inorganic papers
i80
Essehliet al. Y(HP2O7)3H2O doi:10.1107/S1600536807008318 Acta Cryst.(2007). E63, i80–i82 Acta Crystallographica Section E
Structure Reports Online
ISSN 1600-5368
Yttrium hydrogendiphosphate trihydrate
Rachid Essehli,aBrahim El Bali,b*
Michal Dusek,cKarla Fejfarovac
and Mohammed Lachkara
aLaboratoire d’Inge`nierie des Mate`riaux,
Organome´talliques et Mole`culaires, ‘LIMOM’, De´partement de Chimie, Faculte´ des Sciences, BP 1796 Fe`s-Atlas, 30000 Fe`s, Morocco, bLaboratory of Mineral Solid and Analytical
Chemistry, ‘LCSMA’, Department of Chemistry, Faculty of Sciences, University Mohamed I, PO Box 717, 60000 Oujda, Morocco, and c
Institute of Physics, Na Slovance 2, 182 21 Praha 8, Czech Republic
Correspondence e-mail: [email protected]
Key indicators
Single-crystal X-ray study
T= 294 K
Mean(P–O) = 0.002 A˚ H-atom completeness 72% Disorder in solvent or counterion
Rfactor = 0.021
wRfactor = 0.048
Data-to-parameter ratio = 12.7
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
Received 5 February 2007 Accepted 19 February 2007
#2007 International Union of Crystallography All rights reserved
The title compound, Y(HP2O7)3H2O, is isostructural with
Ln(HP2O7)3H2O (Ln = Gd, Er). The YO8 units and
(HP2O7) 3
anions form sheets parallel toab and a network of O—H O hydrogen bonds helps to establish the crystal packing.
Comment
The title compound, (I), is isostructural with ErHP2O73H2O
(Ben Moussa et al., 2004) and GdHP2O73H2O
(Chehimi-Moumen et al., 2001). However, LaHP2O7,3H2O adopts a
different structure in the space groupAba2 (Ben Moussaet al., 2004). Two different structure types are also known for the MHP2O73.5H2O family (Afonin et al., 1990), in which M =
La–Sm crystallize in the orthorhombic system (type I) andM = Sm–Lu crystallize in the triclinic system (type II) (Ben Moussaet al., 2000).
All the atoms in (I) are located on crystallographic general positions. Y is coordinated by six O atoms from diphosphate groups and two water O atoms (Fig. 1). The Y—O and Y— OH2 distances in (I) fall in the ranges 2.2493 (19)–2.594 (3)
and 2.366 (6)–2.4245 (5) A˚ , respectively. Such distances can be compared to the analagous values in ErHP2O73H2O
[2.241 (4)–2.569 (5) and 2.348 (6)–2.414 (5) A˚ ].
The two independent P tetrahedra in (I) share atom O6, with the P—O bridging bonds substantially longer than the terminal bonds (Table 1). The P—O—P angle is 133.11 (12).
Neighboring YO8units form chains alongb. The chains are
[image:1.610.215.444.513.685.2]interconnected by HP2O7anions, forming sheets parallel toab.
Figure 1
The third water molecule is disordered, and is located in the cavities between the sheets (Fig. 2).
The sheets in (I) are connected by a network of O—H O hydrogen bonds involving the HP2O7anions and the
coordi-nated water molecules (Fig. 3 and Table 2).
Experimental
An aqueous solution (10 ml) of YCl36H2O was added dropwise to an
solution (10 ml) of Na4P2O7(0.1 M); the pH of the mixture was
controlled with hydrochloric acid HCl (to pH = 2) and the solution was stirred for two h at room temperature. Colourless crystals of (I) formed after a few days.
