • V = 1283.89 (6) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.08 mm−1

  • T = 200 (2) K

  • 0.5 × 0.4 × 0.2 mm
Data collection

  • Nonius KappaCCD diffractometer

  • Absorption correction: multi-scan (SORTAV; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.398, Tmax = 0.660

  • 4669 measured reflections

  • 16411 independent reflections

  • 4460 reflections with I > 2σ(I)

  • Rint = 0.042
Refinement

  • R[F2 > 2σ(F2)] = 0.022

  • wR(F2) = 0.061

  • S = 1.17

  • 4669 reflections

  • 371 parameters

  • H-atom parameters constrained

  • Δρmax = 0.56 e Å−3

  • Δρmin = −0.97 e Å−3

Table 1
Selected geometric parameters (Å, °)

Nd1—O5 2.386 (2)
Nd1—O3i 2.399 (2)
Nd1—O4ii 2.4120 (19)
Nd1—O1 2.4309 (19)
Nd1—O2iii 2.4443 (19)
Nd1—O7 2.5126 (20)
Nd1—N1 2.618 (2)
Nd1—N2 2.659 (2)
O1—C11 1.252 (3)
O2—C11 1.256 (3)
O3—C22 1.255 (4)
O4—C22 1.252 (3)
O5—C23 1.267 (4)
O6—C23 1.246 (4)
O5—Nd1—O4ii 85.16 (7)
O5—Nd1—O1 85.06 (7)
O3i—Nd1—O1 81.99 (7)
O4ii—Nd1—O1 71.54 (7)
O3i—Nd1—O2iii 72.10 (7)
O4ii—Nd1—O2iii 83.53 (7)
O5—Nd1—O7 73.07 (7)
O4ii—Nd1—O7 70.18 (7)
O2iii—Nd1—O7 69.04 (7)
O5—Nd1—N1 82.69 (7)
O3i—Nd1—N1 84.74 (7)
O2iii—Nd1—N1 85.45 (7)
O7—Nd1—N1 73.68 (7)
O5—Nd1—N2 72.54 (7)
O3i—Nd1—N2 69.59 (7)
O1—Nd1—N2 78.68 (7)
N1—Nd1—N2 61.78 (7)
Symmetry codes: (i) x, y, z+1; (ii) -x+1, -y+1, -z; (iii) -x+1, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O7—H7A⋯O6 0.83 1.92 2.731 (3) 164
O7—H7A⋯O5 0.83 2.53 2.918 (3) 110
O7—H7B⋯O6iv 0.81 2.02 2.811 (3) 165
Symmetry code: (iv) -x, -y+1, -z+1.

Data collection: COLLECT (Nonius, 2000[Nonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: SCALEPACK (Otwinowski & Minor 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: DENZO (Otwinowski & Minor 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536807067396/ww2111sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807067396/ww2111Isup2.hkl

checkCIF report


Comment top

As shown in figure 1, a NdIII cation, one 2,2'-bipyridine (bpy) ligand, one coordinated water molecule, as well as one and a half of the 2,2'-bipyridine-4,4'-dicarboxylate (bpdc) ligands were observed in the crystallographic asymmetric unit. The observation of symmetrical C?O bond lengths range from 1.252 (3) Å to 1.267 (4) Å indicated that all of the carboxyl groups of the bpdc ligands are deprotonated to achieve charge neutrality with the NdIII cation. The formula of the title compound is assigned to be [Nd2(C10H8N2)2(C12H6N2O4)3(H2O)2]n.

The NdIII ion exists in an eight-coordinated environment formed by one water molecule, one chelating bpy ligand, and five monodentate carboxylate groups of the bpdc ligands. The local coordination geometry around NdIII ion is a bicapped trigonal prism polyhedron. Two NdIII centers are bridged by four carboxylate groups to become a Nd2-dimer unit (Figure 2). An inversion center is located at the center of the Nd···Nd axis.

