Poly[μ-aqua-diaqua­(μ3-N′-carboxy­methyl­ethylenediamine-N,N,N′-tri­acetato)oxidopotassium(I)vanadium(IV)]

Zhang, R.-H.; Lu, L.-P.; Li, M.-X.; Zhu, M.-L.

doi:10.1107/S1600536808017030

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 7| July 2008| Page m897

doi:10.1107/S1600536808017030

Open

access

Poly[μ-aqua-diaqua(μ₃-N′-carboxymethylethylenediamine-N,N,N′-triacetato)oxidopotassium(I)vanadium(IV)]

Rui-Hong Zhang,^a Li-Ping Lu,^a Ming-Xia Li ^a and Miao-Li Zhu ^a ^*

^aInstitute of Molecular Science, Key Laboratory of Chemical Biology and Molecular Engineering of the Education Ministry, Shanxi University, Taiyuan, Shanxi 030006, People's Republic of China
^*Correspondence e-mail: miaoli@sxu.edu.cn

(Received 14 May 2008; accepted 5 June 2008; online 7 June 2008)

In the crystal structure of the title compound, [KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]_n, the V^IV ion adopts a distorted octahedral geometry, coordinated by one oxide group, two N and three carboxylate O atoms from the same N′-carboxymethylethylenediamine-N,N,N′-triacetate (HEDTA) ligand. The potassium ion is heptacoordinated by two water molecules, two bridging water molecules and three carboxylate O atoms from three neighbouring HEDTA ligands. The HEDTA ligands and some of the water molecules act as bridges, linking the compound into a three-dimensional architecture via 2₁ screw, c-glide, translation and inversion symmetry operators. Meanwhile, three types of O—H⋯O hydrogen bonds provide an additional stabilization of the three-dimensional architecture.

Related literature

For related literature, see: Crans et al. (2004 ); Khanra et al. (2007 ); Tsuchida et al. (1999 ).

Experimental

Crystal data

[KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]
M_r = 449.31
Monoclinic, P 2₁ /c
a = 6.6701 (13) Å
b = 13.618 (3) Å
c = 18.693 (4) Å
β = 96.150 (2)°
V = 1688.2 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 298 (2) K
0.40 × 0.30 × 0.20 mm

Data collection

Bruker SMART 1K CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ) T_min = 0.714, T_max = 0.840
6813 measured reflections
2957 independent reflections
2613 reflections with I > 2σ(I)
R_int = 0.024

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.088
S = 1.07
2957 reflections
236 parameters
H-atom parameters constrained
Δρ_max = 0.33 e Å⁻³
Δρ_min = −0.22 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8⋯O3ⁱ	0.82	1.75	2.542 (3)	162
O12—H12B⋯O11ⁱⁱ	0.82	2.03	2.802 (3)	157
O11—H11B⋯O4ⁱⁱⁱ	0.82	2.17	2.960 (3)	162
O10—H10B⋯O6ⁱⁱⁱ	0.82	2.20	2.987 (3)	161
O12—H12A⋯O5^iv	0.82	1.99	2.804 (3)	169
O11—H11A⋯O7ⁱⁱ	0.82	1.99	2.801 (3)	169
O10—H10A⋯O12^v	0.82	2.26	2.983 (3)	147
Symmetry codes: (i) -x+1, -y+2, -z; (ii) -x, -y+2, -z+1; (iii) -x+1, -y+2, -z+1; (iv) x-1, y, z; (v) x+1, y, z.

Data collection: SMART (Bruker, 2000 ); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: PLATON (Spek, 2003 ) and publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808017030/fj2120sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808017030/fj2120Isup2.hkl

checkCIF report

Comment top

The vanadium complexes have been attracted great attention because of their versatile properties including biological activities(Crans et al., 2004), magnetic property(Khanra et al., 2007), catalytic abilities (Tsuchida et al., 1999) and so on. Especially, we are interested in the protein tyrosine phosphatase 1B (PTP1B) inhibition activity of vanadium compounds. Thus, the title compound (I) was synthesized and its crystal structure is reported here.

