Two new glaserite-type orthovanadates: Rb2KDy(VO4)2 and Cs1.52K1.48Gd(VO4)2

Rghioui, L.; El Ammari, L.; Assani, A.; Saadi, M.

doi:10.1107/S2056989019008685

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Volume 75| Part 7| July 2019| Pages 1041-1045

https://doi.org/10.1107/S2056989019008685

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Two new glaserite-type orthovanadates: Rb₂KDy(VO₄)₂ and Cs_1.52K_1.48Gd(VO₄)₂

Lotfi Rghioui,^a Lahcen El Ammari,^b ^* Abderrazzak Assani ^b and Mohamed Saadi ^b

^aLaboratoire de Spectroscopie, Modélisation Moléculaire, Matériaux, Nanomatériaux, Eau et Environnement (CERNE2D), Faculty of Sciences, Mohammed V University in Rabat, Avenue Ibn Batouta, BP 1014, Rabat, Morocco, and ^bLaboratoire de Chimie Appliquée des Matériaux, Centre des Sciences des Matériaux, Faculty of Sciences, Mohammed V University in Rabat, Avenue Ibn Batouta, BP 1014, Rabat, Morocco
^*Correspondence e-mail: l_elammari@yahoo.fr

Edited by A. Van der Lee, Université de Montpellier II, France (Received 12 June 2019; accepted 18 June 2019; online 21 June 2019)

The crystal structures of dirubidium potassium dysprosium bis(vanadate), Rb₂KDy(VO₄)₂, and caesium potassium gadolinium bis(vanadate), Cs_1.52K_1.48Gd(VO₄)₂, were solved from single-crystal X-ray diffraction data. Both compounds, synthesized by the reactive flux method, crystallize in the space group P $[\overline{3}]$ m1 with the glaserite structure type. VO₄ tetrahedra are linked to DyO₆ or GdO₆ octahedra by common vertices to form sheets stacking along the c axis. The large twelve-coordinate Cs⁺ or Rb⁺ cations are sandwiched between these layers in tunnels along the a and b axes, while the K⁺ cations, surrounded by ten oxygen atoms, are localized in cavities.

Keywords: crystal structure; crystal growth; X-ray diffraction; Rb₂KDy(VO₄)₂; Cs_1.52K_1.48Gd(VO₄)₂; orthovanadates; IR and Raman spectroscopy.

CCDC references: 1934723; 1934722

1. Chemical context

Many studies have been devoted to phosphates, vanadates and arsenates with the general formula (A,A′)₃Ln(XO₄)₂ (A,A′ = alkaline elements, Ln = rare-earth element and X = P, V, As) because of their outstanding optical properties. This type of compound has numerous possible applications, such as their use in the production of low- and high-pressure mercury lamps or colour television screens (Hong & Chinn, 1976 ). It has been shown that these optical properties are enhanced by the presence of either a rare-earth element or an XO₄ group and are determined by the fine details of the crystal structures of those materials (Benarafa et al., 2005 ; Rghioui et al., 1996 , 1999 , 2006 ). For instance, Parent et al. (1980 ) studied the luminescence phenomenon in Na₃La_1–xNd_x(PO₄)₂ and Na₃La_1–xNd_x(VO₄)₂ and measured the life time of the excited state 4F^3/2 as a function of the Nd³⁺ concentration. From a detailed examination of the emission and excitation spectra, Srivastava et al. (1990 ) highlighted an energy transfer from Ce³⁺ to the Tb³⁺ ion in the K₃La_0.80Ce_0.20(PO₄)₂, K₃La_0.80Tb_0.20(PO₄)₂ and K₃La_1–x–yTb_xCey(PO₄)₂ phosphates. In addition, the band gaps and the life times of Ce³⁺ and Tb³⁺ were determined by Finke et al. (1992 , 1994 ). The optical properties of the La atom in K₃La(PO₄)₂; K₂RbLa(PO₄)₂; Rb₂KLa(PO₄)₂ and Rb₃La(PO₄)₂ phosphates, investigated by FTIR and VUV spectroscopy, have allowed the determination of the values of band-gap energies for K₃La(PO₄)₂ prepared by two different methods (Sasum et al., 1997 ). In addition, Guzik et al. (2007 ) concluded that the emission phenomenon occurs from the charge transfer state in Na₃Lu_1–x–yYb_x(PO₄)₂ and Na₃Y_1–x–yYb_x(PO₄)₂ compounds. More recently, the optical properties of the Eu³⁺ ion were widely investigated in K₃Eu(XO₄)₂ where X = P, As and V, K₂YbHo_1–x–yEu_x(PO₄)₂, K₂CsLn(VO₄)₂ where Ln = La and Gd (Benarafa et al., 2009 ; Rghioui et al., 2015 ; Duke John David et al., 2016 ; Tao et al., 2014 ; Farmer et al., 2014 , 2016 ). In the case of K₃Eu(XO₄)₂, a vibronic coupling mechanism was proposed to explain the process of europium emission observed under 647.1 nm excitation.

From a crystallographic point of view, the related (A,A′)₃Ln(XO₄)₂ compounds with A,A′ = K, Rb and Cs adopt three structure types. The first is a monoclinic system, space group P2₁/m, represented by the phosphate K₃Nd(PO₄)₂. The second one is trigonal, space group P $[\overline{3}]$ , represented by K₃Lu(PO₄)₂, while the third one is also trigonal but in space group P $[\overline{3}]$ m1 and represented by the glaserite K₃Na(SO₄)₂. The present work is a continuation of our structural investigations by X-ray diffraction of the (A,A′)₃Ln(XO₄)₂ system where A,A′ = K, Rb and Cs, Ln = rare earth and X = P, V, As (Rghioui et al., 1999, 2002 , 2007 ). The present paper reports the synthesis and the crystal structure determination of the title compounds by X-ray diffraction at room temperature and vibrational spectroscopy.

2. Structural commentary

Dirubidium potassium dysprosium bis(vanadate), Rb₂KDy(VO₄)₂, and caesium potassium gadolinium bis(vanadate), Cs_1.52K_1.48Gd(VO₄)₂, both compounds crystallize in the space group P $[\overline{3}]$ m1 with the common glaserite, K₃Na(SO₄)₂, structure type (Moonre, 1973 ; Okada & Ossaka, 1980 ). The formulae determined by X-ray diffraction are consistent with the results of chemical analysis. In both structures, all atoms are in special positions of the P $[\overline{3}]$ m1 space group, namely Dy1 in Wyckoff position 1a ( $[\overline{3}]$ m), Rb1 in 1b ( $[\overline{3}]$ m), K1/Rb2, V1 and O2 in 2d (3m) and O1 in 6i (m). The structures of the two vanadates are built up from two independent VO₄ tetrahedra sharing an apex with DyO₆ or GdO₆ octahedra in such a way as to form a layer parallel to the ab plane, as shown in Fig. 1. Three of the six VO₄ tetrahedra surrounding each DyO₆ or GdO₆ octahedron are oriented upwards and the other three down. The concatenation of these polyhedra delimits large tunnels and cavities of site symmetry $[\overline{3}]$ m and 3m in which are located rubidium and a statistical mixture of rubidium and potassium atoms (Fig. 2).

Figure 1
Layer of VO₄ tetrahedra linked to DyO₆ octahedra by vertex sharing in the structure of Rb₂KDy(VO₄)₂.

Figure 2
Three-dimensional view along the a axis of the crystal structure showing Rb⁺ (or Cs⁺) in the channels.

The coordination polyhedron of the mixed site is formed by ten oxygen atoms belonging to three edges, one face and one vertex of five VO₄ tetrahedra as shown in Fig. 3. The K/Rb—O distances range from 2.681 (8) to 3.312 (7) Å. The twelve oxygen atoms surrounding the rubidium atom form an irregular cuboctahedron with Rb—O distances varying between 3.133 (2) and 3.4649 (3) Å. The main interatomic distances and angles are compatible with the values quoted in the literature (Gagné & Hawthorne, 2016 ; Gagné, 2018 ).

Figure 3
View along the c axis of a layer in the structure of the title compounds, showing the cavities in which the K/Rb⁺ (or K/Cs⁺) cations are located.

The three-dimensional structure consists of a basic tetrahedral–octahedral framework, forming layers that stack along the c-axis direction, as shown in Fig. 4. In glaserite-like structures, the large cations are located between the layers in channels running along the a- and b-axis directions and the average size cations are located in the cavities (see Fig. 5).

Figure 4
Three-dimensional view of the crystal structure showing Rb⁺ (or Cs⁺) cations between the layers stacked along the c axis.

Figure 5
Three-dimensional perspective view along c axis of the crystal structure of Rb₂KDy(VO₄)₂.

