Disilver(I) trinickel(II) hydrogenphos­phate bis­(phosphate), Ag2Ni3(HPO4)(PO4)2

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

doi:10.1107/S1600536811021167

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 7| July 2011| Page i40

doi:10.1107/S1600536811021167

Open

access

Disilver(I) trinickel(II) hydrogenphosphate bis(phosphate), Ag₂Ni₃(HPO₄)(PO₄)₂

Abderrazzak Assani,^a ^* Lahcen El Ammari,^a Mohammed Zriouil ^a and Mohamed Saadi ^a

^aLaboratoire de Chimie du Solide Appliquée, Faculté des Sciences, Université Mohammed V-Agdal, Avenue Ibn Battouta, BP 1014, Rabat, Morocco
^*Correspondence e-mail: abder_assani@yahoo.fr

(Received 11 April 2011; accepted 1 June 2011; online 11 June 2011)

The title compound, Ag₂Ni₃(HPO₄)(PO₄)₂, has been synthesized by the hydrothermal method. Its structure is formed by two types of chains running along the b axis. The first chain results from a linear and continuous succession of NiO₆ octahedra linked to PO₄ tetrahedra by a common vertex. The second chain is built up from two adjacent edge-sharing octahedra (dimers) whose ends are linked to two PO₄ tetrahedra by a common edge. Those two types of chains are linked together by the phosphate groups to form polyhedral sheets parallel to the (001) plane. The three-dimensional framework delimits two types of hexagonal tunnels parallel to the a-axis direction, at (x, 1/2, 0) and (x, 0, 1/2), where the Ag atoms are located. Each silver cation is surrounded by eight O atoms. The same Ag⁺ coordination is found in other phosphates with the alluaudite structure, for example, AgMn₃(PO₄)(HPO₄)₂. Moreover, O—H⋯O hydrogen bonds link three PO₄ tetrahedra so as to build a three-dimensional network.

Related literature

For related applications, see: Viter & Nagornyi (2009 ); Gao & Gao (2005 ); Clearfield (1988 ); Trad et al. (2010 ). For compounds with the same structure, see: Assani et al. (2010 , 2011 ); Leroux et al. (1995 ); Ben Smail & Jouini (2002 ).

Experimental

Crystal data

Ag₂Ni₃(HPO₄)(PO₄)₂
M_r = 677.79
Orthorhombic, I m a 2
a = 12.9233 (3) Å
b = 6.5678 (2) Å
c = 10.6629 (3) Å
V = 905.04 (4) Å³
Z = 4
Mo Kα radiation
μ = 10.98 mm⁻¹
T = 296 K
0.25 × 0.13 × 0.08 mm

Data collection

Bruker X8 APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (MULABS; Blessing, 1995 ) T_min = 0.382, T_max = 0.471
3762 measured reflections
1125 independent reflections
1103 reflections with I > 2σ(I)
R_int = 0.017

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.060
S = 1.06
1125 reflections
99 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 1.81 e Å⁻³
Δρ_min = −1.12 e Å⁻³
Absolute structure: Flack (1983 ), 467 Friedel pairs
Flack parameter: 0.55 (3)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7⋯O6ⁱ	0.86	2.06	2.847 (6)	151
Symmetry code: (i) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2005 ); cell refinement: SAINT; data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ) and DIAMOND (Brandenburg, 2006 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811021167/ru2005sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811021167/ru2005Isup2.hkl

checkCIF report

Comment top

As the improvement has arisen in the synthesis of a variety of interesting porous materials and open-framework structures, extensive studies are devoted to the metal phosphates which exhibit a rich structural diversity and have been widely studied as catalysts (Viter & Nagornyi, 2009; Gao & Gao, 2005), ion-exchangers (Clearfield, 1988) and as positive electrode in the lithium and sodium batteries (Trad et al. (2010)).

Within this family of compounds, the resulting anionic frameworks, generally constructed from the alternation of PO₄ tetrahedra connected to metal cations in different coordinate geometry MO_n (with n=4, 5 and 6), generate pores and channels offering suitable environment to accommodate different other cations. In our search for new phosphates with microporous framework, our most attention has been paid to the hydrothermal investigation of the A₂O—MO—P₂O₅ systems, with A = monovalent cations and M = divalent cations. Accordingly, we have succeed, for instance, to isolate new form of silver zinc phosphate (γ-AgZnPO₄) related to the ABW zeolite structure (Assani et al. 2010) while the silver magnesium phosphate, namely AgMg₃(PO₄)(HPO₄)₂, represent a new member of the well known alluaudite-like structure family (Assani et al. 2011). The present paper aims to develop the hydrothermal synthesis and the structural characterization of a new silver nickel phosphate, namely, Ag₂Ni₃(HPO₄)(PO₄)₂.