The X-ray crystallographic analysis shows that there are two metal ion centres in the asymmetric unit of the title compound(Fig 1). V^IV adopts a six coordinated geometry consisting of a O atom(O1) from vanadyl, two N and three carboxyl O atoms(O2, O4 and O6) from same symmetric edta ligand while potassium is hepta-coordinated by two water molecules, two bridging water molecules and three carboxyl O atoms (O3, O5 and O9) respectively from three neighbouring edta ligands with different symmetry. Each edta ligand acts as a bridge simultaneously coordinating to three neighbouring K⁺ ions while coordinating to one vanadium. Neighbouring K⁺ ions are bridged through two coordinated water molecules(O10). As the result of these coordination, the compound is constructed to three-dimensional structure by O9 atom via 2₁-screw, O3 via c-glide & translation and K1 via inversion & translation(Fig 2). Meanwhile, three types of O—H···O hydrogen bonds (Table 1) take part in the stabilization of the three-dimensional architecture(Fig 2). The first type is the coordination water O atoms (O10, O11 and O12) acting as H donors while carboxyl O atoms(O4, O5, O6 and O7) of edta ligands as acceptors. The second is between coordination water molecules[O12—H12B···O11(-x, 2 - y, 1 - z) and O10—H10A···O12(1 + x, y, z)]. The third type of O8—H8···O3(1 - x, 2 - y, -y) hydrogen bond joins neighbouring edta ligands.

Related literature top

For related literature, see: Crans et al. (2004); Khanra et al. (2007); Tsuchida et al. (1999).

Experimental top

All chemicals were of reagent grade, were commercially available and were used without further purification. H4EDTA(11.69 g, 40 mmol) was added to 100 ml of water and neutralized with 11.20 g (80 mmol) of Potassium carbonate. 6.52 g (40 mmol) of VOSO₄ was added to the solution, stirred for 24 h. Evaporation of the solution using a rotary evaporator was concentrated to 20 ml, then the solution with blue flocculent crystals was filtered, The blue crystals were obtained by slow evaporation of the solvent about two days at room temperature.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: PLATON (Spek, 2003) and publCIF (Westrip, 2008).

Figures top

	Fig. 1. A view of the structure of (I) with displacement ellipsoids drawn at the 30% probability level. Symmetry codes: i -x, y + 1/2, -z + 1/2; ii x, -y + 3/2, z - 1/2; iii -x, -y + 2, -z
	Fig. 2. The packing view in the title complex (I).

Poly[µ-aqua-diaqua(µ₃-N'-carboxymethylethylenediamine-N,N,N'- triacetato)oxidopotassium(I)vanadium(IV)] top

Crystal data top

[KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]	F(000) = 924
M_r = 449.31	D_x = 1.768 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3074 reflections
a = 6.6701 (13) Å	θ = 2.1–26.6°
b = 13.618 (3) Å	µ = 0.90 mm⁻¹
c = 18.693 (4) Å	T = 298 K
β = 96.150 (2)°	Block, blue
V = 1688.2 (6) Å³	0.40 × 0.30 × 0.20 mm
Z = 4

Data collection top

Bruker SMART 1K CCD diffractometer	2957 independent reflections
Radiation source: fine-focus sealed tube	2613 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
ω scans	θ_max = 25.0°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −7→7
T_min = 0.714, T_max = 0.840	k = −16→16
6813 measured reflections	l = −12→22

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.088	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0425P)² + 0.6912P] where P = (F_o² + 2F_c²)/3
2957 reflections	(Δ/σ)_max = 0.001
236 parameters	Δρ_max = 0.33 e Å⁻³
0 restraints	Δρ_min = −0.22 e Å⁻³

Crystal data top

[KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]	V = 1688.2 (6) Å³
M_r = 449.31	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 6.6701 (13) Å	µ = 0.90 mm⁻¹
b = 13.618 (3) Å	T = 298 K
c = 18.693 (4) Å	0.40 × 0.30 × 0.20 mm
β = 96.150 (2)°

