Bis(μ-5-carboxyl­ato-1-carboxyl­ato­methyl-2-oxidopyridinium)-κ2 O 5:O 1;κ2 O 1:O 5-[diaqua­(phenan­throline-κ2 N,N′)manganese(II)] dihydrate

Mei-Xiang Jiang; Yun-Long Feng

doi:10.1107/S1600536809017668

. 2009 May 20;65(Pt 6):m654. doi: 10.1107/S1600536809017668

Bis(μ-5-carboxylato-1-carboxylatomethyl-2-oxidopyridinium)-κ² O ⁵:O ¹;κ² O ¹:O ⁵-[diaqua(phenanthroline-κ² N,N′)manganese(II)] dihydrate

Mei-Xiang Jiang ^a, Yun-Long Feng ^a,^*

PMCID: PMC2969745 PMID: 21583018

Abstract

The centrosymmetric binuclear title complex, [Mn₂(C₈H₅NO₅)₂(C₁₂H₈N₂)₂(H₂O)₄]·2H₂O, was obtained by the reaction of manganese chloride with 5-carboxy-1-carboxymethyl-2-oxidopyridinium and 1,10-phenanthroline. The Mn^II atom is coordinated by two N atoms from the 1,10-phenanthroline ligand, two O atoms from two 5-carboxylato-1-carboxylatomethyl-2-oxidopyridinium ligands and two water molecules, leading to a distorted octahedral MnN₂O₄ environment. Intermolecular O—H⋯O hydrogen bonds link neighbouring molecules into a layer structure parallel to (001).

Related literature

For the synthesis of compounds with multicarboxylate ligands and metal centers, see: He et al. (2008 ▶); Huang et al. (2008 ▶); Jiang et al. (2009 ▶); Tong et al. (2005 ▶).

Experimental

Crystal data

[Mn₂(C₈H₅NO₅)₂(C₁₂H₈N₂)₂(H₂O)₄]·2H₂O
M _r = 968.64
Triclinic,
a = 7.7726 (11) Å
b = 9.9519 (14) Å
c = 15.411 (3) Å
α = 98.744 (10)°
β = 103.553 (10)°
γ = 110.252 (7)°
V = 1051.1 (3) Å³
Z = 1
Mo Kα radiation
μ = 0.68 mm⁻¹
T = 293 K
0.60 × 0.15 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.885, T _max = 0.934
19359 measured reflections
4779 independent reflections
3675 reflections with I > 2σ(I)
R _int = 0.171

Refinement

R[F ² > 2σ(F ²)] = 0.051
wR(F ²) = 0.141
S = 1.00
4779 reflections
307 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.81 e Å⁻³
Δρ_min = −0.79 e Å⁻³

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); 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.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809017668/at2783sup1.cif

e-65-0m654-sup1.cif^{(23.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809017668/at2783Isup2.hkl

e-65-0m654-Isup2.hkl^{(234.1KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O4ⁱ	0.831 (16)	1.967 (18)	2.773 (2)	163 (3)
O1W—H1WB⋯O3Wⁱⁱ	0.822 (15)	1.920 (15)	2.730 (2)	169 (3)
O2W—H2WA⋯O4	0.807 (16)	1.998 (15)	2.783 (2)	164 (2)
O2W—H2WA⋯O5	0.807 (16)	2.57 (3)	2.984 (2)	114 (2)
O2W—H2WB⋯O1ⁱⁱⁱ	0.856 (16)	1.959 (16)	2.806 (2)	170 (3)
O3W—H3WA⋯O1	0.833 (17)	1.962 (19)	2.775 (2)	165 (3)

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) .

supplementary crystallographic information

Comment

There is intensely research on the synthesis of compounds with multicarboxylate ligands and metal centers for their potential applications and coloful coordination methods. A large number of these compounds have been synthesized (He et al., 2008; Huang et al., 2008; Jiang et al.,2009; Tong et al., 2005). As illustrated in Fig. 1, the Mn^II atom is coordinated by two nitrogen atoms from one 1,10-phenanthroline molecule, two oxygen atoms from two 5-carboxyl-1-carboxymethyl-2-oxidopyridinium ligands and two wate molecules. Four coordinated atoms of N2, N3, O5 and O2A constitute the base of the octahedral, whereas O1W and O2W atoms occupy the apical position. The intermolecular hydrogen bonds play an important role in the formation of the one-dimensional chain. As shown in Fig. 2. The intermolecular O—H···O hydrogen bonds link the neibouring molecules to a one-dimensional chain.

Experimental

A mixture of 0.5 mmol 5-carboxyl-1-carboxymethyl-2-oxidopyridinium, 0.5 mmol 1,10-phenanthroline and 0.5 mmol of manganese chloride in 10 ml distilled water was stirred for 30 min at 323 K, then the reaction mixture was filtered and well shaped yellow crystals of the title compound was obtained from the mother liquor by slow evaporation at room temperature for several days.