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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 7| July 2012| Pages i59-i60
https://doi.org/10.1107/S1600536812028024

Redetermination of [Pr(NO3)3(H2O)4]·2H2O

Roel Decadt,a Pascal Van Der Voort,a Isabel Van Driessche,a Rik Van Deuna and Kristof Van Heckea*

aDepartment of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 – S3, B-9000 Ghent, Belgium
*Correspondence e-mail: Kristof.VanHecke@UGent.be

(Received 8 June 2012; accepted 20 June 2012; online 27 June 2012)

The structure of the title compound, tetra­aqua­tris­(nitrato-κ2O,O′)praseodymium(III) dihydrate, was redetermined. The structure models derived from the previous determinations [Rumanova et al. (1964[Rumanova, I. M., Volodina, G. F. & Belov, N. V. (1964). Kristallografiya, 9, 642-654.]). Kristallografiya, 9, 642–654; Fuller & Jacobson (1976[Fuller, C. & Jacobson, R. A. (1976). Cryst. Struct. Commun. 5, 349-352.]). Cryst. Struct. Commun. 5, 349–352] were confirmed, but now with all H atoms unambiguously located, revealing a complex O—H⋯O hydrogen-bonding network, extending throughout the whole structure. In the title compound, the coordination environment of the PrIII atom can best be described as a distorted bicapped square anti­prism defined by three bidentate nitrate anions and four water mol­ecules. Additionally, two lattice water mol­ecules are observed in the crystal packing. The title compound is isotypic with several other lanthanide-containing nitrate analogues.

Related literature

For general background and the synthesis of the title compound, see: Liu et al. (2012[Liu, Y. Y., Leus, K., Grzywa, M., Weinberger, D., Strubbe, K., Vrielinck, H., Van Deun, R., Volkmer, D., Van Speybroeck, V. & Van Der Voort, P. (2012). Eur. J. Inorg. Chem. pp. 2819-2827.]). For the original determined structures, see: Fuller & Jacobson (1976[Fuller, C. & Jacobson, R. A. (1976). Cryst. Struct. Commun. 5, 349-352.]); Rumanova et al. (1964[Rumanova, I. M., Volodina, G. F. & Belov, N. V. (1964). Kristallografiya, 9, 642-654.]). For analogous Ln-containing structures (Ln = lanthanide), see: Kawashima et al. (2000[Kawashima, R., Sasaki, M., Satoh, S., Isoda, H., Kino, Y. & Shiozaki, Y. (2000). J. Phys. Soc. Jpn, 69, 3297-3303.]); Rogers et al. (1983[Rogers, D. J., Taylor, N. J. & Toogood, G. E. (1983). Acta Cryst. C39, 939-941.]); Shi & Wang (1990[Shi, B. D. & Wang, J. Z. (1990). Jiegon Huaxue, 9, 164-167.], 1991[Shi, B. D. & Wang, J. Z. (1991). Xiamen Daxue Xuebao, Ziran Kexueban, 30, 55-58.]); Stumpf & Bolte (2001[Stumpf, T. & Bolte, M. (2001). Acta Cryst. E57, i10-i11.]). For related structures of metal-organic compounds, see: Rohde & Urland (2006[Rohde, A. & Urland, W. (2006). Acta Cryst. E62, m3026-m3028.]); Weakley (1982[Weakley, T. J. R. (1982). Inorg. Chim. Acta, 63, 161-168.], 1984[Weakley, T. J. R. (1984). Inorg. Chim. Acta, 95, 317-322.], 1989[Weakley, T. J. R. (1989). Acta Cryst. C45, 525-526.]). For databases of (in)organic structures, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]); Bergerhoff et al. (1983[Bergerhoff, G., Hundt, R., Sievers, R. & Brown, I. D. (1983). J. Chem. Inf. Comput. Sci. 23, 66-69.]); ICSD (2009[ICSD (2009). http://www.fiz-karlsruhe.de/icsd.html.]).

Experimental

Crystal data

  • [Pr(NO3)3(H2O)4]·2H2O

  • Mr = 435.04

  • Triclinic, [P \overline 1]

  • a = 6.7017 (3) Å

  • b = 9.1858 (4) Å

  • c = 11.7010 (6) Å

  • α = 69.118 (4)°

  • β = 88.958 (4)°

  • γ = 69.696 (4)°

  • V = 626.60 (6) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 3.98 mm−1

  • T = 100 K

  • 0.37 × 0.17 × 0.14 mm
Data collection

  • Agilent SuperNova diffractometer with an Atlas detector

  • Absorption correction: numerical [CrysAlis PRO (Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies UK Ltd, Yarnton, England.]), using a multi-faceted crystal model based on expressions derived by Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.375, Tmax = 0.654