As shown in Figure 3, the Nd2-dimer unit is linked through the bpdc ligands to form a layered coordination network. The bpdc ligands present two distinct types of bridging coordination environments, a bis(monodentate) mode as well as a bis(syn,syn-bridging bidentate) mode. Due to the high oxophilicity (hard acid-hard base interaction) of the lanthanide ions, the bipyridine group of the bpdc ligand is not involved in coordination. Two of the bis(syn,syn-bridging bidentate) type bpdc bridging ligands are stacked in a parallel fashion. However, no obvious π–π interactions between the inter-ligand pyridine rings are observed (centroid-to-centroid distance of 4.04 Å and dihedral angle of 19.89°). Both of the hydrogen atoms of the coordinated water molecule O7 serve as hydrogen-bonding donors to form two intra-layer and one inter-layer hydrogen-bonding interactions with the oxygen atoms of the carboxylate groups. It is worthwhile noting that the inter-layer O–H···O hydrogen-bonding interactions play an import role in the stabilization of the layer-to-layer stacking in the crystal structure of the title compound. In addition, several intra-layer C–H···O interactions are also observed for the title compound, despite their weakness.

Solely bpdc-based lanthanide coordination polymers with three-dimensional porous framework structures were previously reported (Wu et al., 2006). The diversity in structure dimensionality between the title compound and the compounds reported by Wu et al. may be attributed to the presence of chelating bpy ligands in the title compound that capped the connectivity of NdIII ions, and leads to a two-dimensional layered network. Further investigations on mixed-ligand coordination modes with lanthanide ions toward the control of structure topology and network dimensionality are in progress.

Related literature top

Solely lanthanide-2,2'-bipyridine-4,4'-dicarboxylate-based coordination polymers with three-dimensional porous framework structures have been previously reported (Wu et al., 2006).

Experimental top

All reagents and solvents were used as obtained without further purification. Nd(NO3)3.6H2O (0.30 mmol, 131.7 mg), 2,2'-bipyridine (0.40 mmol, 62.5 mg), 2,2'-bipyridine-4,4'-dicarboxylic acid (0.15 mmol, 36.8 mg) were dissolved in 5.0 ml of distilled water. The mixture was sealed in a Teflon-lined stainless steel vessel and held at 453 K for 96 h. The vessel was gradually cooled to room temperature, and violet crystals suitable for crystallographic analysis were obtained in the yield of 65% based on 2,2'-bipyridine-4,4'-dicarboxylic acid.

Refinement top

The C-bound H atoms were placed in calculated positions (C—H = 0.93 Å) and refined in the riding-model approximation with Uiso(H) = 1.2 Ueq(C). The N-bound H atoms were observed in a difference Fourier map, but were placed in calculated positions (N—H = 0.86 Å) and refined in the riding-model approximation with Uiso(H) = 1.2 Ueq(N). The H atoms of the coordinated water molecules were located in a difference Fourier map, and refined as riding model with Uiso(H) = 1.5 Ueq(O). A longer Nd(1)—O(7) distance of 2.513 (2) Å is observed may be attributed to the loosely bound water molecule.

Structure description top

As shown in figure 1, a NdIII cation, one 2,2'-bipyridine (bpy) ligand, one coordinated water molecule, as well as one and a half of the 2,2'-bipyridine-4,4'-dicarboxylate (bpdc) ligands were observed in the crystallographic asymmetric unit. The observation of symmetrical C?O bond lengths range from 1.252 (3) Å to 1.267 (4) Å indicated that all of the carboxyl groups of the bpdc ligands are deprotonated to achieve charge neutrality with the NdIII cation. The formula of the title compound is assigned to be [Nd2(C10H8N2)2(C12H6N2O4)3(H2O)2]n.

The NdIII ion exists in an eight-coordinated environment formed by one water molecule, one chelating bpy ligand, and five monodentate carboxylate groups of the bpdc ligands. The local coordination geometry around NdIII ion is a bicapped trigonal prism polyhedron. Two NdIII centers are bridged by four carboxylate groups to become a Nd2-dimer unit (Figure 2). An inversion center is located at the center of the Nd···Nd axis.

