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Crystal structure of octa­kis­(N,N-di­methyl­formamide-κO)europium(III) tetra­cosa-μ2-oxido-dodeca­oxido-μ12-phosphato-dodeca­molybdate(VI)

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aLaboratoire de Physico-chimie des Matériaux, Faculté des Sciences de Monastir, Avenue de l'environnement, 5019 Monastir, University of Monastir, Tunisia, bFaculdade de Medicina, Veterinària, Universidade Tecnica de Lisboa, Avenida da Universidade Tecnica, 1300-477 Lisboa, Portugal, and cREQUIMTE/CQFB Departamento de Quimica, Faculdade de Ciencias e Tecnologia, Universidade Nova de Lisboa, 2829-516 Caparica, Portugal
*Correspondence e-mail: gandour_yassine@hotmail.fr

Edited by M. Weil, Vienna University of Technology, Austria (Received 17 February 2016; accepted 29 February 2016; online 4 March 2016)

In the title salt, [Eu(C3H7NO)8][PMo12O40], the asymmetric unit comprises one α-Keggin-type [PMo12O40]3− polyoxidometalate anion and one distorted dodeca­hedral [Eu(C3H7NO)8]3+ complex cation. In the crystal, the isolated polyoxidometalate anions are packed into hexa­gonally arranged rows extending parallel to [001]. The complex cations are situated between the rows and are linked to the neighbouring anions through weak C—H⋯O hydrogen-bonding inter­actions, leading to the formation of a three-dimensional network structure.

1. Chemical context

Polyoxidometalates (POMs) are versatile metal–oxygen complexes which have attracted inter­est due to their topolog­ical properties and their potential applications in catalysis, photoluminescence, electrochromism and magnetism (Long et al., 2010[Long, D. L., Tsunashima, R. & Cronin, L. (2010). Angew. Chem. Int. Ed. 49, 1736-1758.]; Pope & Müller, 2010[Pope, M. T. & Müller, A. (2010). In Polyoxometalate Chemistry: From TopologyVia Self-Assembly to Applications. Dordrecht: Kluwer.]; Coronado & Gómez-García, 1998[Coronado, E. & Gómez-García, C. J. (1998). Chem. Rev. 98, 273-296.]). Up to date, a variety of strategies have been developed and used to assemble POM-based hybrid materials by controlling reaction factors such as metal ions, organic ligands, POM species, pH, molar ratio of raw materials or reaction environments (Wang et al., 2013[Wang, X., Zhao, D., Tian, A. & Ying, J. (2013). CrystEngComm, 15, 4516-4526.]; Liu et al., 2013[Liu, D., Lu, Y., Tan, H. Q., Chen, W. L., Zhang, Z. M., Li, Y. G. & Wang, E. B. (2013). Chem. Commun. 49, 3673-3675.]). Even with these approaches, the design and synthesis of new stable polyoxidomolybdate complexes are still challenging.

[Scheme 1]

Herein, we report on the synthesis, UV–vis and IR spectra along with the crystal structure of the hybrid europium(III) POM title compound, [Eu(C3H7NO)8][PMo12O40], (I)[link].

2. Structural commentary

The structures of the mol­ecular components of compound (I)[link] are illustrated in Fig. 1[link]. The [PMo12O40]3− polyoxidoanion of (I)[link] exhibits a classical α-Keggin-type structure. The central P atom is tetra­hedrally surrounded with all four oxygen atoms (Oa) linked to four Mo3O13 moieties. The latter species are fused together by sharing corner atoms (Ob) and consist of three MoO6 octa­hedra condensed in a triangular arrangement by sharing edges (Oc). There is also a terminal oxygen atom (Od) in every MoO6 octa­hedron. The P—O bond lengths range from 1.521 (5) Å to 1.536 (4) Å and the Mo—O bond lengths from 1.690 (5) Å to 2.438 (4) Å. The O—P—O angles [109.1 (2)–109.8 (3)°] indicate only a slight distortion of the central PO4 tetra­hedron. The EuIII cation is coordinated by eight di­methyl­formamide ligands through their oxygen atoms with Eu—O distances from 2.369 (5) to 2.416 (6) Å. These values are comparable to those of related oxido-europium(III) species, e.g for the [Eu(thd)3(DMF)2] complex (thd is the ion of 2,2,6,6-tetra­methyl-3,5-hepta­nedione) with Eu—O = 2.494 (5)–2.442 (5) Å (Cunningham & Siever, 1980[Cunningham, J. A. & Sievers, R. E. (1980). Inorg. Chem. 19, 595-604.]). Calculations with the SHAPE software (Alvarez et al., 2005[Alvarez, S., Alemany, P., Casanova, D., Cirera, J., Llunell, M. & Avnir, D. (2005). Coord. Chem. Rev. 249, 1693-1708.]) indicate that the coordination polyhedron of EuIII is a slightly distorted dodeca­hedron approaching mol­ecular D2d symmetry (Casanova et al., 2005[Casanova, D., Llunell, M., Alemany, P. & Alvarez, S. (2005). Chem. Eur. J. 11, 1479-1494.]).

[Figure 1]
Figure 1
The mol­ecular structures of the cation and anion in compound (I)[link], showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity.

3. Supra­molecular features

The unit cell content of the title compound is illustrated in Fig. 2[link]. In the crystal structure of (I)[link], each [Eu(DMF)8]3+ cation is linked to four neighbouring α-Keggin-type [PMo12O40]3− anions through C—H⋯O hydrogen-bonding inter­actions between the methyl groups of the DMF ligands and the terminal-oxygen (Od) and the bridging-oxygen atoms (Ob,c) of the [PMo12O40]3− anions (Fig. 3[link], Table 1[link]). The C(donor)⋯Od(acceptor) distances are between 3.174 (10) and 3.541 (11) Å while the C⋯O(b,c) distances are between 3.289 (11) and 3.473 (12) Å. In the crystal packing, the POM anions are packed into hexa­gonally arranged rows extending parallel to [001] with the [Eu(DMF)8]3+ cations located between the rows (Fig. 4[link]).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C3—H4⋯O31i 0.96 2.72 3.289 (11) 118
C4—H7⋯O36ii 0.96 2.61 3.476 (12) 150
C7—H13⋯O7 0.96 2.65 3.473 (12) 145
C8—H15⋯O28ii 0.96 2.51 3.316 (13) 141
C8—H16⋯O5 0.96 2.58 3.424 (11) 147
C10—H18⋯O28ii 0.93 2.62 3.516 (10) 162
C15—H29⋯O16i 0.96 2.55 3.299 (12) 135
C15—H27⋯O32iii 0.96 2.52 3.440 (10) 160
C15—H28⋯O52iv 0.96 2.29 3.174 (10) 153
C16—H31⋯O6iii 0.96 2.63 3.541 (11) 159
C22—H41⋯O55 0.96 2.53 3.280 (12) 135
C22—H42⋯O11iv 0.96 2.45 3.305 (11) 149
C22—H43⋯O45 0.96 2.61 3.567 (13) 172
C23—H44⋯O17v 0.96 2.52 3.443 (11) 161
C25—H55⋯O24 0.93 2.53 3.337 (11) 145
C25—H55⋯O44 0.93 2.58 3.091 (10) 115
C28—H56⋯O36v 0.93 2.62 3.476 (11) 153
C30—H60⋯O36v 0.96 2.58 3.458 (14) 152
Symmetry codes: (i) [x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z-1]; (ii) [-x+1, -y+1, z-{\script{1\over 2}}]; (iii) x, y, z-1; (iv) [-x+1, -y, z-{\script{1\over 2}}]; (v) [x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z].
[Figure 2]
Figure 2
The contents of the unit cell of complex (I)[link]. H atoms have been omitted for clarity.
[Figure 3]
Figure 3
C—H⋯O hydrogen bonds (dashed lines) link one [Eu(dmf)8]3+ cation to four neighbouring α-Keggin-type [PMo12O40]3− anions. Symmetry codes refer to Table 1[link].
[Figure 4]
Figure 4
The crystal packing of (I)[link] with the [PMo12O40]3− anions in polyhedral representation.

