Di-μ-aqua-bis­(μ-pyridazine-4-carboxyl­ato-κ2N:N′)bis­[triaqua­(pyridazine-4-carboxyl­ato-κ2O,O′)lead(II)] dihydrate

Starosta, W.; Leciejewicz, J.

doi:10.1107/S1600536809039658

metal-organic compounds

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Volume 65| Part 11| November 2009| Page m1291

https://doi.org/10.1107/S1600536809039658

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Di-μ-aqua-bis(μ-pyridazine-4-carboxylato-κ²N:N′)bis[triaqua(pyridazine-4-carboxylato-κ²O,O′)lead(II)] dihydrate

Wojciech Starosta ^a and Janusz Leciejewicz ^a ^*

^aInstitute of Nuclear Chemistry and Technology, ul.Dorodna 16, 03-195 Warszawa, Poland
^*Correspondence e-mail: j.leciejewicz@ichtj.waw.pl

(Received 5 August 2009; accepted 29 September 2009; online 3 October 2009)

The structure of the title compound, [Pb₂(C₅H₃N₂O₂)₄(H₂O)₆]·2H₂O, is composed of dimeric molecules in which two symmetry-related Pb²⁺ ions are bridged by a pair of two pyridazine-4-carboxylate ligand molecules via both heterocyclic N atoms and two water O atoms. Each Pb²⁺ ion is also coordinated by two carboxylate O atoms and three water O atoms, leading to a highly irregular coordination polyhedron around Pb²⁺. The dimers are interconnected by hydrogen bonds between coordinated and uncoordinated water molecules and the carboxylate O atoms. O—H⋯N interactions are also present.

Related literature

For the crystal structure of pyridazine-4-carboxylic acid hydrochloride, see: Starosta & Leciejewicz (2008 ). Centrosymmetric dimeric molecules were reported in the structure of a calcium(II) complex with pyridazine-3-dicarboxylate and water ligands (Starosta & Leciejewicz, 2007 ) and an uranyl complex with the same ligands (Leciejewicz & Starosta, (2009 ). Each dimer shows a different bridging mode.

Experimental

Crystal data

[Pb₂(C₅H₃N₂O₂)₄(H₂O)₆]·2H₂O
M_r = 1086.92
Triclinic, $[P \overline 1]$
a = 7.0762 (14) Å
b = 9.2967 (19) Å
c = 12.830 (3) Å
α = 92.05 (3)°
β = 105.13 (3)°
γ = 102.85 (3)°
V = 790.4 (3) Å³
Z = 1
Mo Kα radiation
μ = 10.73 mm⁻¹
T = 293 K
0.35 × 0.18 × 0.03 mm

Data collection

Kuma KM-4 four-circle diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ) T_min = 0.254, T_max = 0.762
4862 measured reflections
4512 independent reflections
3958 reflections with I > 2σ(I)
R_int = 0.016
3 standard reflections every 200 reflections intensity decay: 1.2%

Refinement

R[F² > 2σ(F²)] = 0.045
wR(F²) = 0.122
S = 1.06
4512 reflections
253 parameters
15 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 5.63 e Å⁻³
Δρ_min = −3.77 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H41⋯O12ⁱ	0.86 (2)	1.93 (2)	2.736 (6)	154 (4)
O4—H42⋯O12ⁱⁱ	0.87 (2)	1.92 (4)	2.754 (6)	161 (11)
O1—H11⋯O5	0.86 (2)	2.08 (3)	2.943 (9)	174 (10)
O1—H12⋯O11ⁱⁱⁱ	0.86 (2)	2.09 (6)	2.849 (7)	146 (9)
O5—H51⋯N22^iv	0.86 (2)	2.23 (5)	3.013 (8)	151 (9)
O5—H52⋯O21^v	0.87 (2)	2.12 (6)	2.897 (8)	149 (10)
O3—H31⋯O12^vi	0.86 (2)	2.09 (7)	2.819 (7)	142 (10)
O3—H32⋯N21^iv	0.86 (2)	2.01 (6)	2.794 (7)	151 (10)
O2—H21⋯O5^vii	0.86 (2)	2.13 (5)	2.906 (8)	150 (9)
O2—H22⋯O11ⁱⁱ	0.86 (2)	2.07 (4)	2.891 (7)	159 (9)
Symmetry codes: (i) -x, -y+1, -z+1; (ii) x-1, y-1, z; (iii) x, y-1, z; (iv) -x+1, -y+1, -z+2; (v) -x+1, -y, -z+2; (vi) -x+1, -y+1, -z+1; (vii) x-1, y, z.

