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CHEMISTRY
ISSN: 2053-2296

Poly[tetra-μ2-L-lactato-indium(III)sodium(I)]

aCollege of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang, Jiangxi 330022, People's Republic of China
*Correspondence e-mail: qyliuchem@hotmail.com

(Received 15 March 2011; accepted 11 April 2011; online 15 April 2011)

The asymmetric unit of the title compound, [InNa(C3H5O3)4]n, consists of one InIII ion, one NaI ion and four crystallographically independent L-lactate monoanions. The coordination of the InIII ion is composed of five carboxyl­ate O and two hy­droxy O atoms in a distorted penta­gonal–bipyramidal coordination geometry. The NaI ion is six-coordinated by four carboxyl­ate O atoms and two hy­droxy O atoms from four L-lactate ligands in a distorted octa­hedral geometry. Each InIII ion is coordinated by four surrounding L-lactate ligands to form an [In(L-lactate)4] unit, which is further linked by NaI ions through Na—O bonds to give a two-dimensional layered structure. Hydrogen bonds between the hy­droxy groups and carboxyl­ate O atoms are observed between neighbouring layers.

Comment

The construction of coordination polymers with desired properties from multifunctional ligands with metal ions is of current inter­est and great importance because these materials can exhibit a variety of physical properties, such as catalysis, mol­ecular magnetism, photoluminescence, adsorption and phase separation (Janiak, 2003[Janiak, C. (2003). J. Chem. Soc. Dalton Trans. pp. 2781-2804.]; Kitagawa et al., 2004[Kitagawa, S., Kitaura, R. & Noro, S. I. (2004). Angew. Chem. Int. Ed. 43, 2334-2375.]; O'Keeffe et al., 2000[O'Keeffe, M., Eddaoudi, M., Li, H. L., Reineke, T. & Yaghi, O. M. (2000). J. Solid State Chem. 152, 3-20.]). The rational synthesis of these materials, however, remains a great challenge. Ionothermal synthesis, a new synthetic methodology developed recently involving the use of an ionic liquid as both solvent and template in the preparation of crystalline solids, offers many advantages over traditional hydro­thermal and solvothermal materials synthesis methods (Parnham & Morris, 2007[Parnham, E. R. & Morris, R. E. (2007). Acc. Chem. Res. 40, 1005-1013.]; Reichert et al., 2006[Reichert, W. M., Holbrey, J. D., Vigour, K. B., Morgan, T. D., Broker, G. A. & Rogers, R. D. (2006). Chem. Commun. pp. 4767-4779.]). Compared with traditional hydro­thermal and solvothermal methods, the change from mol­ecular to ionic reaction media leads to new types of materials being accessible, with structural properties that may be traced directly to the chemistry of the ionic liquid (IL) (Chen et al., 2008[Chen, S. M., Zhang, J. & Bu, X. H. (2008). Inorg. Chem. 47, 5567-5569.]; Zhang et al., 2010[Zhang, N., Liu, Q.-Y., Wang, Y.-L., Shan, Z.-M., Yang, E.-L. & Hu, H.-C. (2010). Inorg. Chem. Commun. 13, 706-710.]). Therefore, the ionic species of ILs may control the structures of the materials formed in ionothermal synthesis. There are some examples in which ILs have been successfully applied to the syntheses of novel coordination compounds (Chen et al., 2009[Chen, W.-X., Ren, Y.-P., Long, L.-S., Huang, R.-B. & Zheng, L.-S. (2009). CrystEngComm, 11, 1522-1525.]; Xu et al., 2007[Xu, L., Choi, E.-Y. & Kwon, Y.-U. (2007). Inorg. Chem. 46, 10670-10680.]). Of particular inter­est is a recent study by Morris and co-workers (Lin et al., 2007[Lin, Z., Slawin, A. M. Z. & Morris, R. E. (2007). J. Am. Chem. Soc. 129, 4880-4881.]) on the use of an enantio­pure anion as one component of the IL to induce homochirality in a nickel(II) structure constructed of entirely achiral building blocks, despite the fact that the anion of the IL is not occluded by the material. Nevertheless, there are still relatively few examples of coordination polymers prepared by ionothermal reaction to date.

[Scheme 1]

The InIII ion is liable to hydrolysis, which limits its use in the construction of coordination compounds under hydro­thermal or solvothermal conditions. However, InIII ions can be used to construct new frameworks under ionothermal conditions because the InIII ion will not hydrolyse in IL solvents. A series of In compounds prepared under ionothermal reaction conditions has been reported recently (Zhang et al., 2008[Zhang, J., Chen, S. M. & Bu, X. H. (2008). Angew. Chem. Int. Ed. 47, 5434-5437.]). We report here the title indium compound, poly[tetra-μ2-L-lactato-indium(III)sodium(I)], (I)[link]. To the best of our knowledge, no indium compound based on the lactate ligand has been reported previously.