Data collection top

Bruker SMART 1K CCD diffractometer	2957 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	2613 reflections with I > 2σ(I)
T_min = 0.714, T_max = 0.840	R_int = 0.024
6813 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.088	H-atom parameters constrained
S = 1.07	Δρ_max = 0.33 e Å⁻³
2957 reflections	Δρ_min = −0.22 e Å⁻³
236 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
V1	0.46422 (6)	1.03027 (3)	0.20517 (2)	0.02305 (14)
N1	0.2470 (3)	0.90064 (14)	0.21295 (10)	0.0229 (4)
N2	0.2025 (3)	1.08521 (14)	0.13790 (10)	0.0226 (4)
C1	0.4610 (4)	0.85480 (18)	0.11714 (13)	0.0268 (5)
C2	0.3056 (4)	0.82187 (17)	0.16472 (13)	0.0272 (5)
H2A	0.1867	0.7994	0.1348	0.033*
H2B	0.3589	0.7668	0.1936	0.033*
C3	0.4930 (4)	0.88638 (17)	0.31905 (13)	0.0274 (6)
C4	0.2772 (4)	0.86957 (19)	0.28900 (13)	0.0288 (6)
H4A	0.2442	0.8005	0.2926	0.035*
H4B	0.1883	0.9067	0.3167	0.035*
C5	0.0432 (4)	0.93920 (17)	0.18987 (13)	0.0260 (5)
H5A	−0.0044	0.9778	0.2283	0.031*
H5B	−0.0499	0.8852	0.1789	0.031*
C6	0.0520 (4)	1.00233 (18)	0.12396 (13)	0.0269 (5)
H6A	−0.0806	1.0296	0.1095	0.032*
H6B	0.0897	0.9620	0.0847	0.032*
C7	0.1193 (4)	1.16469 (18)	0.18111 (13)	0.0281 (6)
H7A	−0.0263	1.1660	0.1706	0.034*
H7B	0.1711	1.2275	0.1669	0.034*
C8	0.1722 (4)	1.15125 (17)	0.26067 (14)	0.0296 (6)
C9	0.2569 (4)	1.12454 (18)	0.06851 (13)	0.0261 (5)
H9A	0.3120	1.0715	0.0420	0.031*
H9B	0.3622	1.1733	0.0785	0.031*
C10	0.0834 (4)	1.17089 (18)	0.02109 (13)	0.0284 (6)
K1	0.31886 (9)	0.85434 (4)	0.49345 (3)	0.03673 (17)
O1	0.6281 (3)	1.11296 (13)	0.19480 (10)	0.0388 (5)
O2	0.5346 (3)	0.94067 (12)	0.12620 (9)	0.0288 (4)
O3	0.5115 (3)	0.79597 (13)	0.07183 (10)	0.0363 (4)
O4	0.5988 (3)	0.94463 (12)	0.28376 (9)	0.0305 (4)
O5	0.5578 (3)	0.84570 (13)	0.37597 (10)	0.0365 (4)
O6	0.3143 (3)	1.08920 (12)	0.28047 (9)	0.0315 (4)
O7	0.0813 (3)	1.19822 (14)	0.30238 (10)	0.0454 (5)
O8	0.1269 (3)	1.20678 (14)	−0.04052 (9)	0.0370 (4)
H8	0.2453	1.1952	−0.0455	0.056*
O9	−0.0876 (3)	1.17595 (15)	0.03675 (10)	0.0412 (5)
O10	0.6764 (3)	0.94372 (15)	0.56121 (11)	0.0502 (5)
H10A	0.7731	0.9205	0.5434	0.075*
H10B	0.6886	0.9215	0.6022	0.075*
O11	0.1732 (3)	0.91295 (14)	0.61935 (10)	0.0474 (5)
