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

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ISSN: 2056-9890

KPr(PO3)4

aUniversité Cadi Ayyad, Laboratoire de la Matière Condensée et de l'Environnement, Faculté des Sciences Semlalia, Département de Chimie, BP 2390, 40000 Marrakech, Morocco, and bUniversité Blaise Pascal, Laboratoire des Matériaux Inorganiques, UMR CNRS 6002, 24 Avenue des Landais, 63177 Aubière, France
*Correspondence e-mail: daniel.avignant@univ-bpclermont.fr

(Received 1 July 2010; accepted 7 July 2010; online 14 July 2010)

Single crystals of the title compound, potassium praseodymium(III) polyphosphate, were obtained by solid-state reaction. The monoclinic non-centrosymmetric structure is isotypic with all other KLn(PO3)4 analogues from Ln = La to Er, inclusive. The crystal structure of these long-chain polyphosphates is built up from infinite crenelated polyphosphate chains of corner-sharing PO4 tetra­hedra with a repeating unit of four tetra­hedra. These chains, running along [100], are arranged in a pseudo-tetra­gonal rod packing and are further linked by isolated PrO8 square anti­prisms [Pr—O = 2.3787 (9)–2.5091 (8) Å], forming a three-dimensional framework. The K+ ions reside in channels parallel to [010] and exhibit a highly distorted coordination sphere by eight O atoms at distances ranging from 2.7908 (9) to 3.1924 (11) Å.

Related literature

Long-chain polyphosphates with general formula AIBIII(PO3)4 have been classified into seven structural types, labelled from I to VII (Jaoudi et al., 2003[Jaoudi, K., Naïli, H., Zouari, N., Mhiri, T. & Daoud, A. (2003). J. Alloys Compd, 354, 104-114.]). All KLn(PO3)4 polyphosphates (Ln is a trivalent rare earth element) reported up to now adopt type III except for KYb(PO3)4 (Palkina et al., 1981[Palkina, K. K., Maksimova, S. I., Chudinova, N. N., Vinogradova, N. V. & Chibiskova, N. T. (1981). Izv. Akad. Nauk. SSSR Neorg. Mater. 17, 110-115.]). For corresponding isotypic crystal structures, see: Zhu et al. (2009[Zhu, J., Cheng, W., Zhang, H. & Wang, Y. (2009). J. Lumin. 129, 1326-1331.]) for Ce and Eu; Horchani-Naifer et al. (2008[Horchani-Naifer, K., Jouini, A. & Férid, M. (2008). Acta Cryst. E64, i34.]) for Y; Parreu et al. (2006[Parreu, I., Carvajal, J. J., Solans, X., Diaz, F. & Aguilo, M. (2006). Chem. Mater. 18, 221-228.]) for Gd and Nd; Xing et al. (1987[Xing, Y., Hu, N. H., Zhou, Q. L., Hong, G. Y. & Yue, S. Y. (1987). Wuli Huaxue Xenbao, 3, 218-221.]) for Tb; Ninghai et al. (1984[Ninghai, H., Yonghua, L., Zhou, Q. L. & Liu, S. Z. (1984). Yingyong Huaxue, 1, 47-50.]) for Eu; Lin et al. (1983[Lin, Y. H., Hu, N. H., Zhou, Q. L. & Liu, S. Z. (1983). Wu Li Hsueh Pao, 32, 675-680.]) for La; Krutik et al. (1980[Krutik, V.M, Pushcharovskii, D. Yu., Pobedimskaya, E.A. & Belov N.V. (1980). Dokl. Akad. Nauk SSSR, 252, 607-610.]) for Er; Hong et al. (1975[Hong, H. Y. (1975). Mater. Res. Bull. 10, 1105-1110.]) for Nd. For a review of the crystal chemistry of phosphates, see: Durif (1995[Durif, A. (1995). Crystal Chemistry of Condensed Phosphates. New York and London: Plenum Press.]). For the cyclo­phosphate structure with the same composition, KPr(PO3)4, see: Zhou et al. (1987[Zhou, Q.-L., Hu, N.-H., Hong, G.-Y. & Yue, S.-Y. (1987). Yingyong Huaxue, 4, 46-50.]).

