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Acta Cryst. (2007). E63, m2203-m2204    [ doi:10.1107/S160053680702884X ]

Reinvestigation of layered poly[aquasodium(I) [[aquasamarium(III)]-di-[mu]-aqua-[mu]3-pyridine-2,6-dicarboxylato-[mu]2-pyridine-2,6-dicarboxylato] trihydrate]

K. Ikarashi, Z. Taoyun, K. Uematsu, K. Toda and M. Sato

Abstract top

The crystal structure of the title compound, {[NaSm(C7H3NO4)2(H2O)4]·3H2O}n, was first reported by van Albada, Gorter & Reedijk [(1999), Polyhedron, 18, 1821-1824]. It has now been reinvestigated and confirmed from single-crystal data, giving greater understanding of the role of the water molecules. The two-dimensional layers found in the compound are built up from six-coordinate NaO6 polyhedra and nine-coordinate SmN2O7 polyhedra. The former share edges with each other along the c axis and the latter are bridged by carboxylate groups of pyridine-2,6-dicarboxylate anions along the b axis. Eight-membered rings of water molecules, connected to one another by hydrogen bonding, are formed in the interlayer spaces.

Comment top

The use of rare earth elements for constructing metal-organic frameworks (MOFs) has been attracted much attention due to their variety of magnetic and optical properties (Benelli & Gatteschi, 2002). Since rare earth ions have a large radius and much affinity for oxygen atoms of ligands, pyridine-2,6-dicarboxylic acid (H2dipic) is widely studied for constructing MOFs containing rare earth elements (Brouca-Cabarrecq et al., 2002;. Duan et al., 2004; Ghosh & Bharadwaj, 2003). Hydrogen-bonding involving water molecules plays an important role in self-assembly processes for building MOF architectures. The structure of the title compound has already been reported (van Albada et al., 1999), but the role of water molecules was not fully understood. We here report the X-ray crystal structure analysis of the compound, and demonstrate a unique hydogen-bonding cluster of water molecules located in interlayer spaces.

A samarium(III) ion is coordinated by two dipic molecules and three water molecules, forming ninefolded coordination environment with four carboxylic oxygen atoms, two dipic nitrogen atoms, and three oxygen atoms of water molecules (Fig.1). All the bond distances for Sm—O and Na—O are comparable to those reported previously (van Albada et al., 1999). The asymmetric unit involves seven water molecules, which are classified into two groups; one is the molecules coordinating metal ions (O1W, O2W, O3W, and O5W) and the other the molecules isolated as a water of crystallization (O4W, O6W, and O7W) with relatively large thermal vibration ellipsoids. The structure can be described as a layered structure, which consists of metallic coordination polymer layers, separated by an interlamellar region populated by water molecules of crystallization. In the layer block, chains are constructed by the ninefolded samarium polyhedra and the sodium octahedra with edge-sharing fashion, running along the direction parallel to the c axis. Each chain is bridged by carboxylate groups of the embedded dipic molecules to adjacent chains, thus forming a two-dimensional network. The interlayer water molecules form unique octamer clusters by hydrogen-bonding, giving eight-membered rings (Fig.2). The atoms O4W, O5W, O6W, and O7W are related to those of the symmetrically equivalent opposite side by the center of symmetry. The rings are tightly fixed to the two-dimensional sheets at the atoms of O5W coordinationg to Na1. In the ring, O4W behaves as hydrogen acceptors while O5W behaves as hydrogen donors, in the hydrogen-bonding scheme. Both the atoms show tetracoordination. On the other hand, the atoms O6W and O7W behave both as hydogen donors and acceptors with tricoordination. The average O···O distance in the ring is 2.796 Å, somewhat longer than that of ice (2.76 Å). The two-dimensional structure of the compound is largely a consequence of hydrogen-bonding interactions among water molecules themselves and the MOF.

Related literature top

For related literature, see: van Albada et al. (1999); Benelli & Gatteschi (2002); Brouca-Cabarrecq et al. (2002); Duan et al. (2004); Ghosh & Bharadwaj (2003).

