Dicobalt(II) lead(II) hydrogenphos­phate(V) phos­phate(V) hydroxide monohydrate

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

doi:10.1107/S1600536812014870

inorganic compounds

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ISSN: 2056-9890

Volume 68| Part 5| May 2012| Page i30

doi:10.1107/S1600536812014870

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Dicobalt(II) lead(II) hydrogenphosphate(V) phosphate(V) hydroxide monohydrate

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

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

(Received 21 March 2012; accepted 4 April 2012; online 18 April 2012)

The title compound, Co₂Pb(HPO₄)(PO₄)OH·H₂O, which was synthesized under hydrothermal conditions, crystallizes in a new structure type. Except for two O atoms in general positions and two Co atoms on centres of symmetry, all other atoms in the asymmetric unit (1 Pb, 2 Co, 2 P, 8 O and 4 H) are located on mirror planes. The structure is built up from two infinite linear chains, viz. ¹_∞[CoO_2/1(H₂O)_2/2O_2/2] and ¹_∞[CoO_2/1(OH)_2/2O_2/2], of edge-sharing CoO₆ octahedra running along [010]. Adjacent chains are linked to each other through PO₄ and PO₃(OH) tetrahedra, leading to the formation of layers parallel to (100). The three-dimensional framework is formed by stacking along [100] of adjacent layers that are held together by distorted PbO₈ polyhedra. Hydrogen bonds of the type O—H⋯O involving the water molecule are very strong, while those O atoms involving the OH groups form weak bifurcated and trifurcated hydrogen bonds.

Related literature

For catalytic properties of phosphates, see: Cheetham et al. (1999 ); Clearfield (1988 ); Trad et al. (2010 ). For compounds with related structures, see: Yakubovich et al. (2001 ); Lee et al. (2008 ); Effenberger (1999 ); Britvin et al. (2002 ); Assani et al. (2010 ). For bond-valence analysis, see: Brown & Altermatt (1985 ). For background to the Inorganic Crystal Structure Database (ICSD), see: Belsky et al. (2002 ).

Experimental

Crystal data

Co₂Pb(HPO₄)(PO₄)OH·H₂O
M_r = 551.02
Monoclinic, P 2₁ /m
a = 7.4299 (1) Å
b = 6.2949 (1) Å
c = 8.9057 (1) Å
β = 113.936 (1)°
V = 380.70 (1) Å³
Z = 2
Mo Kα radiation
μ = 26.83 mm⁻¹
T = 296 K
0.18 × 0.12 × 0.08 mm

Data collection

Bruker X8 APEXII diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1999 ) T_min = 0.029, T_max = 0.117
8321 measured reflections
1601 independent reflections
1558 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.016
wR(F²) = 0.039
S = 1.11
1601 reflections
86 parameters
H-atom parameters constrained
Δρ_max = 1.76 e Å⁻³
Δρ_min = −1.49 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2⋯O6ⁱ	0.86	2.28	3.027 (3)	145
O2—H2⋯O6ⁱⁱ	0.86	2.28	3.027 (3)	145
O7—H7⋯O2ⁱⁱⁱ	0.86	2.20	2.915 (3)	140
O7—H7⋯O3	0.86	2.53	2.986 (2)	114
O7—H7⋯O3^iv	0.86	2.53	2.986 (2)	114
O8—H8A⋯O4^v	0.86	1.79	2.649 (3)	177
O8—H8B⋯O7	0.86	1.65	2.489 (3)	165
Symmetry codes: (i) -x, -y, -z; (ii) $[-x, y-{\script{1\over 2}}, -z]$ ; (iii) -x, -y, -z+1; (iv) $[x, -y+{\script{1\over 2}}, z]$ ; (v) x-1, y, z.

Data collection: APEX2 (Bruker, 2005 ); cell refinement: SAINT (Bruker, 2005); 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: PLATON (Spek, 2009 ) and publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablock global. DOI: 10.1107/S1600536812014870/wm2609sup1.cif

checkCIF report

Comment top

Metal based phosphates are of great interest owing to either their remarkable diversity of structures or their properties and applications in catalysis, as ion-exchangers (Cheetham et al., 1999; Clearfield, 1988) or as positive electrode materials in lithium- and sodium-containing batteries (Trad et al., 2010)). Mainly, our focus of investigation is focused on orthophosphates with (mixed) divalent metals with general formula (M,M')₃(PO₄)₂^.nH₂O (Assani et al., 2010). It has been pointed out that the structural diversity of this family of compounds depends on the size difference of the divalent cations (Effenberger, 1999) and on the degree of hydratation (Yakubovich et al., 2001; Lee et al., 2008. The highest water content known up to date is realised for Mg₃(PO₄)₂^.22H₂O (Britvin et al., 2002). In this work, a new dicobalt lead phosphate(V)] with formula Co₂Pb(HPO₄)(PO₄)OH^.H₂O, was hydrothermally synthesized and structurally characterized.

