Acta Cryst. (2009). E65, m1500 [ doi:10.1107/S1600536809045395 ]
![[mu]](/logos/entities/mu_rmgif.gif)
-2-bromobenzoato)-![[kappa]](/logos/entities/kappa_rmgif.gif)
2O,O':O';3O:O,O']The hydrothermal reaction of SrCO3 and 2-bromobenzoic acid in CH3OH-H2O afforded the SrII title polymeric complex, [Sr(C7H4BrO2)2(H2O)2]n. Within the coordination sphere, the SrII ion is located on a crystallographic twofold axis, and is coordinated by eight O atoms from two water molecules and four carboxylate groups of 2-bromobenzoate ligands in an irregular coordination geometry. Two 3-carboxylate groups of the 2-bromobenzoate anions bridge two symmetry-related SrII atoms, giving rise to a chain structure extending along [001]. The polymeric chains are connected via O-H
O and O-HBr hydrogen bonds interactions into a three-dimensional supramolecular network.
SrCl2.6H2O. (0.533 g, 2.00 mmol) was dissolved in the appropriate amount of water, and then 1M Na2CO3 solution was added. SrCO3 was obtained by filtration, which was then washed with distilled water (5 times). The freshly prepared SrCO3, 2-bromobenzoic acid (0.402 g, 2.00 mmol), CH3OH/H2O (v/v = 1:2, 15 ml) were mixed and stirred for 2.0 h. Subsequently, the resulting cream suspension was heated in a 23 ml Teflon-lined stainless steel autoclave at 433 K for 5800 minutes. After the autoclave was cooled to room temperature according to the procedure at 2600 minutes, the solid was filtered off. The resulting filtrate was allowed to stand at room temperature, and slow evaporation for 6 weeks afforded colorless block-shaped single crystals.
C-bound H atoms were placed in calculated positions, with C—H = 0.93Å and Uiso(H) = 1.2Ueq(C), and were refined using the riding- model approximation. The H atoms of the water molecule were located in a difference Fourier map and refined with an O—H distance restraint of 0.82 (1) Å and Uiso(H) = 1.5Ueq(O).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku, 1998); 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: SHELXL97 (Sheldrick, 2008).
![[Figure 1]](./bh2255fig1thm.gif)
| Fig. 1. The one-dimensional chain structure of the title compound, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. |
![[Figure 2]](./bh2255fig2thm.gif)
| Fig. 2. A packing diagram of the title complex, viewed along the c axis, The O—H···O and O—H···Br hydrogen bonds (dashed lines) in the title compound. |
| [Sr(C7H4BrO2)2(H2O)2] | F(000) = 1008 |
| Mr = 523.68 | Dx = 1.975 Mg m−3 |
| Orthorhombic, Pbcn | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2n 2ab | Cell parameters from 9800 reflections |
| a = 18.740 (4) Å | θ = 3.3–25.0° |
| b = 11.669 (2) Å | µ = 7.62 mm−1 |
| c = 8.0529 (16) Å | T = 290 K |
| V = 1760.9 (6) Å3 | Block, colorless |
| Z = 4 | 0.36 × 0.20 × 0.16 mm |
| Rigaku R-AXIS RAPID diffractometer | 1550 independent reflections |