Experimental

Crystal data
  • KPr(PO3)4

  • Mr = 495.89

  • Monoclinic, P 21

  • a = 7.2872 (2) Å

  • b = 8.4570 (3) Å

  • c = 8.0268 (2) Å

  • β = 91.994 (1)°

  • V = 494.37 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 6.06 mm−1

  • T = 296 K

  • 0.29 × 0.21 × 0.16 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS, APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.448, Tmax = 0.751

  • 45940 measured reflections

  • 13443 independent reflections

  • 13257 reflections with I > 2σ(I)

  • Rint = 0.034

Refinement
  • R[F2 > 2σ(F2)] = 0.018

  • wR(F2) = 0.043

  • S = 1.07

  • 13443 reflections

  • 164 parameters

  • 1 restraint

  • Δρmax = 2.86 e Å−3

  • Δρmin = −2.42 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 6278 Friedel pairs

  • Flack parameter: 0.022 (3)

Table 1
Selected bond lengths (Å)

P1—O6 1.4841 (8)
P1—O12 1.4850 (8)
P1—O5 1.5881 (7)
P1—O10 1.5887 (9)
P2—O11 1.4810 (9)
P2—O7i 1.4822 (8)
P2—O1 1.5926 (8)
P2—O2 1.5941 (8)
P3—O3ii 1.4806 (8)
P3—O4 1.4832 (8)
P3—O5 1.5902 (8)
P3—O1iii 1.5980 (8)
P4—O8iv 1.4777 (8)
P4—O9v 1.4829 (8)
P4—O2 1.5874 (8)
P4—O10 1.5973 (9)
Symmetry codes: (i) [-x+1, y+{\script{1\over 2}}, -z+1]; (ii) [-x, y+{\script{1\over 2}}, -z+1]; (iii) x-1, y, z; (iv) [-x+1, y-{\script{1\over 2}}, -z+1]; (v) x, y, z-1.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). SADABS, APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). SADABS, APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: CaRine (Boudias & Monceau, 1998[Boudias, C. & Monceau, D. (1998). CaRine. CaRine Crystallography, DIVERGENT SA, Compiègne, France.]) and ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

Long chains polyphosphates with general formula AIBIII(PO3)4 have been classified into seven structural types, labelled from I to VII (Durif, 1995; Jaoudi et al. 2003). All long-chains polyphosphates of formula KLn(PO3)4 (Ln = rare earth elements) reported up to now (Zhu et al., 2009; Horchani-Naifer et al., 2008; Parreu et al., 2006; Xing et al., 1987; Ninghai et al., 1984; Lin et al., 1983; Krutik et al., 1980; Hong et al., 1975) adopt type III except for KYb(PO3)4 (Palkina et al. 1981) which is the only presently known member of type V. Most of these potassium polyphosphates are dimorphic and crystallize with both the type III and the type IV polymorphs. KCe(PO3)4 which has been shown to crystallize with either the type II and the type III is the first exception. The second exception is concerned with the Er member of this series presenting the type VII polymorph besides both type III and type IV polymorphs. Moreover, type III long-chain polyphosphates do not exist for monovalent cations other than K+. The structure of the title compound also fits in this type III isotypic series.