  • 10260 measured reflections

  • 2743 independent reflections

  • 2627 reflections with I > 2σ(I)

  • Rint = 0.035
Refinement

  • R[F2 > 2σ(F2)] = 0.017

  • wR(F2) = 0.037

  • S = 1.07

  • 2743 reflections

  • 208 parameters

  • 12 restraints

  • All H-atom parameters refined

  • Δρmax = 0.42 e Å−3

  • Δρmin = −0.60 e Å−3

Table 1
Selected bond lengths (Å)

O1—Pr1 2.5677 (16)
O2—Pr1 2.5790 (15)
O4—Pr1 2.6348 (16)
O5—Pr1 2.6000 (17)
O7—Pr1 2.7307 (15)
O8—Pr1 2.6154 (16)
O10—Pr1 2.4468 (17)
O11—Pr1 2.4287 (17)
O12—Pr1 2.4555 (16)
O13—Pr1 2.4578 (17)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O10—H10A⋯O8i 0.82 (2) 2.10 (2) 2.918 (2) 177 (3)
O10—H10B⋯O14ii 0.82 (2) 1.85 (2) 2.670 (2) 176 (3)
O11—H11A⋯O14i 0.80 (2) 1.94 (2) 2.735 (2) 177 (3)
O11—H11B⋯O15iii 0.80 (2) 1.93 (2) 2.720 (2) 175 (3)
O12—H12A⋯O4iv 0.81 (2) 2.11 (2) 2.925 (2) 174 (3)
O12—H12B⋯O15 0.81 (2) 1.91 (2) 2.713 (2) 175 (3)
O13—H13A⋯O4ii 0.81 (2) 2.38 (2) 3.137 (2) 156 (3)
O13—H13A⋯O8ii 0.81 (2) 2.57 (3) 3.130 (2) 128 (3)
O13—H13B⋯O7v 0.79 (2) 2.24 (2) 3.020 (2) 168 (3)
O13—H13B⋯O9v 0.79 (2) 2.43 (2) 3.046 (2) 136 (3)
O14—H14A⋯O9 0.84 (2) 2.00 (2) 2.826 (2) 169 (3)
O14—H14B⋯O5vi 0.80 (2) 2.26 (2) 2.881 (2) 134 (3)
O14—H14B⋯O3vii 0.80 (2) 2.39 (2) 2.971 (2) 130 (3)
O15—H15B⋯O6ii 0.83 (2) 2.01 (2) 2.824 (2) 169 (3)
O15—H15A⋯O3iv 0.77 (2) 2.56 (2) 3.049 (2) 123 (2)
O15—H15A⋯O3viii 0.77 (2) 2.28 (2) 2.892 (2) 138 (3)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) x-1, y, z; (iii) -x, -y, -z+2; (iv) -x+1, -y, -z+2; (v) -x, -y+1, -z+1; (vi) -x+1, -y+1, -z+1; (vii) -x+2, -y, -z+1; (viii) x-1, y+1, z.

Data collection: CrysAlis PRO (Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies UK Ltd, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2008[Brandenburg, K. (2008). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812028024/wm2647sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812028024/wm2647Isup2.hkl

checkCIF report


Comment top

The title compound was serendipitously obtained in low yield as an undesired product of an experiment aimed at obtaining a PrIII-containing coordination polymer, with dicarboxylate ligands as the connecting moieties, following an earlier successful synthesis of a vanadium metal-organic framework with the same type of linkers (Liu et al., 2012).

The structure of the title compound is analogous to the structures, previously determined, with ICSD entries 22339 (Rumanova et al., 1964) and 123 (Fuller & Jacobson, 1976) (ICSD Version 1.8.1; Bergerhoff et al., 1983; ICSD, 2009). However, in both of the latter structures, the "position of elements of H were undetermined". In the now determined structure, these hydrogen atoms could unambiguously be located from difference Fourier electron density maps, revealing an extended hydrogen bonding network.

The structure of the title compound is isotypic with other [Ln(NO3)3(H2O)4].2H2O analogues, for example for Ln = Nd (ICSD entries 37181 and 71767) (Rogers et al., 1983; Shi & Wang, 1991), Ln = Sm (ICSD entry 69158) (Shi & Wang, 1990) and Ln = Eu (ICSD entry 280528) (Stumpf & Bolte, 2001). Three additional Sm-analogues were reported by Kawashima et al., 2000 (ICSD entries 91511, 91512 and 91513).