| Radiation source: fine-focus sealed tube | 1273 reflections with I > 2σ(I) |
| graphite | Rint = 0.090 |
| ω scans | θmax = 25.0°, θmin = 3.3° |
| Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −22→22 |
| Tmin = 0.170, Tmax = 0.309 | k = −13→13 |
| 12747 measured reflections | l = −9→8 |
| 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)] = 0.042 | H-atom parameters constrained |
| wR(F2) = 0.130 | w = 1/[σ2(Fo2) + (0.0652P)2 + 1.8313P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.14 | (Δ/σ)max < 0.001 |
| 1550 reflections | Δρmax = 0.84 e Å−3 |
| 106 parameters | Δρmin = −0.78 e Å−3 |
| 0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 0 constraints | Extinction coefficient: 0.0016 (6) |
| Primary atom site location: structure-invariant direct methods |
| [Sr(C7H4BrO2)2(H2O)2] | V = 1760.9 (6) Å3 |
| Mr = 523.68 | Z = 4 |
| Orthorhombic, Pbcn | Mo Kα radiation |
| a = 18.740 (4) Å | µ = 7.62 mm−1 |
| b = 11.669 (2) Å | T = 290 K |
| c = 8.0529 (16) Å | 0.36 × 0.20 × 0.16 mm |
| Rigaku R-AXIS RAPID diffractometer | 1550 independent reflections |
| Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 1273 reflections with I > 2σ(I) |
| Tmin = 0.170, Tmax = 0.309 | Rint = 0.090 |
| 12747 measured reflections | θmax = 25.0° |
| R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
| wR(F2) = 0.130 | Δρmax = 0.84 e Å−3 |
| S = 1.14 | Δρmin = −0.78 e Å−3 |
| 1550 reflections | Absolute structure: ? |
| 106 parameters | Flack parameter: ? |
| 0 restraints | Rogers parameter: ? |
| x | y | z | Uiso*/Ueq | ||
| Sr1 | 0.5000 | 0.95347 (6) | 0.2500 | 0.0294 (3) | |
| Br1 | 0.26073 (4) | 1.23028 (6) | 0.28032 (9) | 0.0528 (3) | |
| O1 | 0.4082 (2) | 0.8205 (4) | 0.1116 (5) | 0.0577 (12) | |
| H1A | 0.4050 | 0.8178 | 0.0101 | 0.087* | |
| H1B | 0.3663 | 0.8112 | 0.1371 | 0.087* | |
| O2 | 0.5875 (3) | 1.1245 (4) | 0.2207 (4) | 0.0523 (13) | |
| O3 | 0.4433 (2) | 1.1017 (3) | 0.0190 (4) | 0.0395 (10) | |
| C1 | 0.4152 (3) | 1.1591 (4) | 0.1317 (6) | 0.0335 (12) | |
| C2 | 0.3870 (3) | 1.2758 (4) | 0.0915 (6) | 0.0318 (12) | |
| C3 | 0.3238 (3) | 1.3201 (4) | 0.1490 (6) | 0.0404 (14) | |
| C4 | 0.3005 (4) | 1.4307 (5) | 0.1105 (8) | 0.0475 (16) | |
| H4 | 0.2569 | 1.4575 | 0.1495 | 0.057* | |
| C5 | 0.3434 (5) | 1.4993 (5) | 0.0138 (8) | 0.0549 (19) | |
| H5A | 0.3293 | 1.5739 | −0.0105 | 0.066* | |
| C6 | 0.4068 (5) | 1.4582 (5) | −0.0469 (8) | 0.060 (2) | |
| H6 | 0.4352 | 1.5050 | −0.1129 | 0.072* | |
| C7 | 0.4288 (3) | 1.3487 (5) | −0.0113 (7) | 0.0452 (15) | |
| H7 | 0.4716 | 1.3218 | −0.0549 | 0.054* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Sr1 | 0.0387 (5) | 0.0285 (4) | 0.0210 (4) | 0.000 | 0.0023 (3) | 0.000 |
| Br1 | 0.0460 (5) | 0.0583 (5) | 0.0542 (5) | 0.0021 (3) | 0.0062 (3) | 0.0062 (3) |
| O1 | 0.058 (3) | 0.077 (3) | 0.038 (2) | −0.029 (2) | −0.002 (2) | 0.003 (2) |