4. Synthesis and crystallization

The starting material [(C4H9)4N)4H3][PMo11O39] was prepared using a literature method (Combs-Walker & Hill, 1998[Combs-Walker, L. A. & Hill, C. L. (1991). Inorg. Chem. 30, 4016-4026.]). EuCl3·6H2O (361.41 mg, 1 mmol) and isonicotinic acid (C6H5NO2) (123.11 mg, 1 mmol) were dissolved in 10 ml of di­methyl­formamide. This solution was added dropwise to a yellow di­methyl­formamide solution of [(C4H9)4N)4H3][PMo11O39] (0.33 mmol in 10 ml). The mixture was heated under stirring for 1 h at 333 K. Single crystals of the title compounds were obtained by slow diffusion of 2-propanol through the di­methyl­formamide solution. UV–vis spectrum in di­methyl­formamide: λmax (nm) 315 and 205.

5. FT–IR spectroscopy

The FT–IR spectrum was recorded in the range 4000–400 cm−1 on a Nicolet 470 FT–IR spectrophotometer with pressed KBr pellets.

The FT–IR spectrum of (I)[link] (Fig. 5[link]) exhibits characteristic bands attributed to the stretching and deformation modes of the Mo—O bond vibration of the [PMo12O40]3− anion in the region 1100–400 cm−1. Thus, the asymmetric vibration νas(P—Oa), νas(Mo=Od), νas(Mo—Ob—Mo) and νas(Mo—Oc—Mo) appear at 1065, 951, 885 and 974 cm−1, respectively (Masteri-Farahani & Shahbazi, 2012[Masteri-Farahani, M. & Shahbazi, S. (2012). Inorg. Chem. Commun. 15, 297-300.]). The absorption bands at 1265 and 1657 cm−1 are characteristic of the asymmetric vibration of the C—N and the C=O bonds, respectively. The vibration bands at 1115, 1440, 1385 and 2964 cm−1 are attributed to the vibration ρ(CH3) (rocking vibration), δa(CH3), δs(CH3) and ν(C-H) of the di­methyl­formamide ligand (Durgaprasad et al., 1971[Durgaprasad, G., Sathyanarayana, D. N. & Patel, C. C. (1971). Bull. Chem. Soc. Jpn, 44, 316-322.]).

[Figure 5]
Figure 5
The FT–IR spectrum of (I)[link].

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2[link]. Hydrogen atoms were placed in calculated positions and refined as riding atoms: C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for methine groups and C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl groups. The refined Flack parameter (Parsons et al., 2013[Parsons, S., Flack, H. D. & Wagner, T. (2013). Acta Cryst. B69, 249-259.]) of −0.015 (7) indicates the correct determination of the absolute structure.

Table 2
Experimental details

Crystal data
Chemical formula [Eu(C3H7NO)8][PMo12O40]
Mr 2558.97
Crystal system, space group Orthorhombic, Pna21
Temperature (K) 296
a, b, c (Å) 26.9108 (10), 18.3506 (6), 13.4494 (4)
V3) 6641.7 (4)
Z 4
Radiation type Mo Kα
μ (mm−1) 3.24
Crystal size (mm) 0.20 × 0.18 × 0.17
 
Data collection
Diffractometer Bruker APEXII CCD
Absorption correction Multi-scan (SADABS; Bruker, 2006[Bruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.])
Tmin, Tmax 0.667, 0.747
No. of measured, independent and observed [I > 2σ(I)] reflections 88354, 33285, 19583
Rint 0.075
(sin θ/λ)max−1) 0.849
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.095, 0.98
No. of reflections 33285
No. of parameters 863
No. of restraints 1
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 2.08, −1.80
Absolute structure Flack x determined using 6924 quotients [(I+)−(I)]/[(I+)+(I)]
Absolute structure parameter −0.015 (7)
Computer programs: APEX2 and SAINT (Bruker, 2006[Bruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]), SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]), SHELXL2014 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]), ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]), DIAMOND (Putz & Brandenburg, 2014[Putz, H. & Brandenburg, K. (2014). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).

Supporting information


Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Putz & Brandenburg, 2014); software used to prepare material for publication: WinGX (Farrugia, 2012).