3. Vibrational spectroscopy

The Raman and infrared spectra for Rb₂KDy(VO₄)₂ are shown in Figs. 6 and 7, respectively. Their band assignments given in Table 1 are based on previous works for homologous vanadates (Rghioui et al., 1999, 2012 ; Benarafa et al., 2009). The stretching modes of (VO₄)³⁻ anions are usually found in the region 950–700 cm⁻¹. The peaks observed in the Raman spectrum at 935, 875 and 740 cm⁻¹ as well as the corresponding bands in the infrared spectrum at 925, 830 and 755 cm⁻¹ are all attributed to the symmetric (VO₄)³⁻ and the asymmetric (VO₄)³⁻ vibration. The bending vibrations of (VO₄)³⁻ are seen in the range 390–310 cm⁻¹. As in previous works (Rghioui et al., 2012), the separation between the symmetric and asymmetric bending can not be identified in the vibrational spectra. The bands lying between 230 and 95 cm⁻¹ in the spectra are assigned to the lattice vibrations. They are due to the VO₄ rotation and to the VO₄, K⁺, Rb⁺ and Dy³⁺ translation modes. A comparison of the Raman and infrared bands shows that they are not coincident. This fact confirms the centrosymmetric structure of Rb₂KDy(VO₄)₂ vanadate.

Table 1
Raman and Infrared band assignments (cm⁻¹) for Rb₂KDy(VO₄)₂

Raman	Infrared	Attribution
935	925	Stretching vibrations of VO₄ groups
875	830
740	755

385	377	Deformation modes of VO₄ groups
370	365
340	311

200	230	External modes
160	177
125	130
95	120

Figure 6
Raman spectrum of Rb₂KDy(VO₄)₂.

Figure 7
Infrared spectrum of Rb₂KDy(VO₄)₂.

4. Synthesis and crystallization

Single crystals of Rb₂KDy(VO₄)₂ and Cs_1.52K_1.48Gd(VO₄)₂ were synthesized by the flux method using a mixture of K₂CO₃, Rb₂CO₃ (or Cs₂CO₃ for the Gd compound), Dy₂O₃ (or Gd₂O₃) and V₂O₅ corresponding to 1 mol of K₂RbDy(VO₄)₂ (or Cs_1.52K_1.48Gd(VO₄)₂ and 1 mol of Rb₃VO₄ (or Cs₃VO₄). The reagents were ground in an agate mortar and placed in a platinum crucible. The temperature was raised slowly to 873 K and maintained for 24 h, permitting the carbonates to decompose. A second treatment at the melting temperature of 1273 K was performed, followed by slow cooling at a rate of 4 K h⁻¹ to 673 K and then quickly to ambient temperature. Each thermal treatment was interspersed with grinding. The obtained product was then washed with distilled water in order to eliminate the flux. The resulting product contained single crystals of a suitable size for the X-ray diffraction study.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. In the refinement procedure, the substitutional occupation of the mixed sites was freely refined and restricted to the occupancy of one site for Cs_1.52K_1.48Gd(VO₄)₂ but restricted to 0.5:0.5 for Rb₂KDy(VO₄)₂.

Table 2
Experimental details

	Rb₂KDy(VO₄)₂	Cs_1.52K_1.48Gd(VO₄)₂
Crystal data
M_r	602.42	646.74
Crystal system, space group	Trigonal, P $[\overline{3}]$ m1	Trigonal, P $[\overline{3}]$ m1
Temperature (K)	296	296
a, c (Å)	5.9728 (1), 7.7780 (1)	6.0321 (1), 7.9821 (2)
V (Å³)	240.30 (1)	251.53 (1)
Z	1	1
Radiation type	Mo Kα	Mo Kα
μ (mm⁻¹)	20.10	14.37
Crystal size (mm)	0.35 × 0.28 × 0.25	0.34 × 0.26 × 0.22

Data collection
Diffractometer	Bruker X8 APEX	Bruker X8 APEX
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )	Multi-scan (SADABS; Krause et al., 2015)
T_min, T_max	0.357, 0.749	0.639, 0.747
No. of measured, independent and observed [I > 2σ(I)] reflections	10549, 647, 631	14472, 678, 666
R_int	0.049	0.038
(sin θ/λ)_max (Å⁻¹)	0.926	0.925

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.016, 0.042, 1.11	0.010, 0.028, 1.09
No. of reflections	647	678
No. of parameters	24	25
Δρ_max, Δρ_min (e Å⁻³)	1.35, −1.35	0.63, −0.94
Computer programs: APEX2 and SAINT-Plus (Bruker, 2009 ), SHELXT2014 (Sheldrick, 2015a ), SHELXL2018 (Sheldrick, 2015b ), ORTEP-3 for Windows (Farrugia, 2012 ), DIAMOND (Brandenburg, 2006 ), Mercury (Macrae et al., 2008 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC references: 1934723; 1934722

Crystal structure: contains datablocks I, II, global. DOI: https://doi.org/10.1107/S2056989019008685/vn2149sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989019008685/vn2149Isup2.hkl

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S2056989019008685/vn2149IIsup3.hkl

checkCIF report

Computing details top

For both structures, data collection: APEX2 (Bruker, 2009); cell refinement: SAINT-Plus (Bruker, 2009); data reduction: SAINT-Plus (Bruker, 2009); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a). Program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015b) for (I); SHELXL2018 (Sheldrick, 2015b) for (II). Molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006) for (I); ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008) for (II). For both structures, software used to prepare material for publication: publCIF (Westrip, 2010).

Dirubidium potassium dysprosium bis(vanadate) (I) top

Crystal data top

Rb₂KDy(VO₄)₂	D_x = 4.163 Mg m⁻³
M_r = 602.42	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 647 reflections
a = 5.9728 (1) Å	θ = 2.6–41.1°
c = 7.7780 (1) Å	µ = 20.10 mm⁻¹
V = 240.30 (1) Å³	T = 296 K
Z = 1	Block, colourless
F(000) = 269	0.35 × 0.28 × 0.25 mm

Data collection top

Bruker X8 APEX diffractometer	647 independent reflections
Radiation source: fine-focus sealed tube	631 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.049
φ and ω scans	θ_max = 41.1°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −11→11
T_min = 0.357, T_max = 0.749	k = −11→10
10549 measured reflections	l = −14→14

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0239P)² + 0.1252P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.016	(Δ/σ)_max < 0.001
wR(F²) = 0.042	Δρ_max = 1.35 e Å⁻³
S = 1.11	Δρ_min = −1.35 e Å⁻³
647 reflections	Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
24 parameters	Extinction coefficient: 0.0124 (15)

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Rb1	0.000000	0.000000	0.500000	0.03556 (16)
Dy1	0.000000	0.000000	0.000000	0.00791 (6)
K1	0.333333	0.666667	0.8013 (9)	0.0098 (8)	0.5
Rb2	0.333333	0.666667	0.7969 (5)	0.0191 (6)	0.5
V1	0.333333	0.666667	0.24618 (6)	0.00765 (8)
O1	0.17571 (17)	0.82429 (17)	0.1720 (3)	0.0273 (4)
O2	0.333333	0.666667	0.4567 (4)	0.0389 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.0463 (3)	0.0463 (3)	0.0141 (2)	0.02314 (13)	0.000	0.000
Dy1	0.00565 (6)	0.00565 (6)	0.01243 (8)	0.00282 (3)	0.000	0.000
K1	0.0082 (10)	0.0082 (10)	0.0128 (18)	0.0041 (5)	0.000	0.000
Rb2	0.0194 (7)	0.0194 (7)	0.0185 (12)	0.0097 (4)	0.000	0.000
V1	0.00766 (10)	0.00766 (10)	0.00763 (16)	0.00383 (5)	0.000	0.000
O1	0.0219 (5)	0.0219 (5)	0.0424 (10)	0.0141 (6)	−0.0081 (3)	0.0081 (3)
O2	0.0542 (15)	0.0542 (15)	0.0084 (10)	0.0271 (8)	0.000	0.000

Geometric parameters (Å, º) top

Rb1—O1ⁱ	3.133 (2)	K1—O1^xvii	2.9951 (5)
Rb1—O1ⁱⁱ	3.133 (2)	K1—O1^xviii	2.9951 (6)
Rb1—O1ⁱⁱⁱ	3.133 (2)	K1—O1ⁱⁱⁱ	2.9951 (6)
Rb1—O1^iv	3.133 (2)	K1—O1^xix	2.9951 (5)
Rb1—O1^v	3.133 (2)	K1—O1ⁱ	2.9951 (5)
Rb1—O1^vi	3.133 (2)	K1—O1^xx	3.312 (7)
Rb1—O2^vii	3.4648 (3)	K1—O1^xxi	3.312 (7)
Rb1—O2^viii	3.4648 (3)	K1—O1^xxii	3.312 (7)
Rb1—O2^ix	3.4648 (3)	K1—V1^xx	3.460 (7)
Rb1—O2	3.4648 (3)	K1—V1^vii	3.4681 (8)
Rb1—O2ⁱⁱⁱ	3.4649 (3)	Rb2—O2	2.647 (5)
Rb1—O2^iv	3.4649 (3)	Rb2—O1^xvi	2.9976 (4)
Dy1—O1^x	2.2569 (17)	Rb2—O1^xvii	2.9976 (4)
Dy1—O1^vi	2.2569 (17)	Rb2—O1^xviii	2.9976 (4)
Dy1—O1^xi	2.2569 (17)	Rb2—O1ⁱⁱⁱ	2.9976 (4)
Dy1—O1^iv	2.2569 (17)	Rb2—O1^xix	2.9976 (4)
Dy1—O1^xii	2.2569 (17)	Rb2—O1ⁱ	2.9976 (4)
Dy1—O1ⁱⁱ	2.2569 (17)	Rb2—O1^xx	3.342 (4)
Dy1—K1^xiii	3.779 (3)	Rb2—O1^xxi	3.342 (4)
Dy1—K1^vii	3.779 (3)	Rb2—O1^xxii	3.342 (4)
Dy1—K1^xiv	3.779 (3)	Rb2—V1^vii	3.4646 (4)
Dy1—K1^ix	3.779 (3)	Rb2—V1ⁱⁱⁱ	3.4647 (4)
Dy1—K1^xv	3.779 (3)	V1—O2	1.637 (3)
Dy1—K1ⁱⁱⁱ	3.779 (3)	V1—O1	1.7297 (16)
K1—O2	2.681 (8)	V1—O1^vi	1.7297 (16)
K1—O1^xvi	2.9951 (5)	V1—O1^xxiii	1.7297 (16)