The asymmetric unit of (I)[link] consists of one InIII ion, one NaI ion and four L-lactate monoanions. As depicted in Fig. 1[link], the In1 ion is seven-coordinated by five carboxyl­ate O atoms (O1, O4, O7, O8 and O10) and two hy­droxy O atoms (O3 and O6) from four L-lactate ligands in a penta­gonal–bipyramidal coordination environment, with atoms O6 and O10 occupying the apical positions. The In—O bond lengths range from 2.133 (2) to 2.356 (2) Å and the O—In—O bond angles vary from 55.29 (8) to 164.80 (9)° (Table 1[link]). The Na1 ion is six-coordinated by two carboxyl­ate O atoms [O2 and O5ii; symmetry code: (ii) x − 1, y, z] and two hy­droxy O atoms [O12i and O9iii; symmetry codes: (i) −x + 1, y + [{1\over 2}], −z + [{1\over 2}]; (iii) −x + 1, y − [{1\over 2}], −z + [{1\over 2}]] in a distorted square-planar geometry, with two carboxyl­ate O atoms (O8iii and O11i) in the apical positions. The Na1 ion is surrounded by four L-lactate ligands, with Na1—O distances varying from 2.364 (3) to 2.476 (3) Å (Fig. 1[link] and Table 1[link]). The [NaO6] octa­hedron is distorted, with O—Na—O bond angles varying from 65.13 (8) to 175.47 (11)° (Table 1[link]).

Though all the L-lactate ligands bridge one InIII ion and one NaI ion, the four crystallographically independent L-lactate ligands display three different coordination modes. The first type of L-lactate ligand chelates an InIII ion through its hy­droxy O atom (O3) and one carboxyl­ate O atom (O1), and bridges an NaI ion through its second carboxyl­ate O atom (O2) (Fig. 2[link]). The second type of L-lactate ligand coordination is similar to the first; it chelates an NaI ion through its hy­droxy O atom (O12) and one carboxyl­ate O atom (O11), and bridges an InIII ion through its second carboxyl­ate O atom (O10). The third type of L-lactate ligand employs its carboxyl­ate group (O7 and O8) to chelate an InIII ion, and its hy­droxy O atom (O9) and one of its carboxyl­ate O atoms (O8) to chelate an NaI ion. Therefore, there is a μ2-O (O8) bridge present in this type of L-lactate ligand.

Each InIII ion is coordinated by four surrounding L-lactate ligands to form an [In(L-lactate)4] unit (Fig. 2[link]). Each of these [In(L-lactate)4] units is linked by four neighbouring NaI ions through Na—O bonds to generate a two-dimensional layer along the ab plane (Fig. 3[link]). Within the layer, there are hydrogen bonds between the hy­droxy groups and the carboxyl­ate O atoms [O3⋯O2i and O6⋯O5iv; symmetry code: (iv) −x + 2, y + [{1\over 2}], −z + [{1\over 2}]] (Table 2[link]). The two-dimensional layers are stacked along the c direction to produce the crystal packing (Fig. 4[link]). Inter­layer hydrogen bonds are observed between the hy­droxy groups and the carboxyl­ate O atoms [O9⋯O10v and O12⋯O7vi; symmetry codes: (v) x + [{1\over 2}], −y + [{3\over 2}], −z; (vi) x − [{1\over 2}], −y + [{1\over 2}], −z] (Table 2[link]).

Some coordination compounds incorporating the lactate ligand have been reported previously. Most of them are mononuclear structures, such as [Co(lactate)2(H2O)2]·H2O (Carballo et al., 2002[Carballo, R., Covelo, B., Vázquez-López, E. M., Castiñeiras, A. & Niclós, J. (2002). Z. Anorg. Allg. Chem. 628, 468-472.]), [Mn(lactate)2(H2O)2] (Lis, 1982[Lis, T. (1982). Acta Cryst. B38, 937-939.]) and [Al(lactate)3] (Bombi et al., 1990[Bombi, G. G., Corain, B., Sheikh-Osman, A. A. & Valle, G. C. (1990). Inorg. Chim. Acta, 171, 79-83.]). A few compounds with two-dimensional structures containing bridging lactate ligands have also been reported. However, all of them are homometallic compounds. For example, {[Eu(lactate)2(H2O)2]ClO4}n possesses a cationic two-dimensional laminar layer charged with the perchlorate ions (Qu et al., 2008[Qu, Z.-R., Ye, Q., Zhao, H., Fu, D.-W., Ye, H.-Y., Xiong, R.-G., Akutagawa, T. & Nakamura, T. (2008). Chem. Eur. J. 14, 3452-3456.]). In the [Cu(lactate)2]n complex (Balboa et al., 2007[Balboa, S., Castiñeiras, A., Herle, P. S. & Strähle, J. (2007). Z. Anorg. Allg. Chem. 633, 2420-2424.]), the lactate ligand chelates a CuII ion through its hy­droxy O atom and one carboxyl­ate O atom, and bridges one CuII ion through the second carboxyl­ate O atom, to generate a neutral two-dimensional framework where the basic structural unit is the mononuclear [Cu(lactate)2] unit.

[Figure 1]
Figure 1
The structure of (I)[link], showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Methyl H atoms have been omitted for clarity. [Symmetry codes: (i) −x + 1, y + [{1\over 2}], −z + [{1\over 2}]; (ii) x − 1, y, z; (iii) −x + 1, y − [{1\over 2}], −z + [{1\over 2}].]
[Figure 2]
Figure 2
A view of the [In(L-lactate)4] unit surrounded by four NaI ions. [Symmetry codes: (i) −x + 1, y + [{1\over 2}], −z + [{1\over 2}]; (iii) −x + 1, y − [{1\over 2}], −z + [{1\over 2}]; (vi) x + 1, y, z.]
[Figure 3]
Figure 3
A perspective view of the two-dimensional layered structure of (I)[link]. H atoms have been omitted for clarity. Dashed lines between hy­droxy O and carboxyl­ate O atoms indicate hydrogen bonds. [Symmetry codes: (i) −x + 1, y + [{1\over 2}], −z + [{1\over 2}]; (iv) −x + 2, y + [{1\over 2}], −z + [{1\over 2}].]
[Figure 4]
Figure 4
A view of the packing of (I)[link] along the a axis. H atoms have been omitted for clarity. Dashed lines between hy­droxy O and carboxyl­ate O atoms indicate inter­layer hydrogen bonds.

