Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270111013606/lg3055sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270111013606/lg3055Isup2.hkl |
CCDC reference: 829691
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).
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.
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); 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).
[InNa(C3H5O3)4] | Dx = 1.889 Mg m−3 |
Mr = 494.09 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 4051 reflections |
a = 9.4744 (12) Å | θ = 2.4–27.8° |
b = 9.5803 (12) Å | µ = 1.45 mm−1 |
c = 19.145 (2) Å | T = 296 K |
V = 1737.7 (4) Å3 | Prism, colourless |
Z = 4 | 0.18 × 0.13 × 0.09 mm |
F(000) = 992 |
Bruker APEXII area-detector diffractometer | 4259 independent reflections |
Radiation source: fine-focus sealed tube | 3680 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ω scans | θmax = 29.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→12 |
Tmin = 0.781, Tmax = 0.881 | k = −12→11 |
10916 measured reflections | l = −25→24 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.029 | H 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 reflections | Δρmax = 0.45 e Å−3 |
247 parameters | Δρmin = −0.42 e Å−3 |
0 restraints | Absolute structure: Flack (1983), with 1766 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.03 (2) |
[InNa(C3H5O3)4] | V = 1737.7 (4) Å3 |
Mr = 494.09 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 9.4744 (12) Å | µ = 1.45 mm−1 |
b = 9.5803 (12) Å | T = 296 K |
c = 19.145 (2) Å | 0.18 × 0.13 × 0.09 mm |
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 = 0.881 | Rint = 0.029 |
10916 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.057 | Δρmax = 0.45 e Å−3 |
S = 1.02 | Δρmin = −0.42 e Å−3 |
4259 reflections | Absolute structure: Flack (1983), with 1766 Friedel pairs |
247 parameters | Absolute structure parameter: 0.03 (2) |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
In1 | 0.74771 (3) | 0.528992 (19) | 0.160204 (9) | 0.02032 (6) | |
Na1 | 0.2434 (2) | 0.48419 (11) | 0.39058 (6) | 0.0296 (3) | |
C1 | 0.5051 (4) | 0.4774 (5) | 0.2605 (2) | 0.0243 (9) | |
C2 | 0.4461 (4) | 0.6048 (4) | 0.22333 (18) | 0.0318 (9) | |
H2 | 0.4251 | 0.6776 | 0.2578 | 0.038* | |
C3 | 0.3134 (5) | 0.5677 (6) | 0.1845 (3) | 0.085 (2) | |
H3A | 0.2771 | 0.6493 | 0.1616 | 0.127* | |
H3B | 0.2444 | 0.5329 | 0.2168 | 0.127* | |
H3C | 0.3340 | 0.4973 | 0.1503 | 0.127* | |
C4 | 0.9811 (4) | 0.4819 (5) | 0.26467 (19) | 0.0216 (9) | |
C5 | 0.9469 (4) | 0.6319 (3) | 0.28158 (16) | 0.0243 (7) | |
H5 | 1.0317 | 0.6886 | 0.2742 | 0.029* | |
C6 | 0.9000 (5) | 0.6482 (5) | 0.35579 (17) | 0.0564 (14) | |