Experimental top

The title compound was hydrothermally synthesized at 150°C for 72 h in a 40 ml Teflon-lined steel autoclave under autogenous pressure. The starting solution was prepared by mixing Na2MoO4.2H2O, Sm2O3, NaCl, pyridine-2,6-dicarboxylic acid, and deionized water with a molar ratio of 2:1:2:1:555 (total volume, 15 ml), and its pH value was adjusted to 3.05 by hydrochloric acid. After the hydrothermal reaction, the autoclave was slowly cooled to room temperature, and colorless crystals were produced.

Refinement top

The H atoms bonded to a C atom were positioned geometrically after each cycle in idealized locations and refined as riding on their parent C atoms with C—H = 0.93 Å and Uiso(H) = 1.2Uiso(C atom). All the hydrogen atoms bonded to an O atom of water molecules were located in a difference Fourier map, and isotropically refined with distance restraints of O—H = 0.85 Å and H—H = 0.93 Å, and with Uiso(H) = 1.5Uiso(O atom). The maximum and minimum electron-density peaks are located at 1.23 and 0.82 Å, respectively, from Sm1.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); 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 asymmetric unit of the compound with displacement ellipsoids drawn at the 50% probability level (arbitrary spheres for H atoms).
[Figure 2] Fig. 2. The hydrogen-bondings between water molecules in an eight-membered ring. [Symmetry codes: (i) x + 1, y, z; (ii) -x + 1, y + 1/2, -z + 3/2; (iii) -x + 1, y + 1/2, -z + 1/2; (iv) -x, y + 1/2, -z + 3/2; (v) -x + 1, -y + 1, -z + 1; (vi) -x, -y + 1, -z + 1; (vii) x + 1, -y - 1/2, z - 3/2; (viii) x, -y - 1/2, z - 3/2;].
poly[aquasodium(I) [[aquasamarium(III)]- di-µ-aqua-µ3-pyridine-2,6-dicarboxylato-µ2-pyridine-2,6-dicarboxylato] trihydrate] top
Crystal data top
[NaSm(C7H3NO4)2(H2O)4]·3H2OF(000) = 1244
Mr = 629.66Dx = 1.9 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 19188 reflections
a = 11.2065 (4) Åθ = 2.2–30.0°
b = 17.4485 (3) ŵ = 2.77 mm−1
c = 11.3728 (4) ÅT = 296 K
β = 98.163 (1)°Plate, colourless
V = 2201.27 (12) Å30.30 × 0.18 × 0.04 mm
Z = 4
Data collection top
Rigaku R-AXIS-IV
diffractometer		5944 reflections with I > 2σ(I)
Detector resolution: 10.00 pixels mm-1Rint = 0.046
ω scansθmax = 30.0°, θmin = 1.8°
Absorption correction: numerical
(ABSCOR; Higashi, 1999)		h = −15→15
Tmin = 0.558, Tmax = 0.895k = −22→22
22103 measured reflectionsl = −15→15