H11A	0.1017	0.8743	0.6387	0.071*
H11B	0.2279	0.9442	0.6535	0.071*
O12	−0.0659 (3)	0.90505 (16)	0.44337 (13)	0.0578 (6)
H12A	−0.1676	0.8828	0.4205	0.087*
H12B	−0.0626	0.9615	0.4282	0.087*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.0205 (2)	0.0245 (2)	0.0242 (2)	−0.00226 (16)	0.00252 (16)	−0.00034 (16)
N1	0.0218 (11)	0.0252 (10)	0.0219 (10)	0.0000 (8)	0.0039 (8)	0.0015 (8)
N2	0.0232 (11)	0.0233 (10)	0.0221 (10)	0.0013 (8)	0.0054 (8)	0.0025 (8)
C1	0.0241 (13)	0.0295 (13)	0.0264 (13)	0.0031 (10)	0.0010 (10)	−0.0001 (11)
C2	0.0270 (13)	0.0224 (12)	0.0325 (14)	−0.0007 (10)	0.0042 (11)	−0.0018 (10)
C3	0.0305 (14)	0.0238 (12)	0.0278 (14)	0.0042 (11)	0.0029 (11)	0.0005 (11)
C4	0.0305 (14)	0.0316 (13)	0.0251 (13)	−0.0019 (11)	0.0062 (11)	0.0051 (11)
C5	0.0197 (12)	0.0272 (12)	0.0316 (14)	−0.0025 (10)	0.0044 (10)	−0.0008 (11)
C6	0.0218 (13)	0.0274 (12)	0.0306 (13)	−0.0036 (10)	−0.0017 (10)	−0.0005 (11)
C7	0.0272 (14)	0.0266 (13)	0.0314 (14)	0.0028 (10)	0.0072 (11)	−0.0028 (10)
C8	0.0315 (15)	0.0262 (13)	0.0328 (14)	−0.0052 (11)	0.0104 (11)	−0.0047 (11)
C9	0.0273 (13)	0.0277 (12)	0.0241 (12)	0.0005 (10)	0.0062 (10)	0.0016 (10)
C10	0.0296 (15)	0.0282 (13)	0.0269 (13)	−0.0011 (11)	0.0008 (11)	0.0002 (10)
K1	0.0338 (3)	0.0413 (3)	0.0348 (3)	0.0010 (3)	0.0025 (3)	0.0065 (3)
O1	0.0319 (11)	0.0358 (10)	0.0487 (12)	−0.0090 (8)	0.0045 (9)	−0.0002 (9)
O2	0.0296 (10)	0.0285 (9)	0.0300 (9)	−0.0030 (8)	0.0107 (8)	−0.0029 (7)
O3	0.0370 (11)	0.0372 (10)	0.0363 (10)	−0.0014 (8)	0.0108 (8)	−0.0116 (9)
O4	0.0261 (10)	0.0341 (9)	0.0306 (10)	−0.0011 (8)	0.0002 (7)	0.0061 (8)
O5	0.0387 (11)	0.0381 (10)	0.0311 (10)	0.0021 (8)	−0.0033 (8)	0.0072 (8)
O6	0.0385 (11)	0.0340 (9)	0.0226 (9)	0.0048 (8)	0.0055 (8)	−0.0027 (7)
O7	0.0574 (13)	0.0446 (11)	0.0372 (11)	0.0087 (10)	0.0187 (10)	−0.0100 (9)
O8	0.0336 (11)	0.0506 (12)	0.0272 (10)	0.0050 (9)	0.0050 (8)	0.0086 (9)
O9	0.0268 (11)	0.0532 (12)	0.0443 (12)	0.0067 (9)	0.0071 (9)	0.0162 (9)
O10	0.0508 (13)	0.0523 (12)	0.0461 (12)	−0.0007 (10)	−0.0017 (10)	0.0093 (10)
O11	0.0568 (14)	0.0454 (12)	0.0398 (12)	−0.0081 (10)	0.0037 (10)	0.0008 (9)
O12	0.0492 (14)	0.0465 (12)	0.0727 (16)	−0.0020 (10)	−0.0155 (11)	0.0145 (11)