The asymmetric unit consists of one PrIII cation, three nitrate anions, and in total six water molecules. The PrIII cation is ten-coordinated by the oxygen atoms of three bidentate nitrate anions and four water molecules. Additionally, two lattice water molecules are included in the second coordination sphere of the praseodymium cation. The coordination polyhedron around PrIII can be best described as a distorted bicapped square antiprism (Figure 1). The Pr—O distances range from 2.5677 (16) to 2.7307 (15) Å and from 2.4287 (17) to 2.4578 (17) Å for the coordinating nitrate groups and water molecules, respectively (Table 1). The coordinating nitrate groups are positioned on the same side of the polyhedron, whereas the coordinating water molecules are positioned on the opposite side.

When searching the Cambridge Structural Database (CSD, Version 5.33) (Allen, 2002), another PrIII-complex is found (CSD reference code VAFLOD), containing three nitrate anions and four water molecules in its coordination sphere. However, this complex shows a totally different, approximately twofold symmetry (Weakley, 1989). Other structures of metal-organic complexes of PrIII, coordinated by only nitrate and water molecules are found, showing different coordination assemblies, i.e. a 12-coordinated PrIII atom with five nitrate and two aqua ligands, balanced by two additional counter ions (CSD reference code QERRIP) (Rohde & Urland, 2006), a complex with three nitrate and three aqua ligands (CSD reference code CUKMUQ) (Weakley, 1984), and even the formation of dimers (CSD reference code BUPFIB) (Weakley, 1982) have been previously reported.

In the reported structure, a complex, extended hydrogen bonding network is formed throughout the whole structure, stabilizing the crystal packing, i.e. in total 16 different hydrogen bonds are observed between the coordinating water molecules, nitrate anions and lattice water molecules (Figure 2). In total, eight different symmetry equivalent water or nitrate oxygen atoms are involved in the hydrogen bond network. In fact, the praseodymium complexes are all interconnected through these solvent water molecule hydrogen bonds (Figure 3). The four coordinating water molecules show the following hydrogen bonds: O10 is hydrogen bonded to the symmetry-equivalent water molecule oxygen atom O14 and nitrate O8. Water O11 is hydrogen bonded to the symmetry equivalent waters O14 and O15. Water O12 is hydrogen bonded to the symmetry equivalent nitrate O4 and forms an intramolecular hydrogen bond with water O15. Water O13 shows two bifurcated hydrogen bonds to the symmetry equivalent nitrates O7 and O9 and to O4 and O8. The solvent water molecule O14 forms an intramolecular hydrogen bond with nitrate O9 and a bifurcated hydrogen bond to the symmetry equivalent nitrates O3 and O5. Solvent water molecule O15 forms a bifurcated hydrogen bond to two different symmetry equivalent nitrate O3 atoms and another hydrogen bond to a symmetry equivalent nitrate O6. Details of the hydrogen-bonding geometry are given in Table 2.

Related literature top

For general background and the synthesis of the title compound, see: Liu et al. (2012). For the original determined structures, see: Fuller & Jacobson (1976); Rumanova et al. (1964). For analogous Ln-containing structures (Ln = lanthanide), see: Kawashima et al. (2000); Rogers et al. (1983); Shi & Wang (1990, 1991); Stumpf & Bolte (2001). For related structures of metal-organic compounds, see: Rohde & Urland (2006); Weakley (1982, 1984, 1989). For databases of (in)organic structures, see: Allen (2002); Bergerhoff et al. (1983); ICSD (2009).

Experimental top

The title compound was serendipitously obtained in low yield as a product of an experiment aimed at obtaining a PrIII-containing coordination polymer, with dicarboxylate ligands as the connecting moiety, following an earlier successful synthesis of a vanadium metal-organic framework with the same type of linkers (Liu et al., 2012).

In the synthesis, 0.1 mmol Pr(NO3)3.xH2O, along with 0.3 mmol dicarboxylic acid and four drops of 0.6 M aqueous HNO3 was dissolved in 5 ml of a 1:1 mixture of 1:1 MeOH/H2O. After seven days of heating the mixture to 363 K, the title compound was isolated as colourless crystals, suitable for single-crystal X-ray diffraction analysis.

Refinement top

All hydrogen atoms were located in a difference Fourier electron density map and further refined with isotropic temperature factors fixed at 1.5 times Ueq of the parent atoms, applying a restraint value of 0.84 (2) Å for the O—H distances.

Structure description top

The title compound was serendipitously obtained in low yield as an undesired product of an experiment aimed at obtaining a PrIII-containing coordination polymer, with dicarboxylate ligands as the connecting moieties, following an earlier successful synthesis of a vanadium metal-organic framework with the same type of linkers (Liu et al., 2012).