As shown in Figure 3, the Nd2-dimer unit is linked through the bpdc ligands to form a layered coordination network. The bpdc ligands present two distinct types of bridging coordination environments, a bis(monodentate) mode as well as a bis(syn,syn-bridging bidentate) mode. Due to the high oxophilicity (hard acid-hard base interaction) of the lanthanide ions, the bipyridine group of the bpdc ligand is not involved in coordination. Two of the bis(syn,syn-bridging bidentate) type bpdc bridging ligands are stacked in a parallel fashion. However, no obvious π–π interactions between the inter-ligand pyridine rings are observed (centroid-to-centroid distance of 4.04 Å and dihedral angle of 19.89°). Both of the hydrogen atoms of the coordinated water molecule O7 serve as hydrogen-bonding donors to form two intra-layer and one inter-layer hydrogen-bonding interactions with the oxygen atoms of the carboxylate groups. It is worthwhile noting that the inter-layer O–H···O hydrogen-bonding interactions play an import role in the stabilization of the layer-to-layer stacking in the crystal structure of the title compound. In addition, several intra-layer C–H···O interactions are also observed for the title compound, despite their weakness.

Solely bpdc-based lanthanide coordination polymers with three-dimensional porous framework structures were previously reported (Wu et al., 2006). The diversity in structure dimensionality between the title compound and the compounds reported by Wu et al. may be attributed to the presence of chelating bpy ligands in the title compound that capped the connectivity of NdIII ions, and leads to a two-dimensional layered network. Further investigations on mixed-ligand coordination modes with lanthanide ions toward the control of structure topology and network dimensionality are in progress.

Solely lanthanide-2,2'-bipyridine-4,4'-dicarboxylate-based coordination polymers with three-dimensional porous framework structures have been previously reported (Wu et al., 2006).