O1ⁱ—Rb1—O1ⁱⁱ	180.0	O1^xviii—K1—V1^xx	86.02 (15)
O1ⁱ—Rb1—O1ⁱⁱⁱ	60.33 (5)	O1ⁱⁱⁱ—K1—V1^xx	86.02 (15)
O1ⁱⁱ—Rb1—O1ⁱⁱⁱ	119.67 (5)	O1^xix—K1—V1^xx	86.02 (15)
O1ⁱ—Rb1—O1^iv	119.67 (5)	O1ⁱ—K1—V1^xx	86.02 (15)
O1ⁱⁱ—Rb1—O1^iv	60.33 (5)	O1^xx—K1—V1^xx	29.49 (7)
O1ⁱⁱⁱ—Rb1—O1^iv	180.0	O1^xxi—K1—V1^xx	29.49 (7)
O1ⁱ—Rb1—O1^v	60.33 (5)	O1^xxii—K1—V1^xx	29.49 (7)
O1ⁱⁱ—Rb1—O1^v	119.67 (5)	O2—K1—V1^vii	83.89 (12)
O1ⁱⁱⁱ—Rb1—O1^v	60.33 (5)	O1^xvi—K1—V1^vii	148.26 (4)
O1^iv—Rb1—O1^v	119.67 (5)	O1^xvii—K1—V1^vii	148.26 (4)
O1ⁱ—Rb1—O1^vi	119.67 (5)	O1^xviii—K1—V1^vii	92.20 (4)
O1ⁱⁱ—Rb1—O1^vi	60.33 (5)	O1ⁱⁱⁱ—K1—V1^vii	92.20 (4)
O1ⁱⁱⁱ—Rb1—O1^vi	119.67 (5)	O1^xix—K1—V1^vii	29.92 (3)
O1^iv—Rb1—O1^vi	60.33 (5)	O1ⁱ—K1—V1^vii	29.92 (3)
O1^v—Rb1—O1^vi	180.0	O1^xx—K1—V1^vii	125.60 (19)
O1ⁱ—Rb1—O2^vii	48.95 (6)	O1^xxi—K1—V1^vii	81.25 (8)
O1ⁱⁱ—Rb1—O2^vii	131.05 (6)	O1^xxii—K1—V1^vii	81.25 (8)
O1ⁱⁱⁱ—Rb1—O2^vii	102.09 (5)	V1^xx—K1—V1^vii	96.11 (12)
O1^iv—Rb1—O2^vii	77.91 (5)	O2—Rb2—O1^xvi	94.63 (9)
O1^v—Rb1—O2^vii	102.09 (5)	O2—Rb2—O1^xvii	94.63 (9)
O1^vi—Rb1—O2^vii	77.91 (5)	O1^xvi—Rb2—O1^xvii	63.36 (7)
O1ⁱ—Rb1—O2^viii	131.05 (6)	O2—Rb2—O1^xviii	94.63 (9)
O1ⁱⁱ—Rb1—O2^viii	48.95 (6)	O1^xvi—Rb2—O1^xviii	56.21 (7)
O1ⁱⁱⁱ—Rb1—O2^viii	77.91 (5)	O1^xvii—Rb2—O1^xviii	119.36 (3)
O1^iv—Rb1—O2^viii	102.09 (5)	O2—Rb2—O1ⁱⁱⁱ	94.63 (9)
O1^v—Rb1—O2^viii	77.91 (5)	O1^xvi—Rb2—O1ⁱⁱⁱ	119.36 (3)
O1^vi—Rb1—O2^viii	102.09 (5)	O1^xvii—Rb2—O1ⁱⁱⁱ	56.21 (7)
O2^vii—Rb1—O2^viii	180.00 (11)	O1^xviii—Rb2—O1ⁱⁱⁱ	170.08 (18)
O1ⁱ—Rb1—O2^ix	102.09 (5)	O2—Rb2—O1^xix	94.63 (9)
O1ⁱⁱ—Rb1—O2^ix	77.91 (5)	O1^xvi—Rb2—O1^xix	119.36 (3)
O1ⁱⁱⁱ—Rb1—O2^ix	102.09 (5)	O1^xvii—Rb2—O1^xix	170.08 (18)
O1^iv—Rb1—O2^ix	77.91 (5)	O1^xviii—Rb2—O1^xix	63.36 (7)
O1^v—Rb1—O2^ix	48.95 (6)	O1ⁱⁱⁱ—Rb2—O1^xix	119.36 (3)
O1^vi—Rb1—O2^ix	131.05 (6)	O2—Rb2—O1ⁱ	94.63 (9)
O2^vii—Rb1—O2^ix	119.065 (18)	O1^xvi—Rb2—O1ⁱ	170.08 (18)
O2^viii—Rb1—O2^ix	60.935 (18)	O1^xvii—Rb2—O1ⁱ	119.36 (3)
O1ⁱ—Rb1—O2	77.91 (5)	O1^xviii—Rb2—O1ⁱ	119.36 (3)
O1ⁱⁱ—Rb1—O2	102.09 (5)	O1ⁱⁱⁱ—Rb2—O1ⁱ	63.36 (7)
O1ⁱⁱⁱ—Rb1—O2	77.91 (5)	O1^xix—Rb2—O1ⁱ	56.21 (7)
O1^iv—Rb1—O2	102.09 (5)	O2—Rb2—O1^xx	150.80 (5)
O1^v—Rb1—O2	131.05 (6)	O1^xvi—Rb2—O1^xx	61.07 (8)
O1^vi—Rb1—O2	48.95 (6)	O1^xvii—Rb2—O1^xx	61.07 (8)
O2^vii—Rb1—O2	60.935 (18)	O1^xviii—Rb2—O1^xx	85.09 (8)
O2^viii—Rb1—O2	119.065 (18)	O1ⁱⁱⁱ—Rb2—O1^xx	85.09 (8)
O2^ix—Rb1—O2	180.0	O1^xix—Rb2—O1^xx	110.99 (11)
O1ⁱ—Rb1—O2ⁱⁱⁱ	102.09 (5)	O1ⁱ—Rb2—O1^xx	110.99 (11)
O1ⁱⁱ—Rb1—O2ⁱⁱⁱ	77.91 (5)	O2—Rb2—O1^xxi	150.80 (5)
O1ⁱⁱⁱ—Rb1—O2ⁱⁱⁱ	48.95 (6)	O1^xvi—Rb2—O1^xxi	85.09 (8)
O1^iv—Rb1—O2ⁱⁱⁱ	131.05 (6)	O1^xvii—Rb2—O1^xxi	110.99 (11)
O1^v—Rb1—O2ⁱⁱⁱ	102.09 (5)	O1^xviii—Rb2—O1^xxi	61.07 (8)
O1^vi—Rb1—O2ⁱⁱⁱ	77.91 (5)	O1ⁱⁱⁱ—Rb2—O1^xxi	110.99 (11)
O2^vii—Rb1—O2ⁱⁱⁱ	119.064 (18)	O1^xix—Rb2—O1^xxi	61.07 (8)
O2^viii—Rb1—O2ⁱⁱⁱ	60.936 (18)	O1ⁱ—Rb2—O1^xxi	85.09 (8)
O2^ix—Rb1—O2ⁱⁱⁱ	119.064 (18)	O1^xx—Rb2—O1^xxi	49.99 (8)
O2—Rb1—O2ⁱⁱⁱ	60.935 (18)	O2—Rb2—O1^xxii	150.80 (5)
O1ⁱ—Rb1—O2^iv	77.91 (5)	O1^xvi—Rb2—O1^xxii	110.99 (11)
O1ⁱⁱ—Rb1—O2^iv	102.09 (5)	O1^xvii—Rb2—O1^xxii	85.09 (8)
O1ⁱⁱⁱ—Rb1—O2^iv	131.05 (6)	O1^xviii—Rb2—O1^xxii	110.99 (11)
O1^iv—Rb1—O2^iv	48.95 (6)	O1ⁱⁱⁱ—Rb2—O1^xxii	61.07 (8)
O1^v—Rb1—O2^iv	77.91 (5)	O1^xix—Rb2—O1^xxii	85.09 (8)
O1^vi—Rb1—O2^iv	102.09 (5)	O1ⁱ—Rb2—O1^xxii	61.07 (8)
O2^vii—Rb1—O2^iv	60.936 (18)	O1^xx—Rb2—O1^xxii	49.99 (8)
O2^viii—Rb1—O2^iv	119.064 (18)	O1^xxi—Rb2—O1^xxii	49.99 (8)
O2^ix—Rb1—O2^iv	60.936 (18)	O2—Rb2—V1^vii	84.45 (7)
O2—Rb1—O2^iv	119.065 (18)	O1^xvi—Rb2—V1^vii	148.32 (3)
O2ⁱⁱⁱ—Rb1—O2^iv	180.0	O1^xvii—Rb2—V1^vii	148.32 (3)
O1^x—Dy1—O1^vi	180.00 (12)	O1^xviii—Rb2—V1^vii	92.23 (3)
O1^x—Dy1—O1^xi	88.46 (9)	O1ⁱⁱⁱ—Rb2—V1^vii	92.23 (3)
O1^vi—Dy1—O1^xi	91.54 (9)	O1^xix—Rb2—V1^vii	29.95 (3)
O1^x—Dy1—O1^iv	91.54 (9)	O1ⁱ—Rb2—V1^vii	29.95 (3)
O1^vi—Dy1—O1^iv	88.46 (9)	O1^xx—Rb2—V1^vii	124.76 (11)
O1^xi—Dy1—O1^iv	180.00 (9)	O1^xxi—Rb2—V1^vii	80.89 (5)
O1^x—Dy1—O1^xii	88.46 (9)	O1^xxii—Rb2—V1^vii	80.89 (5)
O1^vi—Dy1—O1^xii	91.54 (9)	O2—Rb2—V1ⁱⁱⁱ	84.45 (7)
O1^xi—Dy1—O1^xii	88.46 (9)	O1^xvi—Rb2—V1ⁱⁱⁱ	92.23 (3)
O1^iv—Dy1—O1^xii	91.54 (9)	O1^xvii—Rb2—V1ⁱⁱⁱ	29.95 (3)
O1^x—Dy1—O1ⁱⁱ	91.54 (9)	O1^xviii—Rb2—V1ⁱⁱⁱ	148.32 (3)
O1^vi—Dy1—O1ⁱⁱ	88.46 (9)	O1ⁱⁱⁱ—Rb2—V1ⁱⁱⁱ	29.95 (3)
O1^xi—Dy1—O1ⁱⁱ	91.54 (9)	O1^xix—Rb2—V1ⁱⁱⁱ	148.32 (3)
O1^iv—Dy1—O1ⁱⁱ	88.46 (9)	O1ⁱ—Rb2—V1ⁱⁱⁱ	92.23 (3)
O1^xii—Dy1—O1ⁱⁱ	180.00 (10)	O1^xx—Rb2—V1ⁱⁱⁱ	80.89 (5)
O1^x—Dy1—K1^xiii	52.42 (5)	O1^xxi—Rb2—V1ⁱⁱⁱ	124.76 (11)
O1^vi—Dy1—K1^xiii	127.58 (5)	O1^xxii—Rb2—V1ⁱⁱⁱ	80.89 (5)
O1^xi—Dy1—K1^xiii	52.42 (5)	V1^vii—Rb2—V1ⁱⁱⁱ	119.07 (2)
O1^iv—Dy1—K1^xiii	127.58 (5)	O2—V1—O1	109.49 (8)
O1^xii—Dy1—K1^xiii	119.51 (12)	O2—V1—O1^vi	109.49 (8)
O1ⁱⁱ—Dy1—K1^xiii	60.49 (12)	O1—V1—O1^vi	109.45 (8)
O1^x—Dy1—K1^vii	127.58 (5)	O2—V1—O1^xxiii	109.49 (8)
O1^vi—Dy1—K1^vii	52.42 (5)	O1—V1—O1^xxiii	109.45 (8)
O1^xi—Dy1—K1^vii	127.58 (5)	O1^vi—V1—O1^xxiii	109.45 (8)
