Potassium nickel(II) gallium phosphate hydrate, K[NiGa2(PO4)3(H2O)2]

Chippindale, A.M.; Sharma, A.V.; Hibble, S.J.

doi:10.1107/S1600536809015438

inorganic compounds

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Volume 65| Part 5| May 2009| Pages i38-i39

doi:10.1107/S1600536809015438

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Potassium nickel(II) gallium phosphate hydrate, K[NiGa₂(PO₄)₃(H₂O)₂]

Ann M. Chippindale,^a ^* Arun V. Sharma ^a and Simon J. Hibble ^a

^aDepartment of Chemistry, University of Reading, Whiteknights, Reading, Berks RG6 6AD, England
^*Correspondence e-mail: a.m.chippindale@rdg.ac.uk

(Received 30 March 2009; accepted 24 April 2009; online 30 April 2009)

The title compound, potassium nickel(II) digallium tris(phosphate) dihydrate, K[NiGa₂(PO₄)₃(H₂O)₂], was synthesized hydrothermally. The structure is constructed from distorted trans-NiO₄(H₂O)₂ octahedra linked through vertices and edges to GaO₅ trigonal bipyramids and PO₄ tetrahedra, forming a three-dimensional framework of formula [NiGa₂(PO₄)₃(H₂O)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 $[\overline{1}]$ ] direction and the other parallel to [001]. These intersect, forming a three-dimensional pore network in which the water molecules 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 molecules 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_r = 558.17
Monoclinic, C 2/c
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 $[Oxford Diffraction, (2006). CrysAlis RED and CrysAlis Pro. Oxford Diffraction Ltd, Abingdon, England. ]$ ) 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[F² > 2σ(F²)] = 0.022
wR(F²) = 0.025
S = 1.04
1667 reflections
103 parameters
3 restraints
Only H-atom coordinates refined
Δρ_max = 0.84 e Å⁻³
Δρ_min = −0.91 e Å⁻³

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—O5^iv	1.5510 (11)
P2—O6^v	1.5348 (12)
P2—O7	1.5434 (12)
Symmetry codes: (i) $[-x, y, -z+{\script{1\over 2}}]$ ; (ii) $[x, -y, z+{\script{1\over 2}}]$ ; (iii) -x, -y, -z; (iv) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]$ .

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⋯O6^iv	0.85 (1)	2.163 (17)	2.976 (2)	161
Symmetry codes: (ii) $[x, -y, z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis Pro (Oxford Diffraction, 2006 $[Oxford Diffraction, (2006). CrysAlis RED and CrysAlis Pro. Oxford Diffraction Ltd, Abingdon, England. ]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 $[Oxford Diffraction, (2006). CrysAlis RED and CrysAlis Pro. Oxford Diffraction Ltd, Abingdon, England. ]$ ); data reduction: CrysAlis RED (Oxford Diffraction, 2006 $[Oxford Diffraction, (2006). CrysAlis RED and CrysAlis Pro. Oxford Diffraction Ltd, Abingdon, England. ]$ ); 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.

Supporting information

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

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

checkCIF report

Comment top

Although the majority of heterometal substituted gallophosphates, MeGaPOs, contain MO₄ (M = Me or Ga) and PO₄ units (Baerlocher et al., 2001), some are known in which the metal atoms have non-tetrahedral geometries. For example, NGP-1 (Lin & Wang, 2005), the only organically templated NiGaPO reported to date, contains Ni and Ga disordered over the same octahedral metal sites, together with GaO₅ and PO₄ units. K[NiGa₂(PO₄)₃(H₂O)₂] is assembled from the same polyhedra as NGP-1 and is isostructural with a number of ammonium transition-metal gallophosphates, NH₄[MeGa₂(PO₄)₃(H₂O)₂] (Me = Mn (Chippindale et al., 1998), Fe, Ni (Bieniok et al., 2008), Co (Chippindale et al., 1996)) and has an aluminium analogue, K[NiAl₂(PO₄)₃(H₂O)₂] (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).

The two phosphorus atoms have tetrahedral geometry (P1, point symmetry C_2v; P2,1). Unlike in NGP-1, the metal atoms are located in two distinct sites; Ga1 in a GaO₅ trigonal bipyramid (1) and Ni1 in an NiO₄(H₂O)₂ distorted octahedron (C_2v), in which the terminal water molecules, H₂O4, lie trans to each other (Fig. 1). Two of the other oxygen atoms in the NiO₆ unit, O2 and O2ⁱ, are two coordinate whilst O3 and O3ⁱ are three coordinate. As expected, the M—O3 (M = Ni, Ga) and P1—O3 bond lengths are the longest M—O and P–O bond lengths observed in the structure. Bond-valence sums (Brese & OKeeffe, 1991) for P1, P2, Ga1 and Ni1 are 4.80, 4.81, 3.22 and 1.93. respectively, which together with the yellow colour of the crystals, confirm the presence of Ni²⁺ in the structure.

