Hydro-thermally synthesized α-Ba(2)P(2)O(7).

Single crystals of α-Ba(2)P(2)O(7), dibarium diphosphate, were obtained under hydro-thermal conditions. The structure belongs to the diphosphate A(2)P(2)O(7) series with A being an alkaline earth cation. α-Ba(2)P(2)O(7) crystallizes isotypically with α-Sr(2)P(2)O(7). All atomic sites have site symmetry m with the exception of two O atoms which reside on general positions. Both Ba(2+) cations are coordinated by nine terminal O atoms from eclipsed diphosphate P(2)O(7) anions to form a three-dimensional network throughout the structure.

Related literature

For general background, see: Brown & Calvo (1970 ▶); ElBelghitti et al. (1995 ▶); Mehdi et al. (1977 ▶); Mohri (2000 ▶). For the uses of alkaline earth diphosphates, see: McKeag & Steward (1955 ▶); Ranby et al. (1955 ▶); Ropp & Mooney (1960 ▶); Srivastava et al. (2003 ▶). For structurally related compounds, see: Calvo (1968 ▶); Barbier & Echard (1998 ▶). For an independent refinement of the α-Ba2P2O7 structure based on data from a crystal grown by solid-state reactions, see: Zakaria et al. (2010 ▶).

Experimental

Crystal data

Ba2P2O7

M = 448.62

Orthorhombic,

a = 9.2842 (19) Å

b = 5.6113 (11) Å

c = 13.796 (3) Å

V = 718.7 (3) Å3

Z = 4

Mo Kα radiation

μ = 11.32 mm−1

T = 298 K

0.45 × 0.15 × 0.15 mm

Data collection

Rigaku AFC-8S Mercury CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.080, T max = 0.281

7205 measured reflections

1854 independent reflections

1510 reflections with I > 2σ(I)

R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.047

wR(F 2) = 0.127

S = 1.11

1854 reflections

58 parameters

Δρmax = 6.71 e Å−3

Δρmin = −3.53 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2001 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810043527/wm2406sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810043527/wm2406Isup2.hkl

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

Ba2P2O7	F(000) = 792
Mr = 448.62	Dx = 4.146 Mg m−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 3690 reflections
a = 9.2842 (19) Å	θ = 2.7–36.3°
b = 5.6113 (11) Å	µ = 11.32 mm−1
c = 13.796 (3) Å	T = 298 K
V = 718.7 (3) Å3	Needle, colorless
Z = 4	0.45 × 0.15 × 0.15 mm

Rigaku AFC-8S Mercury CCD diffractometer	1854 independent reflections
Radiation source: sealed tube	1510 reflections with I > 2σ(I)
graphite	Rint = 0.042
Detector resolution: 14.6306 pixels mm-1	θmax = 36.3°, θmin = 2.6°
ω scans	h = −8→15
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −7→9
Tmin = 0.080, Tmax = 0.281	l = −21→22
7205 measured reflections

Refinement on F2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.047	Secondary atom site location: difference Fourier map
wR(F2) = 0.127	w = 1/[σ2(Fo2) + (0.0617P)2 + 4.9464P] where P = (Fo2 + 2Fc2)/3
S = 1.11	(Δ/σ)max = 0.001
1854 reflections	Δρmax = 6.71 e Å−3
58 parameters	Δρmin = −3.53 e Å−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
Ba1	0.86006 (5)	0.2500	0.41750 (3)	0.01365 (12)
Ba2	0.84160 (5)	0.2500	0.74453 (3)	0.01249 (12)
P1	1.2179 (2)	0.2500	0.45777 (12)	0.0120 (3)
P2	1.4529 (2)	0.2500	0.31494 (13)	0.0120 (3)
O1	1.1427 (4)	0.0289 (8)	0.4204 (3)	0.0163 (8)
O2	1.2271 (6)	0.2500	0.5677 (4)	0.0164 (10)
O3	1.3792 (6)	0.2500	0.4196 (3)	0.0118 (9)*
O4	1.4045 (4)	0.0278 (7)	0.2617 (3)	0.0154 (7)
O5	1.6144 (7)	0.2500	0.3326 (4)	0.0230 (12)

