Potassium nickel(II) gallium phosphate hydrate, K[NiGa(2)(PO(4))(3)(H(2)O)(2)].

The title compound, potassium nickel(II) digallium tris-(phosphate) dihydrate, K[NiGa(2)(PO(4))(3)(H(2)O)(2)], was synthesized hydro-thermally. The structure is constructed from distorted trans-NiO(4)(H(2)O)(2) octa-hedra linked through vertices and edges to GaO(5) trigonal bipyramids and PO(4) tetra-hedra, forming a three-dimensional framework of formula [NiGa(2)(PO(4))(3)(H(2)O)(2)](-). The K, Ni and one P atom lie on special positions (Wyckoff position 4e, site symmetry 2). There are two sets of channels within the framework, one running parallel to the [10] direction and the other parallel to [001]. These inter-sect, forming a three-dimensional pore network in which the water mol-ecules coordinated to the Ni atoms and the K(+) ions required to charge balance the framework reside. The K(+) ions lie in a highly distorted environment surrounded by ten O atoms, six of which are closer than 3.1Å. The coordinated water mol-ecules are within hydrogen-bonding distance to O atoms of bridging Ga-O-P groups.

Related literature

For reviews of open-framework phosphate materials, see: Cheetham et al. (1999 ▶); Harrison (2002 ▶); Maspoch et al. (2007 ▶). For background to heterometal-substituted gallophosphates, MGaPOs, see: Baerlocher et al. (2001 ▶); Lin & Wang (2005 ▶). For related octa­hedral-trigonal bipyramidal silicate structures, see: Rocha & Lin (2005 ▶). For ammonium gallophosphates isostructural to the title compound, see: Chippindale et al. (1996 ▶, 1998 ▶); Bieniok et al. (2008 ▶). For the aluminium analogue, K[NiAl2(PO4)3(H2O)2], see: Meyer & Haushalter (1994 ▶). The same structure type occurs in Cs[Fe3(PO4)3(H2O)2] (Lii & Huang, 1995 ▶) and NH4[CoAl2(PO4)3(H2O)2] (Panz et al., 1998 ▶) and is related to that of (NH4)3Ga2(PO4)3 (Lesage et al., 2004 ▶). For bond-valence sums, see: Brese & O’Keeffe (1991 ▶); For the weighting scheme, see: Prince (1982 ▶); Watkin (1994 ▶).

Experimental

Crystal data

K[NiGa2(PO4)3(H2O)2]

M = 558.17

Monoclinic,

a = 13.2095 (13) Å

b = 10.1733 (9) Å

c = 8.8130 (9) Å

β = 107.680 (10)°

V = 1128.4 (2) Å3

Z = 4

Mo Kα radiation

μ = 7.27 mm−1

T = 150 K

0.09 × 0.08 × 0.06 mm

Data collection

Oxford Diffraction Xcalibur diffractometer

Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006 ▶) T min = 0.54, T max = 0.65

3597 measured reflections

1913 independent reflections

1734 reflections with I > 2σ(I)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.025

S = 1.04

1667 reflections

103 parameters

3 restraints

Only H-atom coordinates refined

Δρmax = 0.84 e Å−3

Δρmin = −0.91 e Å−3

Data collection: CrysAlis Pro (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED (Oxford Diffraction, 2006 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1994 ▶); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003 ▶); molecular graphics: CAMERON (Watkin et al., 1996 ▶); software used to prepare material for publication: CRYSTALS.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809015438/fi2077sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809015438/fi2077Isup2.hkl

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

K[NiGa2(PO4)3(H2O)2]	F(000) = 1080
Mr = 558.17	Dx = 3.286 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3597 reflections
a = 13.2095 (13) Å	θ = 3–32.4°
b = 10.1733 (9) Å	µ = 7.27 mm−1
c = 8.8130 (9) Å	T = 150 K
β = 107.68 (1)°	Block, yellow
V = 1128.4 (2) Å3	0.09 × 0.08 × 0.06 mm
Z = 4

