catena-Poly[[[diaqua­iron(II)]-μ-pyridine-2,5-dicarboxyl­ato-[tetra­aqua­iron(II)]-μ-pyridine-2,5-dicarboxyl­ato] tetra­hydrate]

Xu, H.-Y.; Ma, H.-L.; Xu, M.-T.; Zhao, W.-X.; Guo, B.-G.

doi:10.1107/S1600536808002043

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Page m413

doi:10.1107/S1600536808002043

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catena-Poly[[[diaquairon(II)]-μ-pyridine-2,5-dicarboxylato-[tetraaquairon(II)]-μ-pyridine-2,5-dicarboxylato] tetrahydrate]

Hai-Yun Xu,^a ^* Huai-Ling Ma,^a Mao-Tian Xu,^a Wen-Xian Zhao ^a and Bao-Guo Guo ^a

^aDepartment of Chemistry, Shangqiu Normal College, 476000 Shangqiu, Henan, People's Republic of China
^*Correspondence e-mail: xuhyun@yahoo.cn

(Received 22 December 2007; accepted 20 January 2008; online 25 January 2008)

In the crystal structure of the title compound, {[Fe₂(C₇H₃NO₄)₂(H₂O)₆]·4H₂O}_n, there are two types of coordination for the Fe^II atoms. One Fe^II atom is in a distorted octahedral N₂O₄ environment, with two chelating rings from the pyridinedicarboxylate ligands and two O atoms from the water molecules, while the other is in a distorted octahedral O₆ environment with two O atoms from the pyridinedicarboxylate ligands and four O atoms from the water molecules. Both Fe^II atoms lie on crystallographic centers of symmetry. The complex possesses an infinite chain structure running along the [101] direction. These chains are interconnected by the uncoordinated water molecules through O—H⋯O hydrogen bonds.

Related literature

For related literature, see: Hill (1998 ); Liang et al. (2001 ); Mitzi et al. (1995 ); Moler et al. (2001 ); Zeng et al. (2003 ); Xu et al. (2004 ).

Experimental

Crystal data

[Fe₂(C₇H₃NO₄)₂(H₂O)₆]·4H₂O
M_r = 622.06
Triclinic, $[P \overline 1]$
a = 7.098 (3) Å
b = 8.922 (3) Å
c = 9.720 (2) Å
α = 90.942 (6)°
β = 101.375 (6)°
γ = 108.112 (5)°
V = 571.6 (3) Å³
Z = 1
Mo Kα radiation
μ = 1.36 mm⁻¹
T = 298 (2) K
0.21 × 0.20 × 0.18 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.763, T_max = 0.792
2866 measured reflections
1989 independent reflections
1757 reflections with I > 2σ(I)
R_int = 0.062

Refinement

R[F² > 2σ(F²)] = 0.043
wR(F²) = 0.124
S = 1.06
1989 reflections
166 parameters
H-atom parameters constrained
Δρ_max = 0.65 e Å⁻³
Δρ_min = −0.60 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H9B⋯O8	0.85	2.32	3.159 (6)	171
O9—H9A⋯O6ⁱ	0.85	2.06	2.849 (5)	154
O8—H8B⋯O5ⁱⁱ	0.85	2.55	3.204 (4)	134
O8—H8B⋯O4ⁱⁱ	0.85	2.51	3.171 (4)	136
O8—H8A⋯O3	0.85	2.55	3.177 (4)	132
O8—H8A⋯O2	0.85	2.44	3.201 (4)	149
O5—H5B⋯O7ⁱ	0.85	2.22	2.706 (3)	116
O2—H2B⋯O9ⁱⁱⁱ	0.85	1.94	2.657 (5)	141
O2—H2A⋯O4^iv	0.85	1.99	2.758 (3)	150
O1—H1B⋯O6^v	0.85	1.92	2.715 (3)	156
O1—H1A⋯O8ⁱⁱ	0.85	2.06	2.822 (4)	148
Symmetry codes: (i) -x, -y, -z; (ii) -x+1, -y+1, -z+1; (iii) -x+1, -y, -z+1; (iv) -x+2, -y+1, -z+1; (v) x+1, y+1, z+1.