Crystal data
Y(HP2O7)3H2O Mr= 317.9
Triclinic,P1 a= 6.4297 (7) A˚ b= 6.9042 (4) A˚ c= 9.8272 (10) A˚
= 81.612 (7)
= 80.306 (9)
= 88.413 (7) V= 425.42 (7) A˚3 Z= 2
MoKradiation
= 7.26 mm1 T= 294 K
0.190.080.02 mm
Data collection
Oxford Diffraction four-circle diffractometer with-geometry, model XCalibur-2, with CCD detector Sapphire-2
Absorption correction: analytical (CrysAlis RED; Oxford
Diffraction, 2005) Tmin= 0.335,Tmax= 0.721 5359 measured reflections 1746 independent reflections 1485 reflections withI> 3(I) Rint= 0.030
Refinement
R[F2> 2(F2)] = 0.021 wR(F2) = 0.048 S= 1.21 1746 reflections 137 parameters
H atoms treated by a mixture of independent and constrained refinement
max= 0.32 e A˚3 min=0.38 e A˚3
Table 1
Selected bond lengths (A˚ ).
Y1—O1i
2.2493 (19) Y1—O1ii
2.594 (2) Y1—O2ii 2.4549 (19) Y1—O2iii
2.2951 (19) Y1—O4 2.2827 (18) Y1—O5 2.2940 (19) Y1—O8 2.4245 (19) Y1—O9 2.366 (2)
P1—O1 1.5241 (19) P1—O2 1.531 (2) P1—O4 1.4921 (18) P1—O6 1.604 (2) P2—O3 1.500 (2) P2—O5 1.5006 (19) P2—O6 1.604 (2) P2—O7 1.556 (2)
[image:2.610.314.563.67.284.2]Symmetry codes: (i)x;yþ1;zþ1; (ii)xþ1;y;z; (iii)x;y;zþ1.
Table 2
Hydrogen-bond geometry (A˚ ,).
D—H A D—H H A D A D—H A
O7—H71 O3iv
0.818 (17) 1.779 (17) 2.596 (3) 176 (3) O8—H82 O3v
0.82 (2) 1.96 (2) 2.775 (3) 174 (3) O9—H91 O11 0.817 (17) 2.000 (17) 2.798 (5) 165 (3) O9—H92 O3iii 0.821 (17) 2.09 (2) 2.874 (3) 160 (3) O9—H91 O10 0.817 (17) 2.07 (3) 2.789 (8) 146 (3)
Symmetry codes: (iii)x;y;zþ1; (iv)x;y;zþ2; (v)xþ1;y;zþ1.
The uncoordinated water O atom is disordered over two positions in a 0.427 (4):0.573 (4) ratio. Its H atoms could not be located. The other H atoms were located in difference maps and and refined with a distance restraint of O—H = 0.82 (1) A˚ and withUiso(H) = 1.2Ueq(O).
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduc-tion: CrysAlis RED; program(s) used to solve structure: SIR2002 (Burlaet al., 2003); program(s) used to refine structure:JANA2000 (Petriceket al., 2000); molecular graphics:DIAMOND(Brandenburg
inorganic papers
Acta Cryst.(2007). E63, i80–i82 Essehliet al. Y(HP
2O7)3H2O
i81
Figure 2
The packing of (I), viewed alongb. The pairs of grey polyhedra represent chains of YO8units running alongb. Hydrogen bonds are represented by
[image:2.610.313.563.343.583.2]dashed lines.
Figure 3
The packing of (I), viewed alongc. Hydrogen bonds are represented by dashed lines. Colour key: grey YO8, pink P2O7, red balls O, and black
[image:2.610.46.298.650.715.2]& Putz, 2005); software used to prepare material for publication: JANA2000.
The authors thank the Grant Agency of the Czech Republic (grant No. 202/05/0421).
References
Afonin, E. G. & Pechurova, N. I. (1990).Russ. J. Inorg. Chem.35, 783–785. Ben Moussa, S., Sobrados, I., Iglesias, J. E., Trabelsi-Ayedi, M. & Sanz, J.
(2000).J. Mater. Chem.10, 1973–1978.
Ben Moussa, S., Ventemillas, S., Cabeza, A., Gutierrez-Puebla, E. & Sanz, J. (2004).J. Solid State Chem.177, 2129–2137.
Brandenburg, K. & Putz, H. (2005).DIAMOND. Version 3. Crystal Impact GbR, Bonn, Germany.
Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003).J. Appl. Cryst.36, 1103.
Chehimi-Moumen, F., Ben Hassen-Chehimi, D., Ferid, M. & Trabelsi-Ayadi, M. (2001).Mater. Res. Bull.36, 365–373.
Oxford Diffraction (2005). CrysAlis CCD and CrysAlis RED. Oxford Diffraction, Abingdon, Oxfordshire, England.