The structure of this compound is formed by two types of chains running along the b axis. The first chain (Ni2P2HO₉)∞ is built up from Ni2 and P2 atoms in special Wyckoff position 4 b (m) of the space group Ima2. This chain results from linear and continuous succession of octahedron (Ni2O₆) and P2O₃OH tetrahedron which share a vertex. The second chain (Ni₂P₂O₁₄)n is built up from two adjacent edge sharing octahedra ((Ni1)₂O₁₀ dimmers) whose ends are linked to two P1O₄ tetrahedra by a common edge (Fig.1). Those chains are linked together by the phosphate groups to form polyhedral sheets parallel to the (0 0 1) plane as shown in Fig.2.

The three dimensional framework delimits two types of hexagonal tunnels running along the a direction, at x 1/2 0 and x 0 1/2 (Fig.3). The Ag2 atom is located at centre of tunnels, this explains the high value of its anisotropic displacement U₁₁, whereas Ag1 is slightly shifted from this center (Wyckoff positions: Ag2 at 2a: 0, 0, z and Ag1 at 2 b: 1/4, y, z). However, each Ag⁺ ion is surrounded by 8 O atoms with different Ag–O distances. Indeed, the first coordination environment of Ag2⁺ is almost square planar with four short Ag2—O distances between 2.373 (4) and 2.421 (4) Å and the other four larger distances are in the range of 2.869 (4) to 3.133 (4) Å. A similar coordination surrounding Ag1⁺ is observed with Ag1—O bond lengths in the range of 2.537 (4)–2.616 (4) Å and the longest bonds are situated between 2.661 (4) and 2.963 (4) Å. The same coordination for this cation is found in other phosphate with alluaudite structure like AgMn₃(PO₄)(HPO₄)₂ (Leroux et al. (1995)) and AgNi₃(PO₄)(HPO₄)₂ (Ben Smail & Jouini (2002)).

Moreover, O—H···O hydrogen bondings link two adjacent P2O₄ tetrahedra via a strong hydrogen bond O7–H7···O6 to two P1O₄ tetrahedra through weak bonds O7–H7···O4 in the way to build an infinite three-dimensional network as shown in Table 1.

Related literature top

For related applications, see: Viter & Nagornyi (2009); Gao & Gao (2005); Clearfield (1988); Trad et al. (2010). For compounds with the same structure, see: Assani et al. (2010, 2011); Leroux et al. (1995); Ben Smail & Jouini (2002).

Experimental top

By means of hydrothermal synthesis, we have isolate a new silver nickel phosphate from the reaction mixture of silver nitrate (AgNO₃; 0.1699 g), metallic nickel (Ni; 0.0881 g), 85%wt phosphoric acid (H₃PO₄; 0,10 ml) and water (12 ml). The hydrothermal treatment was conducted in a 23 ml Teflon-lined autoclave under autogeneous pressure at 468 K for two days. After being filtered off, washed with deionized water and air dried, the reaction product consists of a monophasic green powder and some green parallelepipedic crystals corresponding to the title compound.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2 (Bruker, 2005); data reduction: APEX2 (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

	Fig. 1. Partial plot of Ag₂Ni₃(HPO₄)(PO₄)₂ crystal structure. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (i) -x, -y + 1, z; (ii) x + 1/2, -y + 1, z; (iii) x, -y + 3/2, z - 1/2; (iv) -x + 1/2, -y + 3/2, z - 1/2; (v) -x + 1/2, -y + 1/2, z - 1/2; (vi) -x, y + 1/2, z - 1/2; (vii) x + 1/2, y + 1/2, z - 1/2; (viii) x, -y + 1/2, z - 1/2; (ix) -x, -y, z; (x) -x, y + 1/2, z + 1/2; (xi) x, -y + 1/2, z + 1/2; (xii) -x + 1/2, y, z.
	Fig. 2. View along the b axis of polyhedral sheets parallel to the (0 0 1) plane.
	Fig. 3. A three-dimensional polyhedral view of the crystal structure of the Ag₂Ni₃(HPO₄)(PO₄)₂, showing tunnels running along the a direction, at x, 1/2, 0 and x, 0, 1/2.