Geometric parameters (Å, º) top

V1—O1	1.5955 (18)	C7—H7A	0.9700
V1—O6	1.9815 (17)	C7—H7B	0.9700
V1—O2	2.0092 (16)	C8—O7	1.219 (3)
V1—O4	2.0104 (17)	C8—O6	1.294 (3)
V1—N2	2.172 (2)	C9—C10	1.518 (3)
V1—N1	2.298 (2)	C9—H9A	0.9700
N1—C4	1.476 (3)	C9—H9B	0.9700
N1—C5	1.478 (3)	C10—O9	1.210 (3)
N1—C2	1.481 (3)	C10—O8	1.312 (3)
N2—C9	1.484 (3)	K1—O12	2.725 (2)
N2—C7	1.493 (3)	K1—O3ⁱ	2.7539 (19)
N2—C6	1.514 (3)	K1—O11	2.758 (2)
C1—O3	1.238 (3)	K1—O10	2.851 (2)
C1—O2	1.272 (3)	K1—O5	2.851 (2)
C1—C2	1.505 (3)	K1—O9ⁱⁱ	2.900 (2)
C2—H2A	0.9700	K1—O10ⁱⁱⁱ	2.935 (2)
C2—H2B	0.9700	K1—K1ⁱⁱⁱ	4.6380 (14)
C3—O5	1.236 (3)	K1—H12B	3.0701
C3—O4	1.289 (3)	O3—K1^iv	2.7539 (19)
C3—C4	1.505 (4)	O8—H8	0.8200
C4—H4A	0.9700	O9—K1^v	2.900 (2)
C4—H4B	0.9700	O10—K1ⁱⁱⁱ	2.935 (2)
C5—C6	1.509 (3)	O10—H10A	0.8199
C5—H5A	0.9700	O10—H10B	0.8200
C5—H5B	0.9700	O11—H11A	0.8200
C6—H6A	0.9700	O11—H11B	0.8200
C6—H6B	0.9700	O12—H12A	0.8200
C7—C8	1.502 (4)	O12—H12B	0.8200