The crystal structure of the title compound is built from crenelated chains with a repeating unit of four corner-sharing tetrahedra, as displayed in Fig. 1. The chains are further linked by isolated PrO8 square antiprisms to form the three-dimensional framework. Each PrO8 polyhedron (Pr—O distances range from 2.3787 (9) to 2.5091 (8) Å) is connected through vertices to four (PO3) chains stacked in a pseudo-tetragonal rod packing as shown in Fig. 2. Figure 2 also shows that within this pseudo-tetragonal rod packing, two adjacent chains are twisted by ca. 90 ° whereas two opposite chains are parallel. The relative disposition of the chains running along the [100] direction accounts for the strong non-centrosymmetric character of the structure. Figure 3 displays details of the connections between the PrO8 square antiprisms and the four chains surrounding each antiprism. One of the four chains (labelled C1) is attached in a tridentate fashion on a triangular face of the square antiprism whereas the opposite and parallel chain (labelled C2) is connected only through a vertex (Fig. 3a). The two other chains which are adjacent to the first one are attached in a bidentate fashion. The first of these two chains (labelled C3) is linked through a bidentate diphosphate group attached on one side of one square face of the square antiprism (Fig. 3b). The second chain (labelled C4) is connected at the ends of one diagonal of the second square face of the antiprism (Fig. 3c) through corners of the terminal PO4 groups of the crenel-shaped tetraphosphate group corresponding to the repeating unit of the chain. This polyhedral linkage delimits channels running along [010] where the K+ions lie in a highly distorted environment defined by eight oxygen atoms at distances ranging from 2.7908 (9) to 3.1924 (11) Å.

For the cyclophosphate structure with the same composition KPr(PO3)4, see: (Zhou et al., 1987).

Related literature top

Long-chain polyphosphates with general formula AIBIII(PO3)4 have been classified into seven structural types, labelled from I to VII (Jaoudi et al., 2003). All KLn(PO3)4 polyphosphates (Ln is a trivalent rare earth element) reported up to now adopt type III except for KYb(PO3)4 (Palkina et al., 1981). For corresponding isotypic crystal structures, see: Zhu et al. (2009) for Ce and Eu; Horchani-Naifer et al. (2008) for Y; Parreu et al. (2006) for Gd and Nd; Xing et al. (1987) for Tb; Ninghai et al. (1984) for Eu; Lin et al. (1983) for La; Krutik et al. (1980) for Er; Hong et al. (1975) for Nd. For a review of the crystal chemistry of phosphates, see: Durif (1995). For the cyclophosphate structure with the same composition, KPr(PO3)4, see: Zhou et al. (1987).

Experimental top

Crystals of the title compound were synthesized by reacting Pr6O11 with (NH4)H2PO4 and K2CO3 in a platinum crucible. A mixture of these reagents in the molar ratio 14: 66: 20 was used for the synthesis. The mixture has first been heated at 473 K for 12 h and then the temperature has been increased up to 573 K and maintained for 12 h before to be raised at 853 K and kept for 24 additional hours. At the end of this heating step, the muffle furnace was cooled down first to 673 K at the rate of 2 K h-1 and subsequently to room temperature by switching the power off. Single crystals were extracted from the batch by leaching with hot water.

Refinement top

The highest residual peak in the final difference Fourier map was located 0.46 Å from atom Pr and the deepest hole was located 0.47 Å from atom K.

Structure description top

Long chains polyphosphates with general formula AIBIII(PO3)4 have been classified into seven structural types, labelled from I to VII (Durif, 1995; Jaoudi et al. 2003). All long-chains polyphosphates of formula KLn(PO3)4 (Ln = rare earth elements) reported up to now (Zhu et al., 2009; Horchani-Naifer et al., 2008; Parreu et al., 2006; Xing et al., 1987; Ninghai et al., 1984; Lin et al., 1983; Krutik et al., 1980; Hong et al., 1975) adopt type III except for KYb(PO3)4 (Palkina et al. 1981) which is the only presently known member of type V. Most of these potassium polyphosphates are dimorphic and crystallize with both the type III and the type IV polymorphs. KCe(PO3)4 which has been shown to crystallize with either the type II and the type III is the first exception. The second exception is concerned with the Er member of this series presenting the type VII polymorph besides both type III and type IV polymorphs. Moreover, type III long-chain polyphosphates do not exist for monovalent cations other than K+. The structure of the title compound also fits in this type III isotypic series.

