Dilead(II) hydrogen­phosphite dinitrate

Ouarsal, R.; Lachkar, M.; Dušek, M.; Fejfarová, K.; El Bali, B.

doi:10.1107/S1600536809014469

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 5| May 2009| Page i35

doi:10.1107/S1600536809014469

Open

access

Dilead(II) hydrogenphosphite dinitrate

Rachid Ouarsal,^a Mohammed Lachkar,^a Michal Dušek,^b Karla Fejfarová ^b and Brahim El Bali ^c ^*

^aLaboratoire d'Ingénierie des Matériaux Organométalliques et Moléculaires, `LIMOM', Département de Chimie, Faculté des Sciences, BP 1796, Fès-Atlas, 30000 Fès, Morocco, ^bInstitute of Physics, Na Slovance 2, 182 21 Praha 8, Czech Republic, and ^cLaboratory of Mineral, Solid and Analytical Chemistry, `LCSMA', Department of Chemistry, Faculty of Sciences, University Mohamed I, PO Box 717, 60000 Oujda, Morocco
^*Correspondence e-mail: belbali@fso.ump.ma

(Received 14 April 2009; accepted 17 April 2009; online 25 April 2009)

In the title compound, Pb₂(HPO₃)(NO₃)₂, the two distinct Pb²⁺ ions (both with site symmetry m) adopt irregular PbO₁₀ coordination polyhedra. The structure is completed by two distinct nitrate groups (in which one O atom and the N atom have m site symmetry for both ions) and an HPO₃²⁻ anion (in which one O atom and the P and H atoms have m site symmetry). The connectivity of the PbO₁₀, NO₃ and HPO₃ units in the crystal structure results in a three-dimensional network.

Related literature

For related structures, see: Ouarsal et al. (2005a ,b ); Vasić et al. (1981 ). For bond-valence sum calculations, see: Brown & Altermatt (1985 ).

Experimental

Crystal data

Pb₂(HPO₃)(NO₃)₂
M_r = 618.4
Orthorhombic, P m n 2₁
a = 5.4069 (2) Å
b = 10.4079 (6) Å
c = 7.1958 (4) Å
V = 404.94 (4) Å³
Z = 2
Mo Kα radiation
μ = 41.76 mm⁻¹
T = 120 K
0.25 × 0.10 × 0.05 mm

Data collection

Oxford Diffraction CCD diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2005). CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.013, T_max = 0.156
6814 measured reflections
932 independent reflections
919 reflections with I > 3σ(I)
R_int = 0.026

Refinement

R[F² > 2σ(F²)] = 0.012
wR(F²) = 0.030
S = 1.25
932 reflections
78 parameters
1 restraint
Only H-atom coordinates refined
Δρ_max = 0.94 e Å⁻³
Δρ_min = −0.53 e Å⁻³
Absolute structure: Flack (1983 ), with 431 Friedel pairs
Flack parameter: 0.01 (1)

Table 1
Selected bond lengths (Å)

Pb1—O1	2.346 (6)
Pb1—O1ⁱ	3.042 (3)
Pb1—O3ⁱⁱ	2.418 (4)
Pb1—O4ⁱⁱⁱ	2.884 (4)
Pb1—O6^iv	2.881 (7)
Pb1—O6ⁱ	3.168 (4)
Pb2—O2^v	2.7756 (11)
Pb2—O3ⁱⁱ	2.513 (4)
Pb2—O4ⁱⁱ	2.707 (4)
Pb2—O5^vi	2.782 (4)
Pb2—O5^vii	2.948 (4)
Symmetry codes: (i) $[-x+{\script{3\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (ii) -x+1, y, z; (iii) $[x-{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (iv) x, y, z-1; (v) x+1, y+1, z; (vi) $[x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (vii) -x, y+1, z.

