inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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Silver(I) di­aqua­nickel(II) catena-borodiphosphate(V) hydrate, (Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2O

aCentre National pour la Recherche Scientifique et Technique, Division UATRS, Angle Allal AlFassi et Avenue des FAR, Hay Ryad, BP 8027, Rabat, Morocco, and bLaboratoire de Chimie du Solide Appliquée, Faculté des Sciences, Université Mohammed V-Agdal, Avenue Ibn Batouta, BP 1014, Rabat, Morocco
*Correspondence e-mail: b_jaber50@yahoo.com

(Received 15 July 2011; accepted 21 July 2011; online 30 July 2011)

The structure framework of the title compound, (Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2O, is the same as that of its recently published counterpart AgMg(H2O)2[BP2O8]·H2O. In the title structure, the Ag, Ni, B and one O atom are located on special positions (sites symmetry 2). The structure consists of infinite borophosphate helical [BP2O8]3− ribbons, built up from alternate BO4 and PO4 tetra­hedra arranged around the 65 screw axes. The vertex-sharing BO4 and PO4 tetra­hedra form a spiral ribbon of four-membered rings in which BO4 and PO4 groups alternate. The ribbons are connected through slightly distorted NiO4(H2O)2 octa­hedra, four O atoms of which belong to the phosphate groups. The resulting three-dimensional framework is characterized by hexa­gonal channels running along [001]. However, the main difference between the structures of these two compounds lies in the filling ratio of Wyckoff positions 6a and 6b in the tunnels. Indeed, in this work, the refinement of the occupancy rate of sites 6a and 6b shows that the first is occupied by water at 67% and the second is partially occupied by 56.6% of Ag and 21.6% of Ni. In the AgMg(H2O)2[BP2O8]·H2O structure, these two sites are completely occupied by H2O and Ag+, respectively. The title structure is stabilized by O—H⋯O hydrogen bonds between water mol­ecules and O atoms that are part of the helices.

Related literature

For the isotypic Mg analogue, see: Zouihri et al. (2011[Zouihri, H., Saadi, M., Jaber, B. & El Ammari, L. (2011). Acta Cryst. E67, i39.]); Menezes et al. (2008[Menezes, P. W., Hoffmann, S., Prots, Y. & Kniep, R. (2008). Z. Kristallogr. 223, 333-334.]). For other borophosphates, see: Kniep et al. (1998[Kniep, R., Engelhardt, H. & Hauf, C. (1998). Chem. Mater. 10, 2930-2934.]); Ewald et al. (2007[Ewald, B., Huang, Y.-X. & Kniep, R. (2007). Z. Anorg. Allg. Chem. 633, 1517-1540.]); Lin et al. (2008[Lin, J.-R., Huang, Y.-X., Wu, Y.-H. & Zhou, Y. (2008). Acta Cryst. E64, i39-i40.]). For bond valence calculations see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

Experimental

Crystal data
  • (Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2O

  • Mr = 381.35

  • Hexagonal, P 65 22

  • a = 9.3848 (6) Å

  • c = 15.8411 (18) Å

  • V = 1208.28 (18) Å3

  • Z = 6

  • Mo Kα radiation

  • μ = 4.69 mm−1

  • T = 296 K

  • 0.18 × 0.12 × 0.11 mm

Data collection
  • Bruker APEXII CCD detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1999[Sheldrick, G. M. (1999). SADABS. University of Göttingen, Germany.]) Tmin = 0.705, Tmax = 0.741

  • 16974 measured reflections

  • 2043 independent reflections

  • 1912 reflections with I > 2σ(I)

  • Rint = 0.037

Refinement
  • R[F2 > 2σ(F2)] = 0.028

  • wR(F2) = 0.071

  • S = 1.08

  • 2043 reflections

  • 77 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 1.23 e Å−3

  • Δρmin = −0.59 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 779 Friedel pairs

  • Flack parameter: 0.006 (15)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O5—H5A⋯O4i 0.86 1.90 2.728 (2) 161
O5—H5B⋯O2 0.86 1.95 2.762 (2) 156
O6—H6A⋯O3ii 0.89 2.18 2.819 (5) 128
Symmetry codes: (i) [-x+y, -x+1, z+{\script{1\over 3}}]; (ii) [x, x-y+2, -z+{\script{11\over 6}}].

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information


Comment top

A large group of borophosphates is known with a molar ratio of B:P = 1:2 and helical structure type, which consist of loop branched chain anions built from tetrahedral BO4 and PO4 units (Kniep et al., 1998; Ewald et al., 2007; Lin et al. 2008).