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. The atom numbering scheme of the title compound presented in the crystallographically asymmetric unit. The atomic displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. Highlight of coordination environment of the Nd(III) ions. (Key: blue: N; red: O; gray: C; auqa sphere: water molecules; purple sphere: Nd). Hydrogen atoms are omitted for clarity. (Symmetry code: (i) 1–x, 1–y, 1–z) Inset: a view of the bicapped trigonal prism polyhedron around NdIII ion.
[Figure 3] Fig. 3. A view of the layer network of the title compound. (Key: auqa sphere: water molecules; purple polyhedra: Nd) Hydrogen atoms are omitted for clarity.
Poly[diaquabis(2,2'-bipyridine)tris(µ4-2,2'-bipyridine-4,4'- dicarboxylato)dineodymium(III)] top
Crystal data top
[Nd2(C12H6N2O4)3(C10H8N2)2(H2O)2]Z = 2
Mr = 681.72F(000) = 676
Triclinic, P1Dx = 1.763 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.9914 (2) ÅCell parameters from 12726 reflections
b = 12.5409 (3) Åθ = 2.0–25.4°
c = 12.7455 (3) ŵ = 2.08 mm−1
α = 67.809 (2)°T = 200 K
β = 88.645 (2)°Prism, white
γ = 75.437 (1)°0.5 × 0.4 × 0.2 mm
V = 1283.89 (6) Å3
Data collection top
Nonius KappaCCD
diffractometer		4669 independent reflections
Radiation source: sealed tube4460 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 25.3°, θmin = 2.4°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)		h = −10→10
Tmin = 0.398, Tmax = 0.660k = −14→15
16411 measured reflectionsl = −15→15
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0265P)2 + 1.2551P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.022(Δ/σ)max = 0.002
wR(F2) = 0.061Δρmax = 0.56 e Å−3
S = 1.17Δρmin = −0.97 e Å−3
4669 reflectionsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
371 parametersExtinction coefficient: 0.0065 (5)
0 restraints
Crystal data top
[Nd2(C12H6N2O4)3(C10H8N2)2(H2O)2]γ = 75.437 (1)°
Mr = 681.72V = 1283.89 (6) Å3
Triclinic, P1Z = 2
a = 8.9914 (2) ÅMo Kα radiation
b = 12.5409 (3) ŵ = 2.08 mm−1
c = 12.7455 (3) ÅT = 200 K
α = 67.809 (2)°0.5 × 0.4 × 0.2 mm
β = 88.645 (2)°
Data collection top
Nonius KappaCCD
diffractometer		4669 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)		4460 reflections with I > 2σ(I)
Tmin = 0.398, Tmax = 0.660Rint = 0.042
16411 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.061H-atom parameters constrained
S = 1.17Δρmax = 0.56 e Å−3
4669 reflectionsΔρmin = −0.97 e Å−3
371 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.302446 (16)0.648646 (11)0.499494 (11)0.01470 (8)
O10.4250 (2)0.69456 (18)0.32145 (16)0.0229 (5)
O20.6003 (2)0.53012 (18)0.32891 (16)0.0235 (5)
O30.5424 (2)0.65947 (18)−0.43231 (16)0.0223 (4)
O40.7188 (3)0.49332 (18)−0.41903 (17)0.0241 (5)
O50.0710 (2)0.77124 (17)0.38374 (17)0.0225 (4)
O6−0.1170 (3)0.68020 (19)0.39864 (18)0.0284 (5)
O70.0896 (2)0.55410 (18)0.58438 (17)0.0233 (4)
H7A0.01420.59130.53710.035*
H7B0.11410.48490.5920.035*
N10.1807 (3)0.7494 (2)0.6388 (2)0.0215 (5)
N20.3019 (3)0.8746 (2)0.4497 (2)0.0223 (5)
N30.4653 (3)0.7593 (2)−0.0901 (2)0.0258 (6)
N40.7976 (3)0.5136 (3)−0.0406 (2)0.0291 (6)