Octakis(N,N-dimethylformamide-κO)europium(III) tetracosa-µ2-oxido-dodecaoxido-µ12-phosphato-dodecamolybdate(VI) top
Crystal data top
[Eu(C3H7NO)8][PMo12O40]Dx = 2.559 Mg m3
Mr = 2558.97Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pna21Cell parameters from 9528 reflections
a = 26.9108 (10) Åθ = 3.0–32.3°
b = 18.3506 (6) ŵ = 3.24 mm1
c = 13.4494 (4) ÅT = 296 K
V = 6641.7 (4) Å3Prism, yellow
Z = 40.20 × 0.18 × 0.17 mm
F(000) = 4888
Data collection top
Bruker APEXII CCD
diffractometer
19583 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.075
φ and ω scansθmax = 37.1°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2006)
h = 4145
Tmin = 0.667, Tmax = 0.747k = 3131
88354 measured reflectionsl = 2122
33285 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)] = 0.047H-atom parameters constrained
wR(F2) = 0.095 w = 1/[σ2(Fo2) + (0.035P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
33285 reflectionsΔρmax = 2.08 e Å3
863 parametersΔρmin = 1.80 e Å3
1 restraintAbsolute structure: Flack x determined using 6924 quotients [(I+)-(I-)]/[(I+)+(I-)]
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.015 (7)
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 > 2σ(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
Eu10.62226 (2)0.24667 (2)0.27301 (3)0.03117 (7)
Mo10.26680 (2)0.18597 (3)0.63650 (5)0.03332 (13)
Mo20.30169 (2)0.35458 (3)0.55755 (5)0.03366 (13)
Mo30.41829 (3)0.43690 (3)0.64996 (5)0.03387 (13)
Mo40.47559 (2)0.36195 (3)0.85122 (5)0.03004 (12)
Mo50.49335 (2)0.20234 (3)0.68682 (5)0.03324 (13)
Mo60.39245 (3)0.10613 (3)0.60967 (5)0.03505 (14)
Mo70.32991 (3)0.10420 (3)0.85410 (5)0.03838 (15)
Mo80.43839 (3)0.17833 (4)0.93808 (5)0.03661 (14)
Mo90.32843 (3)0.26018 (4)0.99282 (5)0.04260 (17)
Mo100.36044 (2)0.43617 (3)0.87490 (5)0.03517 (14)
Mo110.25072 (2)0.33286 (4)0.78760 (5)0.03541 (14)
Mo120.42166 (3)0.26738 (4)0.49994 (5)0.03432 (13)
P10.37299 (6)0.26883 (8)0.74508 (12)0.0207 (3)
O10.6764 (2)0.1551 (4)0.2093 (5)0.0526 (16)
O20.2228 (2)0.1295 (3)0.5946 (5)0.0453 (14)
O30.26515 (19)0.2607 (3)0.5440 (4)0.0350 (11)
O40.34964 (18)0.4169 (3)0.6033 (4)0.0320 (10)
O50.47195 (19)0.4273 (3)0.7347 (4)0.0325 (11)
O60.5310 (2)0.3873 (3)0.8969 (4)0.0420 (13)
O70.49746 (19)0.2908 (3)0.7483 (4)0.0330 (11)
O80.45951 (19)0.1127 (2)0.6394 (4)0.0355 (11)
O90.32412 (19)0.1439 (3)0.5897 (4)0.0333 (11)
O100.3722 (2)0.0854 (3)0.7370 (4)0.0372 (12)
O110.3952 (2)0.1009 (3)0.9240 (4)0.0407 (13)
O120.45956 (19)0.2814 (3)0.9252 (4)0.0349 (11)
O130.3888 (2)0.2209 (3)1.0310 (4)0.0420 (13)
O140.3515 (2)0.3523 (3)0.9652 (4)0.0374 (12)
O150.30057 (19)0.4081 (3)0.8207 (4)0.0337 (11)
O160.1992 (2)0.3743 (4)0.8289 (5)0.0527 (16)
O170.25496 (19)0.3787 (3)0.6547 (4)0.0363 (11)
O180.22650 (19)0.2506 (3)0.7233 (4)0.0377 (12)
O190.32137 (16)0.2804 (2)0.7018 (3)0.0231 (9)
O200.36948 (17)0.2233 (2)0.8397 (3)0.0257 (9)
O210.39628 (16)0.3431 (2)0.7695 (3)0.0241 (8)
O220.40539 (17)0.2288 (2)0.6696 (3)0.0248 (9)
O230.35674 (19)0.2989 (3)0.5004 (4)0.0344 (11)
O240.4401 (3)0.2850 (4)0.3828 (4)0.0512 (15)
O250.43539 (19)0.3610 (3)0.5671 (4)0.0342 (11)
O260.48598 (18)0.2386 (3)0.5597 (4)0.0340 (11)
O270.4063 (2)0.1693 (3)0.4917 (4)0.0349 (11)
O280.3447 (2)0.5055 (3)0.9514 (5)0.0499 (15)
O290.38277 (19)0.4838 (2)0.7624 (4)0.0361 (11)
O300.43123 (19)0.4244 (3)0.9129 (4)0.0344 (11)
O310.3075 (2)0.1592 (3)0.9607 (4)0.0440 (14)
O320.4708 (2)0.1659 (3)0.8178 (4)0.0341 (11)
O330.4791 (3)0.1462 (4)1.0216 (5)0.0547 (16)
O340.2843 (2)0.1389 (3)0.7637 (4)0.0367 (11)
O350.4338 (2)0.5098 (3)0.5822 (5)0.0488 (15)
O360.2790 (2)0.3974 (3)0.4560 (4)0.0446 (14)
N10.6761 (3)0.4097 (4)0.0486 (6)0.0457 (17)
N20.5963 (3)0.3569 (4)0.5746 (5)0.0438 (16)
N30.7647 (3)0.3614 (4)0.3484 (6)0.0437 (16)
N40.5971 (3)0.1673 (3)0.0459 (5)0.0390 (15)
N50.4821 (3)0.3901 (4)0.2356 (6)0.0476 (18)
O470.6329 (3)0.1665 (4)0.4103 (5)0.0617 (19)
N70.6224 (3)0.0801 (4)0.5252 (5)0.0400 (15)
N80.4832 (3)0.1029 (4)0.2582 (6)0.0474 (17)
N90.7415 (3)0.0838 (4)0.1778 (6)0.0471 (17)
O370.2743 (2)0.2842 (3)0.8971 (4)0.0382 (12)
O380.2989 (3)0.2710 (4)1.1019 (4)0.0632 (19)
O390.3086 (3)0.0201 (3)0.8810 (5)0.0559 (17)
O550.5523 (2)0.1732 (3)0.6856 (5)0.0459 (14)
O400.6550 (2)0.3481 (3)0.1859 (5)0.0490 (14)
C20.6452 (3)0.3714 (4)0.1012 (7)0.046 (2)
H80.61420.36090.07430.055*
C30.7237 (4)0.4299 (5)0.0907 (9)0.061 (3)
H20.71850.45560.15200.092*
H30.74120.46060.04480.092*
H40.74290.38670.10320.092*
C40.6638 (5)0.4329 (6)0.0517 (7)0.067 (3)
H60.68610.41010.09800.101*
H70.66700.48490.05640.101*
H50.63030.41910.06680.101*
O410.6001 (3)0.3175 (4)0.4158 (5)0.0580 (17)
C60.6147 (3)0.3158 (5)0.5037 (7)0.051 (2)
H100.64000.28360.52000.062*
C70.6139 (4)0.3522 (7)0.6749 (7)0.067 (3)
H120.63400.30920.68230.100*
H130.58610.34960.71950.100*
H110.63350.39450.69020.100*