Disilver(I) trinickel(II) hydrogenphosphate bis(phosphate) top

Crystal data top

Ag₂Ni₃(HPO₄)(PO₄)₂	F(000) = 1280
M_r = 677.79	D_x = 4.974 Mg m⁻³
Orthorhombic, Ima2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: I 2 -2a	Cell parameters from 1125 reflections
a = 12.9233 (3) Å	θ = 3.2–29.0°
b = 6.5678 (2) Å	µ = 10.98 mm⁻¹
c = 10.6629 (3) Å	T = 296 K
V = 905.04 (4) Å³	Prism, green
Z = 4	0.25 × 0.13 × 0.08 mm

Data collection top

Bruker X8 APEXII CCD area-detector diffractometer	1125 independent reflections
Radiation source: fine-focus sealed tube	1103 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.017
ϕ and ω scans	θ_max = 29.0°, θ_min = 3.2°
Absorption correction: multi-scan (MULABS; Blessing, 1995)	h = −13→14
T_min = 0.382, T_max = 0.471	k = −16→17
3762 measured reflections	l = −8→8

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.024	H-atom parameters constrained
wR(F²) = 0.060	w = 1/[σ²(F_o²) + (0.0356P)² + 1.7344P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max < 0.001
1125 reflections	Δρ_max = 1.81 e Å⁻³
99 parameters	Δρ_min = −1.12 e Å⁻³
1 restraint	Absolute structure: Flack (1983), 467 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.55 (3)

Crystal data top

Ag₂Ni₃(HPO₄)(PO₄)₂	V = 905.04 (4) Å³
M_r = 677.79	Z = 4
Orthorhombic, Ima2	Mo Kα radiation
a = 12.9233 (3) Å	µ = 10.98 mm⁻¹
b = 6.5678 (2) Å	T = 296 K
c = 10.6629 (3) Å	0.25 × 0.13 × 0.08 mm

Data collection top

Bruker X8 APEXII CCD area-detector diffractometer	1125 independent reflections
Absorption correction: multi-scan (MULABS; Blessing, 1995)	1103 reflections with I > 2σ(I)
T_min = 0.382, T_max = 0.471	R_int = 0.017
3762 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	H-atom parameters constrained
wR(F²) = 0.060	Δρ_max = 1.81 e Å⁻³
S = 1.06	Δρ_min = −1.12 e Å⁻³
1125 reflections	Absolute structure: Flack (1983), 467 Friedel pairs
99 parameters	Absolute structure parameter: 0.55 (3)
1 restraint

Special details top

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.

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) top

	x	y	z	U_iso*/U_eq
Ag1	0.2500	0.60793 (8)	−0.01513 (7)	0.02914 (18)
Ag2	0.0000	0.5000	−0.03769 (5)	0.0443 (2)
Ni1	0.13623 (4)	0.24801 (10)	0.20871 (7)	0.00699 (13)
Ni2	0.0000	0.5000	0.45735 (7)	0.00462 (15)
P1	−0.07279 (7)	0.25722 (19)	0.20677 (13)	0.00587 (19)
P2	0.2500	0.4102 (2)	0.45653 (15)	0.0042 (3)
O1	−0.1343 (3)	0.4456 (5)	0.1739 (3)	0.0091 (7)
O2	0.0044 (3)	0.2070 (6)	0.1000 (3)	0.0056 (6)
O3	0.0036 (3)	0.2785 (5)	0.3204 (3)	0.0072 (8)
O4	−0.1494 (3)	0.0786 (5)	0.2360 (3)	0.0096 (9)
O5	0.1543 (2)	0.5443 (4)	0.4552 (3)	0.0085 (5)
O6	0.2500	0.2617 (8)	0.3420 (5)	0.0090 (12)
O7	0.2500	0.2692 (7)	0.5756 (5)	0.0064 (12)
H7	0.2500	0.3065	0.6529	0.008*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ag1	0.0491 (4)	0.0158 (3)	0.0225 (3)	0.000	0.000	0.0048 (3)
Ag2	0.1145 (7)	0.0083 (2)	0.0101 (3)	−0.0020 (3)	0.000	0.000
Ni1	0.0058 (2)	0.0092 (3)	0.0060 (3)	0.0005 (2)	0.0005 (3)	−0.00135 (19)
Ni2	0.0052 (3)	0.0049 (3)	0.0037 (3)	0.0006 (2)	0.000	0.000
P1	0.0064 (4)	0.0064 (5)	0.0047 (4)	−0.0001 (5)	0.0008 (6)	0.0004 (4)
P2	0.0043 (6)	0.0054 (6)	0.0030 (7)	0.000	0.000	−0.0012 (6)
O1	0.0086 (16)	0.0100 (18)	0.0088 (15)	0.0003 (14)	−0.0017 (10)	−0.0010 (12)
O2	0.0044 (18)	0.0088 (15)	0.0035 (15)	−0.0002 (15)	−0.0010 (12)	−0.0029 (13)
O3	0.012 (2)	0.0044 (17)	0.0049 (15)	0.0009 (15)	−0.0005 (12)	−0.0010 (12)
O4	0.010 (2)	0.0023 (18)	0.016 (2)	−0.0011 (13)	0.0015 (11)	0.0017 (11)
O5	0.0077 (12)	0.0082 (12)	0.0096 (15)	0.0014 (10)	−0.0008 (13)	−0.0003 (12)
O6	0.005 (3)	0.013 (3)	0.009 (2)	0.000	0.000	−0.0007 (16)
O7	0.007 (3)	0.007 (3)	0.005 (2)	0.000	0.000	0.0023 (16)