N5−0.1566 (3)0.9404 (2)−0.0166 (2)0.0234 (5)
C10.1138 (4)0.6873 (3)0.7282 (2)0.0251 (7)
H10.12750.60470.74520.03*
C20.0265 (4)0.7370 (3)0.7965 (3)0.0312 (7)
H2−0.01760.68970.85980.037*
C30.0047 (4)0.8573 (3)0.7704 (3)0.0369 (8)
H3−0.05710.89470.81470.044*
C40.0731 (4)0.9226 (3)0.6797 (3)0.0323 (8)
H40.05921.00550.66110.039*
C50.1628 (4)0.8665 (3)0.6156 (2)0.0221 (6)
C60.2415 (4)0.9319 (3)0.5180 (3)0.0235 (6)
C70.2558 (5)1.0458 (3)0.4987 (3)0.0376 (8)
H70.21341.08440.54810.045*
C80.3316 (5)1.1022 (3)0.4078 (3)0.0426 (9)
H80.34261.17960.39430.051*
C90.3913 (5)1.0454 (3)0.3366 (3)0.0382 (8)
H90.44281.08280.27260.046*
C100.3740 (4)0.9320 (3)0.3610 (3)0.0306 (7)
H100.41570.89250.31210.037*
C110.5080 (3)0.6300 (2)0.2764 (2)0.0178 (6)
C120.4949 (3)0.6758 (2)0.1476 (2)0.0173 (6)
C130.5869 (3)0.6123 (2)0.0900 (2)0.0187 (6)
H130.66110.53940.13090.022*
C140.5690 (3)0.6570 (2)−0.0282 (2)0.0187 (6)
C150.3785 (4)0.8189 (3)−0.0329 (3)0.0306 (8)
H150.30480.8915−0.07540.037*
C160.3893 (4)0.7814 (3)0.0843 (2)0.0248 (7)
H160.32520.82750.12060.03*
C170.6656 (3)0.5932 (2)−0.0944 (2)0.0193 (6)
C180.6182 (3)0.6167 (2)−0.2056 (2)0.0183 (6)
H180.52490.6749−0.24120.022*
C190.7085 (3)0.5544 (2)−0.2641 (2)0.0177 (6)
C200.8448 (4)0.4715 (3)−0.2093 (3)0.0267 (7)
H200.90940.4265−0.24640.032*
C210.8844 (4)0.4559 (3)−0.0993 (3)0.0347 (8)
H210.97950.4007−0.0630.042*
C220.6534 (3)0.5710 (2)−0.3818 (2)0.0182 (6)
C23−0.0411 (3)0.7506 (2)0.3433 (2)0.0190 (6)
C24−0.0843 (3)0.8186 (2)0.2173 (2)0.0197 (6)
C25−0.0014 (3)0.8963 (2)0.1525 (2)0.0189 (6)
H250.0820.90840.1870.023*
C26−0.0414 (3)0.9566 (2)0.0364 (2)0.0181 (6)
C27−0.2347 (4)0.8644 (3)0.0472 (3)0.0307 (7)
H27−0.31580.85190.01070.037*
C28−0.2040 (4)0.8027 (3)0.1641 (3)0.0294 (7)
H28−0.26410.75080.20620.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.02095 (11)0.01231 (10)0.01183 (10)−0.00483 (6)0.00305 (6)−0.00552 (7)
O10.0345 (12)0.0225 (11)0.0154 (10)−0.0109 (9)0.0101 (9)−0.0095 (8)
O20.0321 (12)0.0209 (11)0.0154 (10)−0.0086 (9)0.0020 (8)−0.0036 (8)
O30.0259 (11)0.0226 (11)0.0192 (10)−0.0087 (9)−0.0010 (8)−0.0073 (8)
O40.0366 (12)0.0228 (11)0.0216 (11)−0.0120 (9)0.0075 (9)−0.0157 (9)
O50.0247 (11)0.0169 (10)0.0236 (11)−0.0065 (8)−0.0019 (8)−0.0043 (8)
O60.0287 (12)0.0233 (11)0.0281 (12)−0.0128 (9)0.0017 (9)−0.0007 (9)
O70.0286 (12)0.0204 (10)0.0214 (11)−0.0085 (9)0.0041 (9)−0.0075 (8)
N10.0286 (14)0.0169 (12)0.0195 (13)−0.0039 (10)0.0028 (10)−0.0088 (10)
N20.0296 (14)0.0190 (12)0.0193 (13)−0.0070 (11)0.0024 (10)−0.0081 (10)
N30.0301 (15)0.0262 (14)0.0153 (12)0.0019 (11)−0.0001 (10)−0.0074 (11)
N40.0280 (15)0.0361 (16)0.0196 (13)0.0024 (12)−0.0004 (11)−0.0134 (12)
N50.0254 (14)0.0251 (13)0.0221 (13)−0.0107 (11)0.0017 (10)−0.0091 (11)
C10.0348 (18)0.0187 (15)0.0188 (15)−0.0041 (13)0.0030 (13)−0.0057 (12)
C20.043 (2)0.0305 (17)0.0203 (16)−0.0108 (15)0.0096 (14)−0.0101 (13)
C30.047 (2)0.0352 (19)0.0346 (19)−0.0062 (16)0.0157 (16)−0.0243 (16)
C40.048 (2)0.0223 (16)0.0309 (18)−0.0077 (15)0.0094 (15)−0.0160 (14)
C50.0270 (16)0.0174 (14)0.0233 (15)−0.0044 (12)−0.0005 (12)−0.0101 (12)
