Acta Crystallographica Section E
Structure Reports
Online
ISSN 1600-5368
Caesium gadolinium polyphosphate,
CsGd(PO
3)
4Houcine Naı¨li* and Tahar Mhiri
Laboratoire de l’E´tat Solide, De´partement de Chimie, Faculte´ des Sciences de Sfax, BP 802, 3018 Sfax, Tunisia
Correspondence e-mail: [email protected]
Key indicators
Single-crystal X-ray study T= 292 K
Mean(P–O) = 0.002 A˚ Rfactor = 0.018 wRfactor = 0.046
Data-to-parameter ratio = 42.6
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
#2005 International Union of Crystallography
Printed in Great Britain – all rights reserved
Crystals of CsGd(PO3)4 have been grown by the flux
technique from a mixture of CsH2PO4, Gd2O3 and H3PO4.
CsGd(PO3)4 crystallizes in structure type IV of the
MIMIII(PO3)4 (M I
= alkali metal, MIII = rare earth or Bi)
family of compounds. The structure consists of a
three-dimensional framework made up of spiral (PO3)n chains
linked by GdO8polyhedra. Two infinite (PO3)nchains with a
period of eight tetrahedra run along the [101] direction. Gd and Cs cations are surrounded by eight and eleven O atoms, respectively.
Comment
CsGd(PO3)4 belongs to the family of alkali rare earth
poly-phosphates with the general formulaMIREP4O12(whereM I
=
K, Rb, Na, NH4, Cs andRE = rare earth element). Several
members of this family were synthesized and have been characterized by many authors (Hong, 1975a,b; Koizumi, 1976; Palkinaet al., 1977; Mokhtaret al., 1987). Two different types of structural arrangements are known for these compounds that can generally be classified into seven structure types
denoted by roman numerals: cyclotetraphosphates
MIREP4O12with a ring structure formed by four PO4
tetra-hedra that are joined by bridging O atoms, and polypho-sphates MIRE(PO3)4consisting of helical ribbons formed by
corner-sharing PO4tetrahedra (Jouadiet al., 2003; Ettiset al.,
2003). Previous structure analyses have shown that rare earth polyphosphates with the general formula MIRE(PO3)4
crys-tallize in two crystal systems: orthorhombic with space group
[image:1.610.211.452.519.728.2]Received 3 August 2005 Accepted 11 August 2005 Online 17 August 2005
Figure 1
C2221 (type VII) (M I
= NH4, RE= Y) (Bagieu-Beucher &
Guitel, 1988) or space group Pbna (MI = Li, MIII = Ga)
(Palkinaet al., 1981a), and monoclinic with space groupsC2/c
(Koizumi, 1976; Hamady et al., 1995; Mokhtar et al., 1984)
(type I),P21/n(Palkinaet al., 1981b; Maksimovaet al., 1978)
(types II, IV and V),P21/c(Ben Hassenet al., 1982; Dogoet al.,
1980) or P21 (Yong-Hua et al., 1983; Palkina, Maksimova,
Kuznetsova & Chibiskova, 1978). All these materials have been intensively studied for their electric and optical proper-ties, and some of them have applications in catalysis. Specifi-cally, condensed phosphates of rare earth elements are applied
as laser materials (Danielmeyer & Weber, 1972; Mazurak et
al., 1978). CsGd(PO3)4 was obtained during a systematic
investigation of the pseudo-ternary Cs2O–Gd2O3–P2O5
system. The present paper reports the synthesis and char-acterization of CsGd(PO3)4by single-crystal X-ray diffraction.