Data collection: CrysAlis CCD (Oxford Diffraction, 2005 $[Oxford Diffraction (2005). CrysAlis CCD. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2008 $[Oxford Diffraction (2005). CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SIR2002 (Burla et al., 2003 ); program(s) used to refine structure: JANA2006 (Petříček et al., 2006 ); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ); software used to prepare material for publication: JANA2006.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809014469/hb2952sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809014469/hb2952Isup2.hkl

checkCIF report

Comment top

As part of our ongoing structural stuides of metal hydrogenphosphites (Ouarsal et al. 2005a,b) we now report on the preparation and crystal structure of the title compound, (I).

The structure of (I) consists of two symmetry-independent nitrate groups and one HPO₃ hydrogenphosphite tetrahedron. The Pb atoms are located between them in two different crystallographic positions, both of them being irregularly coordinated by ten O atoms (Fig. 1). In the coordination of Pb1, shorter bonds occur causing larger bond valence sum (Brown & Altermatt, 1985) [2.028 (10) and 1.917 (6) for Pb(1)O₁₀ and Pb(2)O₁₀, respectively]. On the other hand, the mean Pb—O distance is rather larger in Pb(1)O₁₀ than in Pb(2)O₁₀, respectively 2.835 (5) Å and 2.745 (6) Å. These values are comparable to those reported in Pb(H₂PO₄)₂, 2.617 Å (Vasić et al., 1981). One can distinguish the two decahedrons by their respective coordination forms: one monodentate NO₃ and one monodentate HPO₃ occurs in the coordination of Pb1, while two bidentate NO₃ contribute to that of Pb2. Accordingly, the polyhedron Pb(1)O₁₀ turns to be more distorted as Pb(2)O₁₀.

Pb₂(HPO₃)(NO₃)₂ is characterized by a three-dimensional network. Although this is not a layer structure it is convenient from the explanatory point of view to distinguish two layers as indicated in Fig. 2. The slightly rotated view of a layer along [100] (Fig. 3) reveals strips extended in the c directions that are not interconnected within the same layer. Their connection in the b direction is mediated via the neighbouring layer which is shifted so that its Pb atoms fall into the holes. The shortest Pb—O bonds participate in the connection of the two PbO₁₀ units and in the bond towards the HPO₃ tetrahedron. As expected, H1 atom bonded to P is not involved in any hydrogen bonding. Average P—O distance and O—P—O and H—P—O angles are 1.531 (5) Å, 110.4 (2)° and 108.6 (2)° respectively. d_P—H = 1.20 (5) Å. These values lie in the same range as the ones previously reported in known phosphites (Ouarsal et al. 2005b).

Related literature top

For related structures, see: Ouarsal et al. (2005a,b); Vasić et al. (1981). For bond-valence sum calculations, see: Brown & Altermatt (1985).

Experimental top

1.6161 g lead nitrate Pb(NO₃)₂.6H₂O was dissolved in 6 ml of distilled water and added to a solution of 0.4 g phosphorous acid H₃PO₃, dissolved in 5 ml water. The mixture was stirred for 1 h at 333 K, after which time the precipitate obtained was filtered out of the solution. The filtrate was allowed to stand at room temperature until many large, colourless needles of (I) arose. The crystals were recovered by filtration and washed with a water–ethanol (80:20 v/v) mixture.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: JANA2006 (Petříček et al., 2006); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: JANA2006 (Petříček et al., 2006).

Figures top

	Fig. 1. A view of the asymmetric unit and some symmetry-related atoms of (I) showing 60% probability displacement ellipsoids. The various bonds lengths are distinguished by colours and style: indigo-thick up to 2.514 Å, yellow-thick from 2.707 Å to 3.042 Å, yellow-thin-dashed for 3.168 Å. [Symmetry codes: (i) x, y, -1 + z; (ii) 1/2 - x, 1 - y, -1/2 + z; (iii) 3/2 - x, 1 - y, -1/2 + z; (iv) -1/2 - x, 1 - y, -1/2 + z; (v) 1 - x, y, -1 + z; (vi) 1 + x, 1 + y, -1 + z; (vii) -x, 1 + y, -1 + z; (viii) x, 1 + y, -1 + z; (ix) 1/2 + x, 1 - y, -3/2 + z; (x) 1/2 - x, 1 - y, -3/2 + z]
	Fig. 2. A view of the structure of the title compound along [010]. The HPO₃ groups are indicated as pink tetraedra. The bonds to Pb are omitted for clarity. The black thick rectangles denote the layers that will be plotted in more details in Fig. 3.
	Fig. 3. The layers indicated in Fig. 2 in a view along the a direction. The first layer (grey, blue and red atoms) is plotted together with all coordinated O atoms. The various bonds lengths are distinguished by the same way as in Fig. 1.