Data collection: KM-4 Software (Kuma, 1996 $[Kuma (1996). KM-4 Software. Kuma Diffraction Ltd, Wrocław, Poland.]$ ); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 $[Kuma (2001). DATAPROC. Kuma Diffraction Ltd, Wrocław, Poland.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536809039658/bv2128sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809039658/bv2128Isup2.hkl

checkCIF report

Comment top

The structure of the title compound (I) is built of dimeric molecules (Fig.1) in which two symmetry related, nine-coordinate Pb²⁺ ions are chelated by two pairs of pyridazine-4-carboxylate anions via their both hetero-ring atoms, each pair showing different chelating mode: one uses both its hetero-ring N atoms to bridge the metal ions, its deprotonated carboxylate O atoms are left inactive in coordination, the other coordinates the Pb²⁺ions only via carboxylate groups which act as bidentate. In addition, the Pb²⁺ ions are bridged by a pair of water molecules. Three coordinated water O atoms complete the coordination enviroment of Pb²⁺ ions. The coordination geometry around a metal ion is highly irregular. Pyridazine rings are planar with r.m.s. 0.0081 (2)Å (ligand 1) and 0.0030 (2)Å (ligand 2). The coordinated (C27/O21/O22) and non-coordinated (C17/O11/O12) carboxylic groups make dihedral angles of 5.6 (1)° and 11.9 (1)° with their respective pyridazine rings. A packing diagram of (I) displayed in Fig.2 shows how the dimers are linked by a network of hydrogen bonds. Their relevant geometrical parameters are listed in Table 1.

Related literature top

For the crystal structure of pyridazine-4-carboxylic acid hydrochloride, see: Starosta & Leciejewicz, (2008). Centrosymmetric dimeric molecules were reported in the structure of a calcium(II) complex with pyridazine-3-dicarboxylate and water ligands (Starosta & Leciejewicz, 2007) and an uranyl complex with the same ligands (Leciejewicz & Starosta, (2009). Each dimer shows a different bridging mode.

Experimental top

2 Mmol of pyridazine-4-carboxylic acid were dissolved in 100 ml of hot water and boiled for two hours with small excess of Pb(OH)₂. After cooling to room temperature the mixture was filtered and left to crystallize. Few days later colorless single crystals were found in the mother liquid. They were separated, washed with cold ethanol and dried in air.

Structure description top

# Used for convenience to store draft or replaced versions # of the abstract, comment etc. # Its contents will not be output

#==============================================================================

Computing details top

Data collection: KM-4 Software (Kuma, 1996); cell refinement: KM-4 Software (Kuma, 1996); data reduction: DATAPROC (Kuma,2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. A dimer of (1) with atom labelling scheme and 50% probability displacement ellipsoids.
	Fig. 2. Packing diagram of the structure.

Di-µ-aqua-bis(µ-pyridazine-4-carboxylato- κ²N:N')bis[triaqua(pyridazine-4-carboxylato- κ²O,O')lead(II)] dihydrate top

Crystal data top

[Pb₂(C₅H₃N₂O₂)₄(H₂O)₆]·2H₂O	Z = 1
M_r = 1086.92	F(000) = 516
Triclinic, P1	D_x = 2.283 Mg m⁻³
a = 7.0762 (14) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.2967 (19) Å	Cell parameters from 25 reflections
c = 12.830 (3) Å	θ = 6–15°
α = 92.05 (3)°	µ = 10.73 mm⁻¹
β = 105.13 (3)°	T = 293 K
γ = 102.85 (3)°	Plate, colourless
V = 790.4 (3) Å³	0.35 × 0.18 × 0.03 mm