Petricek, V., Dusek, M. & Palatinus, L. (2000).JANA2000. Institute of Physics, Praha, Czech Republic.
inorganic papers
i82
Essehliet al. Y(HPsupporting information
sup-1
Acta Cryst. (2007). E63, i80–i82
supporting information
Acta Cryst. (2007). E63, i80–i82 [https://doi.org/10.1107/S1600536807008318]
Yttrium hydrogendiphosphate trihydrate
Rachid Essehli, Brahim El Bali, Michal Dusek, Karla Fejfarova and Mohammed Lachkar
yttrium hydrogendiphosphate trihydrate
Crystal data
Y(HP2O7)·3H2O Mr = 317.9 Triclinic, P1 Hall symbol: -P 1
a = 6.4297 (7) Å
b = 6.9042 (4) Å
c = 9.8272 (10) Å
α = 81.612 (7)°
β = 80.306 (9)°
γ = 88.413 (7)°
V = 425.42 (7) Å3
Z = 2
F(000) = 308
Dx = 2.481 Mg m−3
Mo Kα radiation, λ = 0.71069 Å Cell parameters from 5359 reflections
θ = 3.2–26.6°
µ = 7.26 mm−1 T = 294 K Blade, colourless 0.19 × 0.08 × 0.02 mm
Data collection
Oxford Diffraction CCD diffractometer
Radiation source: X-ray tube Graphite monochromator
Detector resolution: 8.3438 pixels mm-1
rotation method data acquisition using ω scans Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2005)
Tmin = 0.335, Tmax = 0.721
5359 measured reflections 1746 independent reflections 1485 reflections with I > 3σ(I)
Rint = 0.030
θmax = 26.6°, θmin = 3.2°
h = −8→7
k = −8→8
l = −12→12
Refinement
Refinement on F2 R[F > 3σ(F)] = 0.021
wR(F) = 0.048
S = 1.21 1746 reflections 137 parameters 8 restraints 5 constraints
H atoms treated by a mixture of independent and constrained refinement
Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2]
(Δ/σ)max = 0.020
Δρmax = 0.32 e Å−3
supporting information
sup-2
Acta Cryst. (2007). E63, i80–i82
Special details
Refinement. The refinement was carried out against all reflections. The conventional R-factor is always based on F. The goodness of fit as well as the weighted R-factor are based on F and F2 for refinement carried out on F and F2,
respectively. The threshold expression is used only for calculating R-factors etc. and it is not relevant to the choice of reflections for refinement.
The program used for refinement, Jana2000, uses the weighting scheme based on the experimental expectations, see _refine_ls_weighting_details, that does not force S to be one. Therefore the values of S are usually larger then the ones from the SHELX program.
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
x y z Uiso*/Ueq Occ. (<1)