The crystal structure of the title compound is built from crenelated chains with a repeating unit of four corner-sharing tetrahedra, as displayed in Fig. 1. The chains are further linked by isolated PrO8 square antiprisms to form the three-dimensional framework. Each PrO8 polyhedron (Pr—O distances range from 2.3787 (9) to 2.5091 (8) Å) is connected through vertices to four (PO3) chains stacked in a pseudo-tetragonal rod packing as shown in Fig. 2. Figure 2 also shows that within this pseudo-tetragonal rod packing, two adjacent chains are twisted by ca. 90 ° whereas two opposite chains are parallel. The relative disposition of the chains running along the [100] direction accounts for the strong non-centrosymmetric character of the structure. Figure 3 displays details of the connections between the PrO8 square antiprisms and the four chains surrounding each antiprism. One of the four chains (labelled C1) is attached in a tridentate fashion on a triangular face of the square antiprism whereas the opposite and parallel chain (labelled C2) is connected only through a vertex (Fig. 3a). The two other chains which are adjacent to the first one are attached in a bidentate fashion. The first of these two chains (labelled C3) is linked through a bidentate diphosphate group attached on one side of one square face of the square antiprism (Fig. 3b). The second chain (labelled C4) is connected at the ends of one diagonal of the second square face of the antiprism (Fig. 3c) through corners of the terminal PO4 groups of the crenel-shaped tetraphosphate group corresponding to the repeating unit of the chain. This polyhedral linkage delimits channels running along [010] where the K+ions lie in a highly distorted environment defined by eight oxygen atoms at distances ranging from 2.7908 (9) to 3.1924 (11) Å.

For the cyclophosphate structure with the same composition KPr(PO3)4, see: (Zhou et al., 1987).