Data collection: SMART (Siemens, 1996 ); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; 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: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808002043/is2270sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808002043/is2270Isup2.hkl

checkCIF report

Comment top

Extended frameworks of coordination polymers based on transition metal ions and multifunctional bridging ligands are currently of great interest because of their intriguing topologies and their potential applications (Hill, 1998; Moler et al., 2001; Mitzi et al., 1995). Multi-carboxylate ligands may exhibit various coordination modes to furnish various structures. Recently, many transition metal-organic polymers constructed with multi-carboxylate ligands show varies of novel topology and potential applications in catalysis, materials chemistry and biochemistry (Zeng et al., 2003; Xu et al., 2004; Liang et al., 2001). Pyridine-2,5-dicarboxylic acid (H₂pydc) has unique features because of the presence of two carboxylate groups (O donor atoms) and the pyridine ring (N donor atom), which aids to increase the dimensionality of the assembled covalent network. Therefore, it is most likely that pydc will form low symmetric structures with metals. In this paper, we report the preparation and crystal structure of a new three-dimensional supramolecular complex [Fe₂(pydc)₂(H₂O)₂].4H₂O, (I).

In the complex, (I), there exist two types of coordination geometries around the Fe(II) ions. The Fe1 ions are hexacoordinated in a N₂O₄ environment with two chelating rings from the pydc ligands and two oxygen atoms from the water molecules. The Fe2 ions are also hexacoordinated in an O₆ environment with two oxygen atoms from the pydc ligands and four oxygen atoms from the water molecules. All Fe atoms lie on a crystallographic center of symmetry and the ligand lies on a crystallographic twofold axis. A perspective view of the local coordination environments around the Fe(II) atoms of (I) is shown in Fig. 1. For Fe1 and Fe2, the bond distances of Fe—O (water oxygen), 2.071–2.100 Å, are similar with those of Fe—O (carboxylate oxygen), 2.058–2.080 Å. As presented in Fig. 2, the two kinds of geometries around Fe(II) ions are arranged alternatively to give the one-dimensional polymeric chain. Interestingly, all Fe atoms of one polymeric chain are situated on one line and the neighboring Fe(II) atoms are syn-anti carboxylato bridged with the distance of 5.423 Å. These chains are interconnected by the uncoordinated water molecules through O—H···O hydrogen-bonding interactions and form a two-dimensional layer structure. A three-dimensional supramolecular network is obtained through O—H···O hydrogen-bonding interactions in the layers.

Related literature top

For related literature, see: Hill (1998); Liang et al. (2001); Mitzi et al. (1995); Moler et al. (2001); Zeng et al. (2003); Xu et al. (2004).

Experimental top

A mixture of H₂pydc (0.34 g, 2 mmol), KOH (0.23 g, 4 mmol) and FeSO₄.7H₂O (0.55 g, 2 mmol) in 15 ml of MeOH/H₂O (v/v, 1:1) was sealed in a 25-ml stainless-steel reactor with a teflon liner and was heated at 453 K for 72 h under autogenous pressure. Slow cooling to room temperature yielded 0.36 g (yield 40%) of block red crystals. Anal. Calc. for C₇H₁₃NO₉Fe (%): C 27.03, H 4.21, N 4.50. Found (%): C 27.14, H 4.46, N 4.36.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); 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: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Part of the polymeric structure of the title compound, showing 30% probability displacement ellipsoids and the atom-numbering scheme. The H atoms are omitted for clarity. The suffix A corresponds to symmetry code (2 - x, 1 - y, 1 - z).
	Fig. 2. The three-dimensional supramolecular structure of the title compound. Hydrogen bonds are shown by dashed lines.

catena-Poly[[[diaquairon(II)]-µ-pyridine-2,5-dicarboxylato- [tetraaquairon(II)]-µ-pyridine-2,5-dicarboxylato] tetrahydrate] top