Geometric parameters (Å, º) top

Ag1—O1ⁱ	2.534 (3)	Ni2—O2^xi	2.041 (3)
Ag1—O1ⁱⁱ	2.535 (3)	Ni2—O3ⁱ	2.062 (4)
Ag1—O5ⁱⁱⁱ	2.617 (3)	Ni2—O3	2.062 (4)
Ag1—O5^iv	2.617 (3)	P1—O1	1.511 (4)
Ag1—O7^v	2.659 (5)	P1—O2	1.549 (4)
Ag1—O6^v	2.866 (5)	P1—O4	1.566 (4)
Ag1—O4^vi	2.962 (3)	P1—O3	1.569 (4)
Ag1—O4^vii	2.962 (3)	P2—O5	1.518 (3)
Ag1—Ag2	3.3164 (2)	P2—O5^xii	1.518 (3)
Ag2—O3^vi	2.375 (4)	P2—O6	1.563 (6)
Ag2—O3^viii	2.375 (4)	P2—O7	1.572 (5)
Ag2—O2	2.421 (4)	O1—Ni1ⁱ	2.046 (4)
Ag2—O2ⁱ	2.421 (4)	O1—O4	2.507 (5)
Ag2—O1	2.869 (4)	O1—Ag1ⁱ	2.534 (3)
Ag2—O1ⁱ	2.869 (4)	O2—Ni2^xiii	2.041 (3)
Ag2—O4^viii	3.133 (4)	O3—Ag2^xiv	2.375 (4)
Ag2—O4^vi	3.133 (4)	O4—Ni1^ix	2.172 (4)
Ni1—O1ⁱ	2.046 (4)	O4—Ag1^xv	2.962 (3)
Ni1—O7^v	2.047 (3)	O4—Ag2^xiv	3.133 (4)
Ni1—O6	2.047 (4)	O5—Ag1^xvi	2.617 (3)
Ni1—O2	2.079 (4)	O6—Ni1^xii	2.047 (4)
Ni1—O3	2.097 (4)	O6—Ag1^xvii	2.866 (5)
Ni1—O4^ix	2.172 (4)	O7—Ni1^xi	2.047 (3)
Ni2—O5ⁱ	2.015 (3)	O7—Ni1^xvii	2.047 (3)
Ni2—O5	2.015 (3)	O7—Ag1^xvii	2.659 (5)
Ni2—O2^x	2.041 (3)	O7—H7	0.8600