Oxford Diffraction Xcalibur diffractometer	1734 reflections with I > 2σ(I)
graphite	Rint = 0.018
ω/2θ scans	θmax = 32.6°, θmin = 2.6°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	h = −15→19
Tmin = 0.54, Tmax = 0.65	k = −15→15
3597 measured reflections	l = −13→11
1913 independent reflections

Refinement on F	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022	Only H-atom coordinates refined
wR(F2) = 0.025	Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)] where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)2]2 Ai are: 18.9 -12.3 16.6
S = 1.04	(Δ/σ)max = 0.001
1667 reflections	Δρmax = 0.84 e Å−3
103 parameters	Δρmin = −0.91 e Å−3
3 restraints

	x	y	z	Uiso*/Ueq
Ga1	0.172478 (11)	0.075592 (15)	0.069169 (16)	0.0036
Ni1	0.0000	0.27385 (3)	0.2500	0.0053
K1	0.0000	0.63513 (6)	0.2500	0.0264
P1	0.0000	0.00118 (5)	0.2500	0.0036
P2	0.20870 (3)	0.37358 (4)	0.17941 (4)	0.0043
O1	0.05847 (8)	0.09109 (11)	−0.11504 (12)	0.0063
O2	0.09754 (9)	0.39793 (11)	0.18796 (14)	0.0082
O3	0.07314 (9)	0.09888 (11)	0.19895 (13)	0.0064
O4	0.09834 (9)	0.29514 (12)	0.48612 (14)	0.0111
O5	0.20652 (8)	−0.08860 (10)	0.16197 (12)	0.0061
O6	0.27707 (8)	0.04382 (11)	−0.04158 (13)	0.0070
O7	0.23679 (8)	0.22862 (11)	0.15963 (13)	0.0070
H1	0.135 (3)	0.236 (3)	0.547 (4)	0.0500*
H2	0.136 (3)	0.361 (3)	0.481 (5)	0.0500*

	U11	U22	U33	U12	U13	U23
Ga1	0.00279 (8)	0.00233 (9)	0.00525 (8)	−0.00019 (4)	0.00068 (5)	0.00009 (4)
Ni1	0.00413 (11)	0.00400 (12)	0.00818 (12)	0.0000	0.00228 (8)	0.0000
K1	0.0287 (3)	0.0109 (2)	0.0465 (4)	0.0000	0.0215 (3)	0.0000
P1	0.00246 (18)	0.0030 (2)	0.00514 (19)	0.0000	0.00089 (14)	0.0000
P2	0.00345 (15)	0.00312 (15)	0.00631 (14)	−0.00077 (10)	0.00159 (11)	−0.00031 (10)
O1	0.0048 (4)	0.0058 (4)	0.0066 (4)	0.0003 (3)	−0.0007 (3)	−0.0014 (3)
O2	0.0042 (4)	0.0074 (4)	0.0140 (4)	0.0001 (3)	0.0042 (3)	0.0016 (4)
O3	0.0058 (4)	0.0043 (4)	0.0108 (4)	−0.0002 (3)	0.0051 (3)	0.0010 (3)
O4	0.0106 (5)	0.0083 (4)	0.0115 (5)	−0.0003 (4)	−0.0009 (4)	0.0023 (4)
O5	0.0063 (4)	0.0039 (4)	0.0072 (4)	0.0008 (3)	0.0006 (3)	0.0018 (3)
O6	0.0071 (4)	0.0062 (4)	0.0090 (4)	0.0011 (3)	0.0042 (3)	0.0013 (3)
O7	0.0068 (4)	0.0038 (4)	0.0104 (4)	−0.0017 (3)	0.0029 (3)	−0.0030 (3)