6163 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.081 w = 1/[σ2(Fo2) + (0.0403P)2 + 2.6934P]
where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max < 0.001
6163 reflectionsΔρmax = 0.97 e Å−3
341 parametersΔρmin = −1.28 e Å−3
21 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00064 (16)
Crystal data top
[NaSm(C7H3NO4)2(H2O)4]·3H2OV = 2201.27 (12) Å3
Mr = 629.66Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.2065 (4) ŵ = 2.77 mm−1
b = 17.4485 (3) ÅT = 296 K
c = 11.3728 (4) Å0.30 × 0.18 × 0.04 mm
β = 98.163 (1)°
Data collection top
Rigaku R-AXIS-IV
diffractometer		6163 independent reflections
Absorption correction: numerical
(ABSCOR; Higashi, 1999)		5944 reflections with I > 2σ(I)
Tmin = 0.558, Tmax = 0.895Rint = 0.046
22103 measured reflectionsθmax = 30.0°
Refinement top
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.081Δρmax = 0.97 e Å−3
S = 1.17Δρmin = −1.28 e Å−3
6163 reflectionsAbsolute structure: ?
341 parametersFlack parameter: ?
21 restraintsRogers parameter: ?
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
Sm10.102796 (11)0.181254 (7)0.774431 (10)0.01333 (6)
Na10.08028 (12)0.37858 (7)0.61494 (11)0.0256 (2)
N110.3268 (2)0.15540 (13)0.78946 (18)0.0169 (4)
O110.3317 (2)0.14824 (14)0.48054 (17)0.0274 (5)
O120.18328 (19)0.16788 (12)0.58886 (17)0.0198 (4)
O130.3800 (2)0.17141 (15)1.10109 (19)0.0303 (5)
O140.21058 (18)0.16585 (13)0.97242 (17)0.0210 (4)
C110.2934 (3)0.15591 (16)0.5767 (2)0.0185 (5)
C120.3796 (2)0.15293 (17)0.6910 (2)0.0197 (5)
C130.5037 (3)0.1523 (2)0.6958 (3)0.0342 (7)
H130.53870.14880.62670.041*
C140.5747 (3)0.1570 (3)0.8057 (3)0.0437 (9)
H140.65830.15690.81120.052*
C150.5201 (3)0.1618 (3)0.9069 (3)0.0360 (8)
H150.56610.16650.98130.043*
C160.3956 (3)0.15934 (18)0.8955 (2)0.0210 (5)
C170.3240 (3)0.16562 (17)0.9990 (2)0.0196 (5)
N21−0.0648 (2)0.11795 (13)0.63391 (19)0.0173 (4)
O21−0.03307 (18)0.26630 (11)0.64738 (17)0.0212 (4)
O22−0.2002 (2)0.28990 (13)0.5209 (2)0.0285 (5)
O230.10578 (18)0.04169 (13)0.76633 (17)0.0238 (4)
O240.0160 (2)−0.07055 (12)0.7216 (2)0.0291 (5)
C21−0.1269 (2)0.24589 (16)0.5790 (2)0.0188 (5)
C22−0.1463 (2)0.16042 (17)0.5652 (2)0.0187 (5)
C23−0.2356 (3)0.12771 (19)0.4838 (3)0.0280 (6)
H23−0.29190.15810.43730.034*
C24−0.2390 (3)0.0490 (2)0.4735 (3)0.0345 (7)
H24−0.29720.02560.41870.041*
C25−0.1552 (3)0.00475 (18)0.5450 (3)0.0280 (6)
H25−0.1564−0.04840.53950.034*
C26−0.0693 (2)0.04196 (16)0.6252 (2)0.0190 (5)
C270.0243 (3)−0.00019 (15)0.7095 (2)0.0195 (5)