The structure of the title compound is analogous to the structures, previously determined, with ICSD entries 22339 (Rumanova et al., 1964) and 123 (Fuller & Jacobson, 1976) (ICSD Version 1.8.1; Bergerhoff et al., 1983; ICSD, 2009). However, in both of the latter structures, the "position of elements of H were undetermined". In the now determined structure, these hydrogen atoms could unambiguously be located from difference Fourier electron density maps, revealing an extended hydrogen bonding network.

The structure of the title compound is isotypic with other [Ln(NO3)3(H2O)4].2H2O analogues, for example for Ln = Nd (ICSD entries 37181 and 71767) (Rogers et al., 1983; Shi & Wang, 1991), Ln = Sm (ICSD entry 69158) (Shi & Wang, 1990) and Ln = Eu (ICSD entry 280528) (Stumpf & Bolte, 2001). Three additional Sm-analogues were reported by Kawashima et al., 2000 (ICSD entries 91511, 91512 and 91513).

The asymmetric unit consists of one PrIII cation, three nitrate anions, and in total six water molecules. The PrIII cation is ten-coordinated by the oxygen atoms of three bidentate nitrate anions and four water molecules. Additionally, two lattice water molecules are included in the second coordination sphere of the praseodymium cation. The coordination polyhedron around PrIII can be best described as a distorted bicapped square antiprism (Figure 1). The Pr—O distances range from 2.5677 (16) to 2.7307 (15) Å and from 2.4287 (17) to 2.4578 (17) Å for the coordinating nitrate groups and water molecules, respectively (Table 1). The coordinating nitrate groups are positioned on the same side of the polyhedron, whereas the coordinating water molecules are positioned on the opposite side.

When searching the Cambridge Structural Database (CSD, Version 5.33) (Allen, 2002), another PrIII-complex is found (CSD reference code VAFLOD), containing three nitrate anions and four water molecules in its coordination sphere. However, this complex shows a totally different, approximately twofold symmetry (Weakley, 1989). Other structures of metal-organic complexes of PrIII, coordinated by only nitrate and water molecules are found, showing different coordination assemblies, i.e. a 12-coordinated PrIII atom with five nitrate and two aqua ligands, balanced by two additional counter ions (CSD reference code QERRIP) (Rohde & Urland, 2006), a complex with three nitrate and three aqua ligands (CSD reference code CUKMUQ) (Weakley, 1984), and even the formation of dimers (CSD reference code BUPFIB) (Weakley, 1982) have been previously reported.

In the reported structure, a complex, extended hydrogen bonding network is formed throughout the whole structure, stabilizing the crystal packing, i.e. in total 16 different hydrogen bonds are observed between the coordinating water molecules, nitrate anions and lattice water molecules (Figure 2). In total, eight different symmetry equivalent water or nitrate oxygen atoms are involved in the hydrogen bond network. In fact, the praseodymium complexes are all interconnected through these solvent water molecule hydrogen bonds (Figure 3). The four coordinating water molecules show the following hydrogen bonds: O10 is hydrogen bonded to the symmetry-equivalent water molecule oxygen atom O14 and nitrate O8. Water O11 is hydrogen bonded to the symmetry equivalent waters O14 and O15. Water O12 is hydrogen bonded to the symmetry equivalent nitrate O4 and forms an intramolecular hydrogen bond with water O15. Water O13 shows two bifurcated hydrogen bonds to the symmetry equivalent nitrates O7 and O9 and to O4 and O8. The solvent water molecule O14 forms an intramolecular hydrogen bond with nitrate O9 and a bifurcated hydrogen bond to the symmetry equivalent nitrates O3 and O5. Solvent water molecule O15 forms a bifurcated hydrogen bond to two different symmetry equivalent nitrate O3 atoms and another hydrogen bond to a symmetry equivalent nitrate O6. Details of the hydrogen-bonding geometry are given in Table 2.

For general background and the synthesis of the title compound, see: Liu et al. (2012). For the original determined structures, see: Fuller & Jacobson (1976); Rumanova et al. (1964). For analogous Ln-containing structures (Ln = lanthanide), see: Kawashima et al. (2000); Rogers et al. (1983); Shi & Wang (1990, 1991); Stumpf & Bolte (2001). For related structures of metal-organic compounds, see: Rohde & Urland (2006); Weakley (1982, 1984, 1989). For databases of (in)organic structures, see: Allen (2002); Bergerhoff et al. (1983); ICSD (2009).

Computing details top

Data collection: CrysAlis PRO (Agilent, 2010); cell refinement: CrysAlis PRO (Agilent, 2010); data reduction: CrysAlis PRO (Agilent, 2010); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2008); software used to prepare material for publication: PLATON (Spek, 2009).