The polyphosphate CsGd(PO3)4 is isotypic with
CsEr(PO3)4 (Palkina Maksimova & Kuzentsova, 1978), and
one polymorphic form of the potassium compounds
KBi(PO3)4(Jouadiet al., 2003) and KGd(PO3)4(Rekiket al.,
2004). The crystal structures of CsGd(PO3)4projected on to
theacandbcplanes are shown in Figs. 1 and 2, respectively. The atomic arrangement is characterized by a
three-dimen-sional framework built of helical ribbons (PO3)n that are
formed by corner-sharing of PO4 tetrahedra. Two (PO3)1
chains with a period of eight tetrahedra run along the [101] direction. The Gd atoms are in an eightfold coordination and build dodecahedra arranged two by two along the [101] and
[001] directions (Fig. 3). Although the GdO8dodecahedron is
considerably distorted, no O atom is shared with the adjacent
GdO8 polyhedra. The shortest Gd Gd distance is
5.729 (4) A˚ . The GdO8groups share corners with the
neigh-boring PO4tetrahedra. The scatter of the individual Gd—O
distances, ranging from 2.327 (2) to 2.456 (2) A˚ , displays the irregular shape of this polyhedron. Different to the Gd atom, the Cs atom is surrounded by eleven O atoms. The Cs—O distances vary from 3.077 (2) to 3.588 (3) A˚ . Fig. 4(a) and 4(b)
inorganic papers
Acta Cryst.(2005). E61, i204–i207 Naı¨li and Mhiri CsGd(PO
[image:2.610.55.276.71.287.2]3)4
i205
Figure 2
Projection of the CsGd(PO3)4crystal structure on to thebcplane.
Figure 3
The GdO8dodecahedra, viewed along thebaxis. Intermediate atoms are
[image:2.610.330.535.78.436.2]Cs.
Figure 4
The O-atom coordination around (a) the Gd atom and (b) the Cs atom, drawn with 50% displacement ellipsoids. [Symmetry codes: (i)x+ 1,y, z; (ii)x+3
2,y+ 1 2,z+
1 2; (iii)x+
1 2,y+
1 2,z+
1
2; (iv)x+ 1,y,z+ 1;
(v)x,y+ 1,z; (vi)x+1 2,y
1 2,z+
1
2; (vii)x+ 1 2,y+
1 2,z+
[image:2.610.53.288.318.511.2]depict the environments of the independent Gd and Cs atoms, respectively. The P—O distances are in the ranges 1.593 (2)– 1.617 (2) and 1.480 (3)–1.497 (2) A˚ for the bridging P—Oband
terminal P—Ot O atoms, respectively. The existence of
bridging and terminal O atoms in PO4tetrahedra explains the
three types of O—P—O angles observed. The Ob—P—Ob
angles vary from 97.8 (1) to 102.4 (1), with an average of
99.2, corresponding to the longest P—O bonds. The Ob—P—
Otangles (mean value = 109.3) have the values expected for a
regular tetrahedron, and the Ot—P—Ot angles range from
117.1 (1) to 121.2 (2), corresponding to the shortest P—O
distances. The bridging P—O—P angles vary from 124.6 (1) to
134.6 (2), which are in good agreement with those usually
observed in different types of polyphosphates (Koizumi, 1976; Hong, 1975b; Jouadiet al., 2003).
Although CsGd(PO3)4and KGd(PO3)4(Rekiket al., 2004)
present a similar coordination around the Gd atoms, the polyhedra around the alkali atoms are different. In fact, the coordination around Cs is made up from 11 O atoms, whereas the polyhedron around potassium is formed by only nine O atoms. Although KCe(PO3)4 (type II) (Rzaigui & Ariguib,
1983), CsGd(PO3)4 (type IV), and KYb(PO3)4 (type V)
(Palkina et al., 1979) crystallize in the same space group
(P21/n), the (PO3)1chains in these materials differ from one
another. In the first compound they are repeated after every four PO4tetrahedra along theaaxis. In the second and last,
eight PO4 tetrahedra are repeated along the [101] direction
and thebaxis, respectively.
Experimental
A mixture of CsH2PO4(5.4 g), Gd2O3 (0.4 g) and H3PO4(99%wt,
2.8 g) were mixed in a 10 ml platinum crucible which was placed in a tubular furnance and heated progressively to 473 K over a period of 4 h. The temperature was then kept at 823 K for 48 h before cooling to 323 K at a rate of 40 K d1. The furnance was then switched off.
Single crystals of CsGd(PO3)4 were isolated from the reaction
mixture by washing with hot water and with nitric acid (65%wt) to
eliminate the remaining Gd2O3. The compound obtained is stable
under normal conditions. Its formula was confirmed by chemical analysis [calculated: P 20.44, Cs 21.93, Gd 25.94%; found: P 19.35 (spectrophotometry), Cs 20.25 (AAS), Gd 25.00% (ICP method)].