Experimental

In(NO3)3·4.5H2O (229.2 mg, 0.6 mmol) and the monosodium salt of 5-sulfoisophthalic acid (53.6 mg, 0.2 mmol) were mixed with 1-ethyl-3-methyl­imidazolium L-lactate (0.6 g) in a 25 ml Parr Teflon-lined stainless steel vessel. The vessel was sealed and heated to 413 K. The temperature was maintained for 12 d and then the mixture was allowed to cool naturally to obtain colourless crystals of (I)[link] [yield 51%, based on In(NO3)3·4.5H2O]. IR (KBr pellet, ν, cm−1): 3465, 3391, 3105, 2950, 1638, 1598, 1564, 1473, 1417, 1254, 1124, 1073, 954, 868, 776, 666, 588, 540, 518.

Crystal data
  • [InNa(C3H5O3)4]

  • Mr = 494.09

  • Orthorhombic, P 21 21 21

  • a = 9.4744 (12) Å

  • b = 9.5803 (12) Å

  • c = 19.145 (2) Å

  • V = 1737.7 (4) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.45 mm−1

  • T = 296 K

  • 0.18 × 0.13 × 0.09 mm

Data collection
  • Bruker APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.781, Tmax = 0.881

  • 10916 measured reflections

  • 4259 independent reflections

  • 3680 reflections with I > 2σ(I)

  • Rint = 0.029

Refinement
  • R[F2 > 2σ(F2)] = 0.029

  • wR(F2) = 0.057

  • S = 1.02

  • 4259 reflections

  • 247 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.45 e Å−3

  • Δρmin = −0.42 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), with 1766 Friedel pairs

  • Flack parameter: 0.03 (2)

Table 1
Selected geometric parameters (Å, °)

In1—O10 2.133 (2)
In1—O4 2.162 (2)
In1—O1 2.183 (2)
In1—O6 2.217 (2)
In1—O3 2.255 (2)
In1—O8 2.338 (2)
In1—O7 2.356 (2)
Na1—O12i 2.364 (3)
Na1—O5ii 2.423 (3)
Na1—O2 2.435 (3)
Na1—O8iii 2.437 (2)
Na1—O11i 2.462 (2)
Na1—O9iii 2.476 (3)
O10—In1—O4 122.10 (9)
O10—In1—O1 91.88 (9)
O4—In1—O1 81.77 (10)
O10—In1—O6 164.80 (9)
O4—In1—O6 73.05 (8)
O1—In1—O6 91.77 (10)
O10—In1—O3 83.36 (9)
O1—In1—O3 72.36 (9)
O6—In1—O3 83.70 (9)
O10—In1—O8 93.10 (8)
O6—In1—O8 75.68 (8)
O3—In1—O8 74.12 (8)
O10—In1—O7 87.13 (9)
O4—In1—O7 81.37 (9)
O6—In1—O7 94.55 (9)
O8—In1—O7 55.29 (8)
O12i—Na1—O2 99.82 (12)
O5ii—Na1—O2 88.19 (8)
O12i—Na1—O8iii 110.79 (10)
O5ii—Na1—O8iii 77.75 (9)
O2—Na1—O8iii 85.24 (10)
O12i—Na1—O11i 66.95 (9)
O5ii—Na1—O11i 103.98 (11)
O2—Na1—O11i 98.95 (12)
O8iii—Na1—O11i 175.47 (11)
O12i—Na1—O9iii 84.43 (10)
O5ii—Na1—O9iii 92.82 (11)
O8iii—Na1—O9iii 65.13 (8)
O11i—Na1—O9iii 110.47 (11)
Symmetry codes: (i) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) x-1, y, z; (iii) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3⋯O2i 0.86 (4) 1.76 (4) 2.620 (3) 177 (4)
O6—H6⋯O5iv 0.82 (4) 1.77 (4) 2.578 (4) 170 (4)
O9—H9⋯O10v 0.83 (4) 2.26 (4) 3.087 (4) 173 (4)
O12—H12⋯O7vi 0.87 (4) 2.05 (4) 2.916 (3) 173 (4)
Symmetry codes: (i) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iv) [-x+2, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (v) [x+{\script{1\over 2}}], [-y+{\script{3\over 2}}, -z]; (vi) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z].

H atoms bonded to C atoms were placed in calculated positions and treated using a riding-model approximation, with C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl groups, and C—H = 0.98 Å and Uiso(H) = 1.2Ueq(C) for methyl­idyne groups. Hy­droxy H atoms were located in a difference map and refined with Uiso(H) = 1.5Ueq(O).