Figures top
[Figure 1] Fig. 1. Coordination geometry of the title compound, showing the atom-labelling scheme of the asymmetric unit and 60% probability displacement ellipsoids.
[Figure 2] Fig. 2. Extended hydrogen bond network in the structure of the title compound, with atom-labeling scheme. Hydrogen bonds are indicated. Symmetry equivalent oxygen atoms are colored pink. Symmetry codes (i) 1 - x,-y,1 - z; (ii) 1 - x,-y,2 - z; (iii) 1 - x,1 - y,1 - z; (iv) -x,1 - y,1 - z; (v) -1 + x,y,z; (vi) -x,-y,2 - z; (vii) 2 - x,-y,1 - z; (viii) -1 + x,1 + y,z.
[Figure 3] Fig. 3. Packing diagram of the title compound along the crystallographic a-axis, indicating the extended hydrogen bond network.
Tetraaquatris(nitrato-κ2O,O')praseodymium(III) dihydrate top
Crystal data top
[Pr(NO3)3(H2O)4]·2H2OZ = 2
Mr = 435.04F(000) = 424
Triclinic, P1Dx = 2.306 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.7017 (3) ÅCell parameters from 8040 reflections
b = 9.1858 (4) Åθ = 3.3–29.3°
c = 11.7010 (6) ŵ = 3.98 mm−1
α = 69.118 (4)°T = 100 K
β = 88.958 (4)°Rod, colourless
γ = 69.696 (4)°0.37 × 0.17 × 0.14 mm
V = 626.60 (6) Å3
Data collection top
Agilent SuperNova
diffractometer with an Atlas detector		2743 independent reflections
Radiation source: SuperNova (Mo) X-ray Source2627 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.035
Detector resolution: 10.3693 pixels mm-1θmax = 27.1°, θmin = 3.3°
ω scansh = −8→8
Absorption correction: numerical
[CrysAlis PRO (Agilent, 2010), using a multi-faceted crystal model based on expressions derived by Clark & Reid (1995)]		k = −11→11
Tmin = 0.375, Tmax = 0.654l = −14→14
10260 measured reflections
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)] = 0.017Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.037All H-atom parameters refined
S = 1.07 w = 1/[σ2(Fo2) + (0.0119P)2 + 0.0612P]
where P = (Fo2 + 2Fc2)/3
2743 reflections(Δ/σ)max = 0.001
208 parametersΔρmax = 0.42 e Å−3
12 restraintsΔρmin = −0.60 e Å−3
Crystal data top
[Pr(NO3)3(H2O)4]·2H2Oγ = 69.696 (4)°
Mr = 435.04V = 626.60 (6) Å3
Triclinic, P1Z = 2
a = 6.7017 (3) ÅMo Kα radiation
b = 9.1858 (4) ŵ = 3.98 mm−1
c = 11.7010 (6) ÅT = 100 K
α = 69.118 (4)°0.37 × 0.17 × 0.14 mm
β = 88.958 (4)°
Data collection top
Agilent SuperNova
diffractometer with an Atlas detector		2743 independent reflections
Absorption correction: numerical
[CrysAlis PRO (Agilent, 2010), using a multi-faceted crystal model based on expressions derived by Clark & Reid (1995)]		2627 reflections with I > 2σ(I)
Tmin = 0.375, Tmax = 0.654Rint = 0.035
10260 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01712 restraints
wR(F2) = 0.037All H-atom parameters refined
S = 1.07Δρmax = 0.42 e Å−3
2743 reflectionsΔρmin = −0.60 e Å−3
208 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
N10.6816 (3)−0.2289 (2)0.81616 (17)0.0107 (4)
N20.4207 (3)0.3279 (2)0.82332 (17)0.0111 (4)
N30.4305 (3)0.3335 (2)0.49700 (17)0.0111 (4)