Crystal data
CsGd(PO3)4
Mr= 606.04
Monoclinic,P21=n
a= 10.3229 (2) A˚
b= 8.9307 (2) A˚
c= 11.1826 (2) A˚
= 106.371 (1)
V= 989.13 (3) A˚3
Z= 4
Dx= 4.070 Mg m
3
MoKradiation
Cell parameters from 9641 reflections
= 2–40
= 11.04 mm1
T= 292 (2) K
Block, colourless
0.260.200.16 mm
Data collection
Nonius KappaCCD diffractometer
!scans
Absorption correction: analytical (de Meulenaer & Tompa, 1965)
Tmin= 0.177,Tmax= 0.271
19421 measured reflections 6980 independent reflections
5595 reflections withI> 2(I)
Rint= 0.071
max= 42.1
h=14!19
k=16!15
l=21!20
Refinement
Refinement onF2
R[F2> 2(F2)] = 0.018
wR(F2) = 0.046
S= 1.24
6980 reflections 164 parameters
w= 1/[2
(Fo2) + (0.0187P)2
+ 2.8091P]
whereP= (Fo2+ 2Fc2)/3
(/)max= 0.001
max= 0.89 e A˚
3
min=0.58 e A˚
[image:3.610.312.567.167.480.2]3
Table 1
Selected geometric parameters (A˚ ,).
Gd—O9i
2.327 (2)
Gd—O4 2.349 (2)
Gd—O10i 2.363 (2) Gd—O5ii 2.394 (3) Gd—O7iii 2.403 (2)
Gd—O6iv 2.406 (2)
Gd—O2i
2.426 (2)
Gd—O8v
2.456 (2)
Cs—O4iii 3.077 (2)
Cs—O2vi 3.086 (2) Cs—O5vii 3.087 (2) Cs—O6vi 3.115 (2) Cs—O10i 3.220 (2) Cs—O3i 3.237 (2) Cs—O11vii 3.305 (2)
Cs—O7iii 3.341 (3)
Cs—O8v 3.379 (3) Cs—O12i 3.509 (3) Cs—O7i 3.588 (3)
P1—O7 1.481 (2)
P1—O4 1.484 (2)
P1—O12 1.593 (2)
P1—O3 1.610 (2)
P2—O5 1.480 (3)
P2—O10 1.486 (2)
P2—O3 1.607 (2)
P2—O11 1.617 (2)
P3—O6 1.481 (2)
P3—O2 1.497 (2)
P3—O11 1.603 (2)
P3—O1 1.609 (2)
P4—O9 1.487 (2)
P4—O8 1.492 (2)
P4—O12viii 1.605 (3)
P4—O1 1.608 (2)
O7—P1—O4 118.41 (15)
O7—P1—O12 109.23 (13)
O4—P1—O12 110.44 (14)
O7—P1—O3 108.38 (14)
O4—P1—O3 109.87 (13)
O12—P1—O3 98.69 (14)
O5—P2—O10 121.21 (15)
O5—P2—O3 110.56 (15)
O10—P2—O3 107.91 (13)
O5—P2—O11 106.33 (12)
O10—P2—O11 110.51 (13)
O3—P2—O11 97.80 (13)
O6—P3—O2 117.10 (14)
O6—P3—O11 108.81 (14)
O2—P3—O11 108.89 (13)
O6—P3—O1 107.52 (12)
O2—P3—O1 111.11 (13)
O11—P3—O1 102.39 (12)
O9—P4—O8 117.73 (15)
O9—P4—O12viii
110.27 (15)
O8—P4—O12viii
110.76 (13)
O9—P4—O1 107.87 (12)
O8—P4—O1 110.37 (13)
O12viii
—P4—O1 98.02 (14)
P4—O1—P3 124.64 (13)
P2—O3—P1 129.22 (17)
P3—O11—P2 131.48 (15)
P1—O12—P4v
134.56 (18)
Symmetry codes: (i)x;yþ1;z; (ii) xþ1;y;z; (iii) xþ3 2;yþ
1 2;zþ
1 2; (iv)
xþ1 2;yþ
1 2;zþ
1
2; (v) xþ 1 2;y
1 2;zþ
1
2; (vi) xþ1;y;zþ1; (vii)
xþ1 2;yþ
1 2;zþ
1 2; (viii)x
1 2;y
1 2;z
1 2.