C80.5581 (4)0.4096 (6)0.5489 (8)0.068 (3)
H150.57240.44810.50990.102*
H160.54410.42970.60860.102*
H140.53240.38600.51120.102*
O420.7020 (2)0.2798 (3)0.3417 (5)0.0472 (14)
C100.7180 (3)0.3417 (4)0.3558 (6)0.0430 (18)
H180.69510.37740.37310.052*
C110.8025 (4)0.3079 (6)0.3206 (8)0.062 (3)
H190.78810.26000.32030.093*
H200.82930.30930.36780.093*
H210.81510.31900.25550.093*
C120.7807 (4)0.4351 (6)0.3660 (9)0.067 (3)
H220.75220.46570.37610.100*
H230.79920.45230.30960.100*
H240.80140.43650.42410.100*
O430.6047 (3)0.2262 (3)0.0990 (4)0.0514 (15)
C140.5960 (3)0.1715 (4)0.0515 (6)0.0422 (18)
H260.58810.12940.08660.051*
C150.5833 (4)0.1013 (4)0.0986 (6)0.046 (2)
H280.57980.06200.05190.069*
H290.60870.08940.14610.069*
H270.55230.10880.13250.069*
C160.6085 (4)0.2314 (5)0.1036 (7)0.055 (2)
H310.58070.26410.10210.082*
H300.61530.21750.17100.082*
H320.63720.25510.07590.082*
O440.5498 (2)0.3180 (4)0.2319 (5)0.0528 (16)
C180.5248 (3)0.3674 (4)0.2680 (8)0.0468 (19)
H340.53770.39070.32370.056*
C190.4532 (4)0.4425 (5)0.2893 (9)0.065 (3)
H350.42200.42110.30810.098*
H360.44720.48420.24790.098*
H370.47090.45730.34780.098*
C200.4613 (6)0.3597 (9)0.1481 (9)0.114 (6)
H390.44980.39820.10550.171*
H400.43380.32890.16560.171*
H380.48610.33160.11400.171*
C210.6486 (4)0.1287 (5)0.4775 (6)0.0453 (19)
H470.68160.13490.49620.054*
C220.5722 (3)0.0645 (5)0.4960 (9)0.058 (2)
H410.54990.07910.54810.087*
H420.56870.01320.48410.087*
H430.56450.09090.43640.087*
C230.6432 (4)0.0379 (6)0.6040 (8)0.064 (3)
H440.67760.05030.61200.096*
H460.64030.01300.58840.096*
H450.62570.04800.66460.096*
O450.5562 (2)0.1600 (3)0.2673 (5)0.0503 (14)
C250.5106 (3)0.1617 (4)0.2671 (7)0.0449 (19)
H550.49480.20660.27350.054*
C260.5044 (5)0.0336 (5)0.2361 (11)0.088 (4)
H490.53850.03980.21650.133*
H510.48620.01110.18300.133*
H500.50290.00310.29410.133*
C270.4286 (4)0.1112 (7)0.2546 (9)0.080 (4)
H520.42010.16180.26090.120*
H530.41390.08420.30810.120*
H540.41640.09300.19230.120*
C280.7155 (4)0.1265 (5)0.2333 (7)0.050 (2)
H560.72750.13630.29680.060*
C290.7248 (4)0.0661 (8)0.0795 (9)0.084 (4)
H580.70930.10810.05010.126*
H590.70120.02700.08290.126*
H570.75260.05140.03960.126*
C300.7896 (5)0.0544 (8)0.2084 (9)0.088 (4)
H610.81440.06760.16030.132*
H620.78750.00230.21290.132*
H600.79850.07410.27210.132*
O520.3886 (3)0.0253 (3)0.5521 (5)0.0571 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.03342 (16)0.02974 (14)0.03036 (15)0.00241 (13)0.00034 (15)0.00084 (15)
Mo10.0306 (3)0.0302 (3)0.0392 (3)0.0058 (2)0.0060 (3)0.0007 (3)
Mo20.0306 (3)0.0352 (3)0.0352 (3)0.0008 (2)0.0079 (3)0.0104 (3)
Mo30.0381 (3)0.0250 (3)0.0385 (3)0.0063 (2)0.0028 (3)0.0059 (3)
Mo40.0258 (3)0.0310 (3)0.0333 (3)0.0000 (2)0.0034 (2)0.0058 (3)
Mo50.0281 (3)0.0369 (3)0.0347 (3)0.0098 (2)0.0026 (3)0.0085 (3)
Mo60.0397 (3)0.0252 (3)0.0403 (3)0.0005 (2)0.0023 (3)0.0095 (3)
Mo70.0455 (4)0.0297 (3)0.0399 (4)0.0055 (3)0.0003 (3)0.0121 (3)
Mo80.0409 (4)0.0384 (3)0.0306 (3)0.0043 (3)0.0081 (3)0.0091 (3)
Mo90.0560 (4)0.0450 (4)0.0268 (3)0.0115 (3)0.0128 (3)0.0052 (3)
Mo100.0317 (3)0.0291 (3)0.0447 (4)0.0035 (2)0.0021 (3)0.0131 (3)
Mo110.0238 (3)0.0406 (3)0.0419 (4)0.0031 (2)0.0032 (3)0.0048 (3)
Mo120.0406 (3)0.0386 (3)0.0238 (3)0.0044 (3)0.0064 (3)0.0030 (3)
P10.0222 (7)0.0199 (6)0.0198 (7)0.0017 (5)0.0004 (5)0.0009 (5)
O10.050 (4)0.057 (4)0.051 (4)0.014 (3)0.006 (3)0.014 (3)
O20.040 (3)0.040 (3)0.056 (4)0.009 (2)0.007 (3)0.006 (3)
O30.034 (3)0.036 (3)0.035 (3)0.000 (2)0.009 (2)0.001 (2)
O40.034 (3)0.027 (2)0.035 (3)0.0005 (19)0.003 (2)0.005 (2)
O50.032 (3)0.029 (2)0.037 (3)0.0049 (19)0.000 (2)0.002 (2)
O60.031 (3)0.043 (3)0.052 (3)0.004 (2)0.013 (2)0.009 (3)
O70.030 (3)0.032 (2)0.037 (3)0.0019 (19)0.002 (2)0.004 (2)
O80.038 (3)0.027 (2)0.042 (3)0.008 (2)0.002 (2)0.007 (2)
O90.035 (3)0.031 (2)0.033 (3)0.001 (2)0.005 (2)0.006 (2)
O100.044 (3)0.029 (2)0.039 (3)0.004 (2)0.000 (2)0.001 (2)
O110.051 (3)0.032 (3)0.040 (3)0.004 (2)0.005 (3)0.009 (2)
O120.037 (3)0.035 (3)0.032 (3)0.004 (2)0.001 (2)0.000 (2)
O130.054 (3)0.051 (3)0.021 (2)0.007 (3)0.003 (2)0.004 (2)
O140.043 (3)0.040 (3)0.030 (3)0.006 (2)0.002 (2)0.003 (2)
O150.029 (3)0.032 (2)0.040 (3)0.003 (2)0.002 (2)0.003 (2)
O160.032 (3)0.061 (4)0.065 (4)0.007 (3)0.011 (3)0.009 (3)
O170.031 (3)0.034 (2)0.044 (3)0.007 (2)0.002 (2)0.005 (2)
O180.026 (3)0.040 (3)0.047 (3)0.004 (2)0.003 (2)0.000 (2)
O190.025 (2)0.0205 (19)0.024 (2)0.0017 (16)0.0012 (17)0.0037 (17)
O200.031 (2)0.023 (2)0.023 (2)0.0016 (17)0.0007 (18)0.0042 (18)
O210.027 (2)0.0232 (18)0.022 (2)0.0028 (16)0.0001 (19)0.0043 (18)
O220.030 (2)0.0222 (19)0.022 (2)0.0018 (17)0.0004 (18)0.0021 (17)
O230.035 (3)0.038 (3)0.031 (3)0.002 (2)0.003 (2)0.001 (2)
O240.064 (4)0.061 (4)0.028 (3)0.005 (3)0.016 (3)0.006 (3)
O250.032 (3)0.035 (2)0.036 (3)0.001 (2)0.000 (2)0.003 (2)
O260.029 (2)0.039 (3)0.033 (3)0.006 (2)0.007 (2)0.004 (2)