H6A | 0.8789 | 0.7446 | 0.3648 | 0.085* | |
H6B | 0.9739 | 0.6178 | 0.3865 | 0.085* | |
H6C | 0.8170 | 0.5928 | 0.3636 | 0.085* | |
C7 | 0.8894 (4) | 0.6863 (3) | 0.06632 (17) | 0.0253 (7) | |
C8 | 0.9838 (4) | 0.7789 (4) | 0.02157 (17) | 0.0265 (8) | |
H8 | 0.9957 | 0.7364 | −0.0246 | 0.032* | |
C9 | 1.1264 (4) | 0.7923 (4) | 0.05664 (19) | 0.0367 (9) | |
H9A | 1.1866 | 0.8505 | 0.0288 | 0.055* | |
H9B | 1.1682 | 0.7015 | 0.0614 | 0.055* | |
H9C | 1.1147 | 0.8334 | 0.1020 | 0.055* | |
C10 | 0.6526 (4) | 0.2970 (3) | 0.07842 (16) | 0.0248 (7) | |
C11 | 0.5578 (4) | 0.2150 (3) | 0.02921 (17) | 0.0261 (8) | |
H11 | 0.5508 | 0.2644 | −0.0155 | 0.031* | |
C12 | 0.4134 (4) | 0.2011 (5) | 0.0607 (2) | 0.0495 (11) | |
H12A | 0.3534 | 0.1503 | 0.0294 | 0.074* | |
H12B | 0.3745 | 0.2923 | 0.0687 | 0.074* | |
H12C | 0.4200 | 0.1520 | 0.1043 | 0.074* | |
O1 | 0.6229 (3) | 0.4288 (3) | 0.24191 (13) | 0.0291 (6) | |
O2 | 0.4306 (3) | 0.4265 (3) | 0.30834 (13) | 0.0333 (7) | |
O3 | 0.5494 (3) | 0.6559 (2) | 0.17475 (12) | 0.0272 (6) | |
H3 | 0.553 (4) | 0.745 (4) | 0.1792 (18) | 0.041* | |
O4 | 0.9176 (3) | 0.4232 (2) | 0.21391 (12) | 0.0271 (6) | |
O5 | 1.0742 (3) | 0.4246 (3) | 0.30051 (13) | 0.0287 (7) | |
O6 | 0.8383 (3) | 0.6802 (2) | 0.23555 (12) | 0.0271 (6) | |
H6 | 0.856 (4) | 0.760 (4) | 0.2242 (19) | 0.041* | |
O7 | 0.9266 (3) | 0.5612 (2) | 0.07629 (12) | 0.0342 (6) | |
O8 | 0.7802 (2) | 0.7326 (2) | 0.09477 (11) | 0.0265 (6) | |
O9 | 0.9175 (3) | 0.9112 (3) | 0.01432 (14) | 0.0357 (6) | |
H9 | 0.971 (5) | 0.961 (5) | −0.009 (2) | 0.054* | |
O10 | 0.6278 (3) | 0.4302 (2) | 0.07989 (12) | 0.0312 (6) | |
O11 | 0.7416 (4) | 0.2405 (2) | 0.11515 (11) | 0.0389 (6) | |
O12 | 0.6205 (3) | 0.0815 (3) | 0.01805 (14) | 0.0397 (7) | |
H12 | 0.566 (5) | 0.043 (5) | −0.013 (2) | 0.060* |
U11 | U22 | U33 | U12 | U13 | U23 | |
In1 | 0.02124 (10) | 0.01809 (9) | 0.02163 (9) | 0.00056 (17) | −0.00087 (17) | 0.00144 (8) |
Na1 | 0.0299 (7) | 0.0282 (6) | 0.0307 (6) | −0.0021 (10) | −0.0040 (9) | −0.0015 (5) |
C1 | 0.034 (2) | 0.0155 (18) | 0.023 (2) | −0.0036 (19) | 0.0004 (17) | −0.0001 (19) |
C2 | 0.033 (2) | 0.0273 (19) | 0.036 (2) | 0.0079 (16) | 0.0159 (17) | 0.0079 (15) |
C3 | 0.024 (2) | 0.137 (5) | 0.093 (4) | −0.008 (3) | −0.003 (2) | 0.070 (4) |
C4 | 0.0196 (19) | 0.019 (2) | 0.027 (2) | −0.0005 (17) | 0.0023 (16) | 0.0000 (19) |
C5 | 0.0239 (19) | 0.0198 (16) | 0.0291 (18) | 0.0022 (14) | −0.0063 (14) | 0.0004 (14) |
C6 | 0.080 (4) | 0.060 (3) | 0.029 (2) | 0.038 (3) | −0.006 (2) | −0.0077 (19) |
C7 | 0.032 (2) | 0.0237 (17) | 0.0203 (16) | −0.0028 (14) | 0.0023 (15) | −0.0037 (14) |
C8 | 0.033 (2) | 0.0228 (18) | 0.0237 (17) | 0.0046 (14) | 0.0049 (16) | −0.0011 (14) |