O1W−0.0451 (2)0.12687 (13)0.9033 (2)0.0277 (4)
H1W−0.0940.15910.9270.042*
H2W−0.0840.08630.8800.042*
O2W0.21951 (19)0.30604 (12)0.75680 (18)0.0214 (4)
H3W0.2480.3260.82310.032*
H4W0.2720.3080.7100.032*
O3W0.03015 (19)0.28534 (12)0.89442 (16)0.0199 (4)
H5W0.0060.32470.8540.03*
H6W0.0830.29810.9520.03*
O4W0.2530 (3)−0.05242 (17)0.9220 (2)0.0394 (6)
H7W0.231−0.09930.9240.059*
H8W0.205−0.0290.8680.059*
O5W0.1904 (2)0.49655 (15)0.6342 (2)0.0356 (5)
H9W0.2200.5060.5710.053*
H10W0.2470.4920.6920.053*
O6W0.5694 (4)0.4115 (4)0.7266 (4)0.110 (2)
H11W0.5170.3870.6800.165*
H12W0.6190.4320.6860.165*
O7W0.3811 (4)0.4793 (2)0.8188 (3)0.0625 (9)
H13W0.3900.4500.8790.094*
H14W0.4380.4710.7780.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.01602 (8)0.01226 (9)0.01101 (7)−0.00069 (4)−0.00049 (5)0.00020 (3)
Na10.0319 (6)0.0210 (6)0.0238 (6)−0.0002 (5)0.0037 (5)0.0002 (4)
N110.0193 (10)0.0185 (11)0.0118 (9)0.0019 (8)−0.0016 (7)0.0002 (7)
O110.0312 (11)0.0386 (13)0.0126 (8)0.0042 (9)0.0038 (8)−0.0025 (8)
O120.0197 (9)0.0253 (10)0.0138 (8)−0.0002 (7)0.0004 (7)−0.0016 (7)
O130.0259 (11)0.0509 (15)0.0127 (9)0.0062 (9)−0.0026 (8)−0.0020 (8)
O140.0193 (9)0.0286 (10)0.0147 (8)0.0002 (8)0.0015 (7)0.0014 (7)
C110.0245 (13)0.0156 (13)0.0146 (11)0.0025 (9)−0.0002 (9)−0.0010 (8)
C120.0210 (12)0.0242 (14)0.0140 (10)0.0012 (10)0.0031 (9)−0.0004 (9)
C130.0211 (14)0.060 (2)0.0218 (14)0.0070 (14)0.0054 (11)0.0024 (14)
C140.0154 (14)0.088 (3)0.0279 (16)0.0085 (16)0.0023 (12)−0.0003 (18)
C150.0208 (14)0.065 (2)0.0206 (14)0.0042 (14)−0.0029 (11)−0.0033 (14)
C160.0209 (12)0.0282 (14)0.0129 (11)0.0044 (10)−0.0010 (9)0.0009 (9)
C170.0236 (13)0.0201 (13)0.0143 (11)0.0043 (10)0.0000 (9)0.0007 (9)
N210.0206 (10)0.0140 (11)0.0166 (9)−0.0019 (8)0.0002 (8)0.0002 (7)
O210.0221 (10)0.0172 (10)0.0221 (9)−0.0009 (7)−0.0038 (7)0.0009 (7)
O220.0259 (11)0.0232 (12)0.0339 (11)0.0036 (8)−0.0048 (9)0.0076 (8)
O230.0278 (11)0.0148 (11)0.0264 (10)0.0013 (7)−0.0044 (8)−0.0002 (7)
O240.0401 (13)0.0142 (10)0.0322 (11)−0.0027 (8)0.0026 (9)0.0016 (7)
C210.0206 (12)0.0170 (13)0.0179 (11)0.0002 (9)−0.0003 (9)0.0017 (8)
C220.0191 (12)0.0182 (13)0.0175 (11)−0.0025 (9)−0.0020 (9)0.0026 (9)
C230.0269 (14)0.0286 (16)0.0249 (13)−0.0031 (11)−0.0082 (11)0.0030 (11)
C240.0350 (17)0.0297 (18)0.0338 (16)−0.0102 (13)−0.0128 (13)−0.0042 (12)
C250.0348 (16)0.0182 (15)0.0287 (14)−0.0070 (11)−0.0030 (12)−0.0040 (10)