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND (Brandenburg, 2005[Brandenburg, K. (2005). DIAMOND. Version 3.0. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The construction of coordination polymers with desired properties from multifunctional ligands with metal ions is of current interest and great importance because these materials can exhibit a variety of physical properties, such as catalysis, molecular magnetism, photoluminescence, adsorption and phase separation (Janiak, 2003; Kitagawa et al., 2004; O'Keeffe et al., 2000). The rational synthesis of these materials, however, remains a great challenge. Ionothermal synthesis, a new synthetic methodology developed recently involving the use of an ionic liquid as solvent and template in the preparation of crystalline solids, offers many advantages over traditional hydrothermal and solvothermal materials synthesis methods (Parnham & Morris, 2007; Reichert et al., 2006). Compared with traditional hydrothermal and solvothermal methods, the change from molecular to ionic reaction media leads to new types of materials being accessible, with structural properties that may be traced directly to the chemistry of the ionic liquid (IL) (Chen et al., 2008; Zhang et al., 2010). Therefore, the ionic species of ILs may control the structures of the materials formed in ionothermal synthesis. There are some examples in which ILs have been successfully applied to the syntheses of novel coordination compounds (Chen et al., 2009; Xu et al., 2007). Of particular interest is a recent study by Morris and co-workers (Lin et al., 2007) on the use of an enantiopure anion as one component of the IL to induce homochirality in a nickel(II) structure constructed of entirely achiral building blocks, despite the fact that the anion of the IL is not occluded by the material. Nevertheless, there are still relatively few examples of coordination polymers prepared under ionothermal reaction to date.

The InIII ion is liable to hydrolysis, which limits its use in the construction of coordination compounds under hydrothermal or solvothermal conditions. However, InIII ions can be used to construct new frameworks under ionothermal conditions beacuse the InIII ion will not hydrolyse in IL solvents. A series of In compounds prepared under ionothermal reaction conditions have been reported recently (Zhang et al., 2008). We report here the title indium compound, [InNa(C3H5O3)4]n, (I). To the best of our knowledge, no indium compound based on the lactate ligand has been reported previously.

The asymmetric unit of (I) consists of one InIII ion, one NaI ion and four L-lactate monoanions. As depicted in Fig. 1, the In1 ion is seven-coordinated by five carboxylate O atoms (O1, O4, O7, O8 and O10) and two hydroxy O atoms (O3 and O6) from four L-lactate ligands in a pentagonal–bipyramidal coordination environment, with atoms O6 and O10 occupying the apical positions. The In—O bond lengths range from 2.133 (2) to 2.356 (2) Å and the O—In—O bond angles vary from 55.29 (8) to 164.80 (9)° (Table 1). The Na1 ion is six-coordinated by two carboxylate O atoms [O2 and O5ii; symmetry code: (ii) x - 1, y, z] and two hydroxy O atoms [O12i and O9iii; symmetry codes: (i) -x + 1, y + 1/2, -z + 1/2; (iii) -x + 1, y - 1/2, -z + 1/2] in a distorted square-planar geometry, with two carboxylate O atoms (O8iii and O11i) in the apical positions. The Na1 ion is surrounded by four L-lactate ligands, with Na1—O distances varying from 2.364 (3) to 2.476 (3) Å (Fig. 1 and Table 1). The [NaO6] octahedron is distorted, with O—Na—O bond angles varying from 65.13 (8) to 175.47 (11)° (Table 1).

Though all the L-lactate ligands bridge one InIII ion and one NaI ion, the four crystallographically independent L-lactate ligands display three different coordination modes. The first type of L-lactate ligand chelates an InIII ion through its hydroxy O atom (O3) and one carboxylate O atom (O1), and bridges an NaI ion through its second carboxylate O atom (O2) (Fig. 2). The second type of L-lactate ligand coordination is similar to the first: it chelates an NaI ion through its hydroxy O atom (O12) and one carboxylate O atom (O11), and bridges an InIII ion through its second carboxylate O atom (O10). The third type of L-lactate ligand employs its carboxylate group (O7 and O8) to chelate an InIII ion, and its hydroxy O atom (O9) and one of its carboxylate O atoms (O8) to chelate an NaI ion. Therefore, there is a µ2-O (O8) bridge present in this type of L-lactate ligand.

Each InIII ion is coordinated by four surrounding L-lactate ligands to form an [In(L-lactate)4]- unit (Fig. 2). Each of these [In(L-lactate)4]- units is linked by four neighbouring NaI ions through Na—O bonds to generate a two-dimensional layer along the ab plane (Fig. 3). Within the layer, there are hydrogen bonds between the hydroxy groups and the carboxylate O atoms [O3···O2i and O6···O5iv; symmetry code: (iv) -x + 2, y + 1/2, -z + 1/2] (Table 2). The two-dimensional layers are stacked along the c direction to produce the crystal packing (Fig. 4). Interlayer hydrogen bonds are observed between the hydroxy groups and the carboxylate O atoms [O9···O10v and O12···O7vi; symmetry codes: (v) x + 1/2, -y + 3/2, -z; (vi) x - 1/2, -y + 1/2, -z.] (Table 2).

