Disilver(I) trinickel(II) hydrogenphos-phate bis-(phosphate), Ag(2)Ni(3)(HPO(4))(PO(4))(2).

The title compound, Ag(2)Ni(3)(HPO(4))(PO(4))(2), has been synthesized by the hydro-thermal 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 NiO(6) octa-hedra linked to PO(4) tetra-hedra by a common vertex. The second chain is built up from two adjacent edge-sharing octa-hedra (dimers) whose ends are linked to two PO(4) tetra-hedra 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 hexa-gonal 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, AgMn(3)(PO(4))(HPO(4))(2). Moreover, O-H⋯O hydrogen bonds link three PO(4) tetra-hedra 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 = 677.79

Orthorhombic,

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[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.060

S = 1.06

1125 reflections

99 parameters

1 restraint

H-atom parameters constrained

Δρmax = 1.81 e Å−3

Δρmin = −1.12 e Å−3

Absolute structure: Flack (1983 ▶), 467 Friedel pairs

Flack parameter: 0.55 (3)

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 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811021167/ru2005sup1.cif

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

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

Ag2Ni3(HPO4)(PO4)2	F(000) = 1280
Mr = 677.79	Dx = 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

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

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(Fo2) + (0.0356P)2 + 1.7344P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max < 0.001
1125 reflections	Δρmax = 1.81 e Å−3
99 parameters	Δρmin = −1.12 e Å−3
1 restraint	Absolute structure: Flack (1983), 467 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.55 (3)

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.

	x	y	z	Uiso*/Ueq
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*

	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)