O10.6030 (3)−0.15602 (19)0.70360 (14)0.0153 (4)
O20.5933 (3)−0.15874 (19)0.88855 (14)0.0154 (4)
O30.8379 (3)−0.36072 (19)0.85198 (15)0.0159 (4)
O40.5626 (3)0.18920 (19)0.82739 (15)0.0146 (4)
O50.2358 (3)0.36386 (19)0.77331 (14)0.0147 (4)
O60.4629 (3)0.41926 (19)0.86512 (15)0.0168 (4)
O70.2409 (3)0.37864 (19)0.52158 (15)0.0155 (4)
O80.5621 (2)0.19139 (18)0.56929 (14)0.0124 (3)
O90.4894 (3)0.42152 (19)0.40734 (14)0.0156 (4)
O100.2205 (3)0.0527 (2)0.54042 (15)0.0124 (3)
H10A0.285 (4)−0.016 (3)0.510 (2)0.019*
H10B0.128 (4)0.119 (3)0.483 (2)0.019*
O110.1239 (3)−0.1023 (2)0.77928 (15)0.0149 (4)
H11A0.110 (5)−0.154 (3)0.740 (2)0.022*
H11B0.122 (5)−0.162 (3)0.8474 (18)0.022*
O120.2015 (3)0.0533 (2)0.93368 (15)0.0119 (3)
H12A0.268 (4)−0.009 (3)1.0013 (18)0.018*
H12B0.112 (4)0.126 (3)0.951 (2)0.018*
O13−0.0770 (3)0.2713 (2)0.67182 (16)0.0159 (4)
H13A−0.175 (4)0.241 (3)0.695 (3)0.024*
H13B−0.134 (4)0.366 (2)0.627 (2)0.024*
O140.9130 (3)0.27933 (19)0.35872 (15)0.0121 (3)
H14A0.794 (3)0.326 (3)0.379 (2)0.018*
H14B0.940 (4)0.356 (3)0.311 (2)0.018*
O15−0.1154 (3)0.2943 (2)0.98338 (15)0.0137 (4)
H15B−0.231 (3)0.328 (3)0.941 (2)0.020*
H15A−0.075 (4)0.366 (3)0.976 (3)0.020*
Pr10.305901 (18)0.096024 (13)0.725397 (10)0.00646 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0087 (10)0.0073 (9)0.0132 (10)−0.0035 (8)0.0018 (8)−0.0001 (8)
N20.0138 (10)0.0104 (9)0.0071 (9)−0.0056 (8)0.0001 (8)−0.0001 (8)
N30.0115 (10)0.0089 (9)0.0126 (10)−0.0032 (8)0.0030 (8)−0.0041 (8)
O10.0165 (9)0.0132 (8)0.0087 (8)0.0011 (7)0.0011 (7)−0.0018 (7)
O20.0166 (9)0.0125 (8)0.0111 (8)0.0016 (7)−0.0011 (7)−0.0043 (7)
O30.0125 (9)0.0070 (7)0.0201 (9)0.0008 (7)0.0021 (7)−0.0002 (7)
O40.0136 (9)0.0124 (8)0.0174 (8)−0.0023 (7)0.0001 (7)−0.0073 (7)
O50.0123 (8)0.0088 (7)0.0192 (9)−0.0026 (6)−0.0046 (7)−0.0019 (7)
O60.0242 (10)0.0121 (8)0.0175 (9)−0.0095 (7)−0.0022 (7)−0.0064 (7)
O70.0094 (9)0.0123 (8)0.0196 (9)−0.0011 (7)0.0050 (7)−0.0031 (7)
O80.0091 (8)0.0092 (7)0.0117 (8)−0.0011 (6)−0.0009 (6)0.0021 (6)
O90.0208 (9)0.0103 (8)0.0113 (8)−0.0060 (7)0.0076 (7)0.0008 (7)
O100.0135 (9)0.0107 (8)0.0085 (8)0.0007 (7)−0.0019 (6)−0.0033 (7)
O110.0270 (10)0.0165 (9)0.0085 (8)−0.0152 (8)0.0050 (7)−0.0058 (7)
O120.0131 (9)0.0118 (8)0.0075 (8)−0.0013 (7)0.0015 (6)−0.0028 (7)
O130.0081 (9)0.0101 (8)0.0238 (9)−0.0025 (7)−0.0007 (7)−0.0005 (7)
O140.0136 (9)0.0083 (8)0.0122 (8)−0.0036 (7)0.0026 (7)−0.0019 (7)
O150.0167 (9)0.0107 (8)0.0153 (9)−0.0071 (7)0.0013 (7)−0.0048 (7)
Pr10.00633 (7)0.00570 (7)0.00600 (7)−0.00178 (5)0.00073 (5)−0.00104 (5)
Geometric parameters (Å, º) top
N1—O31.230 (2)O10—Pr12.4468 (17)
N1—O21.261 (3)O10—H10A0.823 (17)
N1—O11.270 (2)O10—H10B0.818 (17)
N1—Pr12.9996 (18)O11—Pr12.4287 (17)
N2—O61.219 (2)O11—H11A0.795 (17)
N2—O51.261 (2)O11—H11B0.796 (17)
N2—O41.284 (2)O12—Pr12.4555 (16)
N3—O91.229 (2)O12—H12A0.814 (16)
N3—O71.255 (2)O12—H12B0.810 (17)
N3—O81.280 (2)O13—Pr12.4578 (17)