Data collection: COLLECT (Nonius, 1998); cell refinement:
SCALEPACK (Otwinowski & Minor, 1997); data reduction:
SCALEPACK and DENZO (Otwinowski & Minor, 1997);
program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure:SHELXL97(Sheldrick, 1997); molecular graphics:DIAMOND(Brandenburg, 1999); software used to prepare material for publication:SHELXL97.
References
Bagieu-Beucher, M. & Guitel, J. C. (1988).Z. Anorg. Allg. Chem.599, 123–
130.
Ben Hassen, D., Ariguib, N. K. & Trabelsi, K. (1982).C. R. Acad. Sci. Paris,
294, 375–381. (In French.)
Brandenburg, K. (1999).DIAMOND. Release 2.1e. Crystal Impact GbR,
Bonn, Germany.
Danielmeyer, H. G. & Weber, H. P. (1972).J. Quant. Electron.8, 805–808.
Dogo, A. M., Pusharovskii, D. Y., Pobedimskaya, E. A. & Belov, N. V. (1980).
Dokl. Akad. Nauk SSSR,251, 1392–1395. (In Russian.)
Ettis, H., Naı¨li, H. & Mhiri, T. (2003).Cryst. Growth Des.3, 599–602. Hamady, A., Jouini, T. & Driss, A. (1995).Acta Cryst.C51, 1970–1972. Hong, H. Y.-P. (1975a).Mater. Res. Bull.10, 635–640.
Jouadi, K., Naı¨li, H., Zouari, N., Mhiri, T. & Daoud, A. (2003). J. Alloys Compd,354, 104–114.
Koizumi, H. (1976).Acta Cryst.B32, 2254–2256.
Maksimova, S. I., Palkina, K. K., Loshchenova, V. B. & Kusnetsov, V. G. (1978).
Zh. Neorg. Khim.23, 2959–2965. (In Russian.)
Mazurak, Z., Ryba-Romanowski, W. & Jezowska-Trabiatowska, B. (1978).J.
Lumin.17, 401–409.
Meulenaer, J. de & Tompa, H. (1965).Acta Cryst.19, 1014–1018.
Mokhtar, F., Ariguib, N. K. & Trabelsi, M. (1987).J. Solid State Chem.69, 1–9.
Mokhtar, F., Doggy, M., Ariguib, N. K. & Trabelsi, M. (1984).J. Solid State
Chem.53, 149–154.
Nonius (1998).COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.
Palkina, K. K., Maksimova, S. I. & Chibiskova, N. T. (1981a).Dokl. Akad.
Nauk. SSSR,257, 357–361. (In Russian.)
Palkina, K. K., Maksimova, S. I. & Chibiskova, N. T. (1981b).Izv. Akad. Nauk. SSSR Neorg. Mater.17, 924–927. (In Russian.)
Palkina, K. K., Maksimova, S. I., Chudinova, N. N., Vinogradova, N. V. &
Chibiskova, N. T. (1979).Izv. Akad. Nauk. SSSR Neorg. Mater.17, 110–117.
(In Russian.)
Palkina, K. K., Maksimova, S. I. & Kuzentsova, V. G. (1978).Izv. Akad. Nauk.
SSSR Neorg. Mater.14, 284–187. (In Russian.)
Palkina, K. K., Maksimova, S. I., Kuznetsova, V. G. & Chibiskova, N. T. (1978).
Koord. Khim.4, 1092–1095. (In Russian.)
Palkina, K. K., Saiffuddinov, V. Z., Kuznetova, V. G. & Chudinova, N. N.
(1977).Dokl. Akad. Nauk SSSR,237, 837–839. (In Russian.)
Rekik, W., Naı¨li, H. & Mhiri, T. (2004).Acta Cryst.C60, i50–i52. Rzaigui, M. & Ariguib, N. K. (1983).J. Solid State Chem.49, 391–398.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
Go¨ttingen, Germany.
Yong-Hua, L., Ning-Hai, H., Qing-Lian, Z. & Shu-Zhen, L. (1983).Acta Phys.