A search in the ICSD (Belsky et al., 2002) reveals that the crystal structure of this phosphate represents a new structure type. A plot of the crystal structure illustrating the most important coordination polyhedra and their mutual connections is represented in Fig. 1. All atoms are in special positions, except two oxygen atoms (O3,O6) in general position of the P2₁/m space group. The crystal structure is built up from three different types of polyhedra more or less distorted, viz. two PbO₈ polyhedra (m symmetry), PO₄ and PO₃(OH) tetrahedra (both with m symmetry) and two CoO₆ octahedra (both with 1 symmetry). The CoO₆ octahedra share edges and form ¹_∞[Co(1)O_2/1(H₂O)_2/2O_2/2] and ¹_∞[Co(2)O_2/1(OH)_2/2O_2/2] chains running parallel to [010], as shown in Fig. 2. Adjacent chains are connected by PO₄ and HPO₄ tetrahedra via vertices, leading to the formation of layers parallel to (100). These layers are in turn linked by sheets of distorted PbO₈ polyhedra as also shown in Fig.2.

Bond valence sum calculations (Brown & Altermatt, 1985) for Pb1²⁺, Co1²⁺, Co2²⁺, P1⁵⁺ and P2⁵⁺ ions are as expected, viz. 1.92, 2.03, 1.93, 5.05 and 5.05 valence units, respectively. The values of the bond valence sums calculated for the oxygen atoms show low values for O2, O7 and O8 when the contribution of H atoms are not considered (i.e. 1.23, 0.88 and 0.75 valence units, respectively). Hence these O atoms are associated with protons and are involved in O—H···O hydrogen bonding (Table 1). H atoms of the water molecule form very strong hydrogen bonds, especially O8–H8B···O7 with an D···A distance less than 2.5 Å. The H atom of the OH^- group (O7) and the hydrogenphosphate group (O2) form weak bifurcated (O2) and trifurcated (O7) hydrogen bonds (Fig. 2, Table 1).

Related literature top

For catalytic properties of phosphates, see: Cheetham et al. (1999); Clearfield (1988); Trad et al. (2010). For compounds with related structures, see: Yakubovich et al. (2001); Lee et al. (2008); Effenberger (1999); Britvin et al. (2002); Assani et al. (2010). For bond-valence analysis, see: Brown & Altermatt (1985). For background to the Inorganic Crystal Structure Database (ICSD), see: Belsky et al. (2002).

Experimental top

The title compound, Co₂Pb(HPO₄)(PO₄)OH^.H₂O, was obtained from the hydrothermal treatment of a reaction mixture of Pb(NO₃)₂, metallic cobalt and 85_wt% phosphoric acid in the molar ratio Pb:Co:P = 1:3:3. The hydrothermal reaction was conducted in a 23 ml Teflon-lined autoclave under autogeneous pressure at 473 K for three days. The product was filtered off, washed with deionized water and air dried. The resulting product consists of pink crystals besides some pink powder.

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: PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Figures top

Fig. 1. A partial three-dimensional plot of the crystal structure of Co₂Pb(HPO₄)(PO₄)OH^.H₂O. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes:(i) -x, y + 1/2, -z; (ii) -x, -y, -z; (iii) x, -y + 1/2, z; (iv) -x, -y, -z + 1; (v) -x - 1, -y, -z; (vi) x + 1, y, z; (vii) -x, -y + 1, -z + 1; (viii) x + 1, -y + 1/2, z + 1; (ix) x + 1, y + 1, z; (x) x, -y - 1/2, z; (xi) x - 1, y - 1, z; (xii) -x, y - 1/2, -z + 1; (xiii) -x - 1, y + 1/2, -z;

Fig. 2. A three-dimensional polyhedral view of the crystal structure of Co₂Pb(HPO₄)(PO₄)OH^.H₂O, showing the stacking of layers along the [100] axis and the hydrogen bonding scheme (dashed lines).