O1—V1—O6	101.82 (9)	O6—C8—C7	116.7 (2)
O1—V1—O2	97.02 (8)	N2—C9—C10	114.7 (2)
O6—V1—O2	160.61 (7)	N2—C9—H9A	108.6
O1—V1—O4	103.90 (9)	C10—C9—H9A	108.6
O6—V1—O4	86.31 (7)	N2—C9—H9B	108.6
O2—V1—O4	93.63 (7)	C10—C9—H9B	108.6
O1—V1—N2	101.83 (9)	H9A—C9—H9B	107.6
O6—V1—N2	80.59 (7)	O9—C10—O8	119.6 (2)
O2—V1—N2	91.17 (7)	O9—C10—C9	124.2 (2)
O4—V1—N2	153.01 (7)	O8—C10—C9	116.2 (2)
O1—V1—N1	174.01 (9)	O12—K1—O3ⁱ	137.71 (6)
O6—V1—N1	84.06 (7)	O12—K1—O11	79.34 (7)
O2—V1—N1	77.21 (7)	O3ⁱ—K1—O11	87.02 (6)
O4—V1—N1	75.13 (7)	O12—K1—O10	139.18 (7)
N2—V1—N1	80.10 (7)	O3ⁱ—K1—O10	76.15 (6)
C4—N1—C5	114.18 (18)	O11—K1—O10	81.47 (7)
C4—N1—C2	111.16 (19)	O12—K1—O5	109.24 (7)
C5—N1—C2	111.99 (19)	O3ⁱ—K1—O5	96.41 (5)
C4—N1—V1	105.01 (14)	O11—K1—O5	161.12 (6)
C5—N1—V1	105.97 (13)	O10—K1—O5	81.36 (6)
C2—N1—V1	107.95 (14)	O12—K1—O9ⁱⁱ	71.57 (6)
C9—N2—C7	110.56 (18)	O3ⁱ—K1—O9ⁱⁱ	71.89 (6)
C9—N2—C6	109.77 (18)	O11—K1—O9ⁱⁱ	100.37 (6)
C7—N2—C6	110.82 (18)	O10—K1—O9ⁱⁱ	147.80 (6)
C9—N2—V1	111.95 (14)	O5—K1—O9ⁱⁱ	98.34 (5)
C7—N2—V1	105.00 (14)	O12—K1—O10ⁱⁱⁱ	71.81 (6)
C6—N2—V1	108.65 (14)	O3ⁱ—K1—O10ⁱⁱⁱ	149.29 (6)
O3—C1—O2	123.8 (2)	O11—K1—O10ⁱⁱⁱ	92.51 (6)
O3—C1—C2	117.8 (2)	O10—K1—O10ⁱⁱⁱ	73.43 (7)
O2—C1—C2	118.4 (2)	O5—K1—O10ⁱⁱⁱ	75.09 (6)
N1—C2—C1	112.82 (19)	O9ⁱⁱ—K1—O10ⁱⁱⁱ	137.93 (6)
N1—C2—H2A	109.0	O12—K1—K1ⁱⁱⁱ	105.52 (5)
C1—C2—H2A	109.0	O3ⁱ—K1—K1ⁱⁱⁱ	113.39 (5)
N1—C2—H2B	109.0	O11—K1—K1ⁱⁱⁱ	86.36 (5)
C1—C2—H2B	109.0	O10—K1—K1ⁱⁱⁱ	37.34 (4)
H2A—C2—H2B	107.8	O5—K1—K1ⁱⁱⁱ	75.22 (4)
O5—C3—O4	123.8 (2)	O9ⁱⁱ—K1—K1ⁱⁱⁱ	171.84 (5)
O5—C3—C4	119.0 (2)	O10ⁱⁱⁱ—K1—K1ⁱⁱⁱ	36.09 (4)
O4—C3—C4	117.2 (2)	O12—K1—H12B	14.8
N1—C4—C3	110.02 (19)	O3ⁱ—K1—H12B	152.2
N1—C4—H4A	109.7	O11—K1—H12B	81.3
C3—C4—H4A	109.7	O10—K1—H12B	126.3
N1—C4—H4B	109.7	O5—K1—H12B	102.8
C3—C4—H4B	109.7	O9ⁱⁱ—K1—H12B	85.4
H4A—C4—H4B	108.2	O10ⁱⁱⁱ—K1—H12B	57.0
N1—C5—C6	109.02 (19)	K1ⁱⁱⁱ—K1—H12B	91.1
N1—C5—H5A	109.9	C1—O2—V1	122.60 (15)
C6—C5—H5A	109.9	C1—O3—K1^iv	134.36 (16)
N1—C5—H5B	109.9	C3—O4—V1	120.32 (16)
C6—C5—H5B	109.9	C3—O5—K1	118.15 (16)
H5A—C5—H5B	108.3	C8—O6—V1	118.11 (15)
C5—C6—N2	111.54 (19)	C10—O8—H8	109.5
C5—C6—H6A	109.3	C10—O9—K1^v	119.74 (16)
N2—C6—H6A	109.3	K1—O10—K1ⁱⁱⁱ	106.57 (7)
C5—C6—H6B	109.3	K1—O10—H10A	108.2
N2—C6—H6B	109.3	K1ⁱⁱⁱ—O10—H10A	100.5
H6A—C6—H6B	108.0	K1—O10—H10B	104.6
N2—C7—C8	112.7 (2)	K1ⁱⁱⁱ—O10—H10B	131.8
N2—C7—H7A	109.1	H10A—O10—H10B	103.5
C8—C7—H7A	109.1	K1—O11—H11A	117.7
N2—C7—H7B	109.1	K1—O11—H11B	130.3
C8—C7—H7B	109.1	H11A—O11—H11B	102.8
H7A—C7—H7B	107.8	K1—O12—H12A	141.4
O7—C8—O6	124.0 (2)	K1—O12—H12B	107.3
O7—C8—C7	119.3 (2)	H12A—O12—H12B	102.5