Sin.32, 675–580.
inorganic papers
Acta Cryst.(2005). E61, i204–i207 Naı¨li and Mhiri CsGd(PO
sup-1
Acta Cryst. (2005). E61, i204–i207
supporting information
Acta Cryst. (2005). E61, i204–i207 [https://doi.org/10.1107/S1600536805025705]
Caesium gadolinium polyphosphate, CsGd(PO
3)
4Houcine Na
ï
li and Tahar Mhiri
Caesium gadolinium polyphosphate
Crystal data CsGd(PO3)4
Mr = 606.04
Monoclinic, P21/n
Hall symbol: -P 2yn a = 10.3229 (2) Å b = 8.9307 (2) Å c = 11.1826 (2) Å β = 106.371 (1)° V = 989.13 (3) Å3
Z = 4
F(000) = 1100 Dx = 4.070 Mg m−3
Mo Kα radiation, λ = 0.71073 Å Cell parameters from 9641 reflections θ = 2–40°
µ = 11.04 mm−1
T = 292 K Needle, colourless 0.26 × 0.20 × 0.16 mm
Data collection Nonius KappaCCD
diffractometer
Radiation source: fine-focus sealed tube Graphite monochromator
Detector resolution: 9 pixels mm-1
ω scans
Absorption correction: analytical (de Meulenaer & Tompa, 1965) Tmin = 0.177, Tmax = 0.271
19421 measured reflections 6980 independent reflections 5595 reflections with I > 2σ(I) Rint = 0.071
θmax = 42.1°, θmin = 3.0°
h = −14→19 k = −16→15 l = −21→20
Refinement Refinement on F2
Least-squares matrix: full R[F2 > 2σ(F2)] = 0.018
wR(F2) = 0.046
S = 1.24 6980 reflections 164 parameters 0 restraints
Primary atom site location: heavy-atom method Secondary atom site location: difference Fourier
map w = 1/[σ2(F
o2) + (0.0187P)2 + 2.8091P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.001
Δρmax = 0.89 e Å−3
Δρmin = −0.58 e Å−3
Special details
Experimental. Data were corrected for Lorentz-polarization effects and an analytical absorption correction (Meulenaer & Tompa, 1965) was applied. The structure was solved in the P 1 21/n 1 space group by the Patterson method (Cs and Gd)
and subsequent difference Fourier syntheses (all other atoms).
supporting information
sup-2
Acta Cryst. (2005). E61, i204–i207
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)
x y z Uiso*/Ueq
