K(2)Ho(PO(4))(WO(4)).

A new compound, dipotassium holmium(III) phosphate(V) tungstate(VI), K(2)Ho(PO(4))(WO(4)), has been obtained during investigation of the K(2)O-P(2)O(5)-WO(3)-HoF(3) phase system using the flux technique. The compound is isotypic with K(2)Bi(PO(4))(WO(4)). Its framework structure consists of flat (∞) (2)[HoPO(4)] layers parallel to (100) that are made up of (∞) (1)[HoO(8)] zigzag chains inter-linked via slightly distorted PO(4) tetra-hedra. WO(4) tetra-hedra are attached above and below these layers, leaving space for the K(+) counter-cations. The HoO(8), PO(4) and WO(4) units exhibit 2 symmetry.

Related literature

For related structures, see: Ben Amara & Dabbabi (1987 ▶); Marsh (1987 ▶); Zatovsky, Terebilenko, Slobodyanik & Baumer (2006 ▶); Zatovsky, Terebilenko, Slobodyanik, Baumer & Shishkin (2006 ▶).

Experimental

Crystal data

K2Ho(PO4)(WO4)

M = 585.95

Orthorhombic,

a = 6.8820 (10) Å

b = 12.1485 (18) Å

c = 19.695 (3) Å

V = 1646.6 (4) Å3

Z = 8

Mo Kα radiation

μ = 24.72 mm−1

T = 293 (2) K

0.10 × 0.09 × 0.07 mm

Data collection

Oxford Diffraction Xcalibur-3 CCD diffractometer

Absorption correction: multi-scan based on the method by Blessing (1995 ▶) T min = 0.102, T max = 0.177

8608 measured reflections

1561 independent reflections

1257 reflections with I > 2σ(I)

R int = 0.055

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.071

S = 1.15

1561 reflections

62 parameters

Δρmax = 1.90 e Å−3

Δρmin = −1.73 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2005 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2005 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680803287X/wm2196sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680803287X/wm2196Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

K2Ho(PO4)(WO4)	F(000) = 2064
Mr = 585.95	Dx = 4.727 Mg m−3
Orthorhombic, Ibca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2c	Cell parameters from 8608 reflections
a = 6.882 (1) Å	θ = 3.4–33.0°
b = 12.1485 (18) Å	µ = 24.72 mm−1
c = 19.695 (3) Å	T = 293 K
V = 1646.6 (4) Å3	Prism, pale beige
Z = 8	0.10 × 0.09 × 0.07 mm

Oxford Diffraction XCalibur-3 CCD diffractometer	1561 independent reflections
Radiation source: fine-focus sealed tube	1257 reflections with I > 2σ(I)
graphite	Rint = 0.055
φ and ω scans	θmax = 33.0°, θmin = 3.4°
Absorption correction: multi-scan based on the method by Blessing (1995)	h = −10→10
Tmin = 0.102, Tmax = 0.177	k = −18→18
8608 measured reflections	l = −30→29

Refinement on F2	0 restraints
Least-squares matrix: full	w = 1/[σ2(Fo2) + (0.0397P)2 + 3.2575P] where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.029	(Δ/σ)max < 0.001
wR(F2) = 0.071	Δρmax = 1.90 e Å−3
S = 1.15	Δρmin = −1.73 e Å−3
1561 reflections	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
62 parameters	Extinction coefficient: 0.00010 (2)

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.

	x	y	z	Uiso*/Ueq
W1	0.5	0.25	0.334530 (12)	0.01088 (5)
Ho1	0.75	0.325113 (17)	0.5	0.00662 (5)
K1	0.96872 (15)	0.07992 (10)	0.34389 (5)	0.0196 (2)
P1	0.75	0.07042 (10)	0.5	0.0065 (2)
O1	0.7088 (4)	0.2796 (3)	0.38536 (17)	0.0146 (7)
O2	0.4420 (6)	0.3643 (4)	0.2845 (2)	0.0269 (8)
O3	0.7308 (4)	−0.0047 (2)	0.43834 (16)	0.0102 (6)
O4	0.9229 (4)	0.1514 (2)	0.49215 (17)	0.0105 (6)