Some coordination compounds with the lactate ligand have been reported previously. Most of them are mononuclear structures, such as [Co(lactate)2(H2O)2](H2O) (Carballo et al., 2002), [Mn(lactate)2(H2O)2] (Lis, 1982) and [Al(lactate)3] (Bombi et al., 1990). A few compounds with two-dimensional structures containing bridging lactate ligands have also been reported. However, all of them are homometallic compounds. For example, the {[Eu(lactate)2(H2O)2](ClO4)}n compound possess a cationic two-dimensional laminar layer charged with the perchlorate ions (Qu et al., 2008). In the [Cu(lactate)2]n complex (Balboa et al., 2007), the lactate ligand chelates a CuII ion through its hydroxy O atom and one carboxylate O atom, and bridges one CuII ion through the second carboxylate O atom, to generate a neutral two-dimensional framework where the basic structrual unit is the mononuclear [Cu(lactate)2] unit.

Related literature top

For related literature, see: Balboa et al. (2007); Bombi et al. (1990); Carballo et al. (2002); Chen et al. (2008, 2009); Janiak (2003); Kitagawa et al. (2004); Lin et al. (2007); Lis (1982); O'Keeffe et al. (2000); Parnham & Morris (2007); Qu et al. (2008); Reichert et al. (2006); Xu et al. (2007); Zhang et al. (2008, 2010).

Experimental top

In(NO3)3.4.5H2O (229.2 mg, 0.6 mmol) and 5-sulfoisophthalic acid monosodium salt (53.6 mg, 0.2 mmol) were mixed with 0.6 g 1-ethyl-3-methylimidazolium-L-lactate in a Parr 25 ml Teflon-lined stainless steel vessel. The vessel was sealed and heated to 413 K. The temperature was maintained for 12 d and then the mixture was cooled naturally to obtain colourless crystals of (I) [yield 51%, based on In(NO3)3.4.5H2O]. Spectroscopic analysis: IR (KBr pellet, ν, cm-1): 3465, 3391, 3105, 2950, 1638, 1598, 1564, 1473, 1417, 1254, 1124, 1073, 954, 868, 776, 666, 588, 540, 518.