O1^iv—Dy1—K1^vii	52.42 (5)	O2—V1—K1^xiv	180.0
O1^xii—Dy1—K1^vii	60.49 (12)	O1—V1—K1^xiv	70.51 (8)
O1ⁱⁱ—Dy1—K1^vii	119.51 (12)	O1^vi—V1—K1^xiv	70.51 (8)
K1^xiii—Dy1—K1^vii	180.0	O1^xxiii—V1—K1^xiv	70.51 (8)
O1^x—Dy1—K1^xiv	119.51 (12)	O2—V1—K1^vii	96.11 (12)
O1^vi—Dy1—K1^xiv	60.49 (12)	O1—V1—K1^vii	154.40 (15)
O1^xi—Dy1—K1^xiv	52.42 (5)	O1^vi—V1—K1^vii	59.72 (4)
O1^iv—Dy1—K1^xiv	127.58 (5)	O1^xxiii—V1—K1^vii	59.72 (4)
O1^xii—Dy1—K1^xiv	52.42 (5)	K1^xiv—V1—K1^vii	83.89 (12)
O1ⁱⁱ—Dy1—K1^xiv	127.58 (5)	O2—V1—K1ⁱⁱⁱ	96.11 (12)
K1^xiii—Dy1—K1^xiv	104.42 (12)	O1—V1—K1ⁱⁱⁱ	59.72 (4)
K1^vii—Dy1—K1^xiv	75.58 (12)	O1^vi—V1—K1ⁱⁱⁱ	59.72 (4)
O1^x—Dy1—K1^ix	60.49 (12)	O1^xxiii—V1—K1ⁱⁱⁱ	154.40 (15)
O1^vi—Dy1—K1^ix	119.51 (12)	K1^xiv—V1—K1ⁱⁱⁱ	83.89 (12)
O1^xi—Dy1—K1^ix	127.58 (5)	K1^vii—V1—K1ⁱⁱⁱ	118.88 (4)
O1^iv—Dy1—K1^ix	52.42 (5)	O2—V1—K1^xviii	96.11 (12)
O1^xii—Dy1—K1^ix	127.58 (5)	O1—V1—K1^xviii	59.72 (4)
O1ⁱⁱ—Dy1—K1^ix	52.42 (5)	O1^vi—V1—K1^xviii	154.40 (15)
K1^xiii—Dy1—K1^ix	75.58 (12)	O1^xxiii—V1—K1^xviii	59.72 (4)
K1^vii—Dy1—K1^ix	104.42 (12)	K1^xiv—V1—K1^xviii	83.89 (12)
K1^xiv—Dy1—K1^ix	180.0	K1^vii—V1—K1^xviii	118.88 (5)
O1^x—Dy1—K1^xv	52.42 (5)	K1ⁱⁱⁱ—V1—K1^xviii	118.88 (4)
O1^vi—Dy1—K1^xv	127.58 (5)	O2—V1—Rb1^xxiv	60.209 (6)
O1^xi—Dy1—K1^xv	119.51 (12)	O1—V1—Rb1^xxiv	49.28 (8)
O1^iv—Dy1—K1^xv	60.49 (12)	O1^vi—V1—Rb1^xxiv	125.09 (3)
O1^xii—Dy1—K1^xv	52.42 (5)	O1^xxiii—V1—Rb1^xxiv	125.09 (3)
O1ⁱⁱ—Dy1—K1^xv	127.58 (5)	K1^xiv—V1—Rb1^xxiv	119.792 (6)
K1^xiii—Dy1—K1^xv	104.42 (12)	K1^vii—V1—Rb1^xxiv	156.32 (12)
K1^vii—Dy1—K1^xv	75.58 (12)	K1ⁱⁱⁱ—V1—Rb1^xxiv	67.75 (7)
K1^xiv—Dy1—K1^xv	104.42 (12)	K1^xviii—V1—Rb1^xxiv	67.75 (7)
K1^ix—Dy1—K1^xv	75.58 (12)	O2—V1—Rb1^xxv	60.209 (6)
O1^x—Dy1—K1ⁱⁱⁱ	127.58 (5)	O1—V1—Rb1^xxv	125.09 (3)
O1^vi—Dy1—K1ⁱⁱⁱ	52.42 (5)	O1^vi—V1—Rb1^xxv	125.09 (3)
O1^xi—Dy1—K1ⁱⁱⁱ	60.49 (12)	O1^xxiii—V1—Rb1^xxv	49.28 (8)
O1^iv—Dy1—K1ⁱⁱⁱ	119.51 (12)	K1^xiv—V1—Rb1^xxv	119.791 (6)
O1^xii—Dy1—K1ⁱⁱⁱ	127.58 (5)	K1^vii—V1—Rb1^xxv	67.76 (7)
O1ⁱⁱ—Dy1—K1ⁱⁱⁱ	52.42 (5)	K1ⁱⁱⁱ—V1—Rb1^xxv	156.32 (12)
K1^xiii—Dy1—K1ⁱⁱⁱ	75.58 (12)	K1^xviii—V1—Rb1^xxv	67.76 (7)
K1^vii—Dy1—K1ⁱⁱⁱ	104.42 (12)	Rb1^xxiv—V1—Rb1^xxv	97.454 (8)
K1^xiv—Dy1—K1ⁱⁱⁱ	75.58 (12)	O2—V1—Rb1	60.209 (6)
K1^ix—Dy1—K1ⁱⁱⁱ	104.42 (12)	O1—V1—Rb1	125.09 (3)
K1^xv—Dy1—K1ⁱⁱⁱ	180.0	O1^vi—V1—Rb1	49.28 (8)
O2—K1—O1^xvi	93.98 (15)	O1^xxiii—V1—Rb1	125.09 (3)
O2—K1—O1^xvii	93.98 (15)	K1^xiv—V1—Rb1	119.791 (6)
O1^xvi—K1—O1^xvii	63.42 (7)	K1^vii—V1—Rb1	67.76 (7)
O2—K1—O1^xviii	93.98 (15)	K1ⁱⁱⁱ—V1—Rb1	67.76 (7)
O1^xvi—K1—O1^xviii	56.26 (7)	K1^xviii—V1—Rb1	156.32 (12)
O1^xvii—K1—O1^xviii	119.52 (4)	Rb1^xxiv—V1—Rb1	97.454 (8)
O2—K1—O1ⁱⁱⁱ	93.98 (15)	Rb1^xxv—V1—Rb1	97.454 (8)
O1^xvi—K1—O1ⁱⁱⁱ	119.52 (4)	O2—V1—Rb2	0.000 (1)
O1^xvii—K1—O1ⁱⁱⁱ	56.26 (7)	O1—V1—Rb2	109.49 (8)
O1^xviii—K1—O1ⁱⁱⁱ	171.3 (3)	O1^vi—V1—Rb2	109.49 (8)
O2—K1—O1^xix	93.98 (15)	O1^xxiii—V1—Rb2	109.49 (8)
O1^xvi—K1—O1^xix	119.52 (4)	K1^xiv—V1—Rb2	180.0
O1^xvii—K1—O1^xix	171.3 (3)	K1^vii—V1—Rb2	96.11 (12)
O1^xviii—K1—O1^xix	63.42 (7)	K1ⁱⁱⁱ—V1—Rb2	96.11 (12)
O1ⁱⁱⁱ—K1—O1^xix	119.52 (4)	K1^xviii—V1—Rb2	96.11 (12)
O2—K1—O1ⁱ	93.98 (15)	Rb1^xxiv—V1—Rb2	60.209 (6)
O1^xvi—K1—O1ⁱ	171.3 (3)	Rb1^xxv—V1—Rb2	60.209 (6)
O1^xvii—K1—O1ⁱ	119.52 (4)	Rb1—V1—Rb2	60.209 (6)
O1^xviii—K1—O1ⁱ	119.52 (4)	V1—O1—Dy1^xxiv	163.14 (14)
O1ⁱⁱⁱ—K1—O1ⁱ	63.42 (7)	V1—O1—K1^xviii	90.36 (6)
O1^xix—K1—O1ⁱ	56.26 (7)	Dy1^xxiv—O1—K1^xviii	90.91 (9)
O2—K1—O1^xx	150.51 (7)	V1—O1—K1ⁱⁱⁱ	90.36 (6)
O1^xvi—K1—O1^xx	61.46 (10)	Dy1^xxiv—O1—K1ⁱⁱⁱ	90.91 (9)
O1^xvii—K1—O1^xx	61.46 (10)	K1^xviii—O1—K1ⁱⁱⁱ	171.3 (3)
O1^xviii—K1—O1^xx	85.65 (13)	V1—O1—Rb1^xxiv	105.98 (10)
O1ⁱⁱⁱ—K1—O1^xx	85.65 (13)	Dy1^xxiv—O1—Rb1^xxiv	90.88 (6)
O1^xix—K1—O1^xx	111.86 (19)	K1^xviii—O1—Rb1^xxiv	85.72 (12)
O1ⁱ—K1—O1^xx	111.86 (19)	K1ⁱⁱⁱ—O1—Rb1^xxiv	85.72 (12)
O2—K1—O1^xxi	150.51 (7)	V1—O1—K1^xiv	80.00 (10)
O1^xvi—K1—O1^xxi	85.65 (13)	Dy1^xxiv—O1—K1^xiv	83.14 (9)
O1^xvii—K1—O1^xxi	111.86 (19)	K1^xviii—O1—K1^xiv	94.35 (13)
O1^xviii—K1—O1^xxi	61.46 (10)	K1ⁱⁱⁱ—O1—K1^xiv	94.35 (13)
O1ⁱⁱⁱ—K1—O1^xxi	111.86 (19)	Rb1^xxiv—O1—K1^xiv	174.02 (9)
O1^xix—K1—O1^xxi	61.46 (10)	V1—O2—Rb2	180.0
O1ⁱ—K1—O1^xxi	85.65 (13)	V1—O2—K1	180.0
O1^xx—K1—O1^xxi	50.47 (12)	Rb2—O2—K1	0.000 (1)
O2—K1—O1^xxii	150.51 (7)	V1—O2—Rb1^xxiv	95.58 (5)
O1^xvi—K1—O1^xxii	111.86 (19)	Rb2—O2—Rb1^xxiv	84.42 (5)
O1^xvii—K1—O1^xxii	85.65 (13)	K1—O2—Rb1^xxiv	84.42 (5)
O1^xviii—K1—O1^xxii	111.86 (19)	V1—O2—Rb1^xxv	95.58 (5)
O1ⁱⁱⁱ—K1—O1^xxii	61.46 (10)	Rb2—O2—Rb1^xxv	84.42 (5)
O1^xix—K1—O1^xxii	85.65 (13)	K1—O2—Rb1^xxv	84.42 (5)
O1ⁱ—K1—O1^xxii	61.46 (10)	Rb1^xxiv—O2—Rb1^xxv	119.065 (18)
O1^xx—K1—O1^xxii	50.47 (12)	V1—O2—Rb1	95.58 (5)
O1^xxi—K1—O1^xxii	50.47 (12)	Rb2—O2—Rb1	84.42 (5)
O2—K1—V1^xx	180.0	K1—O2—Rb1	84.42 (5)
O1^xvi—K1—V1^xx	86.02 (15)	Rb1^xxiv—O2—Rb1	119.065 (18)
O1^xvii—K1—V1^xx	86.02 (15)	Rb1^xxv—O2—Rb1	119.065 (18)