Crystal data top

[Fe₂(C₇H₃NO₄)₂(H₂O)₆]·4H₂O	Z = 1
M_r = 622.06	F(000) = 320
Triclinic, P1	D_x = 1.807 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.098 (3) Å	Cell parameters from 714 reflections
b = 8.922 (3) Å	θ = 2.4–28.2°
c = 9.720 (2) Å	µ = 1.36 mm⁻¹
α = 90.942 (6)°	T = 298 K
β = 101.375 (6)°	Block, red
γ = 108.112 (5)°	0.21 × 0.20 × 0.18 mm
V = 571.6 (3) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	1989 independent reflections
Radiation source: fine-focus sealed tube	1757 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
ϕ and ω scans	θ_max = 25.0°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→6
T_min = 0.763, T_max = 0.792	k = −10→10
2866 measured reflections	l = −11→10

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)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.124	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.081P)² + 0.2244P] where P = (F_o² + 2F_c²)/3
1989 reflections	(Δ/σ)_max < 0.001
166 parameters	Δρ_max = 0.65 e Å⁻³
0 restraints	Δρ_min = −0.60 e Å⁻³

Crystal data top

[Fe₂(C₇H₃NO₄)₂(H₂O)₆]·4H₂O	γ = 108.112 (5)°
M_r = 622.06	V = 571.6 (3) Å³
Triclinic, P1	Z = 1
a = 7.098 (3) Å	Mo Kα radiation
b = 8.922 (3) Å	µ = 1.36 mm⁻¹
c = 9.720 (2) Å	T = 298 K
α = 90.942 (6)°	0.21 × 0.20 × 0.18 mm
β = 101.375 (6)°