Refinement top

H atoms bonded to C atoms were placed in calculated positions and treated using a riding-model approximation, with C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl groups, and C—H = 0.98 Å and Uiso(H) = 1.2Ueq(C) for methylidyne groups. Hydroxy H atoms were located in a difference map and refined with Uiso(H) = 1.5Ueq(O).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Methyl H atoms have been omitted for clarity. [Symmetry codes: (i) -x + 1, y + 1/2, -z + 1/2; (ii) x - 1, y, z; (iii) -x + 1, y - 1/2, -z + 1/2.]
[Figure 2] Fig. 2. A view of the [In(L-lactate)4]- unit surrounded by four NaI ions. [Symmetry codes: (i) -x + 1, y + 1/2, -z + 1/2; (iii) -x + 1, y - 1/2, -z + 1/2; (vi) x + 1, y, z.]
[Figure 3] Fig. 3. A perspective view of the two-dimensional layered structure of (I). H atoms have been omitted for clarity. Dotted lines between hydroxy O and carboxylate O atoms indicate hydrogen bonds. [Symmetry codes: (i) -x + 1, y + 1/2, -z + 1/2; (iv) -x + 2, y + 1/2, -z + 1/2.]
[Figure 4] Fig. 4. A view of the packing of (I), along the a axis. H atoms have been omitted for clarity. Dotted lines between hydroxy O and carboxylate O atoms indicate interlayer hydrogen bonds.
Poly[tetra-µ2-L-lactato-indium(III)sodium(I)] top
Crystal data top
[InNa(C3H5O3)4]Dx = 1.889 Mg m3
Mr = 494.09Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 4051 reflections
a = 9.4744 (12) Åθ = 2.4–27.8°
b = 9.5803 (12) ŵ = 1.45 mm1
c = 19.145 (2) ÅT = 296 K
V = 1737.7 (4) Å3Prism, colourless
Z = 40.18 × 0.13 × 0.09 mm
F(000) = 992
Data collection top
Bruker APEXII area-detector
diffractometer
4259 independent reflections
Radiation source: fine-focus sealed tube3680 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
ω scansθmax = 29.1°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1012
Tmin = 0.781, Tmax = 0.881k = 1211
10916 measured reflectionsl = 2524
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.029H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057 w = 1/[σ2(Fo2) + (0.0226P)2 + 0.1617P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
4259 reflectionsΔρmax = 0.45 e Å3
247 parametersΔρmin = 0.42 e Å3
0 restraintsAbsolute structure: Flack (1983), with 1766 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.03 (2)
Crystal data top
[InNa(C3H5O3)4]V = 1737.7 (4) Å3
Mr = 494.09Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 9.4744 (12) ŵ = 1.45 mm1
b = 9.5803 (12) ÅT = 296 K
c = 19.145 (2) Å0.18 × 0.13 × 0.09 mm
Data collection top
Bruker APEXII area-detector
diffractometer
4259 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3680 reflections with I > 2σ(I)
Tmin = 0.781, Tmax = 0.881Rint = 0.029
10916 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.029H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057Δρmax = 0.45 e Å3
S = 1.02Δρmin = 0.42 e Å3
4259 reflectionsAbsolute structure: Flack (1983), with 1766 Friedel pairs
247 parametersAbsolute structure parameter: 0.03 (2)
0 restraints
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
xyzUiso*/Ueq
In10.74771 (3)0.528992 (19)0.160204 (9)0.02032 (6)
Na10.2434 (2)0.48419 (11)0.39058 (6)0.0296 (3)
C10.5051 (4)0.4774 (5)0.2605 (2)0.0243 (9)
C20.4461 (4)0.6048 (4)0.22333 (18)0.0318 (9)
H20.42510.67760.25780.038*
C30.3134 (5)0.5677 (6)0.1845 (3)0.085 (2)
H3A0.27710.64930.16160.127*
H3B0.24440.53290.21680.127*
H3C0.33400.49730.15030.127*
C40.9811 (4)0.4819 (5)0.26467 (19)0.0216 (9)
C50.9469 (4)0.6319 (3)0.28158 (16)0.0243 (7)
H51.03170.68860.27420.029*
C60.9000 (5)0.6482 (5)0.35579 (17)0.0564 (14)
H6A0.87890.74460.36480.085*
H6B0.97390.61780.38650.085*
H6C0.81700.59280.36360.085*
C70.8894 (4)0.6863 (3)0.06632 (17)0.0253 (7)
C80.9838 (4)0.7789 (4)0.02157 (17)0.0265 (8)
H80.99570.73640.02460.032*
C91.1264 (4)0.7923 (4)0.05664 (19)0.0367 (9)
H9A1.18660.85050.02880.055*
H9B1.16820.70150.06140.055*
H9C1.11470.83340.10200.055*
C100.6526 (4)0.2970 (3)0.07842 (16)0.0248 (7)
C110.5578 (4)0.2150 (3)0.02921 (17)0.0261 (8)
H110.55080.26440.01550.031*
C120.4134 (4)0.2011 (5)0.0607 (2)0.0495 (11)
H12A0.35340.15030.02940.074*
H12B0.37450.29230.06870.074*
H12C0.42000.15200.10430.074*
O10.6229 (3)0.4288 (3)0.24191 (13)0.0291 (6)
O20.4306 (3)0.4265 (3)0.30834 (13)0.0333 (7)
O30.5494 (3)0.6559 (2)0.17475 (12)0.0272 (6)
H30.553 (4)0.745 (4)0.1792 (18)0.041*
O40.9176 (3)0.4232 (2)0.21391 (12)0.0271 (6)
O51.0742 (3)0.4246 (3)0.30051 (13)0.0287 (7)
O60.8383 (3)0.6802 (2)0.23555 (12)0.0271 (6)
H60.856 (4)0.760 (4)0.2242 (19)0.041*
O70.9266 (3)0.5612 (2)0.07629 (12)0.0342 (6)
O80.7802 (2)0.7326 (2)0.09477 (11)0.0265 (6)
O90.9175 (3)0.9112 (3)0.01432 (14)0.0357 (6)
H90.971 (5)0.961 (5)0.009 (2)0.054*
O100.6278 (3)0.4302 (2)0.07989 (12)0.0312 (6)
O110.7416 (4)0.2405 (2)0.11515 (11)0.0389 (6)
O120.6205 (3)0.0815 (3)0.01805 (14)0.0397 (7)
H120.566 (5)0.043 (5)0.013 (2)0.060*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
In10.02124 (10)0.01809 (9)0.02163 (9)0.00056 (17)0.00087 (17)0.00144 (8)
Na10.0299 (7)0.0282 (6)0.0307 (6)0.0021 (10)0.0040 (9)0.0015 (5)
C10.034 (2)0.0155 (18)0.023 (2)0.0036 (19)0.0004 (17)0.0001 (19)
C20.033 (2)0.0273 (19)0.036 (2)0.0079 (16)0.0159 (17)0.0079 (15)
C30.024 (2)0.137 (5)0.093 (4)0.008 (3)0.003 (2)0.070 (4)
C40.0196 (19)0.019 (2)0.027 (2)0.0005 (17)0.0023 (16)0.0000 (19)
C50.0239 (19)0.0198 (16)0.0291 (18)0.0022 (14)0.0063 (14)0.0004 (14)
C60.080 (4)0.060 (3)0.029 (2)0.038 (3)0.006 (2)0.0077 (19)
C70.032 (2)0.0237 (17)0.0203 (16)0.0028 (14)0.0023 (15)0.0037 (14)