C60.0285 (16)0.0194 (15)0.0231 (15)−0.0067 (12)0.0006 (12)−0.0083 (12)
C70.059 (2)0.0209 (16)0.038 (2)−0.0137 (16)0.0098 (17)−0.0158 (15)
C80.065 (3)0.0225 (17)0.045 (2)−0.0208 (17)0.0118 (19)−0.0121 (16)
C90.052 (2)0.0279 (18)0.036 (2)−0.0203 (17)0.0109 (17)−0.0074 (15)
C100.042 (2)0.0252 (16)0.0267 (17)−0.0139 (15)0.0093 (14)−0.0090 (13)
C110.0227 (15)0.0181 (14)0.0152 (14)−0.0121 (12)0.0047 (11)−0.0053 (11)
C120.0224 (15)0.0181 (14)0.0134 (13)−0.0103 (11)0.0049 (11)−0.0053 (11)
C130.0213 (15)0.0167 (13)0.0178 (14)−0.0052 (11)0.0016 (11)−0.0060 (11)
C140.0206 (14)0.0207 (14)0.0160 (14)−0.0063 (12)0.0026 (11)−0.0078 (11)
C150.0338 (18)0.0276 (17)0.0179 (15)0.0100 (14)−0.0024 (13)−0.0063 (13)
C160.0251 (16)0.0271 (16)0.0188 (15)0.0001 (13)0.0043 (12)−0.0096 (13)
C170.0231 (15)0.0188 (14)0.0168 (14)−0.0064 (12)0.0034 (11)−0.0073 (11)
C180.0214 (15)0.0157 (13)0.0188 (14)−0.0066 (11)0.0026 (11)−0.0066 (11)
C190.0252 (15)0.0154 (13)0.0158 (14)−0.0091 (11)0.0037 (11)−0.0073 (11)
C200.0277 (17)0.0299 (17)0.0236 (16)−0.0023 (13)0.0046 (13)−0.0149 (13)
C210.0308 (19)0.039 (2)0.0249 (17)0.0097 (15)−0.0022 (14)−0.0140 (15)
C220.0241 (15)0.0188 (14)0.0171 (14)−0.0145 (12)0.0057 (11)−0.0073 (12)
C230.0207 (15)0.0122 (13)0.0231 (15)−0.0017 (11)0.0005 (12)−0.0070 (11)
C240.0207 (15)0.0157 (13)0.0227 (15)−0.0053 (11)0.0027 (11)−0.0069 (11)
C250.0184 (14)0.0184 (14)0.0233 (15)−0.0055 (11)0.0028 (11)−0.0114 (12)
C260.0177 (14)0.0148 (13)0.0232 (15)−0.0027 (11)0.0040 (11)−0.0097 (12)
C270.0308 (18)0.0354 (18)0.0309 (18)−0.0197 (15)−0.0020 (14)−0.0110 (14)
C280.0313 (18)0.0287 (17)0.0282 (17)−0.0182 (14)0.0015 (13)−0.0044 (14)
Geometric parameters (Å, º) top
Nd1—O52.386 (2)C4—H40.95
Nd1—O3i2.399 (2)C5—C61.484 (4)
Nd1—O4ii2.4120 (19)C6—C71.394 (4)
Nd1—O12.4309 (19)C7—C81.376 (5)
Nd1—O2iii2.4443 (19)C7—H70.95
Nd1—O72.513 (2)C8—C91.376 (5)
Nd1—N12.618 (2)C8—H80.95
Nd1—N22.659 (2)C9—C101.385 (5)
O1—C111.252 (3)C9—H90.95
O2—C111.256 (3)C10—H100.95
O2—Nd1iii2.4443 (19)C11—C121.517 (4)
O3—C221.255 (4)C12—C161.379 (4)
O3—Nd1iv2.399 (2)C12—C131.392 (4)
O4—C221.252 (3)C13—C141.392 (4)
O4—Nd1ii2.4120 (19)C13—H130.95
O5—C231.267 (4)C14—C171.494 (4)
O6—C231.246 (4)C15—C161.384 (4)
O7—H7A0.8298C15—H150.95
O7—H7B0.8078C16—H160.95
N1—C11.341 (4)C17—C181.388 (4)
N1—C51.351 (4)C18—C191.385 (4)
N2—C101.342 (4)C18—H180.95
N2—C61.350 (4)C19—C201.386 (4)
N3—C151.338 (4)C19—C221.512 (4)
N3—C141.344 (4)C20—C211.384 (5)
N4—C211.337 (4)C20—H200.95
N4—C171.343 (4)C21—H210.95
N5—C271.336 (4)C23—C241.512 (4)
N5—C261.347 (4)C24—C281.380 (4)
C1—C21.376 (4)C24—C251.384 (4)
C1—H10.95C25—C261.390 (4)
C2—C31.379 (5)C25—H250.95
C2—H20.95C26—C26v1.488 (6)
C3—C41.374 (5)C27—C281.391 (5)
C3—H30.95C27—H270.95
C4—C51.390 (4)C28—H280.95
O5—Nd1—O3i141.66 (7)C6—C7—H7120.1
O5—Nd1—O4ii85.16 (7)C9—C8—C7119.3 (3)
O3i—Nd1—O4ii123.72 (7)C9—C8—H8120.4
O5—Nd1—O185.06 (7)C7—C8—H8120.4
O3i—Nd1—O181.99 (7)C8—C9—C10118.0 (3)
O4ii—Nd1—O171.54 (7)C8—C9—H9121
O5—Nd1—O2iii142.08 (7)C10—C9—H9121
O3i—Nd1—O2iii72.10 (7)N2—C10—C9123.9 (3)
O4ii—Nd1—O2iii83.53 (7)N2—C10—H10118.1