Dicobalt(II) lead(II) hydrogenphosphate(V) phosphate(V) hydroxide monohydrate top

Crystal data top

Co₂Pb(HPO₄)(PO₄)OH·H₂O	F(000) = 500
M_r = 551.02	D_x = 4.807 Mg m⁻³
Monoclinic, P2₁/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 1601 reflections
a = 7.4299 (1) Å	θ = 2.5–33.5°
b = 6.2949 (1) Å	µ = 26.83 mm⁻¹
c = 8.9057 (1) Å	T = 296 K
β = 113.936 (1)°	Prism, pink
V = 380.70 (1) Å³	0.18 × 0.12 × 0.08 mm
Z = 2

Data collection top

Bruker X8 APEXII diffractometer	1601 independent reflections
Radiation source: fine-focus sealed tube	1558 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
ϕ and ω scans	θ_max = 33.5°, θ_min = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1999)	h = −9→11
T_min = 0.029, T_max = 0.117	k = −9→9
8321 measured reflections	l = −13→13

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.016	H-atom parameters constrained
wR(F²) = 0.039	w = 1/[σ²(F_o²) + (0.0153P)² + 0.885P] where P = (F_o² + 2F_c²)/3
S = 1.11	(Δ/σ)_max = 0.001
1601 reflections	Δρ_max = 1.76 e Å⁻³
86 parameters	Δρ_min = −1.49 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0061 (3)

Crystal data top

Co₂Pb(HPO₄)(PO₄)OH·H₂O	V = 380.70 (1) Å³
M_r = 551.02	Z = 2
Monoclinic, P2₁/m	Mo Kα radiation
a = 7.4299 (1) Å	µ = 26.83 mm⁻¹
b = 6.2949 (1) Å	T = 296 K
c = 8.9057 (1) Å	0.18 × 0.12 × 0.08 mm
β = 113.936 (1)°

Data collection top

Bruker X8 APEXII diffractometer	1601 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1999)	1558 reflections with I > 2σ(I)
T_min = 0.029, T_max = 0.117	R_int = 0.027
8321 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.016	0 restraints
wR(F²) = 0.039	H-atom parameters constrained
S = 1.11	Δρ_max = 1.76 e Å⁻³
1601 reflections	Δρ_min = −1.49 e Å⁻³
86 parameters

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 > 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

	x	y	z	U_iso*/U_eq
Pb1	0.006473 (17)	0.2500	0.232477 (15)	0.01414 (5)
Co1	−0.5000	0.0000	0.0000	0.00717 (8)
Co2	0.5000	0.5000	0.5000	0.00859 (8)
P1	−0.22391 (12)	−0.2500	0.32517 (9)	0.00646 (13)
P2	−0.21025 (11)	0.2500	−0.16270 (9)	0.00642 (13)
O1	−0.3205 (3)	−0.2500	0.4478 (3)	0.0088 (4)
O2	0.0058 (4)	−0.2500	0.4403 (3)	0.0145 (5)
H2	0.0642	−0.2500	0.3744	0.017*
O3	−0.2656 (2)	−0.0469 (3)	0.2228 (2)	0.0102 (3)
O4	0.0041 (4)	0.2500	−0.0355 (3)	0.0160 (5)
O5	−0.3411 (3)	0.2500	−0.0638 (3)	0.0096 (4)
O6	−0.2489 (3)	0.0525 (3)	−0.2742 (2)	0.0135 (3)
O7	−0.4341 (4)	0.2500	0.3936 (3)	0.0100 (4)
H7	−0.3197	0.2500	0.3910	0.012*
O8	−0.6059 (3)	0.2500	0.0885 (3)	0.0086 (4)
H8A	−0.7322	0.2500	0.0522	0.010*
H8B	−0.5660	0.2500	0.1937	0.010*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01157 (7)	0.02066 (8)	0.01059 (7)	0.000	0.00492 (4)	0.000
Co1	0.00890 (17)	0.00553 (19)	0.00703 (16)	0.00041 (14)	0.00319 (14)	0.00011 (13)
Co2	0.01066 (18)	0.0070 (2)	0.00765 (16)	−0.00114 (14)	0.00323 (14)	−0.00053 (13)
P1	0.0091 (3)	0.0062 (3)	0.0048 (3)	0.000	0.0035 (3)	0.000
P2	0.0068 (3)	0.0075 (3)	0.0052 (3)	0.000	0.0028 (2)	0.000
O1	0.0122 (10)	0.0082 (10)	0.0084 (9)	0.000	0.0067 (8)	0.000
O2	0.0080 (10)	0.0233 (14)	0.0106 (10)	0.000	0.0022 (8)	0.000
O3	0.0119 (7)	0.0090 (7)	0.0083 (6)	−0.0011 (6)	0.0027 (5)	0.0010 (6)
O4	0.0073 (10)	0.0287 (15)	0.0101 (10)	0.000	0.0016 (8)	0.000
O5	0.0110 (10)	0.0101 (10)	0.0105 (9)	0.000	0.0071 (8)	0.000
O6	0.0156 (8)	0.0124 (8)	0.0088 (6)	0.0056 (7)	0.0010 (6)	−0.0041 (6)
O7	0.0113 (10)	0.0130 (11)	0.0074 (9)	0.000	0.0055 (8)	0.000
O8	0.0097 (9)	0.0100 (10)	0.0072 (9)	0.000	0.0047 (8)	0.000