Symmetry codes: (i) x−y+1, x, −z+1; (ii) −x+y−1, −x, z; (iii) −x, −y+1, −z+1; (iv) x, y−1, z; (v) y−1, −x+y−1, −z+1; (vi) −y+1, x−y+1, z; (vii) −x+1, −y+1, −z+1; (viii) x−1, y−1, z; (ix) −x, −y, −z+1; (x) y−1, −x+y−1, −z; (xi) −x, −y+1, −z; (xii) x−y+1, x, −z; (xiii) x−1, y−1, z−1; (xiv) x, y, z−1; (xv) x, y−1, z−1; (xvi) x−y+1, x+1, −z+1; (xvii) y−1, −x+y, −z+1; (xviii) −x+1, −y+2, −z+1; (xix) y, −x+y, −z+1; (xx) x, y, z+1; (xxi) −x+y, −x+1, z+1; (xxii) −y+1, x−y+1, z+1; (xxiii) −x+y, −x+1, z; (xxiv) x, y+1, z; (xxv) x+1, y+1, z.

Caesium potassium gadolinium bis(vanadate) (II) top

Crystal data top

Cs_1.52K_1.48Gd(VO₄)₂	D_x = 4.270 Mg m⁻³
M_r = 646.74	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 678 reflections
a = 6.0321 (1) Å	θ = 3.9–41.1°
c = 7.9821 (2) Å	µ = 14.37 mm⁻¹
V = 251.53 (1) Å³	T = 296 K
Z = 1	Block, colourless
F(000) = 286	0.34 × 0.26 × 0.22 mm

Data collection top

Bruker X8 APEX diffractometer	678 independent reflections
Radiation source: fine-focus sealed tube	666 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
φ and ω scans	θ_max = 41.1°, θ_min = 3.9°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −11→11
T_min = 0.639, T_max = 0.747	k = −9→11
14472 measured reflections	l = −14→14

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.014P)² + 0.0871P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.010	(Δ/σ)_max < 0.001
wR(F²) = 0.028	Δρ_max = 0.63 e Å⁻³
S = 1.09	Δρ_min = −0.94 e Å⁻³
678 reflections	Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
25 parameters	Extinction coefficient: 0.0022 (6)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cs1	0.000000	0.000000	0.500000	0.02453 (5)
Gd1	0.000000	0.000000	0.000000	0.00899 (4)
K1	0.333333	0.666667	0.7877 (3)	0.0113 (5)	0.7404 (18)
Cs2	0.333333	0.666667	0.7867 (4)	0.0230 (8)	0.2597 (18)
V1	0.333333	0.666667	0.23977 (4)	0.00899 (5)
O1	0.17704 (10)	0.82296 (10)	0.16910 (16)	0.0265 (2)
O2	0.333333	0.666667	0.4470 (3)	0.0317 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cs1	0.02979 (7)	0.02979 (7)	0.01402 (8)	0.01489 (3)	0.000	0.000
Gd1	0.00627 (4)	0.00627 (4)	0.01444 (6)	0.00313 (2)	0.000	0.000
K1	0.0091 (6)	0.0091 (6)	0.0156 (9)	0.0046 (3)	0.000	0.000
Cs2	0.0200 (9)	0.0200 (9)	0.0288 (14)	0.0100 (5)	0.000	0.000
V1	0.00756 (7)	0.00756 (7)	0.01186 (11)	0.00378 (3)	0.000	0.000
O1	0.0244 (4)	0.0244 (4)	0.0379 (6)	0.0177 (4)	−0.00613 (19)	0.00613 (19)
O2	0.0404 (7)	0.0404 (7)	0.0144 (7)	0.0202 (4)	0.000	0.000