	U11	U22	U33	U12	U13	U23
W1	0.01432 (9)	0.01167 (9)	0.00666 (9)	−0.00095 (8)	0	0
Ho1	0.00652 (9)	0.00523 (9)	0.00811 (10)	0	−0.00005 (9)	0
K1	0.0204 (4)	0.0248 (5)	0.0137 (4)	−0.0002 (4)	0.0021 (3)	0.0039 (4)
P1	0.0064 (5)	0.0034 (5)	0.0098 (6)	0	0.0000 (5)	0
O1	0.0154 (14)	0.0171 (14)	0.0113 (14)	−0.0035 (11)	−0.0012 (11)	−0.0031 (11)
O2	0.0308 (17)	0.0296 (19)	0.0203 (17)	−0.0008 (17)	0.0013 (15)	0.0126 (16)
O3	0.0126 (13)	0.0079 (11)	0.0101 (13)	−0.0018 (10)	−0.0002 (11)	−0.0010 (9)
O4	0.0052 (10)	0.0066 (11)	0.0198 (16)	−0.0017 (9)	0.0011 (10)	−0.0016 (11)

W1—O2i	1.749 (4)	Ho1—K1vii	3.8119 (11)
W1—O2	1.749 (4)	Ho1—K1vi	3.8119 (12)
W1—O1	1.788 (3)	K1—O3	2.683 (3)
W1—O1i	1.788 (3)	K1—O2v	2.689 (4)
W1—K1	3.8352 (12)	K1—O3x	2.747 (3)
W1—K1i	3.8352 (12)	K1—O1vi	2.916 (3)
W1—K1ii	4.0181 (13)	K1—O2xi	2.934 (5)
W1—K1iii	4.0181 (13)	K1—O4	3.063 (3)
W1—K1iv	4.0821 (12)	K1—O1	3.122 (4)
W1—K1v	4.0821 (12)	K1—O2i	3.133 (4)
Ho1—O4vi	2.274 (3)	K1—P1	3.4251 (11)
Ho1—O4vii	2.274 (3)	K1—Ho1vi	3.8119 (11)
Ho1—O1	2.342 (3)	K1—K1iii	3.9511 (13)
Ho1—O1viii	2.342 (3)	P1—O3	1.525 (3)
Ho1—O3ix	2.401 (3)	P1—O3viii	1.525 (3)
Ho1—O3ii	2.401 (3)	P1—O4	1.552 (3)
Ho1—O4viii	2.428 (3)	P1—O4viii	1.552 (3)
Ho1—O4	2.428 (3)	P1—Ho1xii	2.9802 (13)
Ho1—P1ix	2.9802 (13)	P1—K1viii	3.4251 (11)
Ho1—P1	3.0941 (13)
O2i—W1—O2	111.4 (3)	O3x—K1—O4	61.07 (8)
O2i—W1—O1	106.94 (17)	O1vi—K1—O4	69.23 (9)
O2—W1—O1	109.83 (19)	O2xi—K1—O4	130.90 (10)
O2i—W1—O1i	109.83 (19)	O3—K1—O1	76.52 (9)
O2—W1—O1i	106.94 (17)	O2v—K1—O1	100.44 (12)
O1—W1—O1i	111.9 (2)	O3x—K1—O1	117.21 (9)
O4vi—Ho1—O4vii	165.59 (15)	O1vi—K1—O1	84.72 (10)
O4vi—Ho1—O1	94.81 (11)	O2xi—K1—O1	156.62 (10)
O4vii—Ho1—O1	88.59 (11)	O4—K1—O1	58.09 (8)
O4vi—Ho1—O1viii	88.59 (11)	O3—K1—O2i	77.94 (10)
O4vii—Ho1—O1viii	94.81 (11)	O2v—K1—O2i	78.50 (9)
O1—Ho1—O1viii	152.68 (18)	O3x—K1—O2i	156.48 (11)