Long-chain polyphosphates with general formula AIBIII(PO3)4 have been classified into seven structural types, labelled from I to VII (Jaoudi et al., 2003). All KLn(PO3)4 polyphosphates (Ln is a trivalent rare earth element) reported up to now adopt type III except for KYb(PO3)4 (Palkina et al., 1981). For corresponding isotypic crystal structures, see: Zhu et al. (2009) for Ce and Eu; Horchani-Naifer et al. (2008) for Y; Parreu et al. (2006) for Gd and Nd; Xing et al. (1987) for Tb; Ninghai et al. (1984) for Eu; Lin et al. (1983) for La; Krutik et al. (1980) for Er; Hong et al. (1975) for Nd. For a review of the crystal chemistry of phosphates, see: Durif (1995). For the cyclophosphate structure with the same composition, KPr(PO3)4, see: Zhou et al. (1987).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CaRine (Boudias & Monceau, 1998) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. View of the repeating unit of the (PO3) chains. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (vi) -x + 1, y + 1/2, -z + 1; (vii) x, y, z - 1; (viii) -x, y + 1/2, -z + 1; (ix) x - 1, y, z.]
[Figure 2] Fig. 2. Projection along [100] showing the pseudo-tetragonal rod packing of the infinite (PO3) chains.
[Figure 3] Fig. 3. Details of the connections between the (PO3) chains and the PrO8 square antiprisms: a) view showing the tridentate attachement of one chain (C1) and the connection of the second chain (C2) parallel and opposite to the first one. b) view showing the bidentate attachement of the third chain (C3) adjacent and orthogonal to the first one. c) view showing the bidentate attachement of the fourth chain (C4) also orthogonal and adjacent to the first one.
Potassium praseodymium polyphosphate top
Crystal data top
KPr(PO3)4F(000) = 468
Mr = 495.89Dx = 3.331 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 9960 reflections
a = 7.2872 (2) Åθ = 2.8–57.3°
b = 8.4570 (3) ŵ = 6.06 mm1
c = 8.0268 (2) ÅT = 296 K
β = 91.994 (1)°Prism, green
V = 494.37 (3) Å30.29 × 0.21 × 0.16 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer
13443 independent reflections
Radiation source: fine-focus sealed tube13257 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 8.3333 pixels mm-1θmax = 57.4°, θmin = 3.7°
ω and φ scansh = 1717
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
k = 1920
Tmin = 0.448, Tmax = 0.751l = 1818
45940 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.P)2 + 0.0715P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.018(Δ/σ)max = 0.004
wR(F2) = 0.043Δρmax = 2.86 e Å3
S = 1.07Δρmin = 2.42 e Å3
13443 reflectionsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
164 parametersExtinction coefficient: 0.0305 (6)
1 restraintAbsolute structure: Flack (1983), 6278 Friedel pairs
0 constraintsAbsolute structure parameter: 0.022 (3)
Primary atom site location: structure-invariant direct methods
Crystal data top
KPr(PO3)4V = 494.37 (3) Å3
Mr = 495.89Z = 2
Monoclinic, P21Mo Kα radiation
a = 7.2872 (2) ŵ = 6.06 mm1
b = 8.4570 (3) ÅT = 296 K
c = 8.0268 (2) Å0.29 × 0.21 × 0.16 mm
β = 91.994 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
13443 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
13257 reflections with I > 2σ(I)
Tmin = 0.448, Tmax = 0.751Rint = 0.034
45940 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0181 restraint
wR(F2) = 0.043Δρmax = 2.86 e Å3
S = 1.07Δρmin = 2.42 e Å3
13443 reflectionsAbsolute structure: Flack (1983), 6278 Friedel pairs