The aim of this work is the synthesis and the crystal structure of a new borophosphate-hydrate (Ag0.57Ni0.22)Ni(H2O)2[BP2O8],0.67(H2O), which is isotypic with analogue nickel borophosphates A(I)M(H2O)2[BP2O8] H2O (A(I)=Li, Na, K, NH4+; M(II)=Mg, Mn, Fe, Co, Ni, Cu, Zn, Cd) (Zouihri et al., 2011; Menezes et al., 2008).

The anionic partial structure of the title compound contains one–dimensional infinite helices, [BP2O8]3–, which are wound around 65 axis. It is built up from alternate borate (BO4) and phosphate (PO4) tetrahedra, forming a spiral ribbon. The Ni2+ cation is six fold coordinated by four oxygen atoms originating from four phosphate groups and two water molecules as shown in Fig.1. The ribbons are interconnected through slightly distorted NiO4(H2O)2 octahedra. The resulting 3-D framework shows hexagonal tunnels running along c direction where water molecules are located (Fig.2).

The +I, +II, +III and +V oxidation states of the Ag, Ni, B and P atoms were confirmed by bond valence sum calculations (Brown & Altermatt, 1985). The calculated values for the Ag+, NiII+, BIII+ and PV+ ions are as expected, viz. 1.06, 1.89, 3.06 and 4.97, respectively.

The main difference between the structure of this compound and that of his counterpart AgMg(H2O)2[BP2O8],H2O lies in the filling ratio of the Wyckoff positions 6a and 6b in tunnels. Indeed, in this work, the refinement of the occupancy rate of the following sites (symmetry 2) 6a (x, 0, 0) and 6b (x, 2x, 3/4) (space group P6522) shows that the first is occupied by water at 67% and the second is partially occupied by 56.6% of Ag+ and 21.6% of Ni2+ for a total of 78%. While in the case of AgMg(H2O)2[BP2O8],H2O structure these two sites are completely occupied by H2O and Ag+ respectively.

The structure is stabilized by O—H···O hydrogen bonds between water molecules and O atoms that are part of the helices (Fig.1 and Table 1).

Related literature top

For the isotypic Mg analogue, see: Zouihri et al. (2011); Menezes et al. (2008). For similar other borophosphates, see: Kniep et al. (1998); Ewald et al. (2007); Lin et al. (2008). For bond valence calculations see: Brown & Altermatt, (1985).

Experimental top

The compound was hydrothermally synthesized at 453 K for 7 days in a 25 ml Teflon-lined steel autoclave from the mixture of NiCO3, H3BO3, H3PO4 (85%), AgNO3 and 5 mL of distilled water in the molar ratio of 1:4:6:1:165. The brilliant colourless octahedral crystals were recovered and washed with hot water, then dried in air.

Except for boron and hydrogen the presence of the elements were additionally confirmed by EDAX measurements.

Refinement top

The refinement with the sites of Ag and O6 fully occupied led to R = 0.06, Rw = 0.20 and two peaks in the Fourier difference map +4.7 and -3.4 at 0.18 Å from Ni and at 0.35 Å from Ag respectively. While the refinement of the occupancy rate of Ag(0.350 (2)) and O6(0.34 (1)) leads to R = 0.027, Rw = 0.07 and two peaks +1.21 and -0.66 at 0.65Å and 0.52Å from Ag. In the final refinement cycles, the occupancy of O6 was fixed to 0.667. However, the large atomic displacement parameter for this atom indicate disorder or atomic movement along the partially empty tunnel.