Data collection top

Bruker SMART APEX CCD diffractometer	1989 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1757 reflections with I > 2σ(I)
T_min = 0.763, T_max = 0.792	R_int = 0.062
2866 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.043	0 restraints
wR(F²) = 0.124	H-atom parameters constrained
S = 1.06	Δρ_max = 0.65 e Å⁻³
1989 reflections	Δρ_min = −0.60 e Å⁻³
166 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
Fe1	0.5000	0.5000	0.0000	0.0222 (2)
Fe2	1.0000	0.5000	0.5000	0.0258 (2)
C1	0.6446 (4)	0.3738 (3)	0.2523 (3)	0.0270 (6)
C2	0.4924 (4)	0.2309 (3)	0.1667 (3)	0.0275 (6)
C3	0.4514 (5)	0.0824 (3)	0.2147 (3)	0.0330 (7)
H3	0.5126	0.0679	0.3050	0.040*
C4	0.3189 (5)	−0.0438 (3)	0.1270 (3)	0.0331 (7)
H4	0.2889	−0.1449	0.1579	0.040*
C5	0.2302 (4)	−0.0216 (3)	−0.0065 (3)	0.0278 (6)
C6	0.2767 (4)	0.1328 (3)	−0.0474 (3)	0.0279 (6)
H6	0.2161	0.1496	−0.1372	0.033*
C7	0.0905 (4)	−0.1587 (4)	−0.1093 (3)	0.0318 (7)
N1	0.4039 (3)	0.2565 (3)	0.0369 (3)	0.0261 (5)
O1	0.8315 (4)	0.6187 (3)	0.5803 (3)	0.0448 (6)
H1A	0.7132	0.6145	0.5373	0.054*
H1B	0.9150	0.7017	0.6279	0.054*
O2	0.9411 (3)	0.3350 (3)	0.6494 (2)	0.0425 (6)
H2B	0.8576	0.2419	0.6286	0.051*
H2A	1.0460	0.3570	0.7156	0.051*
O3	0.7348 (3)	0.3533 (2)	0.3701 (2)	0.0352 (5)
O4	0.6748 (3)	0.5047 (2)	0.1970 (2)	0.0334 (5)
O5	0.2787 (3)	0.5429 (3)	0.0954 (2)	0.0361 (5)
H5A	0.1792	0.5354	0.0276	0.043*
H5B	0.2288	0.4806	0.1537	0.043*
O6	0.0097 (4)	−0.1287 (3)	−0.2262 (3)	0.0473 (6)
O7	0.0653 (4)	−0.2939 (3)	−0.0688 (3)	0.0430 (6)
O8	0.4663 (4)	0.2880 (4)	0.6019 (3)	0.0640 (8)
H8B	0.4601	0.3105	0.6859	0.077*
H8A	0.5871	0.3270	0.5904	0.077*
O9	0.1591 (7)	−0.0327 (5)	0.4428 (6)	0.1112 (15)
H9B	0.2489	0.0471	0.4912	0.133*
H9A	0.1463	0.0205	0.3718	0.133*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0226 (3)	0.0153 (3)	0.0243 (3)	0.0050 (2)	−0.0034 (2)	−0.0004 (2)
Fe2	0.0269 (4)	0.0200 (3)	0.0247 (3)	0.0056 (2)	−0.0043 (2)	−0.0003 (2)
C1	0.0253 (14)	0.0248 (14)	0.0301 (15)	0.0088 (12)	0.0027 (11)	−0.0011 (11)
C2	0.0261 (14)	0.0260 (14)	0.0284 (15)	0.0082 (12)	0.0021 (11)	−0.0013 (11)
C3	0.0369 (17)	0.0282 (15)	0.0302 (16)	0.0083 (13)	0.0019 (13)	0.0059 (12)
C4	0.0357 (16)	0.0215 (14)	0.0403 (17)	0.0090 (13)	0.0041 (13)	0.0059 (12)
C5	0.0251 (14)	0.0225 (14)	0.0355 (16)	0.0079 (12)	0.0054 (12)	0.0003 (12)
C6	0.0277 (15)	0.0226 (13)	0.0314 (15)	0.0088 (12)	0.0006 (12)	−0.0004 (11)
C7	0.0242 (14)	0.0258 (15)	0.0432 (18)	0.0083 (12)	0.0023 (13)	−0.0049 (13)
N1	0.0259 (12)	0.0187 (11)	0.0308 (13)	0.0071 (10)	−0.0003 (10)	0.0014 (9)
O1	0.0403 (13)	0.0383 (13)	0.0492 (14)	0.0153 (11)	−0.0089 (11)	−0.0151 (11)
O2	0.0407 (13)	0.0349 (12)	0.0411 (13)	0.0033 (10)	−0.0026 (10)	0.0113 (10)
O3	0.0366 (12)	0.0278 (11)	0.0308 (11)	0.0047 (9)	−0.0072 (9)	0.0010 (8)
O4	0.0367 (12)	0.0228 (10)	0.0314 (11)	0.0071 (9)	−0.0096 (9)	−0.0011 (8)
O5	0.0320 (11)	0.0320 (12)	0.0439 (13)	0.0104 (10)	0.0072 (10)	0.0046 (10)
O6	0.0572 (15)	0.0302 (12)	0.0434 (14)	0.0136 (11)	−0.0134 (11)	−0.0088 (10)
O7	0.0367 (13)	0.0198 (11)	0.0632 (16)	0.0040 (10)	−0.0020 (11)	−0.0008 (10)
O8	0.0469 (16)	0.075 (2)	0.066 (2)	0.0196 (16)	0.0038 (14)	0.0019 (16)
O9	0.116 (3)	0.054 (2)	0.163 (5)	0.019 (2)	0.041 (3)	0.000 (2)