Geometric parameters (Å, º) top

Pb1—O4	2.380 (3)	P1—O1	1.531 (2)
Pb1—O6ⁱ	2.5429 (18)	P1—O2	1.595 (3)
Pb1—O6ⁱⁱ	2.5429 (18)	P2—O4	1.535 (3)
Pb1—O3	2.7284 (17)	P2—O6	1.5432 (18)
Pb1—O3ⁱⁱⁱ	2.7284 (17)	P2—O6ⁱⁱⁱ	1.5432 (18)
Pb1—O5	2.846 (2)	P2—O5	1.554 (2)
Pb1—O1^iv	2.857 (2)	O1—Co2^xi	2.2302 (16)
Pb1—O2^iv	2.952 (3)	O1—Co2^xii	2.2302 (16)
Co1—O8	2.0544 (14)	O1—Pb1^iv	2.857 (2)
Co1—O8^v	2.0544 (14)	O2—Pb1^iv	2.952 (3)
Co1—O3^v	2.0624 (16)	O2—H2	0.8600
Co1—O3	2.0624 (16)	O5—Co1^xiii	2.1766 (15)
Co1—O5	2.1766 (15)	O6—Co2^xiv	2.1426 (17)
Co1—O5^v	2.1766 (15)	O6—Pb1ⁱⁱ	2.5429 (18)
Co2—O7^vi	1.9978 (14)	O7—Co2^xv	1.9978 (14)
Co2—O7^vii	1.9978 (14)	O7—Co2^xii	1.9978 (14)
Co2—O6ⁱ	2.1426 (17)	O7—H7	0.8600
Co2—O6^viii	2.1426 (17)	O7—H8B	1.6474
Co2—O1^ix	2.2302 (16)	O8—Co1^xiii	2.0544 (14)
Co2—O1^iv	2.2302 (16)	O8—H8A	0.8600
P1—O3^x	1.5274 (18)	O8—H8B	0.8600
P1—O3	1.5274 (18)