Dilead(II) hydrogenphosphite dinitrate top

Crystal data top

Pb₂(HPO₃)(NO₃)₂	F(000) = 532
M_r = 618.4	D_x = 5.070 Mg m⁻³
Orthorhombic, Pmn2₁	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: P 2ac -2	Cell parameters from 6814 reflections
a = 5.4069 (2) Å	θ = 3.4–26.5°
b = 10.4079 (6) Å	µ = 41.76 mm⁻¹
c = 7.1958 (4) Å	T = 120 K
V = 404.94 (4) Å³	Plate, colourless
Z = 2	0.25 × 0.10 × 0.05 mm

Data collection top

Oxford Diffraction CCD diffractometer	932 independent reflections
Radiation source: X-ray tube	919 reflections with I > 3σ(I)
Graphite monochromator	R_int = 0.026
Detector resolution: 8.3438 pixels mm^-1	θ_max = 26.5°, θ_min = 3.4°
Rotation method data acquisition using ω scans	h = −6→6
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = −13→13
T_min = 0.013, T_max = 0.156	l = −9→9
6814 measured reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/[σ²(I) + 0.0004I²]
R[F² > 2σ(F²)] = 0.012	(Δ/σ)_max = 0.013
wR(F²) = 0.030	Δρ_max = 0.94 e Å⁻³
S = 1.25	Δρ_min = −0.53 e Å⁻³
932 reflections	Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
78 parameters	Extinction coefficient: 48 (5)
1 restraint	Absolute structure: Flack (1983), with 431 Friedel pairs
1 constraint	Absolute structure parameter: 0.01 (1)
Only H-atom coordinates refined

Crystal data top

Pb₂(HPO₃)(NO₃)₂	V = 404.94 (4) Å³
M_r = 618.4	Z = 2
Orthorhombic, Pmn2₁	Mo Kα radiation
a = 5.4069 (2) Å	µ = 41.76 mm⁻¹
b = 10.4079 (6) Å	T = 120 K
c = 7.1958 (4) Å	0.25 × 0.10 × 0.05 mm

Data collection top

Oxford Diffraction CCD diffractometer	932 independent reflections
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	919 reflections with I > 3σ(I)
T_min = 0.013, T_max = 0.156	R_int = 0.026
6814 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.012	Only H-atom coordinates refined
wR(F²) = 0.030	Δρ_max = 0.94 e Å⁻³
S = 1.25	Δρ_min = −0.53 e Å⁻³
932 reflections	Absolute structure: Flack (1983), with 431 Friedel pairs
78 parameters	Absolute structure parameter: 0.01 (1)
1 restraint

Special details top

Refinement. The refinement was carried out against all reflections. The conventional R-factor is always based on F. The goodness of fit as well as the weighted R-factor are based on F and F² for refinement carried out on F and F², respectively. The threshold expression is used only for calculating R-factors etc. and it is not relevant to the choice of reflections for refinement.

The program used for refinement, JANA2000, uses the weighting scheme based on the experimental expectations, see _refine_ls_weighting_details, that does not force S to be one. Therefore the values of S are usually larger then the ones from the SHELX program.