Ag1—O1i	2.534 (3)	Ni2—O2xi	2.041 (3)
Ag1—O1ii	2.535 (3)	Ni2—O3i	2.062 (4)
Ag1—O5iii	2.617 (3)	Ni2—O3	2.062 (4)
Ag1—O5iv	2.617 (3)	P1—O1	1.511 (4)
Ag1—O7v	2.659 (5)	P1—O2	1.549 (4)
Ag1—O6v	2.866 (5)	P1—O4	1.566 (4)
Ag1—O4vi	2.962 (3)	P1—O3	1.569 (4)
Ag1—O4vii	2.962 (3)	P2—O5	1.518 (3)
Ag1—Ag2	3.31641 (16)	P2—O5xii	1.518 (3)
Ag2—O3vi	2.375 (4)	P2—O6	1.563 (6)
Ag2—O3viii	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—Ni2xiii	2.041 (3)
Ag2—O4viii	3.133 (4)	O3—Ag2xiv	2.375 (4)
Ag2—O4vi	3.133 (4)	O4—Ni1ix	2.172 (4)
Ni1—O1i	2.046 (4)	O4—Ag1xv	2.962 (3)
Ni1—O7v	2.047 (3)	O4—Ag2xiv	3.133 (4)
Ni1—O6	2.047 (4)	O5—Ag1xvi	2.617 (3)
Ni1—O2	2.079 (4)	O6—Ni1xii	2.047 (4)
Ni1—O3	2.097 (4)	O6—Ag1xvii	2.866 (5)
Ni1—O4ix	2.172 (4)	O7—Ni1xi	2.047 (3)
Ni2—O5i	2.015 (3)	O7—Ni1xvii	2.047 (3)
Ni2—O5	2.015 (3)	O7—Ag1xvii	2.659 (5)
Ni2—O2x	2.041 (3)	O7—H7	0.8600
O1i—Ag1—O1ii	72.33 (16)	O3viii—Ag2—O4vi	67.92 (11)
O1i—Ag1—O5iii	86.46 (10)	O2—Ag2—O4vi	125.71 (11)
O1ii—Ag1—O5iii	119.74 (11)	O2i—Ag2—O4vi	110.51 (11)
O1i—Ag1—O5iv	119.74 (11)	O1—Ag2—O4vi	177.43 (10)
O1ii—Ag1—O5iv	86.46 (10)	O1i—Ag2—O4vi	102.27 (8)
O5iii—Ag1—O5iv	56.41 (12)	O4viii—Ag2—O4vi	79.25 (12)
O1i—Ag1—O7v	65.26 (11)	Ag1i—Ag2—Ag1	171.68 (3)
O1ii—Ag1—O7v	65.26 (11)	O1i—Ni1—O7v	86.42 (17)
O5iii—Ag1—O7v	148.99 (7)	O1i—Ni1—O6	95.26 (18)
O5iv—Ag1—O7v	148.99 (7)	O7v—Ni1—O6	88.15 (12)
O1i—Ag1—O6v	107.78 (12)	O1i—Ni1—O2	90.92 (15)
O1ii—Ag1—O6v	107.78 (12)	O7v—Ni1—O2	101.25 (13)
O5iii—Ag1—O6v	132.46 (11)	O6—Ni1—O2	169.08 (15)
O5iv—Ag1—O6v	132.46 (11)	O1i—Ni1—O3	89.93 (14)
O7v—Ag1—O6v	53.46 (12)	O7v—Ni1—O3	170.53 (14)
O1i—Ag1—O4vi	116.39 (11)	O6—Ni1—O3	100.89 (14)
O1ii—Ag1—O4vi	164.32 (10)	O2—Ni1—O3	70.05 (11)
O5iii—Ag1—O4vi	74.98 (10)	O1i—Ni1—O4ix	175.34 (13)
O5iv—Ag1—O4vi	98.97 (10)	O7v—Ni1—O4ix	88.97 (17)
O7v—Ag1—O4vi	105.40 (12)	O6—Ni1—O4ix	83.92 (17)
O6v—Ag1—O4vi	57.90 (11)	O2—Ni1—O4ix	90.62 (14)
O1i—Ag1—O4vii	164.32 (10)	O3—Ni1—O4ix	94.73 (14)
O1ii—Ag1—O4vii	116.39 (11)	O5i—Ni2—O5	178.70 (19)
O5iii—Ag1—O4vii	98.97 (10)	O5i—Ni2—O2x	94.43 (14)
O5iv—Ag1—O4vii	74.98 (10)	O5—Ni2—O2x	86.54 (14)
O7v—Ag1—O4vii	105.40 (12)	O5i—Ni2—O2xi	86.55 (14)
O6v—Ag1—O4vii	57.90 (11)	O5—Ni2—O2xi	94.42 (14)
O4vi—Ag1—O4vii	52.10 (14)	O2x—Ni2—O2xi	83.6 (2)
O3vi—Ag2—O3viii	100.81 (18)	O5i—Ni2—O3i	94.10 (14)
O3vi—Ag2—O2	177.72 (14)	O5—Ni2—O3i	84.97 (15)
O3viii—Ag2—O2	76.92 (10)	O2x—Ni2—O3i	93.29 (11)
O3vi—Ag2—O2i	76.92 (10)	O2xi—Ni2—O3i	176.91 (18)
O3viii—Ag2—O2i	177.72 (14)	O5i—Ni2—O3	84.97 (15)
O2—Ag2—O2i	105.35 (15)	O5—Ni2—O3	94.10 (14)
O3vi—Ag2—O1	125.84 (12)	O2x—Ni2—O3	176.91 (18)
O3viii—Ag2—O1	114.65 (11)	O2xi—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)
O3vi—Ag2—O1i	114.65 (11)	O1—P1—O4	109.1 (2)
O3viii—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)
O3vi—Ag2—O4viii	67.92 (11)	O5—P2—O5xii	109.1 (2)
O3viii—Ag2—O4viii	52.70 (12)	O5—P2—O6	110.77 (16)
O2—Ag2—O4viii	110.51 (11)	O5xii—P2—O6	110.77 (16)
O2i—Ag2—O4viii	125.71 (11)	O5—P2—O7	110.44 (16)
O1—Ag2—O4viii	102.27 (8)	O5xii—P2—O7	110.44 (16)
O1i—Ag2—O4viii	177.43 (10)	O6—P2—O7	105.3 (2)
O3vi—Ag2—O4vi	52.70 (12)	P2—O7—H7	127.4

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7···O6xvii	0.86	2.06	2.847 (6)	151.

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) .