	U11	U22	U33	U12	U13	U23
Ba1	0.0139 (2)	0.0148 (2)	0.0122 (2)	0.000	−0.00132 (12)	0.000
Ba2	0.01179 (19)	0.0128 (2)	0.01293 (18)	0.000	0.00048 (12)	0.000
P1	0.0126 (7)	0.0131 (8)	0.0103 (6)	0.000	0.0008 (5)	0.000
P2	0.0105 (7)	0.0119 (7)	0.0138 (7)	0.000	0.0002 (5)	0.000
O1	0.0170 (18)	0.0134 (19)	0.0187 (18)	−0.0009 (14)	0.0018 (12)	0.0001 (13)
O2	0.018 (2)	0.018 (3)	0.013 (2)	0.000	−0.0009 (17)	0.000
O4	0.0149 (17)	0.0108 (17)	0.0205 (15)	−0.0033 (13)	0.0000 (13)	−0.0010 (13)
O5	0.011 (2)	0.037 (3)	0.022 (2)	0.000	0.001 (2)	0.000

Ba1—O5i	2.564 (6)	Ba2—O2viii	2.800 (5)
Ba1—O1ii	2.730 (4)	Ba2—O4ix	2.836 (4)
Ba1—O1iii	2.730 (4)	Ba2—O4x	2.836 (4)
Ba1—O4iv	2.799 (4)	Ba2—O5xi	3.084 (3)
Ba1—O4v	2.799 (4)	Ba2—O5x	3.084 (3)
Ba1—O1vi	2.903 (4)	P1—O1	1.514 (5)
Ba1—O1	2.903 (4)	P1—O1vi	1.514 (5)
Ba1—O2iii	2.9272 (18)	P1—O2	1.519 (6)
Ba1—O2vii	2.9272 (18)	P1—O3	1.588 (6)
Ba1—P2iv	3.320 (2)	P1—Ba1vii	3.3700 (11)
Ba1—P1	3.369 (2)	P1—Ba1iii	3.3700 (11)
Ba1—P1vii	3.3700 (11)	P2—O4	1.515 (4)
Ba2—O1iii	2.765 (4)	P2—O4vi	1.515 (4)
Ba2—O1ii	2.765 (4)	P2—O5	1.519 (6)
Ba2—O4iii	2.767 (4)	P2—O3	1.598 (5)
Ba2—O4ii	2.767 (4)
O5i—Ba1—O1ii	111.47 (14)	O2viii—Ba2—O4x	103.79 (13)
O5i—Ba1—O1iii	111.47 (14)	O4ix—Ba2—O4x	66.70 (16)
O1ii—Ba1—O1iii	69.95 (18)	O1iii—Ba2—O5xi	146.29 (14)
O5i—Ba1—O4iv	74.19 (15)	O1ii—Ba2—O5xi	78.59 (14)
O1ii—Ba1—O4iv	168.60 (12)	O4iii—Ba2—O5xi	129.35 (14)
O1iii—Ba1—O4iv	118.01 (12)	O4ii—Ba2—O5xi	66.99 (14)
O5i—Ba1—O4v	74.19 (15)	O2viii—Ba2—O5xi	71.70 (11)
O1ii—Ba1—O4v	118.01 (13)	O4ix—Ba2—O5xi	49.98 (14)
O1iii—Ba1—O4v	168.60 (12)	O4x—Ba2—O5xi	110.92 (14)
O4iv—Ba1—O4v	52.90 (17)	O1iii—Ba2—O5x	78.59 (14)
O5i—Ba1—O1vi	144.13 (12)	O1ii—Ba2—O5x	146.29 (14)
O1ii—Ba1—O1vi	75.66 (12)	O4iii—Ba2—O5x	66.99 (14)
O1iii—Ba1—O1vi	104.02 (8)	O4ii—Ba2—O5x	129.35 (14)
O4iv—Ba1—O1vi	93.97 (11)	O2viii—Ba2—O5x	71.70 (11)
O4v—Ba1—O1vi	71.85 (11)	O4ix—Ba2—O5x	110.92 (14)
O5i—Ba1—O1	144.13 (12)	O4x—Ba2—O5x	49.98 (14)
O1ii—Ba1—O1	104.02 (8)	O5xi—Ba2—O5x	130.9 (2)
O1iii—Ba1—O1	75.66 (12)	O1—P1—O1vi	110.0 (3)
O4iv—Ba1—O1	71.85 (11)	O1—P1—O2	111.48 (19)
O4v—Ba1—O1	93.97 (11)	O1vi—P1—O2	111.48 (19)