O1ⁱ—Ag1—O1ⁱⁱ	72.33 (16)	O3^viii—Ag2—O4^vi	67.92 (11)
O1ⁱ—Ag1—O5ⁱⁱⁱ	86.46 (10)	O2—Ag2—O4^vi	125.71 (11)
O1ⁱⁱ—Ag1—O5ⁱⁱⁱ	119.74 (11)	O2ⁱ—Ag2—O4^vi	110.51 (11)
O1ⁱ—Ag1—O5^iv	119.74 (11)	O1—Ag2—O4^vi	177.43 (10)
O1ⁱⁱ—Ag1—O5^iv	86.46 (10)	O1ⁱ—Ag2—O4^vi	102.27 (8)
O5ⁱⁱⁱ—Ag1—O5^iv	56.41 (12)	O4^viii—Ag2—O4^vi	79.25 (12)
O1ⁱ—Ag1—O7^v	65.26 (11)	Ag1ⁱ—Ag2—Ag1	171.68 (3)
O1ⁱⁱ—Ag1—O7^v	65.26 (11)	O1ⁱ—Ni1—O7^v	86.42 (17)
O5ⁱⁱⁱ—Ag1—O7^v	148.99 (7)	O1ⁱ—Ni1—O6	95.26 (18)
O5^iv—Ag1—O7^v	148.99 (7)	O7^v—Ni1—O6	88.15 (12)
O1ⁱ—Ag1—O6^v	107.78 (12)	O1ⁱ—Ni1—O2	90.92 (15)
O1ⁱⁱ—Ag1—O6^v	107.78 (12)	O7^v—Ni1—O2	101.25 (13)
O5ⁱⁱⁱ—Ag1—O6^v	132.46 (11)	O6—Ni1—O2	169.08 (15)
O5^iv—Ag1—O6^v	132.46 (11)	O1ⁱ—Ni1—O3	89.93 (14)
O7^v—Ag1—O6^v	53.46 (12)	O7^v—Ni1—O3	170.53 (14)
O1ⁱ—Ag1—O4^vi	116.39 (11)	O6—Ni1—O3	100.89 (14)
O1ⁱⁱ—Ag1—O4^vi	164.32 (10)	O2—Ni1—O3	70.05 (11)
O5ⁱⁱⁱ—Ag1—O4^vi	74.98 (10)	O1ⁱ—Ni1—O4^ix	175.34 (13)
O5^iv—Ag1—O4^vi	98.97 (10)	O7^v—Ni1—O4^ix	88.97 (17)
O7^v—Ag1—O4^vi	105.40 (12)	O6—Ni1—O4^ix	83.92 (17)
O6^v—Ag1—O4^vi	57.90 (11)	O2—Ni1—O4^ix	90.62 (14)
O1ⁱ—Ag1—O4^vii	164.32 (10)	O3—Ni1—O4^ix	94.73 (14)
O1ⁱⁱ—Ag1—O4^vii	116.39 (11)	O5ⁱ—Ni2—O5	178.70 (19)
O5ⁱⁱⁱ—Ag1—O4^vii	98.97 (10)	O5ⁱ—Ni2—O2^x	94.43 (14)
O5^iv—Ag1—O4^vii	74.98 (10)	O5—Ni2—O2^x	86.54 (14)
O7^v—Ag1—O4^vii	105.40 (12)	O5ⁱ—Ni2—O2^xi	86.55 (14)
O6^v—Ag1—O4^vii	57.90 (11)	O5—Ni2—O2^xi	94.42 (14)
O4^vi—Ag1—O4^vii	52.10 (14)	O2^x—Ni2—O2^xi	83.6 (2)
O3^vi—Ag2—O3^viii	100.81 (18)	O5ⁱ—Ni2—O3ⁱ	94.10 (14)
O3^vi—Ag2—O2	177.72 (14)	O5—Ni2—O3ⁱ	84.97 (15)
O3^viii—Ag2—O2	76.92 (10)	O2^x—Ni2—O3ⁱ	93.29 (11)
O3^vi—Ag2—O2ⁱ	76.92 (10)	O2^xi—Ni2—O3ⁱ	176.91 (18)
O3^viii—Ag2—O2ⁱ	177.72 (14)	O5ⁱ—Ni2—O3	84.97 (15)
O2—Ag2—O2ⁱ	105.35 (15)	O5—Ni2—O3	94.10 (14)
O3^vi—Ag2—O1	125.84 (12)	O2^x—Ni2—O3	176.91 (18)
O3^viii—Ag2—O1	114.65 (11)	O2^xi—Ni2—O3	93.29 (11)
O2—Ag2—O1	55.82 (11)	O3ⁱ—Ni2—O3	89.8 (2)
O2ⁱ—Ag2—O1	66.92 (11)	O1—P1—O2	110.0 (2)
O3^vi—Ag2—O1ⁱ	114.65 (11)	O1—P1—O4	109.1 (2)
O3^viii—Ag2—O1ⁱ	125.84 (12)	O2—P1—O4	113.2 (2)
O2—Ag2—O1ⁱ	66.92 (11)	O1—P1—O3	115.89 (19)
O2ⁱ—Ag2—O1ⁱ	55.82 (11)	O2—P1—O3	100.46 (15)
O1—Ag2—O1ⁱ	76.28 (13)	O4—P1—O3	108.1 (2)
O3^vi—Ag2—O4^viii	67.92 (11)	O5—P2—O5^xii	109.1 (2)
O3^viii—Ag2—O4^viii	52.70 (12)	O5—P2—O6	110.77 (16)
O2—Ag2—O4^viii	110.51 (11)	O5^xii—P2—O6	110.77 (16)
O2ⁱ—Ag2—O4^viii	125.71 (11)	O5—P2—O7	110.44 (16)
O1—Ag2—O4^viii	102.27 (8)	O5^xii—P2—O7	110.44 (16)
O1ⁱ—Ag2—O4^viii	177.43 (10)	O6—P2—O7	105.3 (2)
O3^vi—Ag2—O4^vi	52.70 (12)	P2—O7—H7	127.4