O4—Pb1—O6ⁱ	82.12 (5)	O3^v—Co1—O5	88.92 (8)
O4—Pb1—O6ⁱⁱ	82.12 (5)	O3—Co1—O5	91.08 (8)
O6ⁱ—Pb1—O6ⁱⁱ	97.00 (9)	O8—Co1—O5^v	96.95 (6)
O4—Pb1—O3	105.34 (5)	O8^v—Co1—O5^v	83.05 (6)
O6ⁱ—Pb1—O3	171.63 (5)	O3^v—Co1—O5^v	91.08 (8)
O6ⁱⁱ—Pb1—O3	87.90 (7)	O3—Co1—O5^v	88.92 (8)
O4—Pb1—O3ⁱⁱⁱ	105.34 (5)	O5—Co1—O5^v	180.00 (12)
O6ⁱ—Pb1—O3ⁱⁱⁱ	87.90 (7)	O7^vi—Co2—O7^vii	180.0
O6ⁱⁱ—Pb1—O3ⁱⁱⁱ	171.63 (5)	O7^vi—Co2—O6ⁱ	87.93 (9)
O3—Pb1—O3ⁱⁱⁱ	86.46 (8)	O7^vii—Co2—O6ⁱ	92.07 (9)
O4—Pb1—O5	55.64 (7)	O7^vi—Co2—O6^viii	92.07 (9)
O6ⁱ—Pb1—O5	117.25 (4)	O7^vii—Co2—O6^viii	87.93 (9)
O6ⁱⁱ—Pb1—O5	117.25 (4)	O6ⁱ—Co2—O6^viii	180.0
O3—Pb1—O5	65.72 (4)	O7^vi—Co2—O1^ix	100.06 (7)
O3ⁱⁱⁱ—Pb1—O5	65.72 (4)	O7^vii—Co2—O1^ix	79.94 (7)
O4—Pb1—O1^iv	132.09 (7)	O6ⁱ—Co2—O1^ix	93.55 (8)
O6ⁱ—Pb1—O1^iv	67.09 (5)	O6^viii—Co2—O1^ix	86.45 (8)
O6ⁱⁱ—Pb1—O1^iv	67.09 (5)	O7^vi—Co2—O1^iv	79.94 (7)
O3—Pb1—O1^iv	109.06 (5)	O7^vii—Co2—O1^iv	100.06 (7)
O3ⁱⁱⁱ—Pb1—O1^iv	109.06 (5)	O6ⁱ—Co2—O1^iv	86.45 (8)
O5—Pb1—O1^iv	172.27 (6)	O6^viii—Co2—O1^iv	93.55 (8)
O4—Pb1—O2^iv	178.00 (7)	O1^ix—Co2—O1^iv	180.0
O6ⁱ—Pb1—O2^iv	99.18 (5)	O3^x—P1—O3	113.68 (14)
O6ⁱⁱ—Pb1—O2^iv	99.18 (5)	O3^x—P1—O1	112.68 (8)
O3—Pb1—O2^iv	73.26 (5)	O3—P1—O1	112.68 (8)
O3ⁱⁱⁱ—Pb1—O2^iv	73.26 (5)	O3^x—P1—O2	106.78 (8)
O5—Pb1—O2^iv	122.36 (7)	O3—P1—O2	106.78 (8)
O1^iv—Pb1—O2^iv	49.91 (6)	O1—P1—O2	103.32 (13)
O8—Co1—O8^v	180.00 (11)	O4—P2—O6	109.94 (9)
O8—Co1—O3^v	87.37 (8)	O4—P2—O6ⁱⁱⁱ	109.94 (9)
O8^v—Co1—O3^v	92.63 (8)	O6—P2—O6ⁱⁱⁱ	107.30 (15)
O8—Co1—O3	92.63 (8)	O4—P2—O5	106.40 (14)
O8^v—Co1—O3	87.37 (8)	O6—P2—O5	111.63 (9)
O3^v—Co1—O3	180.00 (13)	O6ⁱⁱⁱ—P2—O5	111.63 (9)
O8—Co1—O5	83.05 (6)	H8A—O8—H8B	104.5
O8^v—Co1—O5	96.95 (6)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O6ⁱⁱ	0.86	2.28	3.027 (3)	145
O2—H2···O6^xiv	0.86	2.28	3.027 (3)	145
O7—H7···O2^iv	0.86	2.20	2.915 (3)	140
O7—H7···O3	0.86	2.53	2.986 (2)	114
O7—H7···O3ⁱⁱⁱ	0.86	2.53	2.986 (2)	114
O8—H8A···O4^xv	0.86	1.79	2.649 (3)	177
O8—H8B···O7	0.86	1.65	2.489 (3)	165

Symmetry codes: (ii) −x, −y, −z; (iii) x, −y+1/2, z; (iv) −x, −y, −z+1; (xiv) −x, y−1/2, −z; (xv) x−1, y, z.

Experimental details

Crystal data
Chemical formula	Co₂Pb(HPO₄)(PO₄)OH·H₂O
M_r	551.02
Crystal system, space group	Monoclinic, P2₁/m
Temperature (K)	296
a, b, c (Å)	7.4299 (1), 6.2949 (1), 8.9057 (1)
β (°)	113.936 (1)
V (Å³)	380.70 (1)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	26.83
Crystal size (mm)	0.18 × 0.12 × 0.08

Data collection
Diffractometer	Bruker X8 APEXII diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1999)
T_min, T_max	0.029, 0.117
No. of measured, independent and observed [I > 2σ(I)] reflections	8321, 1601, 1558
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.777

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.016, 0.039, 1.11
No. of reflections	1601
No. of parameters	86
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.76, −1.49

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia,1997) and DIAMOND (Brandenburg, 2006), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O6ⁱ	0.86	2.28	3.027 (3)	144.7
O2—H2···O6ⁱⁱ	0.86	2.28	3.027 (3)	144.7
O7—H7···O2ⁱⁱⁱ	0.86	2.20	2.915 (3)	140.0
O7—H7···O3	0.86	2.53	2.986 (2)	114.4
O7—H7···O3^iv	0.86	2.53	2.986 (2)	114.4
O8—H8A···O4^v	0.86	1.79	2.649 (3)	176.6
O8—H8B···O7	0.86	1.65	2.489 (3)	165.4

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

Acknowledgements

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

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