O270.042 (3)0.038 (3)0.025 (2)0.006 (2)0.002 (2)0.008 (2)
O280.050 (4)0.038 (3)0.062 (4)0.006 (3)0.004 (3)0.024 (3)
O290.038 (3)0.0220 (19)0.048 (3)0.0043 (19)0.001 (2)0.002 (2)
O300.032 (3)0.035 (2)0.036 (3)0.005 (2)0.003 (2)0.013 (2)
O310.051 (4)0.039 (3)0.042 (3)0.002 (2)0.014 (3)0.013 (2)
O320.042 (3)0.030 (2)0.030 (2)0.011 (2)0.002 (2)0.001 (2)
O330.060 (4)0.061 (4)0.043 (3)0.013 (3)0.018 (3)0.010 (3)
O340.041 (3)0.029 (2)0.039 (3)0.005 (2)0.005 (2)0.006 (2)
O350.054 (4)0.038 (3)0.055 (4)0.012 (3)0.002 (3)0.014 (3)
O360.047 (3)0.047 (3)0.040 (3)0.001 (3)0.016 (3)0.015 (3)
N10.060 (5)0.033 (3)0.044 (4)0.002 (3)0.008 (4)0.000 (3)
N20.040 (4)0.056 (4)0.035 (3)0.000 (3)0.004 (3)0.007 (3)
N30.040 (4)0.041 (3)0.050 (4)0.002 (3)0.010 (3)0.007 (3)
N40.041 (4)0.034 (3)0.043 (4)0.005 (3)0.008 (3)0.001 (3)
N50.049 (4)0.039 (3)0.054 (4)0.007 (3)0.000 (3)0.012 (3)
O470.072 (5)0.053 (4)0.060 (4)0.010 (3)0.008 (4)0.023 (3)
N70.043 (4)0.037 (3)0.040 (4)0.005 (3)0.004 (3)0.002 (3)
N80.045 (4)0.047 (4)0.050 (4)0.016 (3)0.006 (3)0.013 (3)
N90.052 (4)0.043 (4)0.047 (4)0.005 (3)0.002 (3)0.001 (3)
O370.040 (3)0.038 (3)0.036 (3)0.003 (2)0.011 (2)0.003 (2)
O380.075 (5)0.085 (5)0.030 (3)0.017 (4)0.026 (3)0.003 (3)
O390.072 (4)0.034 (3)0.061 (4)0.017 (3)0.003 (3)0.017 (3)
O550.036 (3)0.054 (3)0.048 (3)0.017 (3)0.003 (3)0.015 (3)
O400.059 (4)0.041 (3)0.047 (3)0.016 (3)0.004 (3)0.011 (3)
C20.049 (5)0.029 (3)0.060 (6)0.006 (3)0.002 (4)0.003 (4)
C30.051 (6)0.053 (5)0.079 (7)0.004 (4)0.017 (5)0.007 (5)
C40.105 (9)0.059 (6)0.037 (5)0.012 (6)0.002 (5)0.008 (5)
O410.057 (4)0.077 (4)0.040 (3)0.019 (4)0.004 (3)0.016 (3)
C60.050 (5)0.058 (5)0.046 (5)0.014 (4)0.006 (4)0.009 (4)
C70.062 (7)0.103 (9)0.036 (5)0.012 (6)0.012 (5)0.015 (5)
C80.067 (7)0.080 (7)0.056 (6)0.019 (6)0.018 (5)0.007 (6)
O420.041 (3)0.045 (3)0.056 (4)0.006 (3)0.012 (3)0.001 (3)
C100.040 (4)0.042 (4)0.046 (5)0.000 (3)0.003 (4)0.005 (4)
C110.047 (6)0.074 (7)0.066 (6)0.006 (5)0.002 (5)0.018 (5)
C120.057 (6)0.065 (6)0.078 (7)0.023 (5)0.004 (6)0.009 (6)
O430.073 (4)0.047 (3)0.033 (3)0.003 (3)0.010 (3)0.007 (3)
C140.053 (5)0.039 (4)0.034 (4)0.003 (4)0.010 (4)0.000 (4)
C150.061 (6)0.040 (4)0.038 (4)0.011 (4)0.013 (4)0.003 (3)
C160.078 (7)0.042 (4)0.045 (5)0.005 (5)0.003 (5)0.004 (4)
O440.052 (4)0.058 (4)0.049 (4)0.019 (3)0.002 (3)0.000 (3)
C180.045 (5)0.042 (4)0.053 (5)0.003 (3)0.008 (4)0.000 (4)
C190.058 (6)0.044 (5)0.093 (8)0.007 (4)0.007 (6)0.016 (5)
C200.128 (13)0.149 (14)0.064 (8)0.055 (11)0.058 (9)0.021 (9)
C210.049 (5)0.045 (4)0.042 (5)0.010 (4)0.001 (4)0.007 (4)
C220.050 (5)0.044 (5)0.081 (7)0.011 (4)0.005 (5)0.006 (5)
C230.075 (7)0.065 (6)0.051 (6)0.018 (5)0.011 (5)0.023 (5)
O450.041 (3)0.046 (3)0.064 (4)0.013 (3)0.001 (3)0.008 (3)
C250.050 (5)0.039 (4)0.046 (5)0.014 (3)0.003 (4)0.007 (4)
C260.084 (9)0.041 (5)0.140 (13)0.009 (6)0.007 (8)0.008 (6)
C270.052 (6)0.106 (9)0.083 (9)0.023 (6)0.014 (6)0.027 (7)
C280.065 (6)0.044 (4)0.042 (5)0.009 (4)0.001 (4)0.013 (4)
C290.070 (8)0.119 (10)0.063 (7)0.003 (7)0.001 (6)0.047 (7)
C300.095 (10)0.100 (9)0.069 (8)0.057 (8)0.008 (7)0.006 (7)
O520.069 (4)0.035 (3)0.067 (4)0.004 (3)0.007 (4)0.025 (3)
Geometric parameters (Å, º) top
Eu1—O402.369 (5)N1—C31.450 (12)
Eu1—O472.378 (6)N1—C41.452 (12)
Eu1—O12.383 (6)N2—C61.311 (11)
Eu1—O452.387 (5)N2—C71.433 (12)
Eu1—O412.395 (6)N2—C81.455 (12)
Eu1—O442.413 (6)N3—C101.312 (11)
Eu1—O422.415 (6)N3—C121.438 (11)
Eu1—O432.416 (6)N3—C111.463 (12)
Mo1—O21.672 (5)N4—C141.313 (10)
Mo1—O91.836 (5)N4—C161.441 (11)
Mo1—O31.852 (5)N4—C151.452 (10)
Mo1—O341.973 (5)N5—C181.297 (11)
Mo1—O181.986 (5)N5—C201.417 (14)
Mo1—O192.436 (4)N5—C191.433 (12)
Mo2—O361.690 (5)O47—C211.214 (11)
Mo2—O41.831 (5)N7—C211.307 (10)
Mo2—O171.866 (5)N7—C231.427 (12)
Mo2—O231.957 (5)N7—C221.435 (11)
Mo2—O31.993 (5)N8—C251.313 (10)
Mo2—O192.429 (4)N8—C261.427 (13)
Mo3—O351.672 (5)N8—C271.477 (13)
Mo3—O251.842 (5)N9—C281.290 (11)
Mo3—O51.848 (5)N9—C291.435 (13)
Mo3—O41.985 (5)N9—C301.461 (14)
Mo3—O291.985 (5)O40—C21.245 (11)
Mo3—O212.428 (4)C2—H80.9300
Mo4—O61.677 (5)C3—H20.9600
Mo4—O121.834 (5)C3—H30.9600
Mo4—O301.851 (5)C3—H40.9600
Mo4—O51.976 (5)C4—H60.9600
Mo4—O71.992 (5)C4—H70.9600
Mo4—O212.426 (4)C4—H50.9600
Mo5—O551.675 (5)O41—C61.245 (11)
Mo5—O71.825 (5)C6—H100.9300
Mo5—O261.845 (5)C7—H120.9600
Mo5—O321.979 (5)C7—H130.9600
Mo5—O81.985 (5)C7—H110.9600
Mo5—O222.428 (5)C8—H150.9600
Mo6—O521.676 (5)C8—H160.9600
Mo6—O101.837 (5)C8—H140.9600
Mo6—O81.852 (5)O42—C101.228 (9)
Mo6—O91.983 (5)C10—H180.9300
Mo6—O272.000 (5)C11—H190.9600
Mo6—O222.416 (4)C11—H200.9600
Mo7—O391.686 (5)C11—H210.9600
Mo7—O341.842 (6)C12—H220.9600
Mo7—O311.854 (6)C12—H230.9600
Mo7—O101.973 (6)C12—H240.9600
Mo7—O111.994 (6)O43—C141.214 (10)
Mo7—O202.438 (4)C14—H260.9300
Mo8—O331.675 (6)C15—H280.9600