Geometric parameters (Å, º) top

Fe1—O4	2.058 (2)	C4—C5	1.372 (4)
Fe1—O4ⁱ	2.058 (2)	C4—H4	0.9300
Fe1—O5ⁱ	2.100 (2)	C5—C6	1.397 (4)
Fe1—O5	2.100 (2)	C5—C7	1.515 (4)
Fe1—N1	2.125 (2)	C6—N1	1.328 (4)
Fe1—N1ⁱ	2.125 (2)	C6—H6	0.9300
Fe2—O1	2.071 (2)	C7—O6	1.241 (4)
Fe2—O1ⁱⁱ	2.071 (2)	C7—O7	1.245 (4)
Fe2—O3ⁱⁱ	2.080 (2)	O1—H1A	0.8499
Fe2—O3	2.080 (2)	O1—H1B	0.8499
Fe2—O2	2.092 (2)	O2—H2B	0.8500
Fe2—O2ⁱⁱ	2.092 (2)	O2—H2A	0.8501
C1—O3	1.242 (3)	O5—H5A	0.8499
C1—O4	1.268 (4)	O5—H5B	0.8500
C1—C2	1.496 (4)	O8—H8B	0.8500
C2—N1	1.351 (4)	O8—H8A	0.8499
C2—C3	1.376 (4)	O9—H9B	0.8499
C3—C4	1.368 (4)	O9—H9A	0.8500
C3—H3	0.9300

O4—Fe1—O4ⁱ	180.00 (11)	N1—C2—C1	115.5 (2)
O4—Fe1—O5ⁱ	90.89 (9)	C3—C2—C1	122.3 (3)
O4ⁱ—Fe1—O5ⁱ	89.11 (9)	C4—C3—C2	118.8 (3)
O4—Fe1—O5	89.11 (9)	C4—C3—H3	120.6
O4ⁱ—Fe1—O5	90.89 (9)	C2—C3—H3	120.6
O5ⁱ—Fe1—O5	180.00 (6)	C3—C4—C5	120.2 (3)
O4—Fe1—N1	79.00 (8)	C3—C4—H4	119.9
O4ⁱ—Fe1—N1	101.00 (8)	C5—C4—H4	119.9
O5ⁱ—Fe1—N1	88.20 (9)	C4—C5—C6	117.9 (3)
O5—Fe1—N1	91.80 (9)	C4—C5—C7	121.9 (3)
O4—Fe1—N1ⁱ	101.00 (8)	C6—C5—C7	120.2 (3)
O4ⁱ—Fe1—N1ⁱ	79.00 (8)	N1—C6—C5	122.5 (3)
O5ⁱ—Fe1—N1ⁱ	91.80 (9)	N1—C6—H6	118.7
O5—Fe1—N1ⁱ	88.20 (9)	C5—C6—H6	118.7
N1—Fe1—N1ⁱ	180.0	O6—C7—O7	125.1 (3)
O1—Fe2—O1ⁱⁱ	180.00 (12)	O6—C7—C5	118.1 (3)
O1—Fe2—O3ⁱⁱ	90.59 (9)	O7—C7—C5	116.8 (3)
O1ⁱⁱ—Fe2—O3ⁱⁱ	89.41 (9)	C6—N1—C2	118.4 (2)
O1—Fe2—O3	89.41 (9)	C6—N1—Fe1	129.8 (2)
O1ⁱⁱ—Fe2—O3	90.59 (9)	C2—N1—Fe1	111.81 (18)
O3ⁱⁱ—Fe2—O3	180.0	Fe2—O1—H1A	122.3
O1—Fe2—O2	89.15 (10)	Fe2—O1—H1B	107.1
O1ⁱⁱ—Fe2—O2	90.85 (10)	H1A—O1—H1B	122.4
O3ⁱⁱ—Fe2—O2	93.74 (9)	Fe2—O2—H2B	122.9
O3—Fe2—O2	86.26 (9)	Fe2—O2—H2A	108.0
O1—Fe2—O2ⁱⁱ	90.85 (10)	H2B—O2—H2A	122.9
O1ⁱⁱ—Fe2—O2ⁱⁱ	89.15 (10)	C1—O3—Fe2	129.74 (18)
O3ⁱⁱ—Fe2—O2ⁱⁱ	86.26 (9)	C1—O4—Fe1	116.24 (18)
O3—Fe2—O2ⁱⁱ	93.74 (9)	Fe1—O5—H5A	104.8
O2—Fe2—O2ⁱⁱ	180.0	Fe1—O5—H5B	119.7
O3—C1—O4	125.5 (3)	H5A—O5—H5B	105.0
O3—C1—C2	117.1 (2)	H8B—O8—H8A	110.3
O4—C1—C2	117.3 (2)	H9B—O9—H9A	91.5
N1—C2—C3	122.2 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9B···O8	0.85	2.32	3.159 (6)	171
O9—H9A···O6ⁱⁱⁱ	0.85	2.06	2.849 (5)	154
O8—H8B···O5^iv	0.85	2.55	3.204 (4)	134
O8—H8B···O4^iv	0.85	2.51	3.171 (4)	136
O8—H8A···O3	0.85	2.55	3.177 (4)	132
O8—H8A···O2	0.85	2.44	3.201 (4)	149
O5—H5B···O7ⁱⁱⁱ	0.85	2.22	2.706 (3)	116
O2—H2B···O9^v	0.85	1.94	2.657 (5)	141
O2—H2A···O4ⁱⁱ	0.85	1.99	2.758 (3)	150
O1—H1B···O6^vi	0.85	1.92	2.715 (3)	156
O1—H1A···O8^iv	0.85	2.06	2.822 (4)	148