O1—Pr12.5677 (16)O13—H13A0.806 (17)
O2—Pr12.5790 (15)O13—H13B0.791 (17)
O4—Pr12.6348 (16)O14—H14A0.841 (17)
O5—Pr12.6000 (17)O14—H14B0.803 (17)
O7—Pr12.7307 (15)O15—H15B0.827 (17)
O8—Pr12.6154 (16)O15—H15A0.772 (17)
O3—N1—O2121.92 (18)O12—Pr1—O268.79 (5)
O3—N1—O1121.3 (2)O13—Pr1—O2145.75 (6)
O2—N1—O1116.81 (17)O1—Pr1—O249.52 (5)
O3—N1—Pr1178.82 (15)O11—Pr1—O5130.84 (6)
O2—N1—Pr158.64 (10)O10—Pr1—O5132.67 (5)
O1—N1—Pr158.17 (10)O12—Pr1—O569.58 (5)
O6—N2—O5122.21 (19)O13—Pr1—O570.69 (5)
O6—N2—O4121.75 (19)O1—Pr1—O5143.42 (5)
O5—N2—O4116.04 (19)O2—Pr1—O5110.57 (5)
O9—N3—O7121.79 (18)O11—Pr1—O8139.83 (6)
O9—N3—O8120.80 (19)O10—Pr1—O874.17 (5)
O7—N3—O8117.42 (18)O12—Pr1—O8146.05 (5)
N1—O1—Pr196.98 (12)O13—Pr1—O8116.30 (5)
N1—O2—Pr196.69 (11)O1—Pr1—O868.73 (5)
N2—O4—Pr196.44 (12)O2—Pr1—O897.87 (5)
N2—O5—Pr198.76 (13)O5—Pr1—O887.86 (5)
N3—O7—Pr194.96 (11)O11—Pr1—O4140.59 (5)
N3—O8—Pr199.87 (12)O10—Pr1—O4144.15 (5)
Pr1—O10—H10A132.6 (19)O12—Pr1—O476.01 (5)
Pr1—O10—H10B127 (2)O13—Pr1—O4119.27 (6)
H10A—O10—H10B99 (3)O1—Pr1—O495.75 (5)
Pr1—O11—H11A127 (2)O2—Pr1—O468.85 (5)
Pr1—O11—H11B125 (2)O5—Pr1—O448.70 (5)
H11A—O11—H11B101 (3)O8—Pr1—O470.04 (5)
Pr1—O12—H12A131 (2)O11—Pr1—O7130.94 (5)
Pr1—O12—H12B123.3 (19)O10—Pr1—O769.86 (5)
H12A—O12—H12B101 (3)O12—Pr1—O7132.13 (5)
Pr1—O13—H13A126 (2)O13—Pr1—O769.00 (5)
Pr1—O13—H13B130 (2)O1—Pr1—O7110.69 (5)
H13A—O13—H13B104 (3)O2—Pr1—O7144.33 (5)
H14A—O14—H14B104 (3)O5—Pr1—O765.87 (5)
H15B—O15—H15A112 (3)O8—Pr1—O747.74 (5)
O11—Pr1—O1070.89 (6)O4—Pr1—O787.29 (5)
O11—Pr1—O1270.61 (6)O11—Pr1—N179.29 (6)
O10—Pr1—O12139.73 (6)O10—Pr1—N192.07 (5)
O11—Pr1—O1375.51 (6)O12—Pr1—N192.05 (5)
O10—Pr1—O1378.75 (6)O13—Pr1—N1154.78 (5)
O12—Pr1—O1380.71 (6)O1—Pr1—N124.84 (5)
O11—Pr1—O180.55 (6)O2—Pr1—N124.67 (5)
O10—Pr1—O168.87 (5)O5—Pr1—N1129.33 (5)
O12—Pr1—O1115.35 (5)O8—Pr1—N182.83 (5)
O13—Pr1—O1144.58 (6)O4—Pr1—N181.62 (5)
O11—Pr1—O279.84 (6)O7—Pr1—N1129.92 (5)
O10—Pr1—O2114.99 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O8i0.82 (2)2.10 (2)2.918 (2)177 (3)
O10—H10B···O14ii0.82 (2)1.85 (2)2.670 (2)176 (3)
O11—H11A···O14i0.80 (2)1.94 (2)2.735 (2)177 (3)
O11—H11B···O15iii0.80 (2)1.93 (2)2.720 (2)175 (3)
O12—H12A···O4iv0.81 (2)2.11 (2)2.925 (2)174 (3)
O12—H12B···O150.81 (2)1.91 (2)2.713 (2)175 (3)
O13—H13A···O4ii0.81 (2)2.38 (2)3.137 (2)156 (3)
O13—H13A···O8ii0.81 (2)2.57 (3)3.130 (2)128 (3)
O13—H13B···O7v0.79 (2)2.24 (2)3.020 (2)168 (3)
O13—H13B···O9v0.79 (2)2.43 (2)3.046 (2)136 (3)
O14—H14A···O90.84 (2)2.00 (2)2.826 (2)169 (3)
O14—H14B···O5vi0.80 (2)2.26 (2)2.881 (2)134 (3)
O14—H14B···O3vii0.80 (2)2.39 (2)2.971 (2)130 (3)
O15—H15B···O6ii0.83 (2)2.01 (2)2.824 (2)169 (3)
O15—H15A···O3iv0.77 (2)2.56 (2)3.049 (2)123 (2)
O15—H15A···O3viii0.77 (2)2.28 (2)2.892 (2)138 (3)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) −x, −y, −z+2; (iv) −x+1, −y, −z+2; (v) −x, −y+1, −z+1; (vi) −x+1, −y+1, −z+1; (vii) −x+2, −y, −z+1; (viii) x−1, y+1, z.