Data collection top

Kuma KM-4 four-circle diffractometer	3958 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 30.2°, θ_min = 1.7°
Profile data from ω/2θ scans	h = 0→9
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = −13→12
T_min = 0.254, T_max = 0.762	l = −18→16
4862 measured reflections	3 standard reflections every 200 reflections
4512 independent reflections	intensity decay: 1.2%

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.122	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.1029P)²] where P = (F_o² + 2F_c²)/3
4512 reflections	(Δ/σ)_max = 0.002
253 parameters	Δρ_max = 5.63 e Å⁻³
15 restraints	Δρ_min = −3.77 e Å⁻³

Crystal data top

[Pb₂(C₅H₃N₂O₂)₄(H₂O)₆]·2H₂O	γ = 102.85 (3)°
M_r = 1086.92	V = 790.4 (3) Å³
Triclinic, P1	Z = 1
a = 7.0762 (14) Å	Mo Kα radiation
b = 9.2967 (19) Å	µ = 10.73 mm⁻¹
c = 12.830 (3) Å	T = 293 K
α = 92.05 (3)°	0.35 × 0.18 × 0.03 mm
β = 105.13 (3)°

Data collection top

Kuma KM-4 four-circle diffractometer	3958 reflections with I > 2σ(I)
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	R_int = 0.016
T_min = 0.254, T_max = 0.762	3 standard reflections every 200 reflections
4862 measured reflections	intensity decay: 1.2%
4512 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.045	15 restraints
wR(F²) = 0.122	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 5.63 e Å⁻³
4512 reflections	Δρ_min = −3.77 e Å⁻³
253 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 > 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.