O6—V1—N1—C4	−57.66 (15)	N2—C7—C8—O7	−165.0 (2)
O2—V1—N1—C4	127.40 (15)	N2—C7—C8—O6	15.1 (3)
O4—V1—N1—C4	30.08 (14)	C7—N2—C9—C10	−59.1 (3)
N2—V1—N1—C4	−139.11 (15)	C6—N2—C9—C10	63.5 (2)
O6—V1—N1—C5	63.53 (14)	V1—N2—C9—C10	−175.79 (16)
O2—V1—N1—C5	−111.41 (15)	N2—C9—C10—O9	−0.5 (4)
O4—V1—N1—C5	151.27 (15)	N2—C9—C10—O8	179.7 (2)
N2—V1—N1—C5	−17.92 (14)	O3—C1—O2—V1	−175.28 (19)
O6—V1—N1—C2	−176.33 (15)	C2—C1—O2—V1	3.9 (3)
O2—V1—N1—C2	8.74 (14)	O1—V1—O2—C1	171.07 (19)
O4—V1—N1—C2	−88.59 (15)	O6—V1—O2—C1	−22.6 (3)
N2—V1—N1—C2	102.23 (15)	O4—V1—O2—C1	66.57 (19)
O1—V1—N2—C9	42.20 (16)	N2—V1—O2—C1	−86.86 (19)
O6—V1—N2—C9	142.42 (16)	N1—V1—O2—C1	−7.28 (18)
O2—V1—N2—C9	−55.22 (15)	O2—C1—O3—K1^iv	−150.33 (18)
O4—V1—N2—C9	−155.57 (16)	C2—C1—O3—K1^iv	30.5 (3)
N1—V1—N2—C9	−132.03 (15)	O5—C3—O4—V1	−165.98 (18)
O1—V1—N2—C7	−77.80 (15)	C4—C3—O4—V1	12.8 (3)
O6—V1—N2—C7	22.42 (14)	O1—V1—O4—C3	161.53 (18)
O2—V1—N2—C7	−175.22 (14)	O6—V1—O4—C3	60.26 (18)
O4—V1—N2—C7	84.4 (2)	O2—V1—O4—C3	−100.31 (18)
N1—V1—N2—C7	107.97 (14)	N2—V1—O4—C3	−0.5 (3)
O1—V1—N2—C6	163.60 (15)	N1—V1—O4—C3	−24.57 (17)
O6—V1—N2—C6	−96.18 (14)	O4—C3—O5—K1	131.8 (2)
O2—V1—N2—C6	66.17 (14)	C4—C3—O5—K1	−46.9 (3)
O4—V1—N2—C6	−34.2 (2)	O12—K1—O5—C3	17.34 (19)
N1—V1—N2—C6	−10.63 (14)	O3ⁱ—K1—O5—C3	163.20 (17)
C4—N1—C2—C1	−124.2 (2)	O11—K1—O5—C3	−97.2 (2)
C5—N1—C2—C1	106.8 (2)	O10—K1—O5—C3	−121.92 (18)
V1—N1—C2—C1	−9.5 (2)	O9ⁱⁱ—K1—O5—C3	90.64 (18)
O3—C1—C2—N1	−175.9 (2)	O10ⁱⁱⁱ—K1—O5—C3	−46.87 (17)
O2—C1—C2—N1	4.9 (3)	K1ⁱⁱⁱ—K1—O5—C3	−84.25 (17)
C5—N1—C4—C3	−148.1 (2)	O7—C8—O6—V1	−173.6 (2)
C2—N1—C4—C3	84.1 (2)	C7—C8—O6—V1	6.3 (3)
V1—N1—C4—C3	−32.4 (2)	O1—V1—O6—C8	83.24 (19)
O5—C3—C4—N1	−164.2 (2)	O2—V1—O6—C8	−82.9 (3)
O4—C3—C4—N1	17.0 (3)	O4—V1—O6—C8	−173.32 (18)
C4—N1—C5—C6	158.6 (2)	N2—V1—O6—C8	−17.00 (17)
C2—N1—C5—C6	−73.9 (2)	N1—V1—O6—C8	−97.91 (18)
V1—N1—C5—C6	43.5 (2)	O8—C10—O9—K1^v	−41.5 (3)
N1—C5—C6—N2	−57.1 (3)	C9—C10—O9—K1^v	138.70 (19)
C9—N2—C6—C5	161.47 (19)	O12—K1—O10—K1ⁱⁱⁱ	−32.58 (13)
C7—N2—C6—C5	−76.1 (2)	O3ⁱ—K1—O10—K1ⁱⁱⁱ	175.77 (8)
V1—N2—C6—C5	38.7 (2)	O11—K1—O10—K1ⁱⁱⁱ	−95.21 (7)
C9—N2—C7—C8	−146.5 (2)	O5—K1—O10—K1ⁱⁱⁱ	76.92 (7)
C6—N2—C7—C8	91.6 (2)	O9ⁱⁱ—K1—O10—K1ⁱⁱⁱ	168.86 (8)
V1—N2—C7—C8	−25.6 (2)	O10ⁱⁱⁱ—K1—O10—K1ⁱⁱⁱ	0.0