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

Experimental details

Crystal data
Chemical formula	[Fe₂(C₇H₃NO₄)₂(H₂O)₆]·4H₂O
M_r	622.06
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	7.098 (3), 8.922 (3), 9.720 (2)
α, β, γ (°)	90.942 (6), 101.375 (6), 108.112 (5)
V (Å³)	571.6 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	1.36
Crystal size (mm)	0.21 × 0.20 × 0.18

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.763, 0.792
No. of measured, independent and observed [I > 2σ(I)] reflections	2866, 1989, 1757
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.043, 0.124, 1.06
No. of reflections	1989
No. of parameters	166
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.65, −0.60

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), 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
O9—H9B···O8	0.85	2.32	3.159 (6)	171
O9—H9A···O6ⁱ	0.85	2.06	2.849 (5)	154
O8—H8B···O5ⁱⁱ	0.85	2.55	3.204 (4)	134
O8—H8B···O4ⁱⁱ	0.85	2.51	3.171 (4)	136
O8—H8A···O3	0.85	2.55	3.177 (4)	132
O8—H8A···O2	0.85	2.44	3.201 (4)	149
O5—H5B···O7ⁱ	0.85	2.22	2.706 (3)	116
O2—H2B···O9ⁱⁱⁱ	0.85	1.94	2.657 (5)	141
O2—H2A···O4^iv	0.85	1.99	2.758 (3)	150
O1—H1B···O6^v	0.85	1.92	2.715 (3)	156
O1—H1A···O8ⁱⁱ	0.85	2.06	2.822 (4)	148

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

Acknowledgements

The authors thank the Natural Science Foundation of Henan Province (No. 0511020300) for financial support.

References

Hill, C. L. (1998). Chem. Rev. 98, 1–390. Web of Science CrossRef PubMed CAS Google Scholar
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Sheldrick, G. M. (1996). 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
Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Google Scholar
Xu, Y., Han, L., Lin, Z.-Z., Liu, C.-P., Yuan, D.-Q., Zhou, Y.-F. & Hong, M.-C. (2004). Eur. J. Inorg. Chem. pp. 4457–4462. Web of Science CSD CrossRef Google Scholar
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Volume 64| Part 2| February 2008| Page m413

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

catena-Poly[[[di­aqua­iron(II)]-μ-pyridine-2,5-di­carboxyl­ato-[tetra­aqua­iron(II)]-μ-pyridine-2,5-di­carboxyl­ato] tetra­hydrate]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

catena-Poly[[[diaquairon(II)]-μ-pyridine-2,5-dicarboxylato-[tetraaquairon(II)]-μ-pyridine-2,5-dicarboxylato] tetrahydrate]