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

	x	y	z	U_iso*/U_eq
Pb1	0.11555 (3)	0.048890 (18)	0.675973 (14)	0.02300 (9)
O11	0.4666 (8)	0.6974 (5)	0.6607 (4)	0.0360 (10)
O4	−0.2317 (7)	0.0086 (5)	0.5150 (4)	0.0309 (9)
O21	0.2153 (8)	0.1496 (5)	0.8788 (4)	0.0387 (11)
O1	0.3206 (8)	−0.1283 (6)	0.7946 (4)	0.0395 (11)
H11	0.430 (8)	−0.075 (11)	0.838 (5)	0.047*
H12	0.347 (11)	−0.155 (10)	0.736 (4)	0.047*
N12	0.1246 (8)	0.2794 (5)	0.5304 (4)	0.0265 (9)
N11	0.0425 (8)	0.2525 (5)	0.4237 (4)	0.0280 (10)
O22	0.0922 (10)	0.3005 (6)	0.7692 (4)	0.0452 (13)
O12	0.4408 (7)	0.7751 (4)	0.4972 (4)	0.0331 (9)
C17	0.4044 (8)	0.6811 (6)	0.5601 (5)	0.0247 (10)
C14	0.2716 (7)	0.5309 (5)	0.5091 (4)	0.0208 (9)
C13	0.2351 (9)	0.4143 (6)	0.5710 (5)	0.0249 (10)
H13	0.2916	0.4317	0.6458	0.030*
C15	0.1807 (9)	0.5029 (6)	0.3995 (5)	0.0273 (11)
H15	0.1940	0.5769	0.3532	0.033*
C16	0.0682 (10)	0.3600 (7)	0.3606 (5)	0.0309 (12)
H16	0.0079	0.3389	0.2863	0.037*
C24	0.2220 (9)	0.3860 (6)	0.9548 (5)	0.0273 (11)
C27	0.1684 (10)	0.2701 (6)	0.8588 (5)	0.0297 (11)
O5	0.7080 (10)	0.0331 (7)	0.9439 (4)	0.0471 (13)
H51	0.753 (16)	0.123 (4)	0.975 (6)	0.057*
H52	0.682 (16)	−0.024 (7)	0.993 (5)	0.057*
N21	0.3150 (10)	0.6062 (7)	1.1197 (5)	0.0385 (13)
N22	0.2595 (11)	0.6394 (6)	1.0184 (6)	0.0391 (13)
C25	0.2804 (11)	0.3556 (7)	1.0582 (5)	0.0342 (13)
H23	0.2907	0.2606	1.0748	0.041*
C23	0.2131 (11)	0.5332 (7)	0.9376 (5)	0.0325 (12)
H25	0.1731	0.5571	0.8667	0.039*
C26	0.3247 (13)	0.4707 (9)	1.1396 (6)	0.0396 (15)
H26	0.3631	0.4503	1.2115	0.048*
O3	0.4919 (9)	0.1749 (7)	0.7070 (4)	0.0449 (12)
O2	−0.1694 (9)	−0.0786 (7)	0.7638 (5)	0.0490 (14)
H41	−0.277 (8)	0.082 (6)	0.533 (5)	0.07 (3)*
H42	−0.316 (12)	−0.072 (6)	0.521 (10)	0.07 (3)*
H31	0.529 (18)	0.231 (10)	0.661 (6)	0.07 (4)*
H32	0.557 (16)	0.215 (11)	0.771 (3)	0.08 (4)*
H21	−0.172 (17)	−0.018 (9)	0.815 (6)	0.05 (3)*
H22	−0.259 (10)	−0.160 (6)	0.740 (7)	0.04 (2)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02442 (13)	0.01967 (12)	0.02294 (13)	0.00112 (8)	0.00730 (9)	−0.00286 (7)
O11	0.040 (2)	0.026 (2)	0.032 (2)	−0.0024 (18)	0.0027 (19)	−0.0031 (17)
O4	0.029 (2)	0.0177 (18)	0.044 (3)	0.0019 (15)	0.0105 (19)	0.0037 (16)
O21	0.049 (3)	0.029 (2)	0.035 (2)	0.010 (2)	0.008 (2)	−0.0061 (18)
O1	0.041 (3)	0.039 (3)	0.039 (3)	0.012 (2)	0.010 (2)	−0.003 (2)
N12	0.031 (2)	0.0161 (19)	0.032 (2)	0.0016 (17)	0.012 (2)	0.0006 (17)
N11	0.032 (2)	0.0169 (19)	0.032 (2)	0.0005 (17)	0.009 (2)	−0.0032 (17)
O22	0.069 (4)	0.039 (3)	0.025 (2)	0.016 (3)	0.007 (2)	−0.0038 (19)
O12	0.036 (2)	0.0166 (17)	0.046 (3)	−0.0025 (16)	0.016 (2)	0.0023 (16)
C17	0.022 (2)	0.015 (2)	0.036 (3)	0.0028 (17)	0.009 (2)	−0.0044 (18)
C14	0.019 (2)	0.0133 (19)	0.031 (3)	0.0033 (16)	0.0100 (19)	−0.0011 (17)
C13	0.025 (2)	0.020 (2)	0.028 (3)	0.0035 (19)	0.006 (2)	0.0020 (19)
C15	0.030 (3)	0.019 (2)	0.033 (3)	0.003 (2)	0.010 (2)	0.006 (2)
C16	0.032 (3)	0.024 (3)	0.030 (3)	0.000 (2)	0.003 (2)	−0.002 (2)
C24	0.032 (3)	0.023 (2)	0.026 (3)	0.005 (2)	0.007 (2)	−0.0055 (19)
C27	0.038 (3)	0.024 (2)	0.027 (3)	0.004 (2)	0.011 (2)	−0.006 (2)
O5	0.064 (4)	0.042 (3)	0.039 (3)	0.016 (3)	0.017 (3)	0.001 (2)
N21	0.040 (3)	0.037 (3)	0.034 (3)	0.004 (2)	0.009 (2)	−0.013 (2)
N22	0.048 (3)	0.025 (2)	0.042 (3)	0.009 (2)	0.010 (3)	−0.005 (2)
C25	0.048 (4)	0.031 (3)	0.025 (3)	0.013 (3)	0.012 (3)	0.001 (2)
C23	0.044 (3)	0.028 (3)	0.027 (3)	0.013 (2)	0.009 (2)	0.003 (2)
C26	0.052 (4)	0.042 (4)	0.024 (3)	0.010 (3)	0.009 (3)	−0.006 (2)
O3	0.043 (3)	0.051 (3)	0.025 (2)	−0.016 (2)	0.008 (2)	−0.007 (2)
O2	0.045 (3)	0.053 (3)	0.042 (3)	−0.012 (2)	0.023 (2)	−0.011 (2)