Geometric parameters (Å, º) top

Cs1—O1ⁱ	3.2245 (13)	K1—O1^xvii	3.0377 (4)
Cs1—O1ⁱⁱ	3.2245 (13)	K1—O1^xviii	3.0377 (4)
Cs1—O1ⁱⁱⁱ	3.2245 (13)	K1—O1ⁱⁱⁱ	3.0377 (4)
Cs1—O1^iv	3.2245 (13)	K1—O1^xix	3.0377 (4)
Cs1—O1^v	3.2245 (13)	K1—O1ⁱ	3.0377 (4)
Cs1—O1^vi	3.2245 (13)	K1—V1^vii	3.4895 (2)
Cs1—O2^vii	3.5082 (3)	K1—V1ⁱⁱⁱ	3.4895 (2)
Cs1—O2^viii	3.5082 (3)	K1—V1^xviii	3.4895 (2)
Cs1—O2^ix	3.5082 (3)	K1—V1^xx	3.609 (3)
Cs1—O2	3.5083 (3)	Cs2—O2	2.712 (4)
Cs1—O2ⁱⁱⁱ	3.5083 (3)	Cs2—O1^xvi	3.0386 (4)
Cs1—O2^iv	3.5083 (2)	Cs2—O1^xvii	3.0386 (4)
Gd1—O1^x	2.2898 (10)	Cs2—O1^xviii	3.0386 (4)
Gd1—O1^vi	2.2898 (10)	Cs2—O1ⁱⁱⁱ	3.0386 (4)
Gd1—O1^xi	2.2898 (10)	Cs2—O1^xix	3.0386 (4)
Gd1—O1^iv	2.2898 (10)	Cs2—O1ⁱ	3.0386 (4)
Gd1—O1^xii	2.2898 (10)	Cs2—O1^xx	3.462 (3)
Gd1—O1ⁱⁱ	2.2898 (10)	Cs2—O1^xxi	3.462 (3)
Gd1—K1^xiii	3.8732 (12)	Cs2—O1^xxii	3.462 (3)
Gd1—K1^vii	3.8732 (12)	Cs2—V1^vii	3.4890 (2)
Gd1—K1^xiv	3.8731 (12)	Cs2—V1ⁱⁱⁱ	3.4890 (2)
Gd1—K1^ix	3.8731 (12)	V1—O2	1.654 (2)
Gd1—K1^xv	3.8732 (12)	V1—O1	1.7276 (10)
Gd1—K1ⁱⁱⁱ	3.8732 (12)	V1—O1^vi	1.7276 (10)
K1—O2	2.719 (3)	V1—O1^xxiii	1.7276 (10)
K1—O1^xvi	3.0377 (4)