Symmetry codes: (i) −x, −y+1, z; (ii) x+1/2, −y+1, z; (iii) x, −y+3/2, z−1/2; (iv) −x+1/2, −y+3/2, z−1/2; (v) −x+1/2, −y+1/2, z−1/2; (vi) −x, y+1/2, z−1/2; (vii) x+1/2, y+1/2, z−1/2; (viii) x, −y+1/2, z−1/2; (ix) −x, −y, z; (x) −x, y+1/2, z+1/2; (xi) x, −y+1/2, z+1/2; (xii) −x+1/2, y, z; (xiii) −x, y−1/2, z−1/2; (xiv) −x, y−1/2, z+1/2; (xv) x−1/2, y−1/2, z+1/2; (xvi) −x+1/2, −y+3/2, z+1/2; (xvii) −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
O7—H7···O6^xvii	0.86	2.06	2.847 (6)	151

Symmetry code: (xvii) −x+1/2, −y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula	Ag₂Ni₃(HPO₄)(PO₄)₂
M_r	677.79
Crystal system, space group	Orthorhombic, Ima2
Temperature (K)	296
a, b, c (Å)	12.9233 (3), 6.5678 (2), 10.6629 (3)
V (Å³)	905.04 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	10.98
Crystal size (mm)	0.25 × 0.13 × 0.08

Data collection
Diffractometer	Bruker X8 APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (MULABS; Blessing, 1995)
T_min, T_max	0.382, 0.471
No. of measured, independent and observed [I > 2σ(I)] reflections	3762, 1125, 1103
R_int	0.017
(sin θ/λ)_max (Å⁻¹)	0.682

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.060, 1.06
No. of reflections	1125
No. of parameters	99
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.81, −1.12
Absolute structure	Flack (1983), 467 Friedel pairs
Absolute structure parameter	0.55 (3)

Computer programs: APEX2 (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7···O6ⁱ	0.86	2.06	2.847 (6)	151.0

Symmetry code: (i) −x+1/2, −y+1/2, z+1/2.

Acknowledgements

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for the X-ray measurements.

References

Assani, A., Saadi, M. & El Ammari, L. (2010). Acta Cryst. E66, i74. Web of Science CrossRef IUCr Journals Google Scholar
Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2011). Acta Cryst. E67, i5. Web of Science CrossRef IUCr Journals Google Scholar
Ben Smail, R. & Jouini, T. (2002). Acta Cryst. C58, i61–i62. Web of Science CrossRef CAS IUCr Journals Google Scholar
Blessing, R. H. (1995). Acta Cryst. A51, 33–38. CrossRef CAS Web of Science IUCr Journals Google Scholar
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Clearfield, A. (1988). Chem. Rev. 88, 125–148. CrossRef CAS Web of Science Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Gao, D. & Gao, Q. (2005). Microporous Mesoporous Mater. 85, 365–373. CrossRef CAS Google Scholar
Leroux, F., Mar, A., Guyomard, D. & Piffard, Y. (1995). J. Solid State Chem. 117, 206—212. CrossRef Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Trad, K., Carlier, D., Croguennec, L., Wattiaux, A., Ben Amara, M. & Delmas, C. (2010). Chem. Mater. 22, 5554–5562. Web of Science CrossRef CAS Google Scholar
Viter, V. N. & Nagornyi, P. G. (2009). Russ. J. Appl. Chem. 82, 935–939. Web of Science CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.