Gd 0.497879 (11) 0.273491 (14) 0.180789 (11) 0.00726 (4) Cs 0.67903 (2) 0.56590 (3) 0.459719 (19) 0.01910 (6) P1 0.64512 (6) −0.09227 (9) 0.25790 (7) 0.00809 (11) P2 0.45955 (7) −0.32517 (9) 0.13266 (7) 0.00799 (11) P3 0.24454 (6) −0.47205 (9) 0.21423 (6) 0.00771 (11) P4 0.17229 (6) −0.60738 (9) −0.02627 (7) 0.00818 (11) O1 0.13635 (19) −0.5429 (3) 0.09486 (19) 0.0106 (3) O2 0.3514 (2) −0.5836 (3) 0.2739 (2) 0.0111 (3) O3 0.5209 (2) −0.2067 (3) 0.2421 (2) 0.0116 (3) O4 0.6009 (2) 0.0399 (3) 0.1762 (2) 0.0123 (3) O5 0.4394 (2) −0.2544 (3) 0.0091 (2) 0.0133 (3) O6 0.1682 (2) −0.4037 (3) 0.2944 (2) 0.0121 (3) O7 0.7638 (2) −0.1780 (3) 0.2463 (2) 0.0139 (4) O8 0.0641 (2) −0.7111 (3) −0.0963 (2) 0.0126 (4) O9 0.3129 (2) −0.6654 (3) 0.0140 (2) 0.0135 (4) O10 0.5363 (2) −0.4673 (3) 0.1652 (2) 0.0130 (4) O11 0.31122 (19) −0.3412 (3) 0.1532 (2) 0.0106 (3) O12 0.6668 (2) −0.0479 (3) 0.4002 (2) 0.0139 (4)
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
sup-3
Acta Cryst. (2005). E61, i204–i207 Geometric parameters (Å, º)
Gd—O9i 2.327 (2) P2—Csvii 3.7855 (7)
Gd—O4 2.349 (2) P2—Csx 3.8451 (7)
Gd—O10i 2.363 (2) P3—O6 1.481 (2)
Gd—O5ii 2.394 (3) P3—O2 1.497 (2)
Gd—O7iii 2.403 (2) P3—O11 1.603 (2)
Gd—O6iv 2.406 (2) P3—O1 1.609 (2)
Gd—O2i 2.426 (2) P3—Csviii 3.6052 (7)
Gd—O8v 2.456 (2) P4—O9 1.487 (2)
Gd—Cs 4.0936 (3) P4—O8 1.492 (2) Gd—Csvi 4.4703 (3) P4—O12xi 1.605 (3)
Gd—Csvii 4.6417 (3) P4—O1 1.608 (2)
Cs—O4iii 3.077 (2) P4—Csxi 4.0992 (8)
Cs—O2viii 3.086 (2) O2—Gdx 2.426 (2)
Cs—O5ix 3.087 (2) O2—Csviii 3.086 (2)
Cs—O6viii 3.115 (2) O2—Csx 3.684 (2)
Cs—O10i 3.220 (2) O3—Csx 3.236 (2)
Cs—O3i 3.237 (2) O4—Csvi 3.077 (2)
Cs—O11ix 3.305 (2) O5—Gdii 2.394 (3)
Cs—O7iii 3.341 (3) O5—Csvii 3.087 (2)
Cs—O8v 3.379 (3) O6—Gdxii 2.406 (2)
Cs—O12i 3.509 (3) O6—Csviii 3.115 (2)
Cs—O7i 3.588 (3) O7—Gdvi 2.403 (2)
Cs—P3viii 3.6052 (7) O7—Csvi 3.341 (3)
P1—O7 1.481 (2) O7—Csx 3.588 (3)
P1—O4 1.484 (2) O8—Gdxi 2.456 (2)
P1—O12 1.593 (2) O8—Csxi 3.379 (3)
P1—O3 1.610 (2) O9—Gdx 2.327 (2)
P1—Csvi 3.7017 (8) O10—Gdx 2.363 (2)
P1—Csx 3.7537 (8) O10—Csx 3.220 (2)
P2—O5 1.480 (3) O11—Csvii 3.305 (2)
P2—O10 1.486 (2) O12—P4v 1.605 (3)
P2—O3 1.607 (2) O12—Csx 3.509 (3)
P2—O11 1.617 (2)
O9i—Gd—O4 117.72 (9) O3i—Cs—O7i 42.74 (5)
O9i—Gd—O10i 80.10 (9) O11ix—Cs—O7i 80.11 (6)
O4—Gd—O10i 141.43 (8) O7iii—Cs—O7i 80.407 (7)
O9i—Gd—O5ii 70.82 (8) O8v—Cs—O7i 127.81 (6)
O4—Gd—O5ii 71.35 (9) O12i—Cs—O7i 41.36 (6)
O10i—Gd—O5ii 84.91 (9) O4iii—Cs—P3viii 120.02 (4)
O9i—Gd—O7iii 139.47 (9) O2viii—Cs—P3viii 24.29 (4)
O4—Gd—O7iii 74.98 (9) O5ix—Cs—P3viii 90.83 (5)