164 parametersAbsolute structure parameter: 0.022 (3)
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
K0.77227 (5)0.31500 (7)0.72001 (4)0.02909 (8)
Pr0.265282 (4)0.119995 (8)0.757982 (4)0.00552 (1)
P10.50137 (3)0.26677 (3)0.38019 (3)0.00690 (3)
P20.93476 (3)0.24280 (3)0.09865 (3)0.00685 (3)
P30.12252 (3)0.37267 (3)0.39531 (3)0.00674 (3)
P40.60346 (3)0.04117 (3)0.10444 (3)0.00675 (3)
O11.04301 (12)0.23711 (10)0.27436 (11)0.01360 (11)
O20.81354 (11)0.08886 (10)0.12702 (13)0.01412 (12)
O30.03801 (11)0.02642 (9)0.65100 (11)0.01191 (10)
O40.11151 (11)0.31458 (11)0.56903 (9)0.01188 (10)
O50.33093 (10)0.38001 (9)0.34329 (10)0.01061 (9)
O60.66909 (10)0.36646 (10)0.38630 (10)0.01127 (9)
O70.18250 (12)0.11539 (10)0.92653 (10)0.01172 (10)
O80.41427 (12)0.38104 (10)0.82424 (13)0.01527 (12)
O90.53826 (12)0.07174 (11)0.93036 (10)0.01395 (12)
O100.49263 (14)0.16280 (13)0.21526 (13)0.01754 (15)
O111.06463 (16)0.21154 (13)0.03535 (13)0.01866 (16)
O120.46952 (13)0.16652 (11)0.52829 (11)0.01411 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K0.01717 (11)0.0542 (3)0.01579 (10)0.00955 (13)0.00159 (8)0.00090 (12)
Pr0.00546 (1)0.00563 (1)0.00548 (1)0.00032 (1)0.00021 (1)0.00006 (1)
P10.00666 (7)0.00665 (7)0.00750 (7)0.00002 (5)0.00174 (5)0.00055 (5)
P20.00649 (6)0.00695 (7)0.00716 (7)0.00010 (5)0.00069 (5)0.00144 (5)
P30.00623 (6)0.00685 (7)0.00704 (7)0.00079 (5)0.00105 (5)0.00031 (5)
P40.00704 (7)0.00576 (6)0.00735 (7)0.00051 (5)0.00141 (5)0.00019 (5)
O10.0159 (3)0.0098 (2)0.0145 (3)0.0010 (2)0.0082 (2)0.00244 (18)
O20.0083 (2)0.0108 (2)0.0229 (3)0.00354 (17)0.0037 (2)0.0027 (2)
O30.0102 (2)0.0084 (2)0.0168 (3)0.00284 (17)0.00320 (19)0.00037 (18)
O40.0114 (2)0.0160 (3)0.0082 (2)0.0013 (2)0.00038 (16)0.00301 (18)
O50.00730 (18)0.0111 (2)0.0135 (2)0.00173 (16)0.00166 (16)0.00354 (18)
O60.00779 (19)0.0116 (2)0.0145 (2)0.00191 (17)0.00084 (16)0.00167 (19)
O70.0141 (2)0.0103 (2)0.0106 (2)0.00433 (19)0.00116 (18)0.00117 (17)
O80.0131 (3)0.0090 (2)0.0235 (4)0.00183 (19)0.0015 (2)0.0067 (2)
O90.0143 (3)0.0186 (3)0.0087 (2)0.0028 (2)0.00406 (18)0.0001 (2)
O100.0157 (3)0.0201 (3)0.0169 (3)0.0020 (3)0.0016 (2)0.0106 (3)
O110.0206 (4)0.0191 (3)0.0171 (3)0.0030 (3)0.0121 (3)0.0029 (3)
O120.0141 (3)0.0144 (3)0.0142 (3)0.0033 (2)0.0059 (2)0.0074 (2)
Geometric parameters (Å, º) top
K—O4i2.7908 (9)P2—O7vi1.4822 (8)
K—O62.7909 (9)P2—O11.5926 (8)
K—O82.8231 (10)P2—O21.5941 (8)
K—O3i2.8684 (10)P2—Kvii3.2805 (4)
K—O7ii2.9050 (9)P3—O3viii1.4806 (8)
K—O122.9285 (11)P3—O41.4832 (8)
K—O11iii2.9781 (13)P3—O51.5902 (8)
K—O93.1924 (11)P3—O1ix1.5980 (8)
K—P2iii3.2805 (4)P4—O8v1.4777 (8)
K—P13.3360 (4)P4—O9vii1.4829 (8)
Pr—O11iv2.3787 (9)P4—O21.5874 (8)
Pr—O92.4180 (8)P4—O101.5973 (9)
Pr—O122.4414 (8)O1—P3i1.5980 (8)
Pr—O32.4731 (7)O3—P3x1.4806 (8)
Pr—O42.4791 (8)O3—Kix2.8684 (10)
Pr—O6v2.4912 (8)O4—Kix2.7908 (9)
Pr—O72.4928 (8)O6—Prvi2.4912 (8)
Pr—O82.5091 (8)O7—P2v1.4822 (8)
P1—O61.4841 (8)O7—Kxi2.9051 (9)
P1—O121.4850 (8)O8—P4vi1.4776 (8)
P1—O51.5881 (7)O9—P4iii1.4829 (8)
P1—O101.5887 (9)O11—Prxii2.3787 (9)
P2—O111.4810 (9)O11—Kvii2.9782 (13)
O4i—K—O678.26 (2)O12—Pr—O875.38 (3)
O4i—K—O8166.08 (3)O3—Pr—O8136.89 (3)
O6—K—O891.87 (3)O4—Pr—O874.26 (3)
O4i—K—O3i58.32 (3)O6v—Pr—O8140.10 (3)
O6—K—O3i93.61 (3)O7—Pr—O8134.32 (3)
O8—K—O3i133.01 (3)O11iv—Pr—Kix48.64 (3)
O4i—K—O7ii110.62 (3)O9—Pr—Kix147.29 (2)
O6—K—O7ii157.42 (3)O12—Pr—Kix116.78 (2)
O8—K—O7ii75.23 (3)O3—Pr—Kix46.23 (2)