O1vi—Ba1—O1	50.61 (18)	O1—P1—O3	108.79 (19)
O5i—Ba1—O2iii	77.64 (11)	O1vi—P1—O3	108.79 (19)
O1ii—Ba1—O2iii	119.32 (14)	O2—P1—O3	106.1 (3)
O1iii—Ba1—O2iii	52.47 (14)	O4—P2—O4vi	110.7 (3)
O4iv—Ba1—O2iii	71.07 (13)	O4—P2—O5	111.7 (2)
O4v—Ba1—O2iii	121.96 (13)	O4vi—P2—O5	111.7 (2)
O1vi—Ba1—O2iii	131.20 (15)	O4—P2—O3	108.14 (19)
O1—Ba1—O2iii	80.75 (14)	O4vi—P2—O3	108.14 (19)
O5i—Ba1—O2vii	77.64 (11)	O5—P2—O3	106.1 (3)
O1ii—Ba1—O2vii	52.47 (14)	P1—O1—Ba1iii	101.23 (18)
O1iii—Ba1—O2vii	119.32 (14)	P1—O1—Ba2iii	136.0 (2)
O4iv—Ba1—O2vii	121.96 (13)	Ba1iii—O1—Ba2iii	110.49 (16)
O4v—Ba1—O2vii	71.07 (13)	P1—O1—Ba1	94.1 (2)
O1vi—Ba1—O2vii	80.75 (14)	Ba1iii—O1—Ba1	104.34 (12)
O1—Ba1—O2vii	131.20 (15)	Ba2iii—O1—Ba1	106.17 (13)
O2iii—Ba1—O2vii	146.9 (2)	P1—O2—Ba2xii	160.9 (4)
O1iii—Ba2—O1ii	68.95 (18)	P1—O2—Ba1iii	93.11 (12)
O1iii—Ba2—O4iii	72.50 (12)	Ba2xii—O2—Ba1iii	92.31 (11)
O1ii—Ba2—O4iii	109.70 (12)	P1—O2—Ba1vii	93.11 (12)
O1iii—Ba2—O4ii	109.70 (12)	Ba2xii—O2—Ba1vii	92.31 (11)
O1ii—Ba2—O4ii	72.50 (12)	Ba1iii—O2—Ba1vii	146.9 (2)
O4iii—Ba2—O4ii	68.58 (18)	P1—O3—P2	134.7 (4)
O1iii—Ba2—O2viii	141.37 (10)	P2—O4—Ba2iii	136.3 (2)
O1ii—Ba2—O2viii	141.37 (10)	P2—O4—Ba1xiii	96.06 (19)
O4iii—Ba2—O2viii	73.45 (13)	Ba2iii—O4—Ba1xiii	95.85 (12)
O4ii—Ba2—O2viii	73.45 (13)	P2—O4—Ba2xiv	104.2 (2)
O1iii—Ba2—O4ix	109.63 (12)	Ba2iii—O4—Ba2xiv	111.96 (14)
O1ii—Ba2—O4ix	73.36 (12)	Ba1xiii—O4—Ba2xiv	107.08 (13)
O4iii—Ba2—O4ix	176.88 (2)	P2—O5—Ba1xv	162.0 (4)
O4ii—Ba2—O4ix	112.28 (14)	P2—O5—Ba2xiv	93.88 (15)
O2viii—Ba2—O4ix	103.79 (13)	Ba1xv—O5—Ba2xiv	93.56 (13)
O1iii—Ba2—O4x	73.36 (12)	P2—O5—Ba2xvi	93.88 (15)
O1ii—Ba2—O4x	109.63 (12)	Ba1xv—O5—Ba2xvi	93.56 (13)
O4iii—Ba2—O4x	112.28 (14)	Ba2xiv—O5—Ba2xvi	130.9 (2)
O4ii—Ba2—O4x	176.88 (2)

Ba1—O5i	2.564 (6)
Ba1—O1ii	2.730 (4)
Ba1—O4iii	2.799 (4)
Ba1—O1	2.903 (4)
Ba1—O2iv	2.9272 (18)
Ba2—O1iv	2.765 (4)
Ba2—O4ii	2.767 (4)
Ba2—O2v	2.800 (5)
Ba2—O4vi	2.836 (4)
Ba2—O5vii	3.084 (3)
P1—O1	1.514 (5)
P1—O1viii	1.514 (5)
P1—O2	1.519 (6)
P1—O3	1.588 (6)
P2—O4	1.515 (4)
P2—O4viii	1.515 (4)
P2—O5	1.519 (6)
P2—O3	1.598 (5)

P1—O3—P2

134.7 (4)

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