O10i—Gd—O7iii 70.81 (8) O6viii—Cs—P3viii 24.07 (4)
O5ii—Gd—O7iii 78.88 (8) O10i—Cs—P3viii 156.86 (5)
O9i—Gd—O6iv 78.25 (9) O3i—Cs—P3viii 145.75 (5)
supporting information
sup-4
Acta Cryst. (2005). E61, i204–i207
O10i—Gd—O6iv 142.42 (8) O7iii—Cs—P3viii 120.98 (4)
O5ii—Gd—O6iv 115.80 (9) O8v—Cs—P3viii 86.26 (4)
O7iii—Gd—O6iv 140.72 (8) O12i—Cs—P3viii 113.98 (4)
O9i—Gd—O2i 75.57 (8) O7i—Cs—P3viii 142.77 (4)
O4—Gd—O2i 144.84 (8) O7—P1—O4 118.41 (15)
O10i—Gd—O2i 69.77 (8) O7—P1—O12 109.23 (13)
O5ii—Gd—O2i 140.80 (8) O4—P1—O12 110.44 (14)
O7iii—Gd—O2i 117.49 (8) O7—P1—O3 108.38 (14)
O6iv—Gd—O2i 75.27 (9) O4—P1—O3 109.87 (13)
O9i—Gd—O8v 142.91 (8) O12—P1—O3 98.69 (14)
O4—Gd—O8v 79.78 (8) O7—P1—Csvi 64.44 (11)
O10i—Gd—O8v 107.00 (8) O4—P1—Csvi 54.15 (10)
O5ii—Gd—O8v 144.76 (8) O12—P1—Csvi 127.20 (10)
O7iii—Gd—O8v 74.38 (8) O3—P1—Csvi 133.87 (9)
O6iv—Gd—O8v 74.77 (8) O7—P1—Csx 72.13 (11)
O2i—Gd—O8v 73.30 (8) O4—P1—Csx 167.86 (10)
O9i—Gd—Cs 123.81 (7) O12—P1—Csx 68.84 (10)
O4—Gd—Cs 118.09 (5) O3—P1—Csx 59.10 (9)
O10i—Gd—Cs 51.77 (6) Csvi—P1—Csx 136.53 (2)
O5ii—Gd—Cs 122.79 (6) O5—P2—O10 121.21 (15)
O7iii—Gd—Cs 54.71 (7) O5—P2—O3 110.56 (15)
O6iv—Gd—Cs 121.25 (6) O10—P2—O3 107.91 (13)
O2i—Gd—Cs 62.83 (5) O5—P2—O11 106.33 (12)
O8v—Gd—Cs 55.56 (6) O10—P2—O11 110.51 (13)
O9i—Gd—Csvi 109.91 (6) O3—P2—O11 97.80 (13)
O4—Gd—Csvi 40.24 (6) O5—P2—Csvii 51.39 (10)
O10i—Gd—Csvi 102.88 (6) O10—P2—Csvii 157.79 (9)
O5ii—Gd—Csvi 40.87 (5) O3—P2—Csvii 93.82 (9)
O7iii—Gd—Csvi 53.14 (7) O11—P2—Csvii 60.54 (8)
O6iv—Gd—Csvi 113.24 (6) O5—P2—Csx 152.39 (10)
O2i—Gd—Csvi 170.37 (5) O10—P2—Csx 54.57 (10)
O8v—Gd—Csvi 103.94 (6) O3—P2—Csx 56.10 (9)
Cs—Gd—Csvi 107.850 (4) O11—P2—Csx 99.80 (8)
O9i—Gd—Csvii 55.10 (7) Csvii—P2—Csx 143.27 (2)
O4—Gd—Csvii 70.48 (5) O6—P3—O2 117.10 (14)
O10i—Gd—Csvii 135.15 (5) O6—P3—O11 108.81 (14)
O5ii—Gd—Csvii 79.02 (6) O2—P3—O11 108.89 (13)
O7iii—Gd—Csvii 143.41 (7) O6—P3—O1 107.52 (12)
O6iv—Gd—Csvii 37.88 (6) O2—P3—O1 111.11 (13)
O2i—Gd—Csvii 97.94 (5) O11—P3—O1 102.39 (12)
O8v—Gd—Csvii 110.20 (6) O6—P3—Csviii 59.08 (9)
Cs—Gd—Csvii 157.736 (7) O2—P3—Csviii 58.04 (9)
Csvi—Gd—Csvii 91.678 (5) O11—P3—Csviii 127.03 (8)
O4iii—Cs—O2viii 140.42 (6) O1—P3—Csviii 130.57 (9)
O4iii—Cs—O5ix 53.32 (6) O9—P4—O8 117.73 (15)