O1ⁱ—Cs1—O1ⁱⁱ	180.0	O1^xvi—K1—V1^xx	83.48 (6)
O1ⁱ—Cs1—O1ⁱⁱⁱ	59.57 (3)	O1^xvii—K1—V1^xx	83.48 (6)
O1ⁱⁱ—Cs1—O1ⁱⁱⁱ	120.43 (3)	O1^xviii—K1—V1^xx	83.48 (6)
O1ⁱ—Cs1—O1^iv	120.43 (3)	O1ⁱⁱⁱ—K1—V1^xx	83.48 (6)
O1ⁱⁱ—Cs1—O1^iv	59.57 (3)	O1^xix—K1—V1^xx	83.48 (6)
O1ⁱⁱⁱ—Cs1—O1^iv	180.0	O1ⁱ—K1—V1^xx	83.48 (6)
O1ⁱ—Cs1—O1^v	59.57 (3)	V1^vii—K1—V1^xx	93.60 (4)
O1ⁱⁱ—Cs1—O1^v	120.43 (3)	V1ⁱⁱⁱ—K1—V1^xx	93.60 (4)
O1ⁱⁱⁱ—Cs1—O1^v	59.57 (3)	V1^xviii—K1—V1^xx	93.60 (4)
O1^iv—Cs1—O1^v	120.43 (3)	O2—K1—Gd1^xxiv	115.95 (4)
O1ⁱ—Cs1—O1^vi	120.43 (3)	O1^xvi—K1—Gd1^xxiv	36.21 (2)
O1ⁱⁱ—Cs1—O1^vi	59.57 (3)	O1^xvii—K1—Gd1^xxiv	36.21 (2)
O1ⁱⁱⁱ—Cs1—O1^vi	120.43 (3)	O1^xviii—K1—Gd1^xxiv	85.31 (3)
O1^iv—Cs1—O1^vi	59.57 (3)	O1ⁱⁱⁱ—K1—Gd1^xxiv	85.31 (3)
O1^v—Cs1—O1^vi	180.0	O1^xix—K1—Gd1^xxiv	137.69 (7)
O1ⁱ—Cs1—O2^vii	48.07 (4)	O1ⁱ—K1—Gd1^xxiv	137.69 (7)
O1ⁱⁱ—Cs1—O2^vii	131.93 (4)	V1^vii—K1—Gd1^xxiv	157.65 (8)
O1ⁱⁱⁱ—Cs1—O2^vii	100.71 (3)	V1ⁱⁱⁱ—K1—Gd1^xxiv	65.087 (12)
O1^iv—Cs1—O2^vii	79.29 (3)	V1^xviii—K1—Gd1^xxiv	65.087 (12)
O1^v—Cs1—O2^vii	100.71 (3)	V1^xx—K1—Gd1^xxiv	64.05 (4)
O1^vi—Cs1—O2^vii	79.29 (3)	O2—Cs2—O1^xvi	96.67 (7)
O1ⁱ—Cs1—O2^viii	131.93 (4)	O2—Cs2—O1^xvii	96.67 (7)
O1ⁱⁱ—Cs1—O2^viii	48.07 (4)	O1^xvi—Cs2—O1^xvii	63.63 (4)
O1ⁱⁱⁱ—Cs1—O2^viii	79.29 (3)	O2—Cs2—O1^xviii	96.67 (7)
O1^iv—Cs1—O2^viii	100.71 (3)	O1^xvi—Cs2—O1^xviii	55.47 (4)
O1^v—Cs1—O2^viii	79.29 (3)	O1^xvii—Cs2—O1^xviii	118.67 (3)
O1^vi—Cs1—O2^viii	100.71 (3)	O2—Cs2—O1ⁱⁱⁱ	96.67 (7)
O2^vii—Cs1—O2^viii	180.0	O1^xvi—Cs2—O1ⁱⁱⁱ	118.67 (3)
O1ⁱ—Cs1—O2^ix	100.71 (3)	O1^xvii—Cs2—O1ⁱⁱⁱ	55.47 (4)
O1ⁱⁱ—Cs1—O2^ix	79.29 (3)	O1^xviii—Cs2—O1ⁱⁱⁱ	166.04 (13)
O1ⁱⁱⁱ—Cs1—O2^ix	100.71 (3)	O2—Cs2—O1^xix	96.67 (7)
O1^iv—Cs1—O2^ix	79.29 (3)	O1^xvi—Cs2—O1^xix	118.67 (3)
O1^v—Cs1—O2^ix	48.07 (4)	O1^xvii—Cs2—O1^xix	166.04 (13)
O1^vi—Cs1—O2^ix	131.93 (4)	O1^xviii—Cs2—O1^xix	63.63 (4)
O2^vii—Cs1—O2^ix	118.567 (13)	O1ⁱⁱⁱ—Cs2—O1^xix	118.67 (3)
O2^viii—Cs1—O2^ix	61.433 (14)	O2—Cs2—O1ⁱ	96.67 (7)
O1ⁱ—Cs1—O2	79.29 (3)	O1^xvi—Cs2—O1ⁱ	166.04 (13)
O1ⁱⁱ—Cs1—O2	100.71 (3)	O1^xvii—Cs2—O1ⁱ	118.67 (3)
O1ⁱⁱⁱ—Cs1—O2	79.29 (3)	O1^xviii—Cs2—O1ⁱ	118.67 (3)
O1^iv—Cs1—O2	100.71 (3)	O1ⁱⁱⁱ—Cs2—O1ⁱ	63.63 (4)
O1^v—Cs1—O2	131.93 (4)	O1^xix—Cs2—O1ⁱ	55.47 (4)
O1^vi—Cs1—O2	48.07 (4)	O2—Cs2—O1^xx	151.86 (3)
O2^vii—Cs1—O2	61.434 (13)	O1^xvi—Cs2—O1^xx	60.03 (5)
O2^viii—Cs1—O2	118.566 (13)	O1^xvii—Cs2—O1^xx	60.03 (5)
O2^ix—Cs1—O2	180.0	O1^xviii—Cs2—O1^xx	83.15 (6)
O1ⁱ—Cs1—O2ⁱⁱⁱ	100.71 (3)	O1ⁱⁱⁱ—Cs2—O1^xx	83.15 (6)
O1ⁱⁱ—Cs1—O2ⁱⁱⁱ	79.29 (3)	O1^xix—Cs2—O1^xx	108.15 (8)
O1ⁱⁱⁱ—Cs1—O2ⁱⁱⁱ	48.07 (4)	O1ⁱ—Cs2—O1^xx	108.15 (8)
O1^iv—Cs1—O2ⁱⁱⁱ	131.93 (4)	O2—Cs2—O1^xxi	151.86 (3)
O1^v—Cs1—O2ⁱⁱⁱ	100.71 (3)	O1^xvi—Cs2—O1^xxi	83.15 (6)
O1^vi—Cs1—O2ⁱⁱⁱ	79.29 (3)	O1^xvii—Cs2—O1^xxi	108.15 (8)
O2^vii—Cs1—O2ⁱⁱⁱ	118.565 (14)	O1^xviii—Cs2—O1^xxi	60.03 (5)
O2^viii—Cs1—O2ⁱⁱⁱ	61.435 (13)	O1ⁱⁱⁱ—Cs2—O1^xxi	108.15 (8)
O2^ix—Cs1—O2ⁱⁱⁱ	118.565 (14)	O1^xix—Cs2—O1^xxi	60.03 (5)
O2—Cs1—O2ⁱⁱⁱ	61.434 (13)	O1ⁱ—Cs2—O1^xxi	83.15 (6)
O1ⁱ—Cs1—O2^iv	79.29 (3)	O1^xx—Cs2—O1^xxi	48.22 (5)
O1ⁱⁱ—Cs1—O2^iv	100.71 (3)	O2—Cs2—O1^xxii	151.86 (3)
O1ⁱⁱⁱ—Cs1—O2^iv	131.93 (4)	O1^xvi—Cs2—O1^xxii	108.15 (8)
O1^iv—Cs1—O2^iv	48.07 (4)	O1^xvii—Cs2—O1^xxii	83.15 (6)
O1^v—Cs1—O2^iv	79.29 (3)	O1^xviii—Cs2—O1^xxii	108.15 (8)
O1^vi—Cs1—O2^iv	100.71 (3)	O1ⁱⁱⁱ—Cs2—O1^xxii	60.03 (5)
O2^vii—Cs1—O2^iv	61.435 (13)	O1^xix—Cs2—O1^xxii	83.15 (6)
O2^viii—Cs1—O2^iv	118.565 (14)	O1ⁱ—Cs2—O1^xxii	60.03 (5)
O2^ix—Cs1—O2^iv	61.435 (13)	O1^xx—Cs2—O1^xxii	48.22 (5)
O2—Cs1—O2^iv	118.566 (14)	O1^xxi—Cs2—O1^xxii	48.22 (5)
O2ⁱⁱⁱ—Cs1—O2^iv	180.0	O2—Cs2—V1^vii	86.53 (5)
O1^x—Gd1—O1^vi	180.00 (5)	O1^xvi—Cs2—V1^vii	147.92 (2)
O1^x—Gd1—O1^xi	88.78 (5)	O1^xvii—Cs2—V1^vii	147.92 (2)
O1^vi—Gd1—O1^xi	91.22 (5)	O1^xviii—Cs2—V1^vii	92.44 (2)
O1^x—Gd1—O1^iv	91.22 (5)	O1ⁱⁱⁱ—Cs2—V1^vii	92.44 (2)
O1^vi—Gd1—O1^iv	88.78 (5)	O1^xix—Cs2—V1^vii	29.680 (19)
O1^xi—Gd1—O1^iv	180.00 (6)	O1ⁱ—Cs2—V1^vii	29.680 (19)
O1^x—Gd1—O1^xii	88.78 (5)	O1^xx—Cs2—V1^vii	121.61 (8)
O1^vi—Gd1—O1^xii	91.22 (5)	O1^xxi—Cs2—V1^vii	79.51 (4)
O1^xi—Gd1—O1^xii	88.78 (5)	O1^xxii—Cs2—V1^vii	79.51 (4)
O1^iv—Gd1—O1^xii	91.22 (5)	O2—Cs2—V1ⁱⁱⁱ	86.53 (5)
O1^x—Gd1—O1ⁱⁱ	91.22 (5)	O1^xvi—Cs2—V1ⁱⁱⁱ	92.44 (2)
O1^vi—Gd1—O1ⁱⁱ	88.78 (5)	O1^xvii—Cs2—V1ⁱⁱⁱ	29.680 (19)
O1^xi—Gd1—O1ⁱⁱ	91.22 (5)	O1^xviii—Cs2—V1ⁱⁱⁱ	147.91 (2)
O1^iv—Gd1—O1ⁱⁱ	88.78 (5)	O1ⁱⁱⁱ—Cs2—V1ⁱⁱⁱ	29.681 (19)
O1^xii—Gd1—O1ⁱⁱ	180.00 (6)	O1^xix—Cs2—V1ⁱⁱⁱ	147.92 (2)
O1^x—Gd1—K1^xiii	51.601 (16)	O1ⁱ—Cs2—V1ⁱⁱⁱ	92.44 (2)
O1^vi—Gd1—K1^xiii	128.399 (17)	O1^xx—Cs2—V1ⁱⁱⁱ	79.51 (4)
O1^xi—Gd1—K1^xiii	51.602 (16)	O1^xxi—Cs2—V1ⁱⁱⁱ	121.61 (8)
O1^iv—Gd1—K1^xiii	128.398 (16)	O1^xxii—Cs2—V1ⁱⁱⁱ	79.51 (4)
O1^xii—Gd1—K1^xiii	117.93 (5)	V1^vii—Cs2—V1ⁱⁱⁱ	119.638 (11)
O1ⁱⁱ—Gd1—K1^xiii	62.07 (5)	O2—V1—O1	109.06 (5)
O1^x—Gd1—K1^vii	128.399 (17)	O2—V1—O1^vi	109.06 (5)
O1^vi—Gd1—K1^vii	51.601 (16)	O1—V1—O1^vi	109.88 (5)
O1^xi—Gd1—K1^vii	128.398 (16)	O2—V1—O1^xxiii	109.06 (5)
O1^iv—Gd1—K1^vii	51.602 (16)	O1—V1—O1^xxiii	109.88 (5)
O1^xii—Gd1—K1^vii	62.07 (5)	O1^vi—V1—O1^xxiii	109.88 (5)
O1ⁱⁱ—Gd1—K1^vii	117.93 (5)	O2—V1—K1^vii	93.60 (4)
K1^xiii—Gd1—K1^vii	180.0	O1—V1—K1^vii	157.34 (6)