The GaO₅, NiO₆ and PO₄units link together through edge- and vertex-sharing arrangements to give a three-dimensional framework of composition [NiGa₂(PO₄)₃(H₂O)₂]^-. A set of approximately circular channels, running parallel to the [101] direction, contain the water molecules and potassium ions (Fig. 2). A second set of channels, elliptical in shape, run parallel to the c axis (Fig. 3) and intersect with the first set to generate a three-dimensional pore network.

The potassium atom lies in a very distorted coordination environment with six near oxygen atoms (K1···O in range 2.865 (1) to 3.072 (1) Å) with two additional O atoms at 3.397 (1) and two at 3.456 (1) Å). H₂O4 is also involved in hydrogen bonding to Ga—O—P bridging oxygen atoms.

Related literature top

For reviews of open-framework phosphate materials, see: Cheetham et al. (1999); Harrison (2002); Maspoch et al. (2007). For background to heterometal-substituted gallophosphates, MeGaPOs, 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 & OKeeffe (1991); For the weighting scheme, see: Prince (1982); Watkin (1994).

Experimental top

The title compound was prepared hydrothermally from a gel of composition Ga₂O₃: NiCl₂.6H₂O:10H₃PO₄:156H₂O:0.1Si(OEt)₄:5KH₂PO₄which was heated at 433 K for 7 d in a Teflon-lined stainless steel autoclave. The solid product was collected by filtration, washed with deionized water and dried in air. The product consisted of large yellow faceted blocks of the title compound, which could be easily separated from unidentified white powder.

Computing details top

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 (Betteridge et al., 2003).

Figures top

	Fig. 1. Local coordination of the title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. [Symmetry codes: (i) -x, y, -z + 1/2; (ii) x, -y, z + 1/2; (iii) -x, -y, -z; (iv) -x + 1/2, y + 1/2, -z + 1/2; (v) -x + 1/2, -y + 1/2, -z; (viii) x - 1/2, 1/2 - y, 1/2 + z; (ix) -x + 1/2, y + 1/2, z].
	Fig. 2. View of the main channels running parallel to the [1 0 1] direction shown as (a) ball and stick and (b) polyhedral representation. The cross pore distance O1···O5^x is 7.251 (1) Å. The colour of each polyhedron corresponds to the colour of the central atom as defined in Fig. 1. [Symmetry codes: (x) 1/2 - x, 1/2 - y, -z]
	Fig. 3. View along the c axis as (a) ball and stick and (b) polyhedral representation showing the elliptical channels bounded by eight membered rings. The shortest cross channel distances are 4.092 (2) and 4.360 (1) Å for O2···O2^xi and O2···O6^ix respectively. These channels intersect with the main channels shown in Fig.2 to form a 3-D pore network. [Symmetry codes: (ix) -x + 1/2, y + 1/2, z; (xi) -x, 1 - y, z].

potassium nickel(II) digallium tris(phosphate) dihydrate top

Crystal data top

K[NiGa₂(PO₄)₃(H₂O)₂]	F(000) = 1080
M_r = 558.17	D_x = 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

Data collection top

Oxford Diffraction Xcalibur diffractometer	1734 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
ω/2θ scans	θ_max = 32.6°, θ_min = 2.6°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	h = −15→19
T_min = 0.54, T_max = 0.65	k = −15→15
3597 measured reflections	l = −13→11
1913 independent reflections

Refinement top

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/[A₀T₀(x) + A₁T₁(x) ··· + A_n-1]T_n-1(x)] where A_i are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] [1-(deltaF/6*sigmaF)²]² A_i are: 18.9 -12.3 16.6
S = 1.04	(Δ/σ)_max = 0.001
1667 reflections	Δρ_max = 0.84 e Å⁻³
103 parameters	Δρ_min = −0.91 e Å⁻³
3 restraints

Crystal data top

K[NiGa₂(PO₄)₃(H₂O)₂]	V = 1128.4 (2) Å³
M_r = 558.17	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 13.2095 (13) Å	µ = 7.27 mm⁻¹
b = 10.1733 (9) Å	T = 150 K
c = 8.8130 (9) Å	0.09 × 0.08 × 0.06 mm
β = 107.68 (1)°

Data collection top

Oxford Diffraction Xcalibur diffractometer	1913 independent reflections
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	1734 reflections with I > 2σ(I)
T_min = 0.54, T_max = 0.65	R_int = 0.018
3597 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	3 restraints
wR(F²) = 0.025	Only H-atom coordinates refined
S = 1.04	Δρ_max = 0.84 e Å⁻³
1667 reflections	Δρ_min = −0.91 e Å⁻³
103 parameters

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

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—O5^iv	1.5510 (11)
Ni1—O2ⁱ	1.9951 (11)	P2—O6^v	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)	O5^iv—P2—O2	111.12 (6)
O6—Ga1—O7	93.05 (5)	O5^iv—P2—O6^v	110.43 (6)
O2ⁱ—Ni1—O2	101.49 (7)	O5^iv—P2—O7	101.91 (6)
O2—Ni1—O3	95.65 (4)	O6^v—P2—O2	107.68 (6)
O2ⁱ—Ni1—O3	162.84 (5)	O6^v—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—P2^vi	129.28 (7)
O3—Ni1—O4	96.38 (5)	Ga1—O6—P2^v	125.62 (7)
O4ⁱ—Ni1—O3	93.46 (4)	Ga1—O7—P2	139.82 (7)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x, −y, z+1/2; (iii) −x, −y, −z; (iv) −x+1/2, y+1/2, −z+1/2; (v) −x+1/2, −y+1/2, −z; (vi) −x+1/2, y−1/2, −z+1/2.