O1—Nd1—O2iii124.64 (7)C9—C10—H10118.1
O5—Nd1—O773.07 (7)O1—C11—O2125.5 (3)
O3i—Nd1—O7136.56 (7)O1—C11—C12117.3 (2)
O4ii—Nd1—O770.18 (7)O2—C11—C12117.2 (2)
O1—Nd1—O7137.04 (7)C16—C12—C13118.2 (3)
O2iii—Nd1—O769.04 (7)C16—C12—C11120.5 (3)
O5—Nd1—N182.69 (7)C13—C12—C11121.3 (2)
O3i—Nd1—N184.74 (7)C12—C13—C14119.2 (3)
O4ii—Nd1—N1143.82 (8)C12—C13—H13120.4
O1—Nd1—N1140.45 (7)C14—C13—H13120.4
O2iii—Nd1—N185.45 (7)N3—C14—C13122.8 (3)
O7—Nd1—N173.68 (7)N3—C14—C17115.7 (2)
O5—Nd1—N272.54 (7)C13—C14—C17121.5 (3)
O3i—Nd1—N269.59 (7)N3—C15—C16124.1 (3)
O4ii—Nd1—N2144.11 (7)N3—C15—H15118
O1—Nd1—N278.68 (7)C16—C15—H15118
O2iii—Nd1—N2130.91 (7)C12—C16—C15118.8 (3)
O7—Nd1—N2126.03 (7)C12—C16—H16120.6
N1—Nd1—N261.78 (7)C15—C16—H16120.6
C11—O1—Nd1132.49 (18)N4—C17—C18122.9 (3)
C11—O2—Nd1iii152.00 (19)N4—C17—C14116.5 (2)
C22—O3—Nd1iv124.74 (17)C18—C17—C14120.6 (3)
C22—O4—Nd1ii148.51 (19)C19—C18—C17119.3 (3)
C23—O5—Nd1134.30 (17)C19—C18—H18120.3
Nd1—O7—H7A105C17—C18—H18120.3
Nd1—O7—H7B109.2C18—C19—C20118.4 (3)
H7A—O7—H7B109.9C18—C19—C22120.3 (3)
C1—N1—C5118.2 (3)C20—C19—C22121.2 (3)
C1—N1—Nd1118.68 (19)C21—C20—C19118.3 (3)
C5—N1—Nd1122.42 (19)C21—C20—H20120.8
C10—N2—C6117.7 (3)C19—C20—H20120.8
C10—N2—Nd1120.7 (2)N4—C21—C20124.2 (3)
C6—N2—Nd1121.29 (19)N4—C21—H21117.9
C15—N3—C14116.9 (3)C20—C21—H21117.9
C21—N4—C17116.9 (3)O4—C22—O3125.5 (3)
C27—N5—C26117.3 (3)O4—C22—C19117.3 (3)
N1—C1—C2123.4 (3)O3—C22—C19117.1 (2)
N1—C1—H1118.3O6—C23—O5125.5 (3)
C2—C1—H1118.3O6—C23—C24118.5 (3)
C1—C2—C3118.2 (3)O5—C23—C24116.1 (2)
C1—C2—H2120.9C28—C24—C25118.7 (3)
C3—C2—H2120.9C28—C24—C23121.0 (3)
C4—C3—C2119.4 (3)C25—C24—C23120.3 (3)
C4—C3—H3120.3C24—C25—C26119.4 (3)
C2—C3—H3120.3C24—C25—H25120.3
C3—C4—C5119.6 (3)C26—C25—H25120.3
C3—C4—H4120.2N5—C26—C25122.4 (3)
C5—C4—H4120.2N5—C26—C26v116.1 (3)
N1—C5—C4121.2 (3)C25—C26—C26v121.5 (3)
N1—C5—C6116.8 (3)N5—C27—C28123.8 (3)
C4—C5—C6122.0 (3)N5—C27—H27118.1
N2—C6—C7121.3 (3)C28—C27—H27118.1
N2—C6—C5116.7 (3)C24—C28—C27118.4 (3)
C7—C6—C5121.9 (3)C24—C28—H28120.8
C8—C7—C6119.8 (3)C27—C28—H28120.8
C8—C7—H7120.1
Symmetry codes: (i) x, y, z+1; (ii) −x+1, −y+1, −z; (iii) −x+1, −y+1, −z+1; (iv) x, y, z−1; (v) −x, −y+2, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O60.831.922.731 (3)164
O7—H7A···O50.832.532.918 (3)110
O7—H7B···O6vi0.812.022.811 (3)165
Symmetry code: (vi) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Nd2(C12H6N2O4)3(C10H8N2)2(H2O)2]
Mr681.72
Crystal system, space groupTriclinic, P1
Temperature (K)200
a, b, c (Å)8.9914 (2), 12.5409 (3), 12.7455 (3)
α, β, γ (°)67.809 (2), 88.645 (2), 75.437 (1)
V (Å3)1283.89 (6)
Z2
Radiation typeMo Kα
µ (mm−1)2.08
Crystal size (mm)0.5 × 0.4 × 0.2
Data collection
DiffractometerNonius KappaCCD
Absorption correctionMulti-scan
(SORTAV; Blessing, 1995)
Tmin, Tmax0.398, 0.660
No. of measured, independent and
observed [I > 2σ(I)] reflections		16411, 4669, 4460
Rint0.042
(sin θ/λ)max (Å−1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.061, 1.17
No. of reflections4669
No. of parameters371
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.56, −0.97