O1^x—Gd1—K1^xiv	117.93 (5)	O1^vi—V1—K1^vii	60.518 (16)
O1^vi—Gd1—K1^xiv	62.07 (5)	O1^xxiii—V1—K1^vii	60.518 (16)
O1^xi—Gd1—K1^xiv	51.602 (16)	O2—V1—K1ⁱⁱⁱ	93.60 (4)
O1^iv—Gd1—K1^xiv	128.398 (16)	O1—V1—K1ⁱⁱⁱ	60.517 (16)
O1^xii—Gd1—K1^xiv	51.602 (16)	O1^vi—V1—K1ⁱⁱⁱ	60.518 (16)
O1ⁱⁱ—Gd1—K1^xiv	128.398 (16)	O1^xxiii—V1—K1ⁱⁱⁱ	157.34 (6)
K1^xiii—Gd1—K1^xiv	102.28 (4)	K1^vii—V1—K1ⁱⁱⁱ	119.610 (10)
K1^vii—Gd1—K1^xiv	77.72 (4)	O2—V1—K1^xviii	93.60 (4)
O1^x—Gd1—K1^ix	62.07 (5)	O1—V1—K1^xviii	60.517 (16)
O1^vi—Gd1—K1^ix	117.93 (5)	O1^vi—V1—K1^xviii	157.34 (6)
O1^xi—Gd1—K1^ix	128.398 (16)	O1^xxiii—V1—K1^xviii	60.518 (16)
O1^iv—Gd1—K1^ix	51.602 (16)	K1^vii—V1—K1^xviii	119.610 (10)
O1^xii—Gd1—K1^ix	128.398 (16)	K1ⁱⁱⁱ—V1—K1^xviii	119.609 (10)
O1ⁱⁱ—Gd1—K1^ix	51.602 (16)	O2—V1—K1^xiv	180.0
K1^xiii—Gd1—K1^ix	77.72 (4)	O1—V1—K1^xiv	70.94 (5)
K1^vii—Gd1—K1^ix	102.28 (4)	O1^vi—V1—K1^xiv	70.94 (5)
K1^xiv—Gd1—K1^ix	180.0	O1^xxiii—V1—K1^xiv	70.94 (5)
O1^x—Gd1—K1^xv	51.602 (16)	K1^vii—V1—K1^xiv	86.40 (4)
O1^vi—Gd1—K1^xv	128.398 (16)	K1ⁱⁱⁱ—V1—K1^xiv	86.40 (4)
O1^xi—Gd1—K1^xv	117.93 (5)	K1^xviii—V1—K1^xiv	86.40 (4)
O1^iv—Gd1—K1^xv	62.07 (5)	O2—V1—Cs1^xxv	59.187 (4)
O1^xii—Gd1—K1^xv	51.602 (16)	O1—V1—Cs1^xxv	49.87 (5)
O1ⁱⁱ—Gd1—K1^xv	128.398 (16)	O1^vi—V1—Cs1^xxv	124.970 (19)
K1^xiii—Gd1—K1^xv	102.28 (4)	O1^xxiii—V1—Cs1^xxv	124.970 (19)
K1^vii—Gd1—K1^xv	77.72 (4)	K1^vii—V1—Cs1^xxv	152.79 (5)
K1^xiv—Gd1—K1^xv	102.28 (4)	K1ⁱⁱⁱ—V1—Cs1^xxv	66.64 (3)
K1^ix—Gd1—K1^xv	77.72 (4)	K1^xviii—V1—Cs1^xxv	66.64 (3)
O1^x—Gd1—K1ⁱⁱⁱ	128.398 (16)	K1^xiv—V1—Cs1^xxv	120.814 (4)
O1^vi—Gd1—K1ⁱⁱⁱ	51.602 (16)	O2—V1—Cs1^xxvi	59.187 (4)
O1^xi—Gd1—K1ⁱⁱⁱ	62.07 (5)	O1—V1—Cs1^xxvi	124.969 (19)
O1^iv—Gd1—K1ⁱⁱⁱ	117.93 (5)	O1^vi—V1—Cs1^xxvi	124.970 (19)
O1^xii—Gd1—K1ⁱⁱⁱ	128.398 (16)	O1^xxiii—V1—Cs1^xxvi	49.87 (5)
O1ⁱⁱ—Gd1—K1ⁱⁱⁱ	51.602 (16)	K1^vii—V1—Cs1^xxvi	66.65 (3)
K1^xiii—Gd1—K1ⁱⁱⁱ	77.72 (4)	K1ⁱⁱⁱ—V1—Cs1^xxvi	152.78 (5)
K1^vii—Gd1—K1ⁱⁱⁱ	102.28 (4)	K1^xviii—V1—Cs1^xxvi	66.65 (3)
K1^xiv—Gd1—K1ⁱⁱⁱ	77.72 (4)	K1^xiv—V1—Cs1^xxvi	120.813 (4)
K1^ix—Gd1—K1ⁱⁱⁱ	102.28 (4)	Cs1^xxv—V1—Cs1^xxvi	96.109 (5)
K1^xv—Gd1—K1ⁱⁱⁱ	180.0	O2—V1—Cs1	59.187 (4)
O2—K1—O1^xvi	96.52 (6)	O1—V1—Cs1	124.969 (19)
O2—K1—O1^xvii	96.52 (6)	O1^vi—V1—Cs1	49.87 (5)
O1^xvi—K1—O1^xvii	63.65 (4)	O1^xxiii—V1—Cs1	124.970 (19)
O2—K1—O1^xviii	96.52 (6)	K1^vii—V1—Cs1	66.65 (3)
O1^xvi—K1—O1^xviii	55.49 (4)	K1ⁱⁱⁱ—V1—Cs1	66.65 (3)
O1^xvii—K1—O1^xviii	118.73 (2)	K1^xviii—V1—Cs1	152.78 (5)
O2—K1—O1ⁱⁱⁱ	96.52 (6)	K1^xiv—V1—Cs1	120.813 (4)
O1^xvi—K1—O1ⁱⁱⁱ	118.73 (2)	Cs1^xxv—V1—Cs1	96.109 (5)
O1^xvii—K1—O1ⁱⁱⁱ	55.49 (4)	Cs1^xxvi—V1—Cs1	96.109 (5)
O1^xviii—K1—O1ⁱⁱⁱ	166.32 (11)	O2—V1—Cs2	0.0
O2—K1—O1^xix	96.52 (6)	O1—V1—Cs2	109.06 (5)
O1^xvi—K1—O1^xix	118.73 (2)	O1^vi—V1—Cs2	109.06 (5)
O1^xvii—K1—O1^xix	166.32 (11)	O1^xxiii—V1—Cs2	109.06 (5)
O1^xviii—K1—O1^xix	63.65 (4)	K1^vii—V1—Cs2	93.60 (4)
O1ⁱⁱⁱ—K1—O1^xix	118.73 (2)	K1ⁱⁱⁱ—V1—Cs2	93.60 (4)
O2—K1—O1ⁱ	96.52 (6)	K1^xviii—V1—Cs2	93.60 (4)
O1^xvi—K1—O1ⁱ	166.32 (11)	K1^xiv—V1—Cs2	180.0
O1^xvii—K1—O1ⁱ	118.73 (2)	Cs1^xxv—V1—Cs2	59.187 (4)
O1^xviii—K1—O1ⁱ	118.73 (2)	Cs1^xxvi—V1—Cs2	59.187 (4)
O1ⁱⁱⁱ—K1—O1ⁱ	63.65 (4)	Cs1—V1—Cs2	59.187 (4)
O1^xix—K1—O1ⁱ	55.49 (4)	V1—O1—Gd1^xxv	162.94 (8)
O2—K1—V1^vii	86.40 (4)	V1—O1—K1^xviii	89.81 (3)
O1^xvi—K1—V1^vii	147.94 (2)	Gd1^xxv—O1—K1^xviii	92.19 (4)
O1^xvii—K1—V1^vii	147.94 (2)	V1—O1—K1ⁱⁱⁱ	89.81 (3)
O1^xviii—K1—V1^vii	92.45 (2)	Gd1^xxv—O1—K1ⁱⁱⁱ	92.19 (4)
O1ⁱⁱⁱ—K1—V1^vii	92.45 (2)	K1^xviii—O1—K1ⁱⁱⁱ	166.32 (11)
O1^xix—K1—V1^vii	29.676 (19)	V1—O1—Cs1^xxv	105.95 (5)
O1ⁱ—K1—V1^vii	29.676 (19)	Gd1^xxv—O1—Cs1^xxv	91.12 (4)
O2—K1—V1ⁱⁱⁱ	86.40 (4)	K1^xviii—O1—Cs1^xxv	83.48 (5)
O1^xvi—K1—V1ⁱⁱⁱ	92.45 (2)	K1ⁱⁱⁱ—O1—Cs1^xxv	83.48 (5)
O1^xvii—K1—V1ⁱⁱⁱ	29.675 (19)	V1—O2—Cs2	180.0
O1^xviii—K1—V1ⁱⁱⁱ	147.94 (2)	V1—O2—K1	180.0
O1ⁱⁱⁱ—K1—V1ⁱⁱⁱ	29.676 (19)	Cs2—O2—K1	0.0
O1^xix—K1—V1ⁱⁱⁱ	147.94 (2)	V1—O2—Cs1^xxv	96.93 (3)
O1ⁱ—K1—V1ⁱⁱⁱ	92.45 (2)	Cs2—O2—Cs1^xxv	83.07 (3)
V1^vii—K1—V1ⁱⁱⁱ	119.610 (10)	K1—O2—Cs1^xxv	83.07 (3)
O2—K1—V1^xviii	86.40 (4)	V1—O2—Cs1^xxvi	96.93 (3)
O1^xvi—K1—V1^xviii	29.675 (19)	Cs2—O2—Cs1^xxvi	83.07 (3)
O1^xvii—K1—V1^xviii	92.45 (2)	K1—O2—Cs1^xxvi	83.07 (3)
O1^xviii—K1—V1^xviii	29.676 (19)	Cs1^xxv—O2—Cs1^xxvi	118.566 (13)
O1ⁱⁱⁱ—K1—V1^xviii	147.94 (2)	V1—O2—Cs1	96.93 (3)
O1^xix—K1—V1^xviii	92.45 (2)	Cs2—O2—Cs1	83.07 (3)
O1ⁱ—K1—V1^xviii	147.94 (2)	K1—O2—Cs1	83.07 (3)
V1^vii—K1—V1^xviii	119.610 (10)	Cs1^xxv—O2—Cs1	118.566 (13)
V1ⁱⁱⁱ—K1—V1^xviii	119.609 (10)	Cs1^xxvi—O2—Cs1	118.566 (13)
O2—K1—V1^xx	180.0

Raman and Infrared band assignments (cm^-1) for Rb₂KDy(VO₄)₂ top

Raman	Infrared	Attribution
935	925	Stretching
875	830	vibrations of
740	755	VO₄ groups

385	377	Deformation
370	365	modes of
340	311	VO₄ groups

200	230	External
160	177	modes
125	130
95	120

Acknowledgements

The authors thank the Faculty of Science at the Mohammed V University in Rabat, Morocco, for the X-ray measurements.

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Volume 75| Part 7| July 2019| Pages 1041-1045

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