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8···O3^vi	0.82	1.75	2.542 (3)	162
O12—H12B···O11^vii	0.82	2.03	2.802 (3)	157
O11—H11B···O4ⁱⁱⁱ	0.82	2.17	2.960 (3)	162
O10—H10B···O6ⁱⁱⁱ	0.82	2.20	2.987 (3)	161
O12—H12A···O5^viii	0.82	1.99	2.804 (3)	169
O11—H11A···O7^vii	0.82	1.99	2.801 (3)	169
O10—H10A···O12^ix	0.82	2.26	2.983 (3)	147

Symmetry codes: (iii) −x+1, −y+2, −z+1; (vi) −x+1, −y+2, −z; (vii) −x, −y+2, −z+1; (viii) x−1, y, z; (ix) x+1, y, z.

Experimental details

Crystal data
Chemical formula	[KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]
M_r	449.31
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	298
a, b, c (Å)	6.6701 (13), 13.618 (3), 18.693 (4)
β (°)	96.150 (2)
V (Å³)	1688.2 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.90
Crystal size (mm)	0.40 × 0.30 × 0.20

Data collection
Diffractometer	Bruker SMART 1K CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2000)
T_min, T_max	0.714, 0.840
No. of measured, independent and observed [I > 2σ(I)] reflections	6813, 2957, 2613
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.088, 1.07
No. of reflections	2957
No. of parameters	236
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.33, −0.22

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL/PC (Sheldrick, 2008), PLATON (Spek, 2003) and publCIF (Westrip, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8···O3ⁱ	0.82	1.75	2.542 (3)	162.1
O12—H12B···O11ⁱⁱ	0.82	2.03	2.802 (3)	156.8
O11—H11B···O4ⁱⁱⁱ	0.82	2.17	2.960 (3)	161.7
O10—H10B···O6ⁱⁱⁱ	0.82	2.20	2.987 (3)	161.1
O12—H12A···O5^iv	0.82	1.99	2.804 (3)	169.3
O11—H11A···O7ⁱⁱ	0.82	1.99	2.801 (3)	169.2
O10—H10A···O12^v	0.82	2.26	2.983 (3)	146.5

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

Acknowledgements

The authors acknowledge financial support from the National Natural Science Foundation of China (grant No. 20471033), the Provincial Natural Science Foundation of Shanxi Province of China (grant No. 20051013) and the Overseas Returned Scholar Foundation of Shanxi Province of China in 2006.

References

Bruker (2000). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Crans, D. C., Smee, J. J., Gaidamauskas, E. & Yang, L. (2004). Chem. Rev. 104, 849–902. Web of Science CrossRef PubMed CAS Google Scholar
Khanra, S., Kloth, M., Mansaray, H., Muryn, C. A., Tuna, F., Sanudo, E. C., Helliwell, M., McInnes, E. J. L. & Winpenny, R. E. P. (2007). Angew. Chem. Int. Ed. 46, 5568–5571. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2000). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tsuchida, E., Oyaizu, K., Listiani Dewi, E., Imai, T. & Anson, F. C. (1999). Inorg. Chem. 38, 3704–3708. Web of Science CrossRef PubMed CAS Google Scholar
Westrip, S. P. (2008). publCIF. In preparation. Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.