C9 | 0.034 (2) | 0.039 (2) | 0.037 (2) | −0.0011 (18) | 0.0059 (18) | 0.0003 (17) |
C10 | 0.0251 (19) | 0.0284 (18) | 0.0209 (16) | −0.0058 (15) | 0.0015 (14) | −0.0040 (14) |
C11 | 0.035 (2) | 0.0156 (16) | 0.0275 (17) | 0.0014 (14) | −0.0070 (15) | −0.0021 (13) |
C12 | 0.034 (3) | 0.052 (3) | 0.062 (3) | −0.009 (2) | −0.006 (2) | −0.013 (2) |
O1 | 0.0270 (15) | 0.0249 (14) | 0.0354 (14) | 0.0068 (11) | 0.0075 (12) | 0.0107 (12) |
O2 | 0.0410 (18) | 0.0241 (15) | 0.0349 (16) | 0.0030 (14) | 0.0168 (14) | 0.0095 (13) |
O3 | 0.0323 (14) | 0.0143 (11) | 0.0348 (14) | −0.0010 (10) | 0.0106 (11) | 0.0048 (10) |
O4 | 0.0303 (15) | 0.0183 (12) | 0.0327 (14) | 0.0050 (11) | −0.0054 (11) | −0.0058 (11) |
O5 | 0.0281 (16) | 0.0233 (14) | 0.0347 (15) | 0.0043 (13) | −0.0076 (13) | −0.0022 (12) |
O6 | 0.0347 (15) | 0.0134 (12) | 0.0331 (13) | 0.0007 (11) | −0.0124 (11) | 0.0033 (10) |
O7 | 0.0445 (17) | 0.0195 (13) | 0.0385 (14) | 0.0033 (11) | 0.0089 (12) | 0.0018 (11) |
O8 | 0.0252 (18) | 0.0300 (12) | 0.0244 (10) | −0.0013 (10) | 0.0047 (10) | −0.0023 (9) |
O9 | 0.0386 (16) | 0.0256 (13) | 0.0429 (15) | 0.0057 (12) | 0.0088 (13) | 0.0109 (12) |
O10 | 0.0431 (16) | 0.0186 (12) | 0.0320 (13) | −0.0054 (11) | −0.0009 (12) | −0.0040 (10) |
O11 | 0.0370 (15) | 0.0399 (13) | 0.0397 (12) | −0.0017 (19) | −0.0129 (19) | −0.0079 (10) |
O12 | 0.0471 (18) | 0.0239 (13) | 0.0481 (16) | 0.0074 (12) | −0.0173 (14) | −0.0151 (12) |
In1—O10 | 2.133 (2) | C6—H6B | 0.9600 |
In1—O4 | 2.162 (2) | C6—H6C | 0.9600 |
In1—O1 | 2.183 (2) | C7—O8 | 1.250 (4) |
In1—O6 | 2.217 (2) | C7—O7 | 1.264 (4) |
In1—O3 | 2.255 (2) | C7—C8 | 1.523 (5) |
In1—O8 | 2.338 (2) | C8—O9 | 1.422 (4) |
In1—O7 | 2.356 (2) | C8—C9 | 1.514 (5) |
Na1—O12i | 2.364 (3) | C8—H8 | 0.9800 |
Na1—O5ii | 2.423 (3) | C9—H9A | 0.9600 |
Na1—O2 | 2.435 (3) | C9—H9B | 0.9600 |
Na1—O8iii | 2.437 (2) | C9—H9C | 0.9600 |
Na1—O11i | 2.462 (2) | C10—O11 | 1.224 (4) |
Na1—O9iii | 2.476 (3) | C10—O10 | 1.298 (4) |
C1—O2 | 1.254 (4) | C10—C11 | 1.521 (5) |
C1—O1 | 1.261 (4) | C11—O12 | 1.426 (4) |
C1—C2 | 1.520 (5) | C11—C12 | 1.501 (5) |
C2—O3 | 1.436 (4) | C11—H11 | 0.9800 |
C2—C3 | 1.503 (6) | C12—H12A | 0.9600 |
C2—H2 | 0.9800 | C12—H12B | 0.9600 |
C3—H3A | 0.9600 | C12—H12C | 0.9600 |
C3—H3B | 0.9600 | O3—H3 | 0.86 (4) |
C3—H3C | 0.9600 | O5—Na1iv | 2.423 (3) |
C4—O5 | 1.245 (4) | O6—H6 | 0.82 (4) |
C4—O4 | 1.273 (4) | O8—Na1i | 2.437 (2) |
C4—C5 | 1.509 (6) | O9—Na1i | 2.476 (3) |
C5—O6 | 1.431 (4) | O9—H9 | 0.83 (4) |
C5—C6 | 1.497 (4) | O11—Na1iii | 2.462 (2) |
C5—H5 | 0.9800 | O12—Na1iii | 2.364 (3) |
C6—H6A | 0.9600 | O12—H12 | 0.87 (4) |
O10—In1—O4 | 122.10 (9) | C4—C5—H5 | 108.8 |