| O2 | 0.076 (4) | 0.053 (3) | 0.028 (2) | −0.026 (2) | 0.007 (2) | −0.0068 (18) |
| O3 | 0.052 (3) | 0.041 (2) | 0.0251 (19) | 0.0051 (18) | 0.0075 (17) | −0.0051 (16) |
| C1 | 0.034 (3) | 0.039 (3) | 0.028 (3) | 0.007 (2) | 0.000 (2) | −0.001 (2) |
| C2 | 0.037 (3) | 0.031 (3) | 0.027 (3) | 0.008 (2) | −0.003 (2) | −0.006 (2) |
| C3 | 0.060 (4) | 0.035 (3) | 0.026 (3) | 0.008 (3) | −0.010 (3) | 0.000 (2) |
| C4 | 0.053 (4) | 0.043 (3) | 0.047 (4) | 0.011 (3) | −0.009 (3) | −0.006 (3) |
| C5 | 0.080 (6) | 0.034 (3) | 0.052 (4) | 0.010 (3) | −0.011 (4) | 0.001 (3) |
| C6 | 0.087 (6) | 0.046 (4) | 0.047 (4) | −0.014 (4) | −0.006 (4) | 0.012 (3) |
| C7 | 0.047 (4) | 0.044 (3) | 0.045 (3) | −0.005 (3) | 0.004 (3) | 0.000 (3) |
| Sr1—O3i | 2.498 (3) | O3—C1 | 1.244 (6) |
| Sr1—O3ii | 2.498 (3) | O3—Sr1i | 2.498 (3) |
| Sr1—O1 | 2.570 (4) | C1—O2iii | 1.257 (6) |
| Sr1—O1iii | 2.570 (4) | C1—C2 | 1.496 (7) |
| Sr1—O2 | 2.594 (4) | C2—C3 | 1.373 (8) |
| Sr1—O2iii | 2.594 (4) | C2—C7 | 1.422 (8) |
| Sr1—O3iii | 2.753 (4) | C3—C4 | 1.397 (8) |
| Sr1—O3 | 2.753 (4) | C4—C5 | 1.376 (10) |
| Sr1—C1iii | 3.031 (5) | C4—H4 | 0.9300 |
| Sr1—C1 | 3.031 (5) | C5—C6 | 1.371 (11) |
| Br1—C3 | 1.901 (6) | C5—H5A | 0.9300 |
| O1—H1A | 0.8200 | C6—C7 | 1.373 (9) |
| O1—H1B | 0.8200 | C6—H6 | 0.9300 |
| O2—C1iii | 1.257 (6) | C7—H7 | 0.9300 |
| O3i—Sr1—O3ii | 150.14 (16) | O2—Sr1—Sr1iv | 83.55 (8) |
| O3i—Sr1—O1 | 75.71 (13) | O2iii—Sr1—Sr1iv | 73.25 (8) |
| O3ii—Sr1—O1 | 86.32 (12) | O3iii—Sr1—Sr1iv | 35.34 (7) |
| O3i—Sr1—O1iii | 86.32 (12) | O3—Sr1—Sr1iv | 119.25 (7) |
| O3ii—Sr1—O1iii | 75.71 (13) | C1iii—Sr1—Sr1iv | 59.36 (10) |
| O1—Sr1—O1iii | 105.7 (2) | C1—Sr1—Sr1iv | 95.59 (10) |
| O3i—Sr1—O2 | 81.37 (12) | O3i—Sr1—Sr1i | 39.61 (8) |
| O3ii—Sr1—O2 | 123.12 (11) | O3ii—Sr1—Sr1i | 154.76 (9) |
| O1—Sr1—O2 | 147.99 (12) | O1—Sr1—Sr1i | 74.84 (9) |
| O1iii—Sr1—O2 | 94.65 (16) | O1iii—Sr1—Sr1i | 125.16 (9) |
| O3i—Sr1—O2iii | 123.12 (11) | O2—Sr1—Sr1i | 73.25 (8) |
| O3ii—Sr1—O2iii | 81.37 (12) | O2iii—Sr1—Sr1i | 83.55 (8) |
| O1—Sr1—O2iii | 94.65 (16) | O3iii—Sr1—Sr1i | 119.25 (7) |
| O1iii—Sr1—O2iii | 147.99 (12) | O3—Sr1—Sr1i | 35.34 (7) |
| O2—Sr1—O2iii | 79.4 (2) | C1iii—Sr1—Sr1i | 95.59 (10) |
| O3i—Sr1—O3iii | 125.68 (15) | C1—Sr1—Sr1i | 59.36 (9) |
| O3ii—Sr1—O3iii | 74.95 (13) | Sr1iv—Sr1—Sr1i | 149.82 (4) |
| O1—Sr1—O3iii | 158.51 (13) | Sr1—O1—H1A | 120.4 |
| O1iii—Sr1—O3iii | 80.09 (12) | Sr1—O1—H1B | 127.8 |
| O2—Sr1—O3iii | 48.25 (10) | H1A—O1—H1B | 99.9 |
| O2iii—Sr1—O3iii | 72.51 (13) | C1iii—O2—Sr1 | 97.8 (3) |
| O3i—Sr1—O3 | 74.95 (13) | C1—O3—Sr1i | 162.0 (3) |
| O3ii—Sr1—O3 | 125.68 (15) | C1—O3—Sr1 | 90.5 (3) |
| O1—Sr1—O3 | 80.09 (12) | Sr1i—O3—Sr1 | 105.05 (13) |
| O1iii—Sr1—O3 | 158.51 (13) | O3—C1—O2iii | 122.3 (5) |
| O2—Sr1—O3 | 72.51 (13) | O3—C1—C2 | 118.8 (4) |