The electrical neutrality of the molecule led us to put some nickel in the site of Ag. The refinement of this model leads to the ratio Ag/Ni about 0.47. In the site occupied by a mixture of Ag+ and Ni2+, the cations are constrained to have the same positional and displacement parameters and the sum of the occupancy rate is restrained to fit the charge balance. The highest peak and the minimum peak in the difference map are at 0.66 Å and 0.52 Å respectively from Ag1 atom. The O-bound H atoms were initially located in a difference map and refined with O—H distance restraints of 0.86 (1). In the last cycles they were refined in the riding model approximation with Uiso(H) set to 1.5Ueq(O). The 779 Friedel opposite reflections are not merged.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (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
[Figure 1] Fig. 1. Partial plot of (Ag0.57Ni0.22)Ni(H2O)2[BP2O8],0.67(H2O) crystal structure showing plyhedra linkage. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (i) -y + 1, -x + 1, -z + 13/6; (ii) y - 1, -x + y, z + 1/6; (iii) y - 1, x, -z + 5/3; (iv) x, x-y + 1, -z + 11/6; (v) -x + y - 1, y, -z + 3/2; (vi) -x, -x + y, -z + 4/3; (vii) y, x + 1, -z + 5/3; (viii) x-y + 1, -y + 2, -z + 2.
[Figure 2] Fig. 2. Projection view of the (Ag0.57Ni0.22)Ni(H2O)2[BP2O8],0.67(H2O) framework structure showing tunnel running along c direction where water molecules are located.
Silver diaquanickel(II) catena-borodiphosphate(V) hydrate top
Crystal data top
(Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2ODx = 3.145 Mg m3
Mr = 381.35Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6522Cell parameters from 1912 reflections
Hall symbol: P 65 2 ( 0 0 1)θ = 3.6–36.9°
a = 9.3848 (6) ŵ = 4.69 mm1
c = 15.8411 (18) ÅT = 296 K
V = 1208.28 (18) Å3Prism, colourless
Z = 60.18 × 0.12 × 0.11 mm
F(000) = 1118
Data collection top
Bruker APEXII CCD detector
diffractometer
2043 independent reflections
Radiation source: fine-focus sealed tube1912 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ω and ϕ scansθmax = 36.9°, θmin = 3.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1999)
h = 1415
Tmin = 0.705, Tmax = 0.741k = 1315
16974 measured reflectionsl = 2526
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.071 w = 1/[σ2(Fo2) + (0.043P)2 + 0.3826P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
2043 reflectionsΔρmax = 1.23 e Å3
77 parametersΔρmin = 0.59 e Å3
1 restraintAbsolute structure: Flack (1983), 777 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.006 (15)
Crystal data top
(Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2OZ = 6
Mr = 381.35Mo Kα radiation
Hexagonal, P6522µ = 4.69 mm1
a = 9.3848 (6) ÅT = 296 K
c = 15.8411 (18) Å0.18 × 0.12 × 0.11 mm
V = 1208.28 (18) Å3
Data collection top
Bruker APEXII CCD detector
diffractometer
2043 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1999)
1912 reflections with I > 2σ(I)
Tmin = 0.705, Tmax = 0.741Rint = 0.037
16974 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.071Δρmax = 1.23 e Å3
S = 1.08Δρmin = 0.59 e Å3
2043 reflectionsAbsolute structure: Flack (1983), 777 Friedel pairs
77 parametersAbsolute structure parameter: 0.006 (15)
1 restraint
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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
xyzUiso*/UeqOcc. (<1)
Ag10.18588 (3)0.81412 (3)1.08330.03293 (14)0.567 (2)
Ni10.18588 (3)0.81412 (3)1.08330.03293 (14)0.2167 (12)
Ni20.10776 (4)0.553882 (19)0.91670.00726 (7)
P0.17053 (5)0.78027 (5)0.75196 (3)0.00600 (8)
B0.15242 (15)0.6952 (3)0.75000.0068 (4)
O10.13668 (19)0.61873 (17)0.79010 (8)0.0111 (2)
O20.31964 (17)0.93224 (18)0.78587 (8)0.0111 (2)
O30.02186 (17)0.80809 (17)0.76714 (8)0.0088 (2)
O40.18247 (16)0.76331 (16)0.65399 (8)0.0084 (2)
O50.29029 (19)0.79869 (19)0.94467 (10)0.0150 (3)
H5A0.37510.80660.96980.022*
H5B0.32900.85710.89970.022*
O60.1235 (7)1.00001.00000.135 (5)0.67
H6A0.12381.05241.04710.203*0.67
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0385 (2)0.0385 (2)0.0261 (2)0.0225 (2)0.00270 (16)0.00270 (16)
Ni10.0385 (2)0.0385 (2)0.0261 (2)0.0225 (2)0.00270 (16)0.00270 (16)
Ni20.00732 (13)0.00740 (10)0.00704 (11)0.00366 (6)0.0000.00101 (9)
P0.00595 (16)0.00698 (16)0.00472 (14)0.00296 (13)0.00006 (13)0.00092 (13)
B0.0085 (7)0.0070 (9)0.0046 (8)0.0035 (4)0.0006 (7)0.000
O10.0162 (6)0.0098 (5)0.0080 (5)0.0069 (5)0.0009 (4)0.0024 (4)
O20.0068 (5)0.0109 (6)0.0104 (5)0.0004 (4)0.0005 (4)0.0007 (4)
O30.0053 (5)0.0102 (5)0.0107 (5)0.0037 (4)0.0001 (4)0.0022 (4)
O40.0111 (5)0.0107 (5)0.0051 (4)0.0066 (5)0.0010 (4)0.0016 (4)
O50.0112 (6)0.0138 (6)0.0159 (6)0.0033 (5)0.0028 (5)0.0037 (5)
O60.045 (2)0.112 (7)0.271 (12)0.056 (3)0.077 (4)0.154 (8)
Geometric parameters (Å, º) top
Ag1—O52.4389 (17)Ni2—O52.1152 (16)
Ag1—O5i2.4389 (17)Ni2—O5ii2.1152 (16)
Ag1—O62.480 (4)P—O11.5108 (14)
Ag1—O6i2.480 (4)P—O21.5117 (15)
Ag1—O1ii2.6569 (15)P—O31.5611 (14)
Ag1—O1iii2.6569 (15)P—O41.5698 (13)
Ni2—O2iv2.0610 (14)B—O3vi1.462 (2)
Ni2—O2v2.0610 (14)B—O31.462 (2)
Ni2—O1ii2.0733 (13)B—O4vii1.477 (2)
Ni2—O12.0733 (13)B—O4iv1.477 (2)
O5—Ag1—O5i132.92 (8)O2v—Ni2—O5ii88.46 (7)
O5—Ag1—O678.79 (10)O1ii—Ni2—O5ii88.16 (6)
O5i—Ag1—O6147.60 (8)O1—Ni2—O5ii82.71 (6)
O5—Ag1—O6i147.60 (8)O5—Ni2—O5ii90.93 (10)
O5i—Ag1—O6i78.79 (10)O1—P—O2115.82 (8)
O6—Ag1—O6i71.1 (2)O1—P—O3110.43 (8)
O2iv—Ni2—O2v92.40 (9)O2—P—O3105.70 (8)
O2iv—Ni2—O1ii87.94 (5)O1—P—O4106.47 (7)
O2v—Ni2—O1ii101.12 (6)O2—P—O4111.57 (8)
O2iv—Ni2—O1101.12 (6)O3—P—O4106.52 (7)
O2v—Ni2—O187.94 (5)O3vi—B—O3102.25 (19)
O1ii—Ni2—O1166.98 (9)O3vi—B—O4vii112.61 (8)
O2iv—Ni2—O588.46 (7)O3—B—O4vii113.91 (7)
O2v—Ni2—O5176.10 (6)O3vi—B—O4iv113.91 (7)
O1ii—Ni2—O582.71 (6)O3—B—O4iv112.61 (8)
O1—Ni2—O588.16 (6)O4vii—B—O4iv102.02 (18)
O2iv—Ni2—O5ii176.10 (6)
Symmetry codes: (i) y+1, x+1, z+13/6; (ii) x, xy+1, z+11/6; (iii) x+y, x+1, z+1/3; (iv) y1, x+y, z+1/6; (v) y1, x, z+5/3; (vi) x+y1, y, z+3/2; (vii) x, x+y, z+4/3.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O4iii0.861.902.728 (2)161
O5—H5B···O20.861.952.762 (2)156
O6—H6A···O3viii0.892.182.819 (5)128
Symmetry codes: (iii) x+y, x+1, z+1/3; (viii) x, xy+2, z+11/6.