C260.0233 (12)0.0159 (12)0.0171 (11)−0.0041 (9)0.0008 (9)−0.0017 (8)
C270.0283 (13)0.0134 (12)0.0174 (11)0.0006 (9)0.0051 (9)0.0007 (8)
O1W0.0303 (11)0.0241 (11)0.0311 (11)−0.0060 (8)0.0124 (9)−0.0066 (8)
O2W0.0251 (10)0.0217 (10)0.0175 (9)−0.0034 (8)0.0031 (7)−0.0020 (7)
O3W0.0260 (10)0.0184 (10)0.0144 (8)0.0001 (7)−0.0004 (7)−0.0009 (6)
O4W0.0395 (14)0.0407 (16)0.0358 (13)0.0055 (11)−0.0021 (10)0.0070 (11)
O5W0.0414 (14)0.0278 (13)0.0396 (13)0.0008 (10)0.0124 (11)0.0022 (10)
O6W0.055 (2)0.204 (6)0.077 (3)−0.058 (3)0.026 (2)−0.071 (4)
O7W0.071 (2)0.065 (2)0.054 (2)−0.0094 (18)0.0177 (17)0.0094 (16)
Geometric parameters (Å, °) top
Sm1—O142.4144 (19)C15—H150.93
Sm1—O122.4213 (19)C16—C171.520 (4)
Sm1—O232.437 (2)N21—C261.330 (3)
Sm1—O212.4460 (19)N21—C221.338 (3)
Sm1—O3W2.478 (2)O21—C211.267 (3)
Sm1—N112.533 (2)O22—C211.243 (3)
Sm1—N212.540 (2)O23—C271.272 (3)
Sm1—O1W2.547 (2)O24—C271.240 (3)
Sm1—O2W2.562 (2)O24—Na1iv2.445 (3)
Sm1—Na13.8831 (12)C21—C221.512 (4)
Sm1—Na1i4.0532 (12)C22—C231.386 (4)
Na1—O212.392 (2)C23—C241.379 (5)
Na1—O5W2.394 (3)C23—H230.93
Na1—O2W2.434 (3)C24—C251.387 (5)
Na1—O24ii2.445 (3)C24—H240.93
Na1—O14iii2.456 (2)C25—C261.389 (4)
Na1—O1Wiii2.610 (3)C25—H250.93
Na1—Sm1iii4.0532 (12)C26—C271.509 (4)
Na1—H4W2.58O1W—Na1i2.610 (3)
N11—C161.338 (3)O1W—H1W0.851
N11—C121.339 (3)O1W—H2W0.854
O11—C111.238 (3)O2W—H3W0.848
O12—C111.278 (3)O2W—H4W0.849
O13—C171.243 (3)O3W—H5W0.851
O14—C171.264 (3)O3W—H6W0.845
O14—Na1i2.456 (2)O4W—H7W0.856
C11—C121.506 (4)O4W—H8W0.855
C12—C131.384 (4)O5W—H9W0.848
C13—C141.385 (5)O5W—H10W0.852
C13—H130.93O6W—H11W0.854
C14—C151.380 (5)O6W—H12W0.854
C14—H140.93O7W—H13W0.851
C15—C161.383 (4)O7W—H14W0.852
O14—Sm1—O12127.10 (7)O2W—Na1—H4W19.2
O14—Sm1—O2385.20 (7)O24ii—Na1—H4W106.6
O12—Sm1—O2382.06 (7)O14iii—Na1—H4W65.6
O14—Sm1—O21143.66 (7)O1Wiii—Na1—H4W132.6
O12—Sm1—O2179.70 (7)Sm1—Na1—H4W52.0
O23—Sm1—O21126.48 (6)Sm1iii—Na1—H4W96.7
O14—Sm1—O3W74.21 (7)C16—N11—C12119.3 (2)
O12—Sm1—O3W137.98 (7)C16—N11—Sm1119.38 (17)
O23—Sm1—O3W139.51 (7)C12—N11—Sm1120.03 (17)
O21—Sm1—O3W69.82 (7)C11—O12—Sm1126.48 (17)
O14—Sm1—N1163.73 (7)C17—O14—Sm1125.19 (17)
O12—Sm1—N1163.47 (7)C17—O14—Na1i120.86 (17)
O23—Sm1—N1178.80 (7)Sm1—O14—Na1i112.64 (9)
O21—Sm1—N11132.52 (7)O11—C11—O12125.1 (2)
O3W—Sm1—N11119.57 (7)O11—C11—C12119.9 (3)
O14—Sm1—N21139.98 (7)O12—C11—C12115.0 (2)
O12—Sm1—N2175.13 (7)N11—C12—C13121.8 (3)
O23—Sm1—N2163.55 (7)N11—C12—C11114.5 (2)
O21—Sm1—N2163.22 (7)C13—C12—C11123.5 (2)