O10—In1—O1 | 91.88 (9) | C5—C6—H6A | 109.5 |
O4—In1—O1 | 81.77 (10) | C5—C6—H6B | 109.5 |
O10—In1—O6 | 164.80 (9) | H6A—C6—H6B | 109.5 |
O4—In1—O6 | 73.05 (8) | C5—C6—H6C | 109.5 |
O1—In1—O6 | 91.77 (10) | H6A—C6—H6C | 109.5 |
O10—In1—O3 | 83.36 (9) | H6B—C6—H6C | 109.5 |
O4—In1—O3 | 144.51 (8) | O8—C7—O7 | 120.1 (3) |
O1—In1—O3 | 72.36 (9) | O8—C7—C8 | 121.6 (3) |
O6—In1—O3 | 83.70 (9) | O7—C7—C8 | 118.3 (3) |
O10—In1—O8 | 93.10 (8) | O9—C8—C9 | 111.2 (3) |
O4—In1—O8 | 123.19 (9) | O9—C8—C7 | 108.4 (3) |
O1—In1—O8 | 145.26 (8) | C9—C8—C7 | 108.9 (3) |
O6—In1—O8 | 75.68 (8) | O9—C8—H8 | 109.5 |
O3—In1—O8 | 74.12 (8) | C9—C8—H8 | 109.5 |
O10—In1—O7 | 87.13 (9) | C7—C8—H8 | 109.5 |
O4—In1—O7 | 81.37 (9) | C8—C9—H9A | 109.5 |
O1—In1—O7 | 159.40 (9) | C8—C9—H9B | 109.5 |
O6—In1—O7 | 94.55 (9) | H9A—C9—H9B | 109.5 |
O3—In1—O7 | 127.81 (8) | C8—C9—H9C | 109.5 |
O8—In1—O7 | 55.29 (8) | H9A—C9—H9C | 109.5 |
O12i—Na1—O5ii | 168.59 (12) | H9B—C9—H9C | 109.5 |
O12i—Na1—O2 | 99.82 (12) | O11—C10—O10 | 123.2 (3) |
O5ii—Na1—O2 | 88.19 (8) | O11—C10—C11 | 122.3 (3) |
O12i—Na1—O8iii | 110.79 (10) | O10—C10—C11 | 114.5 (3) |
O5ii—Na1—O8iii | 77.75 (9) | O12—C11—C12 | 111.1 (3) |
O2—Na1—O8iii | 85.24 (10) | O12—C11—C10 | 108.1 (3) |
O12i—Na1—O11i | 66.95 (9) | C12—C11—C10 | 109.6 (3) |
O5ii—Na1—O11i | 103.98 (11) | O12—C11—H11 | 109.3 |
O2—Na1—O11i | 98.95 (12) | C12—C11—H11 | 109.3 |
O8iii—Na1—O11i | 175.47 (11) | C10—C11—H11 | 109.3 |
O12i—Na1—O9iii | 84.43 (10) | C11—C12—H12A | 109.5 |
O5ii—Na1—O9iii | 92.82 (11) | C11—C12—H12B | 109.5 |
O2—Na1—O9iii | 149.32 (10) | H12A—C12—H12B | 109.5 |
O8iii—Na1—O9iii | 65.13 (8) | C11—C12—H12C | 109.5 |
O11i—Na1—O9iii | 110.47 (11) | H12A—C12—H12C | 109.5 |
O2—C1—O1 | 124.1 (4) | H12B—C12—H12C | 109.5 |
O2—C1—C2 | 116.6 (4) | C1—O1—In1 | 121.3 (3) |
O1—C1—C2 | 119.3 (3) | C1—O2—Na1 | 142.5 (3) |
O3—C2—C3 | 109.3 (3) | C2—O3—In1 | 117.67 (19) |
O3—C2—C1 | 109.1 (3) | C2—O3—H3 | 108 (3) |
C3—C2—C1 | 110.4 (4) | In1—O3—H3 | 121 (3) |
O3—C2—H2 | 109.3 | C4—O4—In1 | 120.5 (3) |
C3—C2—H2 | 109.3 | C4—O5—Na1iv | 139.2 (3) |
C1—C2—H2 | 109.3 | C5—O6—In1 | 117.89 (18) |
C2—C3—H3A | 109.5 | C5—O6—H6 | 109 (3) |
C2—C3—H3B | 109.5 | In1—O6—H6 | 121 (3) |
H3A—C3—H3B | 109.5 | C7—O7—In1 | 91.5 (2) |
C2—C3—H3C | 109.5 | C7—O8—In1 | 92.69 (19) |
H3A—C3—H3C | 109.5 | C7—O8—Na1i | 118.5 (2) |
H3B—C3—H3C | 109.5 | In1—O8—Na1i | 138.69 (10) |
O5—C4—O4 | 124.1 (4) | C8—O9—Na1i | 116.9 (2) |
O5—C4—C5 | 117.0 (4) | C8—O9—H9 | 107 (3) |
O4—C4—C5 | 118.9 (3) | Na1i—O9—H9 | 128 (3) |
O6—C5—C6 | 109.7 (3) | C10—O10—In1 | 110.8 (2) |
O6—C5—C4 | 109.3 (3) | C10—O11—Na1iii | 117.1 (2) |
C6—C5—C4 | 111.5 (3) | C11—O12—Na1iii | 118.0 (2) |
O6—C5—H5 | 108.8 | C11—O12—H12 | 104 (3) |