Ga1—O1	1.8556 (11)	P1—O1ii	1.5279 (11)
Ga1—O3	1.9994 (11)	P1—O1iii	1.5279 (11)
Ga1—O5	1.8541 (10)	P1—O3	1.5452 (11)
Ga1—O6	1.9455 (11)	P1—O3i	1.5452 (11)
Ga1—O7	1.8357 (11)	P2—O2	1.5135 (11)
Ni1—O2	1.9951 (11)	P2—O5iv	1.5510 (11)
Ni1—O2i	1.9951 (11)	P2—O6v	1.5348 (12)
Ni1—O3	2.1374 (11)	P2—O7	1.5434 (12)
Ni1—O3i	2.1374 (11)	O4—H1	0.850 (10)
Ni1—O4	2.1030 (12)	O4—H2	0.848 (10)
Ni1—O4i	2.1030 (12)
O1—Ga1—O3	89.49 (5)	O4i—Ni1—O4	168.18 (7)
O1—Ga1—O5	119.09 (5)	O1ii—P1—O1iii	104.18 (9)
O1—Ga1—O6	94.97 (5)	O1ii—P1—O3	114.14 (6)
O1—Ga1—O7	116.97 (5)	O1iii—P1—O3	112.42 (6)
O3—Ga1—O5	88.16 (5)	O3i—P1—O1ii	112.42 (6)
O3—Ga1—O6	174.93 (4)	O3i—P1—O1iii	114.14 (6)
O3—Ga1—O7	87.06 (5)	O3i—P1—O3	99.94 (8)
O5—Ga1—O6	87.57 (5)	O2—P2—O7	115.61 (6)
O5—Ga1—O7	123.66 (5)	O5iv—P2—O2	111.12 (6)
O6—Ga1—O7	93.05 (5)	O5iv—P2—O6v	110.43 (6)
O2i—Ni1—O2	101.49 (7)	O5iv—P2—O7	101.91 (6)
O2—Ni1—O3	95.65 (4)	O6v—P2—O2	107.68 (6)
O2i—Ni1—O3	162.84 (5)	O6v—P2—O7	110.02 (6)
O2—Ni1—O4	87.12 (5)	Ga1—O1—P1iii	135.47 (7)
O2i—Ni1—O4	85.41 (5)	Ga1—O3—Ni1	129.51 (5)
O3i—Ni1—O2	162.84 (5)	Ga1—O3—P1	131.86 (7)
O3i—Ni1—O2i	95.65 (4)	Ni1—O2—P2	128.84 (7)
O3i—Ni1—O3	67.23 (6)	Ni1—O3—P1	96.42 (5)
O3i—Ni1—O4	93.46 (4)	Ni1—O4—H1	128 (3)
O3i—Ni1—O4i	96.38 (5)	Ni1—O4—H2	103 (3)
O4i—Ni1—O2	85.41 (5)	H1—O4—H2	111 (3)
O4i—Ni1—O2i	87.12 (5)	Ga1—O5—P2vi	129.28 (7)
O3—Ni1—O4	96.38 (5)	Ga1—O6—P2v	125.62 (7)
O4i—Ni1—O3	93.46 (4)	Ga1—O7—P2	139.82 (7)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H1···O5ii	0.85 (1)	1.90 (1)	2.741 (2)	172
O4—H2···O6iv	0.85 (1)	2.16 (2)	2.976 (2)	161

Table 1

Selected geometric parameters (Å, °)

Ga1—O1	1.8556 (11)
Ga1—O3	1.9994 (11)
Ga1—O5	1.8541 (10)
Ga1—O6	1.9455 (11)
Ga1—O7	1.8357 (11)
Ni1—O2	1.9951 (11)
Ni1—O2i	1.9951 (11)
Ni1—O3	2.1374 (11)
Ni1—O3i	2.1374 (11)
Ni1—O4	2.1030 (12)
Ni1—O4i	2.1030 (12)
P1—O1ii	1.5279 (11)
P1—O1iii	1.5279 (11)
P1—O3	1.5452 (11)
P1—O3i	1.5452 (11)
P2—O2	1.5135 (11)
P2—O5iv	1.5510 (11)
P2—O6v	1.5348 (12)
P2—O7	1.5434 (12)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H1⋯O5ii	0.85 (1)	1.896 (11)	2.741 (2)	172
O4—H2⋯O6iv	0.85 (1)	2.163 (17)	2.976 (2)	161

Symmetry codes: (ii) ; (iv) .