O3i—K—O7ii108.78 (3)O4—Pr—Kix44.44 (2)
O4i—K—O12115.71 (3)O6v—Pr—Kix120.771 (19)
O6—K—O1252.38 (2)O7—Pr—Kix97.96 (2)
O8—K—O1263.48 (3)O8—Pr—Kix91.99 (2)
O3i—K—O1283.86 (3)O11iv—Pr—K120.16 (3)
O7ii—K—O12131.14 (3)O9—Pr—K51.68 (2)
O4i—K—O11iii70.23 (2)O12—Pr—K45.47 (3)
O6—K—O11iii147.28 (3)O3—Pr—K155.08 (2)
O8—K—O11iii120.66 (3)O4—Pr—K94.44 (2)
O3i—K—O11iii62.54 (3)O6v—Pr—K97.156 (19)
O7ii—K—O11iii50.31 (2)O7—Pr—K127.02 (2)
O12—K—O11iii136.81 (3)O8—Pr—K43.25 (2)
O4i—K—O9136.58 (3)Kix—Pr—K130.558 (15)
O6—K—O9118.49 (3)O6—P1—O12116.70 (5)
O8—K—O956.95 (3)O6—P1—O5107.54 (5)
O3i—K—O979.85 (3)O12—P1—O5110.52 (5)
O7ii—K—O970.04 (3)O6—P1—O10110.55 (5)
O12—K—O966.11 (2)O12—P1—O10110.38 (6)
O11iii—K—O981.08 (3)O5—P1—O1099.78 (5)
O4i—K—P2iii96.054 (18)O6—P1—K55.97 (3)
O6—K—P2iii174.10 (2)O12—P1—K61.30 (4)
O8—K—P2iii94.00 (2)O5—P1—K121.03 (3)
O3i—K—P2iii81.93 (2)O10—P1—K138.98 (4)
O7ii—K—P2iii26.858 (16)O11—P2—O7vi115.17 (6)
O12—K—P2iii130.40 (2)O11—P2—O1109.17 (6)
O11iii—K—P2iii26.821 (17)O7vi—P2—O1114.25 (5)
O9—K—P2iii64.676 (17)O11—P2—O2109.22 (6)
O4i—K—P198.784 (19)O7vi—P2—O2111.14 (5)
O6—K—P126.147 (16)O1—P2—O296.24 (5)
O8—K—P174.92 (2)O11—P2—Kvii65.14 (5)
O3i—K—P190.78 (2)O7vi—P2—Kvii62.31 (3)
O7ii—K—P1150.12 (2)O1—P2—Kvii167.90 (4)
O12—K—P126.409 (16)O2—P2—Kvii95.76 (4)
O11iii—K—P1153.20 (3)O3viii—P3—O4119.42 (5)
O9—K—P192.400 (19)O3viii—P3—O5107.01 (5)
P2iii—K—P1156.78 (2)O4—P3—O5110.07 (4)
O4i—K—P4vi148.57 (3)O3viii—P3—O1ix109.79 (4)
O6—K—P4vi96.19 (2)O4—P3—O1ix107.65 (5)
O8—K—P4vi21.809 (17)O5—P3—O1ix101.41 (5)
O3i—K—P4vi152.95 (2)O3viii—P3—Kix90.09 (4)
O7ii—K—P4vi65.122 (18)O5—P3—Kix150.30 (3)
O12—K—P4vi82.33 (2)O1ix—P3—Kix95.04 (4)
O11iii—K—P4vi115.28 (2)O8v—P4—O9vii119.69 (6)
O9—K—P4vi73.308 (19)O8v—P4—O2106.59 (5)
P2iii—K—P4vi89.502 (11)O9vii—P4—O2109.84 (5)
P1—K—P4vi87.099 (10)O8v—P4—O10108.77 (6)
O4i—K—P3i20.271 (16)O9vii—P4—O10105.12 (6)
O6—K—P3i58.589 (17)O2—P4—O10106.09 (5)
O8—K—P3i147.16 (3)O8v—P4—Kv45.22 (4)
O3i—K—P3i68.374 (19)O9vii—P4—Kv103.55 (4)
O7ii—K—P3i126.64 (2)O2—P4—Kv145.07 (4)
O12—K—P3i102.092 (19)O10—P4—Kv73.90 (4)
O11iii—K—P3i90.45 (2)P2—O1—P3i132.40 (6)
O9—K—P3i147.36 (2)P4—O2—P2136.74 (6)
P2iii—K—P3i115.882 (11)P3x—O3—Pr136.64 (5)
P1—K—P3i81.085 (10)P3x—O3—Kix126.63 (4)
P4vi—K—P3i137.479 (17)Pr—O3—Kix95.26 (3)
O11iv—Pr—O999.75 (4)P3—O4—Pr139.19 (5)
O11iv—Pr—O12151.63 (3)P3—O4—Kix119.05 (4)
O9—Pr—O1287.04 (3)Pr—O4—Kix97.10 (3)
O11iv—Pr—O377.45 (4)P1—O5—P3132.48 (5)
O9—Pr—O3148.45 (3)P1—O6—Prvi130.14 (5)
O12—Pr—O3110.50 (3)P1—O6—K97.89 (4)
O11iv—Pr—O486.26 (3)Prvi—O6—K122.05 (3)
O9—Pr—O4143.85 (3)P2v—O7—Pr136.16 (5)
O12—Pr—O472.87 (3)P2v—O7—Kxi90.83 (4)
O3—Pr—O467.70 (3)Pr—O7—Kxi132.10 (3)
O11iv—Pr—O6v137.47 (3)P4vi—O8—Pr147.72 (6)
O9—Pr—O6v87.33 (3)P4vi—O8—K112.97 (5)
O12—Pr—O6v69.86 (3)Pr—O8—K99.24 (3)
O3—Pr—O6v75.34 (3)P4iii—O9—Pr143.02 (6)
O4—Pr—O6v112.14 (3)P4iii—O9—K116.82 (5)
O11iv—Pr—O773.45 (4)Pr—O9—K91.87 (3)
O9—Pr—O776.38 (3)P1—O10—P4144.49 (7)
O12—Pr—O7134.75 (3)P2—O11—Prxii171.29 (7)
O3—Pr—O772.70 (3)P2—O11—Kvii88.04 (5)
O4—Pr—O7138.54 (3)Prxii—O11—Kvii94.52 (4)
O6v—Pr—O767.60 (3)P1—O12—Pr144.39 (5)
O11iv—Pr—O880.66 (4)P1—O12—K92.29 (5)
O9—Pr—O871.69 (3)Pr—O12—K98.06 (3)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1/2, z+2; (iii) x, y, z+1; (iv) x1, y, z+1; (v) x+1, y1/2, z+1; (vi) x+1, y+1/2, z+1; (vii) x, y, z1; (viii) x, y+1/2, z+1; (ix) x1, y, z; (x) x, y1/2, z+1; (xi) x+1, y1/2, z+2; (xii) x+1, y, z1.