C80.033 (2)0.0228 (18)0.0237 (17)0.0046 (14)0.0049 (16)0.0011 (14)
C90.034 (2)0.039 (2)0.037 (2)0.0011 (18)0.0059 (18)0.0003 (17)
C100.0251 (19)0.0284 (18)0.0209 (16)0.0058 (15)0.0015 (14)0.0040 (14)
C110.035 (2)0.0156 (16)0.0275 (17)0.0014 (14)0.0070 (15)0.0021 (13)
C120.034 (3)0.052 (3)0.062 (3)0.009 (2)0.006 (2)0.013 (2)
O10.0270 (15)0.0249 (14)0.0354 (14)0.0068 (11)0.0075 (12)0.0107 (12)
O20.0410 (18)0.0241 (15)0.0349 (16)0.0030 (14)0.0168 (14)0.0095 (13)
O30.0323 (14)0.0143 (11)0.0348 (14)0.0010 (10)0.0106 (11)0.0048 (10)
O40.0303 (15)0.0183 (12)0.0327 (14)0.0050 (11)0.0054 (11)0.0058 (11)
O50.0281 (16)0.0233 (14)0.0347 (15)0.0043 (13)0.0076 (13)0.0022 (12)
O60.0347 (15)0.0134 (12)0.0331 (13)0.0007 (11)0.0124 (11)0.0033 (10)
O70.0445 (17)0.0195 (13)0.0385 (14)0.0033 (11)0.0089 (12)0.0018 (11)
O80.0252 (18)0.0300 (12)0.0244 (10)0.0013 (10)0.0047 (10)0.0023 (9)
O90.0386 (16)0.0256 (13)0.0429 (15)0.0057 (12)0.0088 (13)0.0109 (12)
O100.0431 (16)0.0186 (12)0.0320 (13)0.0054 (11)0.0009 (12)0.0040 (10)
O110.0370 (15)0.0399 (13)0.0397 (12)0.0017 (19)0.0129 (19)0.0079 (10)
O120.0471 (18)0.0239 (13)0.0481 (16)0.0074 (12)0.0173 (14)0.0151 (12)
Geometric parameters (Å, º) top
In1—O102.133 (2)C6—H6B0.9600
In1—O42.162 (2)C6—H6C0.9600
In1—O12.183 (2)C7—O81.250 (4)
In1—O62.217 (2)C7—O71.264 (4)
In1—O32.255 (2)C7—C81.523 (5)
In1—O82.338 (2)C8—O91.422 (4)
In1—O72.356 (2)C8—C91.514 (5)
Na1—O12i2.364 (3)C8—H80.9800
Na1—O5ii2.423 (3)C9—H9A0.9600
Na1—O22.435 (3)C9—H9B0.9600
Na1—O8iii2.437 (2)C9—H9C0.9600
Na1—O11i2.462 (2)C10—O111.224 (4)
Na1—O9iii2.476 (3)C10—O101.298 (4)
C1—O21.254 (4)C10—C111.521 (5)
C1—O11.261 (4)C11—O121.426 (4)
C1—C21.520 (5)C11—C121.501 (5)
C2—O31.436 (4)C11—H110.9800
C2—C31.503 (6)C12—H12A0.9600
C2—H20.9800C12—H12B0.9600
C3—H3A0.9600C12—H12C0.9600
C3—H3B0.9600O3—H30.86 (4)
C3—H3C0.9600O5—Na1iv2.423 (3)
C4—O51.245 (4)O6—H60.82 (4)
C4—O41.273 (4)O8—Na1i2.437 (2)
C4—C51.509 (6)O9—Na1i2.476 (3)
C5—O61.431 (4)O9—H90.83 (4)
C5—C61.497 (4)O11—Na1iii2.462 (2)
C5—H50.9800O12—Na1iii2.364 (3)
C6—H6A0.9600O12—H120.87 (4)
O10—In1—O4122.10 (9)C4—C5—H5108.8
O10—In1—O191.88 (9)C5—C6—H6A109.5
O4—In1—O181.77 (10)C5—C6—H6B109.5
O10—In1—O6164.80 (9)H6A—C6—H6B109.5
O4—In1—O673.05 (8)C5—C6—H6C109.5
O1—In1—O691.77 (10)H6A—C6—H6C109.5
O10—In1—O383.36 (9)H6B—C6—H6C109.5
O4—In1—O3144.51 (8)O8—C7—O7120.1 (3)
O1—In1—O372.36 (9)O8—C7—C8121.6 (3)
O6—In1—O383.70 (9)O7—C7—C8118.3 (3)
O10—In1—O893.10 (8)O9—C8—C9111.2 (3)
O4—In1—O8123.19 (9)O9—C8—C7108.4 (3)
O1—In1—O8145.26 (8)C9—C8—C7108.9 (3)
O6—In1—O875.68 (8)O9—C8—H8109.5
O3—In1—O874.12 (8)C9—C8—H8109.5
O10—In1—O787.13 (9)C7—C8—H8109.5
O4—In1—O781.37 (9)C8—C9—H9A109.5
O1—In1—O7159.40 (9)C8—C9—H9B109.5
O6—In1—O794.55 (9)H9A—C9—H9B109.5
O3—In1—O7127.81 (8)C8—C9—H9C109.5
O8—In1—O755.29 (8)H9A—C9—H9C109.5
O12i—Na1—O5ii168.59 (12)H9B—C9—H9C109.5
O12i—Na1—O299.82 (12)O11—C10—O10123.2 (3)
O5ii—Na1—O288.19 (8)O11—C10—C11122.3 (3)
O12i—Na1—O8iii110.79 (10)O10—C10—C11114.5 (3)
O5ii—Na1—O8iii77.75 (9)O12—C11—C12111.1 (3)
O2—Na1—O8iii85.24 (10)O12—C11—C10108.1 (3)
O12i—Na1—O11i66.95 (9)C12—C11—C10109.6 (3)
O5ii—Na1—O11i103.98 (11)O12—C11—H11109.3
O2—Na1—O11i98.95 (12)C12—C11—H11109.3
O8iii—Na1—O11i175.47 (11)C10—C11—H11109.3
O12i—Na1—O9iii84.43 (10)C11—C12—H12A109.5
O5ii—Na1—O9iii92.82 (11)C11—C12—H12B109.5
O2—Na1—O9iii149.32 (10)H12A—C12—H12B109.5
O8iii—Na1—O9iii65.13 (8)C11—C12—H12C109.5
O11i—Na1—O9iii110.47 (11)H12A—C12—H12C109.5
O2—C1—O1124.1 (4)H12B—C12—H12C109.5
O2—C1—C2116.6 (4)C1—O1—In1121.3 (3)
O1—C1—C2119.3 (3)C1—O2—Na1142.5 (3)
O3—C2—C3109.3 (3)C2—O3—In1117.67 (19)
O3—C2—C1109.1 (3)C2—O3—H3108 (3)
C3—C2—C1110.4 (4)In1—O3—H3121 (3)
O3—C2—H2109.3C4—O4—In1120.5 (3)
C3—C2—H2109.3C4—O5—Na1iv139.2 (3)
C1—C2—H2109.3C5—O6—In1117.89 (18)
C2—C3—H3A109.5C5—O6—H6109 (3)
C2—C3—H3B109.5In1—O6—H6121 (3)
H3A—C3—H3B109.5C7—O7—In191.5 (2)
C2—C3—H3C109.5C7—O8—In192.69 (19)
H3A—C3—H3C109.5C7—O8—Na1i118.5 (2)
H3B—C3—H3C109.5In1—O8—Na1i138.69 (10)
O5—C4—O4124.1 (4)C8—O9—Na1i116.9 (2)
O5—C4—C5117.0 (4)C8—O9—H9107 (3)
O4—C4—C5118.9 (3)Na1i—O9—H9128 (3)
O6—C5—C6109.7 (3)C10—O10—In1110.8 (2)
O6—C5—C4109.3 (3)C10—O11—Na1iii117.1 (2)
C6—C5—C4111.5 (3)C11—O12—Na1iii118.0 (2)
O6—C5—H5108.8C11—O12—H12104 (3)
C6—C5—H5108.8Na1iii—O12—H12131 (3)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x1, y, z; (iii) x+1, y1/2, z+1/2; (iv) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O2i0.86 (4)1.76 (4)2.620 (3)177 (4)
O6—H6···O5v0.82 (4)1.77 (4)2.578 (4)170 (4)
O9—H9···O10vi0.83 (4)2.26 (4)3.087 (4)173 (4)
O12—H12···O7vii0.87 (4)2.05 (4)2.916 (3)173 (4)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (v) x+2, y+1/2, z+1/2; (vi) x+1/2, y+3/2, z; (vii) x1/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula[InNa(C3H5O3)4]
Mr494.09
Crystal system, space groupOrthorhombic, P212121
Temperature (K)296
a, b, c (Å)9.4744 (12), 9.5803 (12), 19.145 (2)
V3)1737.7 (4)
Z4
Radiation typeMo Kα
µ (mm1)1.45
Crystal size (mm)0.18 × 0.13 × 0.09
Data collection
DiffractometerBruker APEXII area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.781, 0.881
No. of measured, independent and
observed [I > 2σ(I)] reflections
10916, 4259, 3680
Rint0.029
(sin θ/λ)max1)0.683
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.057, 1.02
No. of reflections4259
No. of parameters247
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.45, 0.42
Absolute structureFlack (1983), with 1766 Friedel pairs
Absolute structure parameter0.03 (2)