Experimental details

Crystal data
Chemical formula[Pr(NO3)3(H2O)4]·2H2O
Mr435.04
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)6.7017 (3), 9.1858 (4), 11.7010 (6)
α, β, γ (°)69.118 (4), 88.958 (4), 69.696 (4)
V (Å3)626.60 (6)
Z2
Radiation typeMo Kα
µ (mm−1)3.98
Crystal size (mm)0.37 × 0.17 × 0.14
Data collection
DiffractometerAgilent SuperNova
diffractometer with an Atlas detector
Absorption correctionNumerical
[CrysAlis PRO (Agilent, 2010), using a multi-faceted crystal model based on expressions derived by Clark & Reid (1995)]
Tmin, Tmax0.375, 0.654
No. of measured, independent and
observed [I > 2σ(I)] reflections		10260, 2743, 2627
Rint0.035
(sin θ/λ)max (Å−1)0.641
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.017, 0.037, 1.07
No. of reflections2743
No. of parameters208
No. of restraints12
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å−3)0.42, −0.60

Computer programs: CrysAlis PRO (Agilent, 2010), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2008), PLATON (Spek, 2009).

Selected bond lengths (Å) top
O1—Pr12.5677 (16)O8—Pr12.6154 (16)
O2—Pr12.5790 (15)O10—Pr12.4468 (17)
O4—Pr12.6348 (16)O11—Pr12.4287 (17)
O5—Pr12.6000 (17)O12—Pr12.4555 (16)
O7—Pr12.7307 (15)O13—Pr12.4578 (17)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O8i0.823 (17)2.096 (18)2.918 (2)177 (3)
O10—H10B···O14ii0.818 (16)1.853 (17)2.670 (2)176 (3)
O11—H11A···O14i0.795 (17)1.940 (18)2.735 (2)177 (3)
O11—H11B···O15iii0.796 (17)1.926 (18)2.720 (2)175 (3)
O12—H12A···O4iv0.814 (16)2.113 (17)2.925 (2)174 (3)
O12—H12B···O150.810 (17)1.905 (18)2.713 (2)175 (3)
O13—H13A···O4ii0.806 (17)2.38 (2)3.137 (2)156 (3)
O13—H13A···O8ii0.806 (17)2.57 (3)3.130 (2)128 (3)
O13—H13B···O7v0.791 (17)2.241 (18)3.020 (2)168 (3)
O13—H13B···O9v0.791 (17)2.43 (2)3.046 (2)136 (3)
O14—H14A···O90.841 (17)1.996 (18)2.826 (2)169 (3)
O14—H14B···O5vi0.803 (17)2.26 (2)2.881 (2)134 (3)
O14—H14B···O3vii0.803 (17)2.39 (2)2.971 (2)130 (3)
O15—H15B···O6ii0.827 (17)2.008 (18)2.824 (2)169 (3)
O15—H15A···O3iv0.772 (17)2.56 (2)3.049 (2)123 (2)
O15—H15A···O3viii0.772 (17)2.28 (2)2.892 (2)138 (3)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) −x, −y, −z+2; (iv) −x+1, −y, −z+2; (v) −x, −y+1, −z+1; (vi) −x+1, −y+1, −z+1; (vii) −x+2, −y, −z+1; (viii) x−1, y+1, z.
 

Acknowledgements

This research was co-funded by the Ghent University, GOA grant No. 01 G00710. RVD thanks the FWO-Flanders for financial support (research project G.0081.10 N).

References

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ISSN: 2056-9890
Volume 68| Part 7| July 2012| Pages i59-i60
https://doi.org/10.1107/S1600536812028024
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