Y1 0.37257 (4) 0.26045 (4) 0.45331 (3) 0.00917 (9) P1 −0.19333 (11) 0.23357 (10) 0.56158 (8) 0.0093 (2) P2 0.05684 (11) 0.14192 (11) 0.78774 (8) 0.0130 (2) O1 −0.3372 (3) 0.4128 (3) 0.5584 (2) 0.0133 (6) O2 −0.3314 (3) 0.0712 (3) 0.5339 (2) 0.0145 (7) O3 0.0671 (3) −0.0742 (3) 0.8353 (2) 0.0190 (7) O4 0.0146 (3) 0.2582 (3) 0.4672 (2) 0.0145 (6) O5 0.2422 (3) 0.2328 (3) 0.6874 (2) 0.0186 (7) O6 −0.1529 (3) 0.1807 (3) 0.7195 (2) 0.0175 (7) O7 0.0109 (4) 0.2607 (3) 0.9125 (2) 0.0239 (7) O8 0.6667 (3) 0.3602 (3) 0.2693 (2) 0.0219 (7) O9 0.2880 (3) 0.2676 (4) 0.2275 (2) 0.0273 (8)
O10 0.4997 (11) 0.1008 (12) 0.0009 (7) 0.0687 (19) 0.427 (4) O11 0.5105 (8) 0.3288 (10) −0.0454 (5) 0.0687 (19) 0.573 (4) H71 −0.008 (5) 0.200 (4) 0.9915 (15) 0.0287*
H91 0.364 (3) 0.267 (5) 0.1520 (16) 0.0327* H92 0.170 (2) 0.229 (5) 0.223 (3) 0.0327* H81 0.732 (3) 0.462 (2) 0.262 (3) 0.0263* H82 0.748 (3) 0.274 (3) 0.244 (3) 0.0263*
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
supporting information
sup-3
Acta Cryst. (2007). E63, i80–i82
Geometric parameters (Å, º)
Y1—O1i 2.2493 (19) P2—O3 1.500 (2)
Y1—O1ii 2.594 (2) P2—O5 1.5006 (19)
Y1—O2ii 2.4549 (19) P2—O6 1.604 (2)
Y1—O2iii 2.2951 (19) P2—O7 1.556 (2)
Y1—O4 2.2827 (18) O7—H71 0.818 (17)
Y1—O5 2.2940 (19) O8—H81 0.817 (18)
Y1—O8 2.4245 (19) O8—H82 0.82 (2)
Y1—O9 2.366 (2) O9—H91 0.817 (17)
P1—O1 1.5241 (19) O9—H92 0.818 (19)
P1—O2 1.531 (2) O10—O10iv 1.395 (12)
P1—O4 1.4921 (18) O10—O11 1.573 (11)
P1—O6 1.604 (2)
O1ii—Y1—O1i 68.00 (6) O4—Y1—O5 75.19 (7)
O1ii—Y1—O2ii 56.78 (6) O4—Y1—O8 134.71 (7)
O1ii—Y1—O2iii 122.87 (6) O4—Y1—O9 70.55 (7)
O1ii—Y1—O4 140.61 (7) O5—Y1—O8 146.41 (8)
O1ii—Y1—O5 75.61 (7) O5—Y1—O9 145.58 (7)
O1ii—Y1—O8 70.84 (7) O8—Y1—O9 67.09 (8)
O1ii—Y1—O9 135.72 (7) O1—P1—O2 103.80 (11)
O1i—Y1—O1ii 68.00 (6) O1—P1—O4 115.73 (11)
O1i—Y1—O2ii 124.52 (7) O1—P1—O6 106.23 (11)
O1i—Y1—O2iii 167.60 (7) O2—P1—O4 114.54 (12)
O1i—Y1—O4 85.39 (7) O2—P1—O6 107.18 (11)
O1i—Y1—O5 88.53 (7) O4—P1—O6 108.75 (11)
O1i—Y1—O8 80.81 (7) O3—P2—O5 117.12 (12)
O1i—Y1—O9 91.93 (8) O3—P2—O6 106.80 (12)
O2ii—Y1—O2iii 67.10 (7) O3—P2—O7 112.06 (12)
O2ii—Y1—O4 142.75 (6) O5—P2—O6 109.51 (11)
O2ii—Y1—O5 83.24 (7) O5—P2—O7 108.35 (13)
O2ii—Y1—O8 77.06 (6) O6—P2—O7 101.89 (12)
O2ii—Y1—O9 123.33 (7) P1—O6—P2 133.11 (12)
O2iii—Y1—O2ii 67.10 (7) P2—O7—H71 118 (2)
O2iii—Y1—O4 82.23 (7) H81—O8—H82 109 (2)
O2iii—Y1—O5 88.80 (7) H91—O9—H92 109 (3)
O2iii—Y1—O8 107.71 (7) O10iv—O10—O11 162.9 (7)
O2iii—Y1—O9 83.48 (8)
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x+1, y, z; (iii) −x, −y, −z+1; (iv) −x+1, −y, −z.
Hydrogen-bond geometry (Å, º)
D—H···A D—H H···A D···A D—H···A
O7—H71···O3v 0.818 (17) 1.779 (17) 2.596 (3) 176 (3)
O8—H82···O3vi 0.82 (2) 1.96 (2) 2.775 (3) 174 (3)
supporting information
sup-4
Acta Cryst. (2007). E63, i80–i82
O9—H92···O3iii 0.821 (17) 2.09 (2) 2.874 (3) 160 (3)
O9—H91···O10 0.817 (17) 2.07 (3) 2.789 (8) 146 (3)