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

	x	y	z	U_iso*/U_eq
Pb1	0.5	0.47428 (2)	0.20948	0.01003 (7)
Pb2	0.5	0.84356 (2)	0.37011 (5)	0.01002 (8)
O1	0.5	0.4667 (5)	0.5354 (8)	0.0147 (15)
P1	0.5	0.34607 (15)	0.6573 (3)	0.0083 (5)
N1	0	−0.0035 (6)	0.4972 (8)	0.0103 (17)
O2	0	−0.0975 (5)	0.3893 (8)	0.0155 (14)
N2	0.5	0.7144 (6)	0.7547 (8)	0.0134 (18)
O3	0.2358 (7)	0.6561 (4)	0.2748 (5)	0.0109 (10)
O4	0.7011 (7)	0.7548 (3)	0.6898 (6)	0.0205 (11)
O5	−0.2007 (7)	0.0434 (3)	0.5539 (6)	0.0194 (11)
O6	0.5	0.6317 (6)	0.8801 (10)	0.033 (2)
H1	0.5	0.248 (4)	0.568 (10)	0.0099*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.00890 (14)	0.01098 (13)	0.01022 (12)	0	0	−0.00077 (12)
Pb2	0.00891 (15)	0.01137 (12)	0.00978 (12)	0	0	−0.00032 (9)
O1	0.012 (3)	0.020 (2)	0.013 (2)	0	0	0.002 (2)
P1	0.0048 (9)	0.0110 (8)	0.0091 (9)	0	0	0.0017 (5)
N1	0.011 (3)	0.013 (2)	0.007 (3)	0	0	0.000 (2)
O2	0.012 (3)	0.015 (2)	0.019 (2)	0	0	−0.006 (2)
N2	0.019 (4)	0.011 (3)	0.010 (3)	0	0	0.000 (2)
O3	0.0055 (18)	0.0151 (16)	0.0123 (17)	−0.0002 (15)	0.0003 (14)	−0.0033 (11)
O4	0.0123 (19)	0.0226 (16)	0.027 (2)	−0.0012 (15)	−0.0004 (16)	0.0012 (17)
O5	0.013 (2)	0.0235 (17)	0.0222 (16)	0.0054 (16)	0.0001 (18)	−0.0102 (17)
O6	0.049 (4)	0.030 (3)	0.019 (3)	0	0	0.015 (3)

Geometric parameters (Å, º) top

Pb1—O1	2.346 (6)	Pb2—O4ⁱⁱⁱ	2.707 (4)
Pb1—O1ⁱ	3.042 (3)	Pb2—O5^vii	2.948 (4)
Pb1—O1ⁱⁱ	3.042 (3)	Pb2—O5ⁱ	2.782 (4)
Pb1—O3	2.418 (4)	Pb2—O5^viii	2.782 (4)
Pb1—O3ⁱⁱⁱ	2.418 (4)	Pb2—O5^ix	2.948 (4)
Pb1—O4ⁱⁱ	2.884 (4)	P1—O1	1.532 (6)
Pb1—O4^iv	2.884 (4)	P1—O3^x	1.530 (4)
Pb1—O6^v	2.881 (7)	P1—O3^xi	1.530 (4)
Pb1—O6ⁱ	3.168 (4)	P1—H1	1.20 (5)
Pb1—O6ⁱⁱ	3.168 (4)	N1—O2	1.249 (8)
Pb2—O2^vi	2.7756 (11)	N1—O5	1.258 (5)
Pb2—O2^vii	2.7756 (11)	N1—O5^xii	1.258 (5)
Pb2—O3	2.513 (4)	N2—O4	1.255 (5)
Pb2—O3ⁱⁱⁱ	2.513 (4)	N2—O4ⁱⁱⁱ	1.255 (5)
Pb2—O4	2.707 (4)	N2—O6	1.247 (9)