Mo8—O111.844 (6)C15—H290.9600
Mo8—O321.853 (5)C15—H270.9600
Mo8—O121.983 (5)C16—H310.9600
Mo8—O131.987 (6)C16—H300.9600
Mo8—O202.423 (4)C16—H320.9600
Mo9—O381.680 (6)O44—C181.229 (10)
Mo9—O141.838 (6)C18—H340.9300
Mo9—O131.851 (6)C19—H350.9600
Mo9—O311.984 (6)C19—H360.9600
Mo9—O371.993 (6)C19—H370.9600
Mo9—O202.433 (5)C20—H390.9600
Mo10—O281.690 (5)C20—H400.9600
Mo10—O151.842 (5)C20—H380.9600
Mo10—O291.847 (6)C21—H470.9300
Mo10—O141.976 (5)C22—H410.9600
Mo10—O301.984 (5)C22—H420.9600
Mo10—O212.420 (4)C22—H430.9600
Mo11—O161.676 (6)C23—H440.9600
Mo11—O371.836 (5)C23—H460.9600
Mo11—O181.857 (5)C23—H450.9600
Mo11—O151.976 (5)O45—C251.227 (10)
Mo11—O171.979 (5)C25—H550.9300
Mo11—O192.423 (4)C26—H490.9600
Mo12—O241.684 (5)C26—H510.9600
Mo12—O231.840 (5)C26—H500.9600
Mo12—O271.850 (5)C27—H520.9600
Mo12—O251.976 (5)C27—H530.9600
Mo12—O261.980 (5)C27—H540.9600
Mo12—O222.428 (4)C28—H560.9300
P1—O191.521 (5)C29—H580.9600
P1—O201.526 (5)C29—H590.9600
P1—O221.527 (5)C29—H570.9600
P1—O211.536 (4)C30—H610.9600
O1—C281.219 (11)C30—H620.9600
N1—C21.297 (11)C30—H600.9600
O40—Eu1—O47145.6 (2)O26—Mo12—O2272.45 (18)
O40—Eu1—O198.6 (2)O19—P1—O20109.8 (3)
O47—Eu1—O176.7 (2)O19—P1—O22109.5 (3)
O40—Eu1—O45141.7 (2)O20—P1—O22109.1 (2)
O47—Eu1—O4572.7 (2)O19—P1—O21109.3 (2)
O1—Eu1—O4588.5 (2)O20—P1—O21109.5 (3)
O40—Eu1—O4193.6 (2)O22—P1—O21109.6 (3)
O47—Eu1—O4175.1 (3)C28—O1—Eu1137.4 (6)
O1—Eu1—O41145.4 (2)Mo1—O3—Mo2124.5 (3)
O45—Eu1—O41101.7 (2)Mo2—O4—Mo3151.4 (3)
O40—Eu1—O4476.2 (2)Mo3—O5—Mo4125.8 (3)
O47—Eu1—O44127.6 (2)Mo5—O7—Mo4151.7 (3)
O1—Eu1—O44142.6 (2)Mo6—O8—Mo5124.8 (2)
O45—Eu1—O4475.6 (2)Mo1—O9—Mo6151.6 (3)
O41—Eu1—O4471.8 (2)Mo6—O10—Mo7151.5 (3)
O40—Eu1—O4270.2 (2)Mo8—O11—Mo7125.5 (3)
O47—Eu1—O4275.6 (2)Mo4—O12—Mo8152.1 (3)
O1—Eu1—O4276.8 (2)Mo9—O13—Mo8124.6 (3)
O45—Eu1—O42147.4 (2)Mo9—O14—Mo10151.8 (3)
O41—Eu1—O4277.2 (2)Mo10—O15—Mo11151.4 (3)
O44—Eu1—O42132.0 (2)Mo2—O17—Mo11124.8 (3)
O40—Eu1—O4373.5 (2)Mo11—O18—Mo1124.6 (3)
O47—Eu1—O43132.8 (2)P1—O19—Mo11126.2 (2)
O1—Eu1—O4370.2 (2)P1—O19—Mo2125.7 (2)
O45—Eu1—O4373.7 (2)Mo11—O19—Mo289.23 (14)
O41—Eu1—O43144.3 (2)P1—O19—Mo1126.1 (2)
O44—Eu1—O4372.8 (2)Mo11—O19—Mo188.93 (15)
O42—Eu1—O43125.7 (2)Mo2—O19—Mo188.80 (15)
O2—Mo1—O9102.7 (3)P1—O20—Mo8126.5 (3)
O2—Mo1—O3102.4 (3)P1—O20—Mo9125.6 (2)
O9—Mo1—O395.8 (2)Mo8—O20—Mo988.87 (15)
O2—Mo1—O34101.0 (3)P1—O20—Mo7125.7 (3)
O9—Mo1—O3485.0 (2)Mo8—O20—Mo789.20 (14)
O3—Mo1—O34155.8 (2)Mo9—O20—Mo789.09 (15)
O2—Mo1—O18100.5 (3)P1—O21—Mo10126.1 (3)
O9—Mo1—O18155.7 (2)P1—O21—Mo4125.6 (2)
O3—Mo1—O1886.5 (2)Mo10—O21—Mo489.12 (14)
O34—Mo1—O1883.2 (2)P1—O21—Mo3126.0 (3)
O2—Mo1—O19171.9 (2)Mo10—O21—Mo389.13 (13)
O9—Mo1—O1985.20 (18)Mo4—O21—Mo389.11 (14)
O3—Mo1—O1974.36 (18)P1—O22—Mo6126.0 (3)
O34—Mo1—O1981.65 (18)P1—O22—Mo5126.1 (3)
O18—Mo1—O1972.08 (18)Mo6—O22—Mo589.19 (14)
O36—Mo2—O4103.7 (2)P1—O22—Mo12126.0 (2)
O36—Mo2—O17102.2 (3)Mo6—O22—Mo1289.10 (14)
O4—Mo2—O1795.3 (2)Mo5—O22—Mo1288.42 (15)
O36—Mo2—O23101.5 (3)Mo12—O23—Mo2152.1 (3)
O4—Mo2—O2385.7 (2)Mo3—O25—Mo12152.5 (3)
O17—Mo2—O23155.4 (2)Mo5—O26—Mo12124.5 (3)
O36—Mo2—O398.6 (3)Mo12—O27—Mo6123.9 (3)
O4—Mo2—O3156.8 (2)Mo10—O29—Mo3125.1 (2)
O17—Mo2—O386.4 (2)Mo4—O30—Mo10124.8 (3)
O23—Mo2—O383.5 (2)Mo7—O31—Mo9125.8 (3)
O36—Mo2—O19170.1 (2)Mo8—O32—Mo5151.7 (3)
O4—Mo2—O1985.87 (18)Mo7—O34—Mo1152.0 (3)
O17—Mo2—O1973.79 (19)C2—N1—C3119.4 (8)
O23—Mo2—O1981.74 (18)C2—N1—C4121.4 (9)
O3—Mo2—O1972.30 (18)C3—N1—C4119.2 (8)
O35—Mo3—O25102.3 (3)C6—N2—C7121.7 (8)
O35—Mo3—O5102.5 (3)C6—N2—C8118.4 (8)
O25—Mo3—O596.1 (2)C7—N2—C8119.9 (8)
O35—Mo3—O4102.0 (3)C10—N3—C12122.2 (8)
O25—Mo3—O484.4 (2)C10—N3—C11120.0 (7)
O5—Mo3—O4154.8 (2)C12—N3—C11117.8 (8)
O35—Mo3—O29100.9 (3)C14—N4—C16119.6 (7)
O25—Mo3—O29155.3 (2)C14—N4—C15122.0 (7)
O5—Mo3—O2987.0 (2)C16—N4—C15118.2 (7)
O4—Mo3—O2982.7 (2)C18—N5—C20120.2 (9)
O35—Mo3—O21171.5 (2)C18—N5—C19121.8 (9)
O25—Mo3—O2185.71 (19)C20—N5—C19117.9 (10)
O5—Mo3—O2173.44 (19)C21—O47—Eu1166.5 (7)
O4—Mo3—O2181.45 (17)C21—N7—C23121.6 (8)
O29—Mo3—O2171.66 (17)C21—N7—C22120.6 (8)
O6—Mo4—O12103.5 (3)C23—N7—C22117.7 (8)
O6—Mo4—O30103.7 (2)C25—N8—C26121.7 (9)
O12—Mo4—O3096.0 (2)C25—N8—C27118.5 (9)
O6—Mo4—O599.6 (2)C26—N8—C27118.9 (9)
O12—Mo4—O5155.3 (2)C28—N9—C29120.0 (9)
O30—Mo4—O587.0 (2)C28—N9—C30122.9 (9)
O6—Mo4—O7100.0 (2)C29—N9—C30117.0 (9)
O12—Mo4—O785.3 (2)Mo11—O37—Mo9151.5 (3)
O30—Mo4—O7155.2 (2)C2—O40—Eu1130.2 (5)
O5—Mo4—O782.0 (2)O40—C2—N1123.4 (9)
O6—Mo4—O21170.8 (2)O40—C2—H8118.3
O12—Mo4—O2185.6 (2)N1—C2—H8118.3
O30—Mo4—O2173.97 (19)N1—C3—H2109.5
O5—Mo4—O2171.54 (18)N1—C3—H3109.5
O7—Mo4—O2181.47 (18)H2—C3—H3109.5
O55—Mo5—O7103.4 (3)N1—C3—H4109.5
O55—Mo5—O26102.0 (3)H2—C3—H4109.5
O7—Mo5—O2696.1 (2)H3—C3—H4109.5
O55—Mo5—O32101.0 (3)N1—C4—H6109.5
O7—Mo5—O3285.1 (2)N1—C4—H7109.5
O26—Mo5—O32156.0 (2)H6—C4—H7109.5
O55—Mo5—O899.6 (3)N1—C4—H5109.5