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
In1—O102.133 (2)Na1—O12i2.364 (3)
In1—O42.162 (2)Na1—O5ii2.423 (3)
In1—O12.183 (2)Na1—O22.435 (3)
In1—O62.217 (2)Na1—O8iii2.437 (2)
In1—O32.255 (2)Na1—O11i2.462 (2)
In1—O82.338 (2)Na1—O9iii2.476 (3)
In1—O72.356 (2)
O10—In1—O4122.10 (9)O8—In1—O755.29 (8)
O10—In1—O191.88 (9)O12i—Na1—O299.82 (12)
O4—In1—O181.77 (10)O5ii—Na1—O288.19 (8)
O10—In1—O6164.80 (9)O12i—Na1—O8iii110.79 (10)
O4—In1—O673.05 (8)O5ii—Na1—O8iii77.75 (9)
O1—In1—O691.77 (10)O2—Na1—O8iii85.24 (10)
O10—In1—O383.36 (9)O12i—Na1—O11i66.95 (9)
O1—In1—O372.36 (9)O5ii—Na1—O11i103.98 (11)
O6—In1—O383.70 (9)O2—Na1—O11i98.95 (12)
O10—In1—O893.10 (8)O8iii—Na1—O11i175.47 (11)
O6—In1—O875.68 (8)O12i—Na1—O9iii84.43 (10)
O3—In1—O874.12 (8)O5ii—Na1—O9iii92.82 (11)
O10—In1—O787.13 (9)O8iii—Na1—O9iii65.13 (8)
O4—In1—O781.37 (9)O11i—Na1—O9iii110.47 (11)
O6—In1—O794.55 (9)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x1, y, z; (iii) x+1, y1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O2i0.86 (4)1.76 (4)2.620 (3)177 (4)
O6—H6···O5iv0.82 (4)1.77 (4)2.578 (4)170 (4)
O9—H9···O10v0.83 (4)2.26 (4)3.087 (4)173 (4)
O12—H12···O7vi0.87 (4)2.05 (4)2.916 (3)173 (4)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (iv) x+2, y+1/2, z+1/2; (v) x+1/2, y+3/2, z; (vi) x1/2, y+1/2, z.
 

Acknowledgements

This work was support by the National Natural Science Foundation of China (grant No. 20901033), the Scientific Research Foundation for the Returned Overseas Chinese Scholars (SEM), the NSF of Jiangxi Provincial (grant No. 2009GZH0056) and the Project of Education Department of Jiangxi Province (grant Nos. GJJ10016 and GJJ11381).

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