O4vi—Ho1—O3ix	88.91 (10)	O1vi—K1—O2i	131.64 (12)
O4vii—Ho1—O3ix	78.65 (10)	O2xi—K1—O2i	103.49 (13)
O1—Ho1—O3ix	133.18 (11)	O4—K1—O2i	101.64 (9)
O1viii—Ho1—O3ix	73.88 (12)	O1—K1—O2i	54.04 (10)
O4vi—Ho1—O3ii	78.65 (10)	O3—P1—O3viii	106.4 (2)
O4vii—Ho1—O3ii	88.91 (10)	O3—P1—O4	111.52 (16)
O1—Ho1—O3ii	73.88 (12)	O3viii—P1—O4	113.10 (16)
O1viii—Ho1—O3ii	133.18 (12)	O3—P1—O4viii	113.10 (16)
O3ix—Ho1—O3ii	61.17 (15)	O3viii—P1—O4viii	111.52 (16)
O4vi—Ho1—O4viii	126.77 (7)	O4—P1—O4viii	101.3 (2)
O4vii—Ho1—O4viii	67.63 (12)	W1—O1—Ho1	133.20 (16)
O1—Ho1—O4viii	78.27 (12)	W1—O1—K1vi	124.93 (16)
O1viii—Ho1—O4viii	78.03 (12)	Ho1—O1—K1vi	92.27 (11)
O3ix—Ho1—O4viii	133.56 (10)	W1—O1—K1	99.08 (14)
O3ii—Ho1—O4viii	143.86 (10)	Ho1—O1—K1	111.49 (12)
O4vi—Ho1—O4	67.63 (12)	K1vi—O1—K1	86.88 (9)
O4vii—Ho1—O4	126.77 (8)	W1—O2—K1v	132.6 (2)
O1—Ho1—O4	78.03 (12)	W1—O2—K1ii	115.89 (19)
O1viii—Ho1—O4	78.27 (12)	K1v—O2—K1ii	95.86 (13)
O3ix—Ho1—O4	143.86 (10)	W1—O2—K1i	99.64 (16)
O3ii—Ho1—O4	133.56 (10)	K1v—O2—K1i	120.18 (15)
O4viii—Ho1—O4	59.26 (13)	K1ii—O2—K1i	81.21 (11)
O3—K1—O2v	152.62 (12)	P1—O3—Ho1xii	96.20 (15)
O3—K1—O3x	78.69 (8)	P1—O3—K1	105.64 (14)
O2v—K1—O3x	124.78 (11)	Ho1xii—O3—K1	130.32 (12)
O3—K1—O1vi	119.65 (10)	P1—O3—K1iii	142.66 (16)
O2v—K1—O1vi	86.67 (12)	Ho1xii—O3—K1iii	95.30 (9)
O3x—K1—O1vi	60.35 (9)	K1—O3—K1iii	93.37 (11)
O3—K1—O2xi	93.55 (11)	P1—O4—Ho1vi	146.28 (18)
O2v—K1—O2xi	78.59 (14)	P1—O4—Ho1	99.72 (13)
O3x—K1—O2xi	80.53 (10)	Ho1vi—O4—Ho1	111.83 (11)
O1vi—K1—O2xi	118.34 (11)	P1—O4—K1	89.66 (13)
O3—K1—O4	52.05 (8)	Ho1vi—O4—K1	89.92 (10)
O2v—K1—O4	148.06 (12)	Ho1—O4—K1	110.96 (11)

Table 1

Selected bond lengths (Å)

W1—O2	1.749 (4)
W1—O1	1.788 (3)
Ho1—O4i	2.274 (3)
Ho1—O1	2.342 (3)
Ho1—O3ii	2.401 (3)
Ho1—O4	2.428 (3)
P1—O3	1.525 (3)
P1—O4	1.552 (3)

Symmetry codes: (i) ; (ii) .