O7—Mo5—O8155.5 (2)H6—C4—H5109.5
O26—Mo5—O887.2 (2)H7—C4—H5109.5
O32—Mo5—O882.3 (2)C6—O41—Eu1132.0 (6)
O55—Mo5—O22170.7 (2)O41—C6—N2123.9 (9)
O7—Mo5—O2285.67 (19)O41—C6—H10118.1
O26—Mo5—O2274.59 (18)N2—C6—H10118.1
O32—Mo5—O2281.61 (18)N2—C7—H12109.5
O8—Mo5—O2271.80 (17)N2—C7—H13109.5
O52—Mo6—O10103.3 (3)H12—C7—H13109.5
O52—Mo6—O8102.5 (3)N2—C7—H11109.5
O10—Mo6—O895.8 (2)H12—C7—H11109.5
O52—Mo6—O9100.9 (3)H13—C7—H11109.5
O10—Mo6—O985.6 (2)N2—C8—H15109.5
O8—Mo6—O9155.5 (2)N2—C8—H16109.5
O52—Mo6—O2799.1 (3)H15—C8—H16109.5
O10—Mo6—O27156.2 (2)N2—C8—H14109.5
O8—Mo6—O2787.2 (2)H15—C8—H14109.5
O9—Mo6—O2782.1 (2)H16—C8—H14109.5
O52—Mo6—O22170.8 (3)C10—O42—Eu1127.1 (5)
O10—Mo6—O2285.69 (19)O42—C10—N3125.4 (8)
O8—Mo6—O2274.14 (18)O42—C10—H18117.3
O9—Mo6—O2281.56 (18)N3—C10—H18117.3
O27—Mo6—O2272.40 (17)N3—C11—H19109.5
O39—Mo7—O34103.4 (3)N3—C11—H20109.5
O39—Mo7—O31102.8 (3)H19—C11—H20109.5
O34—Mo7—O3196.1 (3)N3—C11—H21109.5
O39—Mo7—O10102.0 (3)H19—C11—H21109.5
O34—Mo7—O1085.3 (2)H20—C11—H21109.5
O31—Mo7—O10154.1 (2)N3—C12—H22109.5
O39—Mo7—O1199.8 (3)N3—C12—H23109.5
O34—Mo7—O11155.4 (2)H22—C12—H23109.5
O31—Mo7—O1186.4 (3)N3—C12—H24109.5
O10—Mo7—O1182.1 (2)H22—C12—H24109.5
O39—Mo7—O20170.4 (3)H23—C12—H24109.5
O34—Mo7—O2085.93 (18)C14—O43—Eu1132.6 (5)
O31—Mo7—O2073.5 (2)O43—C14—N4124.7 (8)
O10—Mo7—O2080.88 (19)O43—C14—H26117.6
O11—Mo7—O2071.30 (18)N4—C14—H26117.6
O33—Mo8—O11102.1 (3)N4—C15—H28109.5
O33—Mo8—O32103.5 (3)N4—C15—H29109.5
O11—Mo8—O3296.5 (2)H28—C15—H29109.5
O33—Mo8—O12101.9 (3)N4—C15—H27109.5
O11—Mo8—O12155.0 (2)H28—C15—H27109.5
O32—Mo8—O1284.6 (2)H29—C15—H27109.5
O33—Mo8—O1398.9 (3)N4—C16—H31109.5
O11—Mo8—O1386.8 (3)N4—C16—H30109.5
O32—Mo8—O13156.0 (2)H31—C16—H30109.5
O12—Mo8—O1382.7 (2)N4—C16—H32109.5
O33—Mo8—O20170.4 (3)H31—C16—H32109.5
O11—Mo8—O2074.0 (2)H30—C16—H32109.5
O32—Mo8—O2085.74 (19)C18—O44—Eu1138.8 (6)
O12—Mo8—O2081.23 (18)O44—C18—N5126.1 (9)
O13—Mo8—O2072.31 (19)O44—C18—H34117.0
O38—Mo9—O14103.1 (3)N5—C18—H34117.0
O38—Mo9—O13102.6 (3)N5—C19—H35109.5
O14—Mo9—O1396.7 (3)N5—C19—H36109.5
O38—Mo9—O3199.6 (3)H35—C19—H36109.5
O14—Mo9—O31155.6 (2)N5—C19—H37109.5
O13—Mo9—O3186.9 (3)H35—C19—H37109.5
O38—Mo9—O37101.1 (3)H36—C19—H37109.5
O14—Mo9—O3785.0 (2)N5—C20—H39109.5
O13—Mo9—O37155.1 (2)N5—C20—H40109.5
O31—Mo9—O3781.9 (2)H39—C20—H40109.5
O38—Mo9—O20170.6 (3)N5—C20—H38109.5
O14—Mo9—O2086.07 (19)H39—C20—H38109.5
O13—Mo9—O2074.19 (19)H40—C20—H38109.5
O31—Mo9—O2071.60 (19)O47—C21—N7124.6 (9)
O37—Mo9—O2081.18 (18)O47—C21—H47117.7
O28—Mo10—O15103.4 (3)N7—C21—H47117.7
O28—Mo10—O29103.0 (3)N7—C22—H41109.5
O15—Mo10—O2995.3 (2)N7—C22—H42109.5
O28—Mo10—O14100.5 (3)H41—C22—H42109.5
O15—Mo10—O1485.4 (2)N7—C22—H43109.5
O29—Mo10—O14155.7 (2)H41—C22—H43109.5
O28—Mo10—O3099.6 (3)H42—C22—H43109.5
O15—Mo10—O30155.7 (2)N7—C23—H44109.5
O29—Mo10—O3087.1 (2)N7—C23—H46109.5
O14—Mo10—O3082.7 (2)H44—C23—H46109.5
O28—Mo10—O21171.0 (2)N7—C23—H45109.5
O15—Mo10—O2185.38 (19)H44—C23—H45109.5
O29—Mo10—O2174.00 (18)H46—C23—H45109.5
O14—Mo10—O2181.87 (18)C25—O45—Eu1136.7 (6)
O30—Mo10—O2172.04 (17)O45—C25—N8122.8 (8)
O16—Mo11—O37104.0 (3)O45—C25—H55118.6
O16—Mo11—O18103.5 (3)N8—C25—H55118.6
O37—Mo11—O1895.7 (2)N8—C26—H49109.5
O16—Mo11—O1599.8 (3)N8—C26—H51109.5
O37—Mo11—O1585.6 (2)H49—C26—H51109.5
O18—Mo11—O15155.6 (2)N8—C26—H50109.5
O16—Mo11—O1798.8 (3)H49—C26—H50109.5
O37—Mo11—O17155.7 (2)H51—C26—H50109.5
O18—Mo11—O1786.8 (2)N8—C27—H52109.5
O15—Mo11—O1782.4 (2)N8—C27—H53109.5
O16—Mo11—O19170.7 (3)H52—C27—H53109.5
O37—Mo11—O1985.24 (19)N8—C27—H54109.5
O18—Mo11—O1974.38 (19)H52—C27—H54109.5
O15—Mo11—O1981.50 (18)H53—C27—H54109.5
O17—Mo11—O1972.16 (18)O1—C28—N9125.3 (9)
O24—Mo12—O23102.9 (3)O1—C28—H56117.4
O24—Mo12—O27101.4 (3)N9—C28—H56117.4
O23—Mo12—O2795.4 (2)N9—C29—H58109.5
O24—Mo12—O25101.9 (3)N9—C29—H59109.5
O23—Mo12—O2584.4 (2)H58—C29—H59109.5
O27—Mo12—O25156.2 (2)N9—C29—H57109.5
O24—Mo12—O26100.0 (3)H58—C29—H57109.5
O23—Mo12—O26155.8 (2)H59—C29—H57109.5
O27—Mo12—O2687.7 (2)N9—C30—H61109.5
O25—Mo12—O2683.2 (2)N9—C30—H62109.5
O24—Mo12—O22171.3 (3)H61—C30—H62109.5
O23—Mo12—O2285.27 (19)N9—C30—H60109.5
O27—Mo12—O2274.48 (18)H61—C30—H60109.5
O25—Mo12—O2281.80 (18)H62—C30—H60109.5
O2—Mo1—O3—Mo2171.0 (3)O22—P1—O21—Mo10175.5 (3)
O9—Mo1—O3—Mo284.6 (3)O19—P1—O21—Mo4175.3 (3)
O34—Mo1—O3—Mo26.0 (8)O20—P1—O21—Mo455.0 (4)
O18—Mo1—O3—Mo271.1 (3)O22—P1—O21—Mo464.6 (4)
O19—Mo1—O3—Mo21.3 (3)O19—P1—O21—Mo364.9 (3)
O36—Mo2—O4—Mo3129.9 (6)O20—P1—O21—Mo3174.7 (3)
O17—Mo2—O4—Mo3126.1 (6)O22—P1—O21—Mo355.1 (3)
O23—Mo2—O4—Mo329.1 (6)O19—P1—O22—Mo664.7 (3)
O3—Mo2—O4—Mo333.1 (10)O20—P1—O22—Mo655.5 (4)
O19—Mo2—O4—Mo352.9 (6)O21—P1—O22—Mo6175.3 (3)
O35—Mo3—O5—Mo4169.8 (3)O19—P1—O22—Mo5174.7 (3)
O25—Mo3—O5—Mo486.2 (3)O20—P1—O22—Mo565.1 (3)
O4—Mo3—O5—Mo43.4 (7)O21—P1—O22—Mo554.8 (4)
O29—Mo3—O5—Mo469.3 (3)O19—P1—O22—Mo1255.5 (4)