O3W—Sm1—N21113.19 (7)C12—C13—C14118.8 (3)
N11—Sm1—N21127.06 (7)C12—C13—H13120.6
O14—Sm1—O1W72.65 (7)C14—C13—H13120.6
O12—Sm1—O1W145.01 (7)C15—C14—C13119.3 (3)
O23—Sm1—O1W70.31 (7)C15—C14—H14120.4
O21—Sm1—O1W99.49 (8)C13—C14—H14120.4
O3W—Sm1—O1W70.40 (7)C14—C15—C16118.7 (3)
N11—Sm1—O1W127.92 (8)C14—C15—H15120.6
N21—Sm1—O1W73.54 (7)C16—C15—H15120.6
O14—Sm1—O2W88.52 (7)N11—C16—C15122.0 (3)
O12—Sm1—O2W75.89 (7)N11—C16—C17113.7 (2)
O23—Sm1—O2W146.73 (7)C15—C16—C17124.2 (3)
O21—Sm1—O2W73.75 (7)O13—C17—O14125.4 (3)
O3W—Sm1—O2W68.38 (7)O13—C17—C16118.5 (3)
N11—Sm1—O2W69.18 (7)O14—C17—C16116.0 (2)
N21—Sm1—O2W131.34 (7)C26—N21—C22119.5 (2)
O1W—Sm1—O2W137.96 (7)C26—N21—Sm1119.82 (18)
O14—Sm1—Na1121.67 (6)C22—N21—Sm1120.60 (18)
O12—Sm1—Na171.69 (5)C21—O21—Na1123.25 (17)
O23—Sm1—Na1150.29 (5)C21—O21—Sm1125.80 (18)
O21—Sm1—Na136.14 (5)Na1—O21—Sm1106.76 (8)
O3W—Sm1—Na166.59 (5)C27—O23—Sm1125.49 (18)
N11—Sm1—Na1100.81 (6)C27—O24—Na1iv119.5 (2)
N21—Sm1—Na195.65 (5)O22—C21—O21125.5 (3)
O1W—Sm1—Na1126.50 (6)O22—C21—C22118.7 (2)
O2W—Sm1—Na137.82 (5)O21—C21—C22115.8 (2)
O14—Sm1—Na1i34.01 (5)N21—C22—C23122.0 (3)
O12—Sm1—Na1i152.80 (5)N21—C22—C21114.2 (2)
O23—Sm1—Na1i77.40 (5)C23—C22—C21123.7 (3)
O21—Sm1—Na1i127.06 (5)C24—C23—C22118.4 (3)
O3W—Sm1—Na1i65.96 (5)C24—C23—H23120.8
N11—Sm1—Na1i94.89 (5)C22—C23—H23120.8
N21—Sm1—Na1i110.38 (5)C23—C24—C25119.8 (3)
O1W—Sm1—Na1i38.75 (6)C23—C24—H24120.1
O2W—Sm1—Na1i113.29 (5)C25—C24—H24120.1
Na1—Sm1—Na1i131.76 (2)C24—C25—C26118.3 (3)
O21—Na1—O5W165.54 (10)C24—C25—H25120.9
O21—Na1—O2W77.07 (8)C26—C25—H25120.9
O5W—Na1—O2W96.48 (9)N21—C26—C25122.0 (3)
O21—Na1—O24ii83.03 (8)N21—C26—C27115.0 (2)
O5W—Na1—O24ii84.01 (9)C25—C26—C27122.9 (3)
O2W—Na1—O24ii89.74 (8)O24—C27—O23124.9 (3)
O21—Na1—O14iii102.81 (8)O24—C27—C26119.8 (3)
O5W—Na1—O14iii89.13 (9)O23—C27—C26115.3 (2)
O2W—Na1—O14iii83.57 (8)Sm1—O1W—Na1i103.62 (8)
O24ii—Na1—O14iii169.83 (10)Sm1—O1W—H1W115
O21—Na1—O1Wiii83.36 (8)Na1i—O1W—H1W91
O5W—Na1—O1Wiii108.58 (9)Sm1—O1W—H2W118
O2W—Na1—O1Wiii143.37 (9)Na1i—O1W—H2W116
O24ii—Na1—O1Wiii118.45 (9)H1W—O1W—H2W108.8
O14iii—Na1—O1Wiii70.89 (7)Na1—O2W—Sm1101.97 (8)
O21—Na1—Sm137.10 (5)Na1—O2W—H3W120
O5W—Na1—Sm1136.15 (8)Sm1—O2W—H3W114
O2W—Na1—Sm140.21 (5)Na1—O2W—H4W90
O24ii—Na1—Sm188.46 (6)Sm1—O2W—H4W119
O14iii—Na1—Sm191.32 (6)H3W—O2W—H4W109.6
O1Wiii—Na1—Sm1112.90 (6)Sm1—O3W—H5W113
O21—Na1—Sm1iii92.45 (6)Sm1—O3W—H6W112
O5W—Na1—Sm1iii101.99 (7)H5W—O3W—H6W110.0