Experimental details

Crystal data
Chemical formulaKPr(PO3)4
Mr495.89
Crystal system, space groupMonoclinic, P21
Temperature (K)296
a, b, c (Å)7.2872 (2), 8.4570 (3), 8.0268 (2)
β (°) 91.994 (1)
V3)494.37 (3)
Z2
Radiation typeMo Kα
µ (mm1)6.06
Crystal size (mm)0.29 × 0.21 × 0.16
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.448, 0.751
No. of measured, independent and
observed [I > 2σ(I)] reflections
45940, 13443, 13257
Rint0.034
(sin θ/λ)max1)1.186
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.018, 0.043, 1.07
No. of reflections13443
No. of parameters164
No. of restraints1
Δρmax, Δρmin (e Å3)2.86, 2.42
Absolute structureFlack (1983), 6278 Friedel pairs
Absolute structure parameter0.022 (3)

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), CaRine (Boudias & Monceau, 1998) and ORTEP-3 for Windows (Farrugia, 1997), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
P1—O61.4841 (8)P3—O3ii1.4806 (8)
P1—O121.4850 (8)P3—O41.4832 (8)
P1—O51.5881 (7)P3—O51.5902 (8)
P1—O101.5887 (9)P3—O1iii1.5980 (8)
P2—O111.4810 (9)P4—O8iv1.4777 (8)
P2—O7i1.4822 (8)P4—O9v1.4829 (8)
P2—O11.5926 (8)P4—O21.5874 (8)
P2—O21.5941 (8)P4—O101.5973 (9)
Symmetry codes: (i) x+1, y+1/2, z+1; (ii) x, y+1/2, z+1; (iii) x1, y, z; (iv) x+1, y1/2, z+1; (v) x, y, z1.
 

References

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