Hydrogen-bond geometry (Å, º) top

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···O6^iv	0.85 (1)	2.16 (2)	2.976 (2)	161

Symmetry codes: (ii) x, −y, z+1/2; (iv) −x+1/2, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	K[NiGa₂(PO₄)₃(H₂O)₂]
M_r	558.17
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	150
a, b, c (Å)	13.2095 (13), 10.1733 (9), 8.8130 (9)
β (°)	107.68 (1)
V (Å³)	1128.4 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	7.27
Crystal size (mm)	0.09 × 0.08 × 0.06

Data collection
Diffractometer	Oxford Diffraction Xcalibur diffractometer
Absorption correction	Multi-scan (CrysAlis RED; Oxford Diffraction, 2006)
T_min, T_max	0.54, 0.65
No. of measured, independent and observed [I > 2σ(I)] reflections	3597, 1913, 1734
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.758

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.025, 1.04
No. of reflections	1667
No. of parameters	103
No. of restraints	3
H-atom treatment	Only H-atom coordinates refined
Δρ_max, Δρ_min (e Å⁻³)	0.84, −0.91

Computer programs: CrysAlis PRO (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SIR92 (Altomare et al., 1994), CRYSTALS (Betteridge et al., 2003), CAMERON (Watkin et al., 1996).

Selected geometric parameters (Å, º) top

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

O1—Ga1—O3	89.49 (5)	O4ⁱ—Ni1—O3	93.46 (4)
O1—Ga1—O5	119.09 (5)	O4ⁱ—Ni1—O4	168.18 (7)
O1—Ga1—O6	94.97 (5)	O1ⁱⁱ—P1—O1ⁱⁱⁱ	104.18 (9)
O1—Ga1—O7	116.97 (5)	O1ⁱⁱ—P1—O3	114.14 (6)
O3—Ga1—O5	88.16 (5)	O1ⁱⁱⁱ—P1—O3	112.42 (6)
O3—Ga1—O6	174.93 (4)	O3ⁱ—P1—O1ⁱⁱ	112.42 (6)
O3—Ga1—O7	87.06 (5)	O3ⁱ—P1—O1ⁱⁱⁱ	114.14 (6)
O5—Ga1—O6	87.57 (5)	O3ⁱ—P1—O3	99.94 (8)
O5—Ga1—O7	123.66 (5)	O2—P2—O7	115.61 (6)
O6—Ga1—O7	93.05 (5)	O5^iv—P2—O2	111.12 (6)
O2ⁱ—Ni1—O2	101.49 (7)	O5^iv—P2—O6^v	110.43 (6)
O2—Ni1—O3	95.65 (4)	O5^iv—P2—O7	101.91 (6)
O2ⁱ—Ni1—O3	162.84 (5)	O6^v—P2—O2	107.68 (6)
O2—Ni1—O4	87.12 (5)	O6^v—P2—O7	110.02 (6)
O2ⁱ—Ni1—O4	85.41 (5)	Ga1—O1—P1ⁱⁱⁱ	135.47 (7)
O3ⁱ—Ni1—O2	162.84 (5)	Ga1—O3—Ni1	129.51 (5)
O3ⁱ—Ni1—O2ⁱ	95.65 (4)	Ga1—O3—P1	131.86 (7)
O3ⁱ—Ni1—O3	67.23 (6)	Ni1—O2—P2	128.84 (7)
O3ⁱ—Ni1—O4	93.46 (4)	Ni1—O3—P1	96.42 (5)
O3ⁱ—Ni1—O4ⁱ	96.38 (5)	Ga1—O5—P2^vi	129.28 (7)
O4ⁱ—Ni1—O2	85.41 (5)	Ga1—O6—P2^v	125.62 (7)
O4ⁱ—Ni1—O2ⁱ	87.12 (5)	Ga1—O7—P2	139.82 (7)
O3—Ni1—O4	96.38 (5)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x, −y, z+1/2; (iii) −x, −y, −z; (iv) −x+1/2, y+1/2, −z+1/2; (v) −x+1/2, −y+1/2, −z; (vi) −x+1/2, y−1/2, −z+1/2.

Hydrogen-bond geometry (Å, º) top

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···O6^iv	0.85 (1)	2.163 (17)	2.976 (2)	161

Symmetry codes: (ii) x, −y, z+1/2; (iv) −x+1/2, y+1/2, −z+1/2.

Acknowledgements

The authors thank the EPSRC for a grant in support of a single-crystal diffractometer.

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