O21—Mo3—O5—Mo42.5 (3)O20—P1—O22—Mo12175.7 (3)
O55—Mo5—O7—Mo4129.4 (6)O21—P1—O22—Mo1264.4 (4)
O26—Mo5—O7—Mo4126.7 (6)O24—Mo12—O23—Mo2130.2 (6)
O32—Mo5—O7—Mo429.2 (6)O27—Mo12—O23—Mo2126.8 (6)
O8—Mo5—O7—Mo430.1 (10)O25—Mo12—O23—Mo229.3 (6)
O22—Mo5—O7—Mo452.8 (6)O26—Mo12—O23—Mo230.3 (10)
O52—Mo6—O8—Mo5168.5 (4)O22—Mo12—O23—Mo252.9 (6)
O10—Mo6—O8—Mo586.5 (3)O35—Mo3—O25—Mo12132.4 (7)
O9—Mo6—O8—Mo55.7 (8)O5—Mo3—O25—Mo12123.3 (7)
O27—Mo6—O8—Mo569.8 (3)O4—Mo3—O25—Mo1231.3 (6)
O22—Mo6—O8—Mo52.7 (3)O29—Mo3—O25—Mo1227.3 (10)
O2—Mo1—O9—Mo6129.2 (6)O21—Mo3—O25—Mo1250.5 (6)
O3—Mo1—O9—Mo6126.6 (6)O55—Mo5—O26—Mo12169.1 (3)
O34—Mo1—O9—Mo629.1 (6)O7—Mo5—O26—Mo1285.8 (3)
O18—Mo1—O9—Mo632.2 (10)O32—Mo5—O26—Mo125.8 (7)
O19—Mo1—O9—Mo652.9 (6)O8—Mo5—O26—Mo1269.8 (3)
O52—Mo6—O10—Mo7128.1 (7)O22—Mo5—O26—Mo122.0 (3)
O8—Mo6—O10—Mo7127.5 (7)O24—Mo12—O27—Mo6169.1 (3)
O9—Mo6—O10—Mo727.9 (7)O23—Mo12—O27—Mo686.6 (3)
O27—Mo6—O10—Mo731.2 (11)O25—Mo12—O27—Mo61.8 (8)
O22—Mo6—O10—Mo754.0 (7)O26—Mo12—O27—Mo669.4 (3)
O33—Mo8—O11—Mo7168.8 (4)O22—Mo12—O27—Mo63.0 (3)
O32—Mo8—O11—Mo785.8 (4)O28—Mo10—O29—Mo3168.8 (3)
O12—Mo8—O11—Mo75.2 (8)O15—Mo10—O29—Mo386.1 (3)
O13—Mo8—O11—Mo770.3 (4)O14—Mo10—O29—Mo34.4 (8)
O20—Mo8—O11—Mo72.2 (3)O30—Mo10—O29—Mo369.6 (3)
O6—Mo4—O12—Mo8128.2 (6)O21—Mo10—O29—Mo32.5 (3)
O30—Mo4—O12—Mo8126.1 (6)O6—Mo4—O30—Mo10168.6 (3)
O5—Mo4—O12—Mo830.3 (10)O12—Mo4—O30—Mo1085.9 (4)
O7—Mo4—O12—Mo829.0 (6)O5—Mo4—O30—Mo1069.4 (3)
O21—Mo4—O12—Mo852.8 (6)O7—Mo4—O30—Mo105.8 (8)
O38—Mo9—O13—Mo8169.0 (4)O21—Mo4—O30—Mo102.2 (3)
O14—Mo9—O13—Mo885.8 (4)O39—Mo7—O31—Mo9168.4 (4)
O31—Mo9—O13—Mo869.9 (4)O34—Mo7—O31—Mo986.3 (4)
O37—Mo9—O13—Mo86.8 (9)O10—Mo7—O31—Mo95.5 (8)
O20—Mo9—O13—Mo81.9 (3)O11—Mo7—O31—Mo969.2 (4)
O38—Mo9—O14—Mo10131.0 (7)O20—Mo7—O31—Mo92.4 (3)
O13—Mo9—O14—Mo10124.3 (7)O33—Mo8—O32—Mo5132.1 (7)
O31—Mo9—O14—Mo1027.0 (11)O11—Mo8—O32—Mo5123.8 (7)
O37—Mo9—O14—Mo1030.7 (6)O12—Mo8—O32—Mo531.1 (7)
O20—Mo9—O14—Mo1050.8 (6)O13—Mo8—O32—Mo527.1 (11)
O28—Mo10—O15—Mo11128.4 (6)O20—Mo8—O32—Mo550.5 (6)
O29—Mo10—O15—Mo11126.9 (6)O39—Mo7—O34—Mo1131.2 (6)
O14—Mo10—O15—Mo1128.7 (6)O31—Mo7—O34—Mo1124.0 (6)
O30—Mo10—O15—Mo1132.1 (10)O10—Mo7—O34—Mo130.0 (6)
O21—Mo10—O15—Mo1153.5 (6)O11—Mo7—O34—Mo129.3 (10)
O36—Mo2—O17—Mo11168.2 (3)O20—Mo7—O34—Mo151.1 (6)
O4—Mo2—O17—Mo1186.5 (3)O16—Mo11—O37—Mo9127.0 (6)
O23—Mo2—O17—Mo114.5 (7)O18—Mo11—O37—Mo9127.6 (6)
O3—Mo2—O17—Mo1170.2 (3)O15—Mo11—O37—Mo928.0 (6)
O19—Mo2—O17—Mo112.4 (3)O17—Mo11—O37—Mo932.5 (10)
O16—Mo11—O18—Mo1168.6 (4)O19—Mo11—O37—Mo953.8 (6)
O37—Mo11—O18—Mo185.5 (4)Eu1—O40—C2—N1154.9 (6)
O15—Mo11—O18—Mo16.6 (8)C3—N1—C2—O403.1 (13)
O17—Mo11—O18—Mo170.3 (3)C4—N1—C2—O40177.2 (8)
O19—Mo11—O18—Mo12.1 (3)Eu1—O41—C6—N2176.3 (7)
O20—P1—O19—Mo1155.7 (3)C7—N2—C6—O41179.1 (10)
O22—P1—O19—Mo11175.5 (3)C8—N2—C6—O412.5 (15)
O21—P1—O19—Mo1164.4 (3)Eu1—O42—C10—N3146.6 (7)
O20—P1—O19—Mo2175.9 (3)C12—N3—C10—O42180.0 (9)
O22—P1—O19—Mo264.3 (3)C11—N3—C10—O420.5 (14)
O21—P1—O19—Mo255.8 (4)Eu1—O43—C14—N4165.4 (6)
O20—P1—O19—Mo164.6 (3)C16—N4—C14—O430.9 (14)
O22—P1—O19—Mo155.2 (3)C15—N4—C14—O43176.1 (8)
O21—P1—O19—Mo1175.3 (3)Eu1—O44—C18—N5169.7 (7)
O19—P1—O20—Mo8175.4 (3)C20—N5—C18—O443.2 (16)
O22—P1—O20—Mo855.4 (4)C19—N5—C18—O44172.7 (9)
O21—P1—O20—Mo864.6 (4)Eu1—O47—C21—N7167 (2)
O19—P1—O20—Mo964.7 (4)C23—N7—C21—O47179.5 (9)
O22—P1—O20—Mo9175.3 (3)C22—N7—C21—O474.0 (14)
O21—P1—O20—Mo955.3 (4)Eu1—O45—C25—N8176.5 (6)
O19—P1—O20—Mo754.7 (4)C26—N8—C25—O457.7 (16)
O22—P1—O20—Mo765.4 (4)C27—N8—C25—O45177.4 (9)
O21—P1—O20—Mo7174.7 (3)Eu1—O1—C28—N9169.7 (7)
O19—P1—O21—Mo1055.4 (4)C29—N9—C28—O10.5 (16)
O20—P1—O21—Mo1064.9 (3)C30—N9—C28—O1176.3 (11)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H4···O31i0.962.723.289 (11)118
C4—H7···O36ii0.962.613.476 (12)150
C7—H13···O70.962.653.473 (12)145
C8—H15···O28ii0.962.513.316 (13)141
C8—H16···O50.962.583.424 (11)147
C10—H18···O28ii0.932.623.516 (10)162
C15—H29···O16i0.962.553.299 (12)135
C15—H27···O32iii0.962.523.440 (10)160
C15—H28···O52iv0.962.293.174 (10)153
C16—H31···O6iii0.962.633.541 (11)159
C22—H41···O550.962.533.280 (12)135
C22—H42···O11iv0.962.453.305 (11)149
C22—H43···O450.962.613.567 (13)172
C23—H44···O17v0.962.523.443 (11)161
C25—H55···O240.932.533.337 (11)145
C25—H55···O440.932.583.091 (10)115
C28—H56···O36v0.932.623.476 (11)153
C30—H60···O36v0.962.583.458 (14)152
Symmetry codes: (i) x+1/2, y+1/2, z1; (ii) x+1, y+1, z1/2; (iii) x, y, z1; (iv) x+1, y, z1/2; (v) x+1/2, y+1/2, z.
 

Acknowledgements

The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia. The authors are grateful to the Portuguese Fundacão para a Ciencias e Tecnologia (FCT) for support through projects SFRH/BPD/24889/2005 and PTDC/BIAPRO/ 103980/2008 and for funding the purchase of the single-crystal diffractometer.

References

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