Computer programs: COLLECT (Nonius, 2000), DENZO and SCALEPACK (Otwinowski & Minor 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Nd1—O52.386 (2)Nd1—N22.659 (2)
Nd1—O3i2.399 (2)O1—C111.252 (3)
Nd1—O4ii2.4120 (19)O2—C111.256 (3)
Nd1—O12.4309 (19)O3—C221.255 (4)
Nd1—O2iii2.4443 (19)O4—C221.252 (3)
Nd1—O72.513 (2)O5—C231.267 (4)
Nd1—N12.618 (2)O6—C231.246 (4)
O5—Nd1—O4ii85.16 (7)O5—Nd1—N182.69 (7)
O5—Nd1—O185.06 (7)O3i—Nd1—N184.74 (7)
O3i—Nd1—O181.99 (7)O2iii—Nd1—N185.45 (7)
O4ii—Nd1—O171.54 (7)O7—Nd1—N173.68 (7)
O3i—Nd1—O2iii72.10 (7)O5—Nd1—N272.54 (7)
O4ii—Nd1—O2iii83.53 (7)O3i—Nd1—N269.59 (7)
O5—Nd1—O773.07 (7)O1—Nd1—N278.68 (7)
O4ii—Nd1—O770.18 (7)N1—Nd1—N261.78 (7)
O2iii—Nd1—O769.04 (7)
Symmetry codes: (i) x, y, z+1; (ii) −x+1, −y+1, −z; (iii) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O60.831.922.731 (3)164
O7—H7A···O50.832.532.918 (3)110
O7—H7B···O6iv0.812.022.811 (3)165
Symmetry code: (iv) −x, −y+1, −z+1.
 

Acknowledgements

The authors gratefully acknowledge the financial support of the National Science Council and Fu Jen Catholic University, Taiwan.

References

First citationBlessing, R. H. (1995). Acta Cryst. A51, 33–38.  CrossRef CAS Web of Science IUCr Journals Google Scholar
 First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
 First citationFarrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.  CrossRef CAS IUCr Journals Google Scholar
 First citationNonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.  Google Scholar
 First citationOtwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.  Google Scholar
 First citationSheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.  Google Scholar
 First citationWu, J.-Y., Yeh, T.-T., Wen, Y.-S., Twu, J. & Lu, K.-L. (2006). Cryst. Growth Des. 6, 467–473.  Web of Science CSD CrossRef CAS Google Scholar

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ISSN: 2056-9890
Volume 64| Part 1| January 2008| Pages m260-m261
https://doi.org/10.1107/S1600536807067396
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