O2W—Na1—Sm1iii112.23 (6)H7W—O4W—H8W108.0
O24ii—Na1—Sm1iii156.07 (7)Na1—O5W—H9W111
O14iii—Na1—Sm1iii33.35 (5)Na1—O5W—H10W108
O1Wiii—Na1—Sm1iii37.64 (5)H9W—O5W—H10W109.3
Sm1—Na1—Sm1iii102.07 (3)H11W—O6W—H12W108.7
O21—Na1—H4W88.4H13W—O7W—H14W109.1
O5W—Na1—H4W89.1
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x, y+1/2, −z+3/2; (iii) x, −y+1/2, z−1/2; (iv) −x, y−1/2, −z+3/2.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O22i0.851.932.753 (3)162
O1W—H2W···O5Wiv0.851.962.794 (3)165
O2W—H3W···O11i0.851.952.790 (3)169
O2W—H4W···O13iii0.851.882.725 (3)170
O3W—H5W···O24ii0.852.022.853 (3)166
O3W—H6W···O12i0.851.892.725 (3)173
O4W—H7W···O22iv0.862.082.907 (4)163
O4W—H8W···O230.861.942.779 (3)168
O5W—H9W···O4Wiii0.851.962.784 (4)163
O5W—H10W···O7W0.851.942.791 (5)177
O6W—H11W···O13iii0.851.952.789 (5)168
O6W—H12W···O4Wv0.852.032.858 (5)163
O7W—H13W···O11i0.852.222.989 (4)151
O7W—H14W···O6W0.851.962.754 (7)155
Symmetry codes: (i) x, −y+1/2, z+1/2; (iv) −x, y−1/2, −z+3/2; (iii) x, −y+1/2, z−1/2; (ii) −x, y+1/2, −z+3/2; (v) −x+1, y+1/2, −z+3/2.
Table 1
Selected geometric parameters (Å) top
Sm1—O142.4144 (19)Sm1—O2W2.562 (2)
Sm1—O122.4213 (19)Na1—O212.392 (2)
Sm1—O232.437 (2)Na1—O5W2.394 (3)
Sm1—O212.4460 (19)Na1—O2W2.434 (3)
Sm1—O3W2.478 (2)Na1—O24i2.445 (3)
Sm1—N112.533 (2)Na1—O14ii2.456 (2)
Sm1—N212.540 (2)Na1—O1Wii2.610 (3)
Sm1—O1W2.547 (2)
Symmetry codes: (i) −x, y+1/2, −z+3/2; (ii) x, −y+1/2, z−1/2.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O22iii0.851.932.753 (3)162
O1W—H2W···O5Wiv0.851.962.794 (3)165
O2W—H3W···O11iii0.851.952.790 (3)169
O2W—H4W···O13ii0.851.882.725 (3)170
O3W—H5W···O24i0.852.022.853 (3)166
O3W—H6W···O12iii0.851.892.725 (3)173
O4W—H7W···O22iv0.862.082.907 (4)163
O4W—H8W···O230.861.942.779 (3)168
O5W—H9W···O4Wii0.851.962.784 (4)163
O5W—H10W···O7W0.851.942.791 (5)177
O6W—H11W···O13ii0.851.952.789 (5)168
O6W—H12W···O4Wv0.852.032.858 (5)163
O7W—H13W···O11iii0.852.222.989 (4)151
O7W—H14W···O6W0.851.962.754 (7)155
Symmetry codes: (iii) x, −y+1/2, z+1/2; (iv) −x, y−1/2, −z+3/2; (ii) x, −y+1/2, z−1/2; (i) −x, y+1/2, −z+3/2; (v) −x+1, y+1/2, −z+3/2.
Acknowledgements top

This work was supported by a Grant-in-Aid for Scientific Research (No. 440, Panoscopic Assembling and High Ordered Functions for Rare Earth Materials, and No. 17042012) from the Ministry of Education, Culture, Sports, Science and Technology.

references
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