Experimental details

Crystal data
Chemical formula(Ag0.57Ni0.22)Ni(H2O)2[BP2O8]·0.67H2O
Mr381.35
Crystal system, space groupHexagonal, P6522
Temperature (K)296
a, c (Å)9.3848 (6), 15.8411 (18)
V3)1208.28 (18)
Z6
Radiation typeMo Kα
µ (mm1)4.69
Crystal size (mm)0.18 × 0.12 × 0.11
Data collection
DiffractometerBruker APEXII CCD detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1999)
Tmin, Tmax0.705, 0.741
No. of measured, independent and
observed [I > 2σ(I)] reflections
16974, 2043, 1912
Rint0.037
(sin θ/λ)max1)0.845
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.071, 1.08
No. of reflections2043
No. of parameters77
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.23, 0.59
Absolute structureFlack (1983), 777 Friedel pairs
Absolute structure parameter0.006 (15)

Computer programs: APEX2 (Bruker, 2005), SAINT (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···AD—HH···AD···AD—H···A
O5—H5A···O4i0.861.902.728 (2)160.7
O5—H5B···O20.861.952.762 (2)155.9
O6—H6A···O3ii0.892.182.819 (5)128.0
Symmetry codes: (i) x+y, x+1, z+1/3; (ii) x, xy+2, z+11/6.
 

Acknowledgements

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

References

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