Geometric parameters (Å, º) top

Pb1—O3	2.578 (6)	C13—H13	0.9300
Pb1—O21	2.593 (5)	C15—C16	1.386 (8)
Pb1—O2	2.638 (6)	C15—H15	0.9300
Pb1—O22	2.647 (5)	C16—H16	0.9300
Pb1—O1	2.688 (6)	C24—C25	1.343 (9)
Pb1—O4	2.707 (5)	C24—C23	1.406 (8)
O11—C17	1.242 (8)	C24—C27	1.517 (8)
O4—H41	0.86 (2)	O5—H51	0.86 (2)
O4—H42	0.87 (2)	O5—H52	0.87 (2)
O21—C27	1.254 (8)	N21—C26	1.308 (10)
O1—H11	0.86 (2)	N21—N22	1.324 (10)
O1—H12	0.86 (2)	N22—C23	1.328 (8)
N12—C13	1.327 (7)	C25—C26	1.390 (9)
N12—N11	1.331 (7)	C25—H23	0.9300
N11—C16	1.320 (8)	C23—H25	0.9300
O22—C27	1.208 (8)	C26—H26	0.9300
O12—C17	1.241 (7)	O3—H31	0.86 (2)
C17—C14	1.514 (7)	O3—H32	0.86 (2)
C14—C15	1.373 (8)	O2—H21	0.86 (2)
C14—C13	1.385 (7)	O2—H22	0.86 (2)

O3—Pb1—O21	79.05 (17)	N12—C13—H13	118.0
O3—Pb1—O2	146.72 (18)	C14—C13—H13	118.0
O21—Pb1—O2	70.88 (18)	C14—C15—C16	117.4 (5)
O3—Pb1—O22	85.5 (2)	C14—C15—H15	121.3
O21—Pb1—O22	49.16 (16)	C16—C15—H15	121.3
O2—Pb1—O22	85.5 (2)	N11—C16—C15	123.2 (6)
O3—Pb1—O1	74.2 (2)	N11—C16—H16	118.4
O21—Pb1—O1	71.28 (16)	C15—C16—H16	118.4
O2—Pb1—O1	82.8 (2)	C25—C24—C23	117.0 (5)
O22—Pb1—O1	119.77 (16)	C25—C24—C27	123.0 (6)
O3—Pb1—O4	137.65 (16)	C23—C24—C27	120.1 (6)
O21—Pb1—O4	132.46 (16)	O22—C27—O21	124.6 (6)
O2—Pb1—O4	75.25 (18)	O22—C27—C24	119.1 (6)
O22—Pb1—O4	96.49 (16)	O21—C27—C24	116.3 (6)
O1—Pb1—O4	135.76 (15)	H51—O5—H52	107 (3)
Pb1—O4—H41	100.9 (17)	C26—N21—N22	120.3 (6)
Pb1—O4—H42	110 (8)	N21—N22—C23	119.1 (6)
H41—O4—H42	107 (3)	C24—C25—C26	117.9 (6)
C27—O21—Pb1	93.8 (4)	C24—C25—H23	121.1
Pb1—O1—H11	110 (8)	C26—C25—H23	121.1
Pb1—O1—H12	87 (7)	N22—C23—C24	122.7 (6)
H11—O1—H12	109 (3)	N22—C23—H25	118.7
C13—N12—N11	118.9 (5)	C24—C23—H25	118.7
C16—N11—N12	119.9 (5)	N21—C26—C25	123.0 (7)
C27—O22—Pb1	92.3 (4)	N21—C26—H26	118.5
O12—C17—O11	126.7 (5)	C25—C26—H26	118.5
O12—C17—C14	116.7 (5)	Pb1—O3—H31	120 (8)
O11—C17—C14	116.6 (5)	Pb1—O3—H32	117 (8)
C15—C14—C13	116.5 (5)	H31—O3—H32	109 (4)
C15—C14—C17	122.0 (5)	Pb1—O2—H21	108 (7)
C13—C14—C17	121.5 (5)	Pb1—O2—H22	127 (6)
N12—C13—C14	124.0 (5)	H21—O2—H22	124 (10)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4—H41···O12ⁱ	0.86 (2)	1.93 (2)	2.736 (6)	154 (4)
O4—H42···O12ⁱⁱ	0.87 (2)	1.92 (4)	2.754 (6)	161 (11)
O1—H11···O5	0.86 (2)	2.08 (3)	2.943 (9)	174 (10)
O1—H12···O11ⁱⁱⁱ	0.86 (2)	2.09 (6)	2.849 (7)	146 (9)
O5—H51···N22^iv	0.86 (2)	2.23 (5)	3.013 (8)	151 (9)
O5—H52···O21^v	0.87 (2)	2.12 (6)	2.897 (8)	149 (10)
O3—H31···O12^vi	0.86 (2)	2.09 (7)	2.819 (7)	142 (10)
O3—H32···N21^iv	0.86 (2)	2.01 (6)	2.794 (7)	151 (10)
O2—H21···O5^vii	0.86 (2)	2.13 (5)	2.906 (8)	150 (9)
O2—H22···O11ⁱⁱ	0.86 (2)	2.07 (4)	2.891 (7)	159 (9)