O2viii—Cs—O5ix 96.88 (6) O9—P4—O12xi 110.27 (15)
O4iii—Cs—O6viii 98.08 (6) O8—P4—O12xi 110.76 (13)
sup-5
Acta Cryst. (2005). E61, i204–i207
O5ix—Cs—O6viii 84.10 (7) O8—P4—O1 110.37 (13)
O4iii—Cs—O10i 71.13 (6) O12xi—P4—O1 98.02 (14)
O2viii—Cs—O10i 148.23 (6) O9—P4—Csxi 68.78 (11)
O5ix—Cs—O10i 110.95 (6) O8—P4—Csxi 51.52 (10)
O6viii—Cs—O10i 146.29 (6) O12xi—P4—Csxi 147.33 (10)
O4iii—Cs—O3i 87.83 (6) O1—P4—Csxi 113.58 (10)
O2viii—Cs—O3i 121.78 (6) P4—O1—P3 124.64 (13)
O5ix—Cs—O3i 91.24 (6) P3—O2—Gdx 128.98 (13)
O6viii—Cs—O3i 168.04 (6) P3—O2—Csviii 97.67 (11)
O10i—Cs—O3i 45.60 (6) Gdx—O2—Csviii 133.35 (8)
O4iii—Cs—O11ix 98.82 (6) P3—O2—Csx 117.04 (12)
O2viii—Cs—O11ix 57.71 (6) Gdx—O2—Csx 81.30 (5)
O5ix—Cs—O11ix 45.50 (6) Csviii—O2—Csx 76.36 (5)
O6viii—Cs—O11ix 75.83 (6) P2—O3—P1 129.22 (17)
O10i—Cs—O11ix 136.34 (6) P2—O3—Csx 99.57 (11)
O3i—Cs—O11ix 93.04 (6) P1—O3—Csx 95.63 (9)
O4iii—Cs—O7iii 46.53 (6) P1—O4—Gd 139.09 (15)
O2viii—Cs—O7iii 141.67 (6) P1—O4—Csvi 102.84 (11)
O5ix—Cs—O7iii 99.49 (6) Gd—O4—Csvi 110.23 (8)
O6viii—Cs—O7iii 99.30 (6) P2—O5—Gdii 142.75 (16)
O10i—Cs—O7iii 49.74 (6) P2—O5—Csvii 106.61 (12)
O3i—Cs—O7iii 92.32 (6) Gdii—O5—Csvii 108.63 (8)
O11ix—Cs—O7iii 144.65 (5) P3—O6—Gdxii 149.17 (14)
O4iii—Cs—O8v 96.15 (6) P3—O6—Csviii 96.85 (10)
O2viii—Cs—O8v 95.79 (6) Gdxii—O6—Csviii 113.81 (8)
O5ix—Cs—O8v 141.91 (6) P1—O7—Gdvi 148.91 (15)
O6viii—Cs—O8v 77.96 (6) P1—O7—Csvi 91.98 (12)
O10i—Cs—O8v 71.86 (6) Gdvi—O7—Csvi 89.35 (8)
O3i—Cs—O8v 111.88 (5) P1—O7—Csx 84.74 (12)
O11ix—Cs—O8v 151.33 (6) Gdvi—O7—Csx 94.45 (7)
O7iii—Cs—O8v 51.83 (6) Csvi—O7—Csx 176.20 (7)
O4iii—Cs—O12i 88.42 (6) P4—O8—Gdxi 128.81 (15)
O2viii—Cs—O12i 97.18 (6) P4—O8—Csxi 108.26 (11)
O5ix—Cs—O12i 58.71 (6) Gdxi—O8—Csxi 87.61 (7)
O6viii—Cs—O12i 127.37 (6) P4—O9—Gdx 146.63 (15)
O10i—Cs—O12i 85.11 (6) P2—O10—Gdx 139.94 (13)
O3i—Cs—O12i 41.99 (5) P2—O10—Csx 103.33 (12)
O11ix—Cs—O12i 51.61 (5) Gdx—O10—Csx 93.03 (7)
O7iii—Cs—O12i 120.93 (6) P3—O11—P2 131.48 (15)
O8v—Cs—O12i 153.46 (5) P3—O11—Csvii 132.32 (10)
O4iii—Cs—O7i 50.73 (6) P2—O11—Csvii 94.24 (10)
O2viii—Cs—O7i 136.04 (6) P1—O12—P4v 134.56 (18)
O5ix—Cs—O7i 53.70 (6) P1—O12—Csx 86.12 (10)
O6viii—Cs—O7i 136.57 (5) P4v—O12—Csx 139.26 (12)
O10i—Cs—O7i 60.35 (6)