O1—Pb1—O1ⁱ	114.73 (10)	O2^vii—Pb2—O5ⁱ	64.37 (14)
O1—Pb1—O1ⁱⁱ	114.73 (10)	O2^vii—Pb2—O5^viii	109.11 (14)
O1—Pb1—O3	80.31 (13)	O2^vii—Pb2—O5^ix	110.88 (13)
O1—Pb1—O3ⁱⁱⁱ	80.31 (13)	O3—Pb2—O3ⁱⁱⁱ	69.28 (12)
O1—Pb1—O4ⁱⁱ	91.22 (13)	O3—Pb2—O4	101.25 (12)
O1—Pb1—O4^iv	91.22 (13)	O3—Pb2—O4ⁱⁱⁱ	74.85 (12)
O1—Pb1—O6^v	147.26 (18)	O3—Pb2—O5^vii	169.07 (12)
O1—Pb1—O6ⁱ	66.48 (13)	O3—Pb2—O5ⁱ	109.08 (12)
O1—Pb1—O6ⁱⁱ	66.48 (13)	O3—Pb2—O5^viii	83.30 (11)
O1ⁱ—Pb1—O1ⁱⁱ	125.41 (13)	O3—Pb2—O5^ix	110.97 (11)
O1ⁱ—Pb1—O3	52.92 (13)	O3ⁱⁱⁱ—Pb2—O4	74.85 (12)
O1ⁱ—Pb1—O3ⁱⁱⁱ	116.57 (13)	O3ⁱⁱⁱ—Pb2—O4ⁱⁱⁱ	101.25 (12)
O1ⁱ—Pb1—O4ⁱⁱ	130.14 (13)	O3ⁱⁱⁱ—Pb2—O5^vii	110.97 (11)
O1ⁱ—Pb1—O4^iv	69.42 (12)	O3ⁱⁱⁱ—Pb2—O5ⁱ	83.30 (11)
O1ⁱ—Pb1—O6^v	63.03 (9)	O3ⁱⁱⁱ—Pb2—O5^viii	109.08 (12)
O1ⁱ—Pb1—O6ⁱ	58.09 (14)	O3ⁱⁱⁱ—Pb2—O5^ix	169.07 (12)
O1ⁱ—Pb1—O6ⁱⁱ	171.25 (15)	O4—Pb2—O4ⁱⁱⁱ	47.35 (12)
O1ⁱⁱ—Pb1—O3	116.57 (13)	O4—Pb2—O5^vii	68.85 (11)
O1ⁱⁱ—Pb1—O3ⁱⁱⁱ	52.92 (13)	O4—Pb2—O5ⁱ	133.06 (12)
O1ⁱⁱ—Pb1—O4ⁱⁱ	69.42 (12)	O4—Pb2—O5^viii	174.94 (11)
O1ⁱⁱ—Pb1—O4^iv	130.14 (13)	O4—Pb2—O5^ix	94.59 (12)
O1ⁱⁱ—Pb1—O6^v	63.03 (9)	O4ⁱⁱⁱ—Pb2—O5^vii	94.59 (12)
O1ⁱⁱ—Pb1—O6ⁱ	171.25 (15)	O4ⁱⁱⁱ—Pb2—O5ⁱ	174.94 (11)
O1ⁱⁱ—Pb1—O6ⁱⁱ	58.09 (14)	O4ⁱⁱⁱ—Pb2—O5^viii	133.06 (12)
O3—Pb1—O3ⁱⁱⁱ	72.44 (12)	O4ⁱⁱⁱ—Pb2—O5^ix	68.85 (11)
O3—Pb1—O4ⁱⁱ	171.11 (12)	O5^vii—Pb2—O5ⁱ	81.63 (12)
O3—Pb1—O4^iv	109.00 (12)	O5^vii—Pb2—O5^viii	106.42 (11)
O3—Pb1—O6^v	73.43 (14)	O5^vii—Pb2—O5^ix	66.57 (11)
O3—Pb1—O6ⁱ	72.12 (14)	O5ⁱ—Pb2—O5^viii	45.92 (11)