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

Experimental details

Crystal data
Chemical formula	[Pb₂(C₅H₃N₂O₂)₄(H₂O)₆]·2H₂O
M_r	1086.92
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	7.0762 (14), 9.2967 (19), 12.830 (3)
α, β, γ (°)	92.05 (3), 105.13 (3), 102.85 (3)
V (Å³)	790.4 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	10.73
Crystal size (mm)	0.35 × 0.18 × 0.03

Data collection
Diffractometer	Kuma KM-4 four-circle
Absorption correction	Analytical (CrysAlis RED; Oxford Diffraction, 2008)
T_min, T_max	0.254, 0.762
No. of measured, independent and observed [I > 2σ(I)] reflections	4862, 4512, 3958
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.707

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.045, 0.122, 1.06
No. of reflections	4512
No. of parameters	253
No. of restraints	15
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	5.63, −3.77

Computer programs: KM-4 Software (Kuma, 1996), DATAPROC (Kuma,2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4—H41···O12ⁱ	0.86 (2)	1.93 (2)	2.736 (6)	154 (4)
O4—H42···O12ⁱⁱ	0.87 (2)	1.92 (4)	2.754 (6)	161 (11)
O1—H11···O5	0.86 (2)	2.08 (3)	2.943 (9)	174 (10)
O1—H12···O11ⁱⁱⁱ	0.86 (2)	2.09 (6)	2.849 (7)	146 (9)
O5—H51···N22^iv	0.86 (2)	2.23 (5)	3.013 (8)	151 (9)
O5—H52···O21^v	0.87 (2)	2.12 (6)	2.897 (8)	149 (10)
O3—H31···O12^vi	0.86 (2)	2.09 (7)	2.819 (7)	142 (10)
O3—H32···N21^iv	0.86 (2)	2.01 (6)	2.794 (7)	151 (10)
O2—H21···O5^vii	0.86 (2)	2.13 (5)	2.906 (8)	150 (9)
O2—H22···O11ⁱⁱ	0.86 (2)	2.07 (4)	2.891 (7)	159 (9)

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

References

Kuma (1996). KM-4 Software. Kuma Diffraction Ltd, Wrocław, Poland. Google Scholar
Kuma (2001). DATAPROC. Kuma Diffraction Ltd, Wrocław, Poland. Google Scholar
Leciejewicz, J. & Starosta, W. (2009). Acta Cryst. E65, m94. Web of Science CSD CrossRef IUCr Journals Google Scholar
Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Starosta, W. & Leciejewicz, J. (2007). Acta Cryst. E63, m1662–m1663. Web of Science CSD CrossRef IUCr Journals Google Scholar
Starosta, W. & Leciejewicz, J. (2008). Acta Cryst. E64, o461. Web of Science CSD CrossRef IUCr Journals Google Scholar

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Volume 65| Part 11| November 2009| Page m1291

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