C6—C5—H5 | 108.8 | Na1iii—O12—H12 | 131 (3) |
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; (iv) x+1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2i | 0.86 (4) | 1.76 (4) | 2.620 (3) | 177 (4) |
O6—H6···O5v | 0.82 (4) | 1.77 (4) | 2.578 (4) | 170 (4) |
O9—H9···O10vi | 0.83 (4) | 2.26 (4) | 3.087 (4) | 173 (4) |
O12—H12···O7vii | 0.87 (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) x−1/2, −y+1/2, −z. |
Experimental details
Crystal data | |
Chemical formula | [InNa(C3H5O3)4] |
Mr | 494.09 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 296 |
a, b, c (Å) | 9.4744 (12), 9.5803 (12), 19.145 (2) |
V (Å3) | 1737.7 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.45 |
Crystal size (mm) | 0.18 × 0.13 × 0.09 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.781, 0.881 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10916, 4259, 3680 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.683 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.057, 1.02 |
No. of reflections | 4259 |
No. of parameters | 247 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.45, −0.42 |
Absolute structure | Flack (1983), with 1766 Friedel pairs |
Absolute structure parameter | 0.03 (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).
In1—O10 | 2.133 (2) | Na1—O12i | 2.364 (3) |
In1—O4 | 2.162 (2) | Na1—O5ii | 2.423 (3) |
In1—O1 | 2.183 (2) | Na1—O2 | 2.435 (3) |
In1—O6 | 2.217 (2) | Na1—O8iii | 2.437 (2) |
In1—O3 | 2.255 (2) | Na1—O11i | 2.462 (2) |
In1—O8 | 2.338 (2) | Na1—O9iii | 2.476 (3) |
In1—O7 | 2.356 (2) | ||
O10—In1—O4 | 122.10 (9) | O8—In1—O7 | 55.29 (8) |
O10—In1—O1 | 91.88 (9) | O12i—Na1—O2 | 99.82 (12) |
O4—In1—O1 | 81.77 (10) | O5ii—Na1—O2 | 88.19 (8) |
O10—In1—O6 | 164.80 (9) | O12i—Na1—O8iii | 110.79 (10) |
O4—In1—O6 | 73.05 (8) | O5ii—Na1—O8iii | 77.75 (9) |
O1—In1—O6 | 91.77 (10) | O2—Na1—O8iii | 85.24 (10) |
O10—In1—O3 | 83.36 (9) | O12i—Na1—O11i | 66.95 (9) |
O1—In1—O3 | 72.36 (9) | O5ii—Na1—O11i | 103.98 (11) |
O6—In1—O3 | 83.70 (9) | O2—Na1—O11i | 98.95 (12) |
O10—In1—O8 | 93.10 (8) | O8iii—Na1—O11i | 175.47 (11) |
O6—In1—O8 | 75.68 (8) | O12i—Na1—O9iii | 84.43 (10) |
O3—In1—O8 | 74.12 (8) | O5ii—Na1—O9iii | 92.82 (11) |
O10—In1—O7 | 87.13 (9) | O8iii—Na1—O9iii | 65.13 (8) |
O4—In1—O7 | 81.37 (9) | O11i—Na1—O9iii | 110.47 (11) |
O6—In1—O7 | 94.55 (9) |
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. |
D—H···A | D—H | H···A | D···A | 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+1/2, −z+1/2; (iv) −x+2, y+1/2, −z+1/2; (v) x+1/2, −y+3/2, −z; (vi) x−1/2, −y+1/2, −z. |
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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.