O3—Pb1—O6ⁱⁱ	134.56 (15)	O5ⁱ—Pb2—O5^ix	106.42 (11)
O3ⁱⁱⁱ—Pb1—O4ⁱⁱ	109.00 (12)	O5^viii—Pb2—O5^ix	81.63 (12)
O3ⁱⁱⁱ—Pb1—O4^iv	171.11 (12)	Pb1—O1—P1	126.8 (3)
O3ⁱⁱⁱ—Pb1—O6^v	73.43 (14)	O1—P1—O3^x	109.20 (18)
O3ⁱⁱⁱ—Pb1—O6ⁱ	134.56 (15)	O1—P1—O3^xi	109.20 (18)
O3ⁱⁱⁱ—Pb1—O6ⁱⁱ	72.12 (14)	O1—P1—H1	113 (3)
O4ⁱⁱ—Pb1—O4^iv	68.18 (11)	O3^x—P1—O3^xi	112.8 (2)
O4ⁱⁱ—Pb1—O6^v	115.45 (13)	O3^x—P1—H1	106.4 (16)
O4ⁱⁱ—Pb1—O6ⁱ	102.09 (13)	O3^xi—P1—H1	106.4 (16)
O4ⁱⁱ—Pb1—O6ⁱⁱ	41.64 (14)	O2—N1—O5	120.4 (3)
O4^iv—Pb1—O6^v	115.45 (13)	O2—N1—O5^xii	120.4 (3)
O4^iv—Pb1—O6ⁱ	41.64 (14)	O5—N1—O5^xii	119.3 (5)
O4^iv—Pb1—O6ⁱⁱ	102.09 (13)	Pb2^xiii—O2—Pb2^xiv	153.8 (2)
O6^v—Pb1—O6ⁱ	121.12 (11)	Pb2^xiii—O2—N1	101.78 (11)
O6^v—Pb1—O6ⁱⁱ	121.12 (11)	O4—N2—O4ⁱⁱⁱ	120.0 (5)
O6ⁱ—Pb1—O6ⁱⁱ	117.19 (15)	O4—N2—O6	120.0 (3)
O2^vi—Pb2—O2^vii	153.82 (14)	O4ⁱⁱⁱ—N2—O6	120.0 (3)
O2^vi—Pb2—O3	68.37 (13)	Pb1—O3—Pb2	108.96 (14)
O2^vi—Pb2—O3ⁱⁱⁱ	137.63 (13)	Pb1—O3—P1ⁱ	111.9 (2)
O2^vi—Pb2—O4	115.10 (14)	Pb2—O3—P1ⁱ	129.5 (2)
O2^vi—Pb2—O4ⁱⁱⁱ	69.02 (14)	Pb1^xv—O4—Pb2	123.29 (14)
O2^vi—Pb2—O5^vii	110.88 (13)	Pb1^xv—O4—N2	101.0 (3)
O2^vi—Pb2—O5ⁱ	109.11 (14)	Pb2—O4—N2	94.7 (3)
O2^vi—Pb2—O5^viii	64.37 (14)	Pb2^xiii—O5—Pb2^x	151.56 (16)
O2^vi—Pb2—O5^ix	44.54 (13)	Pb2^xiii—O5—N1	93.1 (3)
O2^vii—Pb2—O3	137.63 (13)	Pb2^x—O5—N1	95.3 (3)
O2^vii—Pb2—O3ⁱⁱⁱ	68.37 (13)	Pb1^xvi—O6—N2	171.0 (5)
O2^vii—Pb2—O4	69.02 (14)	Pb1^xvi—O6—O4	148.84 (17)
O2^vii—Pb2—O4ⁱⁱⁱ	115.10 (14)	Pb1^xvi—O6—O4ⁱⁱⁱ	148.84 (17)
O2^vii—Pb2—O5^vii	44.54 (13)

Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) −x+3/2, −y+1, z−1/2; (iii) −x+1, y, z; (iv) x−1/2, −y+1, z−1/2; (v) x, y, z−1; (vi) x, y+1, z; (vii) x+1, y+1, z; (viii) x+1/2, −y+1, z−1/2; (ix) −x, y+1, z; (x) −x+1/2, −y+1, z+1/2; (xi) x+1/2, −y+1, z+1/2; (xii) −x, y, z; (xiii) x−1, y−1, z; (xiv) x, y−1, z; (xv) −x+3/2, −y+1, z+1/2; (xvi) x, y, z+1.

Experimental details

Crystal data
Chemical formula	Pb₂(HPO₃)(NO₃)₂
M_r	618.4
Crystal system, space group	Orthorhombic, Pmn2₁
Temperature (K)	120
a, b, c (Å)	5.4069 (2), 10.4079 (6), 7.1958 (4)
V (Å³)	404.94 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	41.76
Crystal size (mm)	0.25 × 0.10 × 0.05

Data collection
Diffractometer	Oxford Diffraction CCD diffractometer
Absorption correction	Analytical (CrysAlis RED; Oxford Diffraction, 2008)
T_min, T_max	0.013, 0.156
No. of measured, independent and observed [I > 3σ(I)] reflections	6814, 932, 919
R_int	0.026
(sin θ/λ)_max (Å⁻¹)	0.628

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.012, 0.030, 1.25
No. of reflections	932
No. of parameters	78
No. of restraints	1
H-atom treatment	Only H-atom coordinates refined
Δρ_max, Δρ_min (e Å⁻³)	0.94, −0.53
Absolute structure	Flack (1983), with 431 Friedel pairs
Absolute structure parameter	0.01 (1)

Computer programs: CrysAlis CCD (Oxford Diffraction, 2005), CrysAlis RED (Oxford Diffraction, 2008), SIR97 (Altomare et al., 1999), JANA2006 (Petříček et al., 2006), DIAMOND (Brandenburg & Putz, 2005).

Selected bond lengths (Å) top

Pb1—O1	2.346 (6)	Pb2—O2^v	2.7756 (11)
Pb1—O1ⁱ	3.042 (3)	Pb2—O3ⁱⁱ	2.513 (4)
Pb1—O3ⁱⁱ	2.418 (4)	Pb2—O4ⁱⁱ	2.707 (4)
Pb1—O4ⁱⁱⁱ	2.884 (4)	Pb2—O5^vi	2.782 (4)
Pb1—O6^iv	2.881 (7)	Pb2—O5^vii	2.948 (4)
Pb1—O6ⁱ	3.168 (4)

Symmetry codes: (i) −x+3/2, −y+1, z−1/2; (ii) −x+1, y, z; (iii) x−1/2, −y+1, z−1/2; (iv) x, y, z−1; (v) x+1, y+1, z; (vi) x+1/2, −y+1, z−1/2; (vii) −x, y+1, z.

Acknowledgements

This work was supported by the Grant Agency of the Czech Republic (grant No. 202/06/0757).

References

Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247. CrossRef CAS Web of Science IUCr Journals Google Scholar
Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. CrossRef IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Ouarsal, R., El Bali, B., Lachkar, M., Dusek, M. & Fejfarova, K. (2005a). Acta Cryst. E61, i168–i170. Web of Science CrossRef IUCr Journals Google Scholar
Ouarsal, R., El Bali, B., Lachkar, M., Dusek, M. & Fejfarova, K. (2005b). Acta Cryst. E61, i171–i173. Web of Science CrossRef IUCr Journals Google Scholar
Oxford Diffraction (2005). CrysAlis CCD. Oxford Diffraction Ltd, Abingdon, England. Google Scholar
Oxford Diffraction (2005). CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England. Google Scholar
Petříček, V., Dušek, M. & Palatinus, L. (2006). JANA2006. Institute of Physics, Prague, Czech Republic. http://www-xray.fzu.cz/jana/jana.html Google Scholar
Vasić, P., Prelesnik, B., Herak, R. & Čurić, M. (1981). Acta Cryst. B37, 660–662. CrossRef Web of Science IUCr Journals Google Scholar