| O2iii—Sr1—O3 | 48.25 (10) | O2iii—C1—C2 | 118.9 (4) |
| O3iii—Sr1—O3 | 102.18 (15) | O3—C1—Sr1 | 65.3 (3) |
| O3i—Sr1—C1iii | 104.69 (13) | O2iii—C1—Sr1 | 58.0 (3) |
| O3ii—Sr1—C1iii | 98.88 (13) | C2—C1—Sr1 | 166.8 (4) |
| O1—Sr1—C1iii | 164.74 (14) | C3—C2—C7 | 116.5 (5) |
| O1iii—Sr1—C1iii | 89.49 (15) | C3—C2—C1 | 125.1 (5) |
| O2—Sr1—C1iii | 24.26 (12) | C7—C2—C1 | 118.4 (5) |
| O2iii—Sr1—C1iii | 72.16 (16) | C2—C3—C4 | 122.8 (6) |
| O3iii—Sr1—C1iii | 24.23 (11) | C2—C3—Br1 | 121.1 (4) |
| O3—Sr1—C1iii | 85.27 (13) | C4—C3—Br1 | 116.0 (5) |
| O3i—Sr1—C1 | 98.88 (13) | C5—C4—C3 | 118.7 (6) |
| O3ii—Sr1—C1 | 104.69 (13) | C5—C4—H4 | 120.6 |
| O1—Sr1—C1 | 89.49 (15) | C3—C4—H4 | 120.6 |
| O1iii—Sr1—C1 | 164.74 (14) | C6—C5—C4 | 120.2 (6) |
| O2—Sr1—C1 | 72.16 (16) | C6—C5—H5A | 119.9 |
| O2iii—Sr1—C1 | 24.26 (12) | C4—C5—H5A | 119.9 |
| O3iii—Sr1—C1 | 85.27 (13) | C5—C6—C7 | 120.8 (7) |
| O3—Sr1—C1 | 24.23 (11) | C5—C6—H6 | 119.6 |
| C1iii—Sr1—C1 | 75.3 (2) | C7—C6—H6 | 119.6 |
| O3i—Sr1—Sr1iv | 154.76 (9) | C6—C7—C2 | 120.8 (6) |
| O3ii—Sr1—Sr1iv | 39.61 (8) | C6—C7—H7 | 119.6 |
| O1—Sr1—Sr1iv | 125.16 (9) | C2—C7—H7 | 119.6 |
| O1iii—Sr1—Sr1iv | 74.84 (9) |
| Symmetry codes: (i) −x+1, −y+2, −z; (ii) x, −y+2, z+1/2; (iii) −x+1, y, −z+1/2; (iv) −x+1, −y+2, −z+1. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1A···O2i | 0.82 | 1.98 | 2.753 (5) | 156 |
| O1—H1B···Br1v | 0.82 | 2.81 | 3.603 (2) | 164 |
| Symmetry codes: (i) −x+1, −y+2, −z; (v) −x+1/2, y−1/2, z. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1A···O2i | 0.82 | 1.98 | 2.753 (5) | 156 |
| O1—H1B···Br1ii | 0.82 | 2.81 | 3.603 (2) | 164 |
| Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1/2, y−1/2, z. |
The author gratefully acknowledges the financial support of the Education office of Zhejiang Province (grant No. 20051316).
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Metal ions with 2-bromobenzoato ligands can form, among others, mononuclear, dinuclear complexes (Zhang et al., 2005, 2008; Zhang, 2006; Wang et al., 2003) but very few reports on one-dimensional chain structures complexes including 2-bromobenzoato ligands have been published.
In this paper, we would like to report the synthesis and crystal structure of a one-dimensional chain complex including 2-bromobenzoato and Strontium(II). The crystal structure of the title compound is similar to previously published structures (Zhang, 2008; Karipides et al., 1988). Within the title compound, each SrII ion is located on a crystallographic two-fold axis and is coordinated by eight O atoms from two water molecules and four carboxyl groups of 2-bromobenzoic acid anions in an irregular coordination geometry. Two µ3-carboxyl groups of the 2-bromobenzoic anions bridge two symmetry related Strontium atoms, giving rise to a one-dimensional chain structure extending along the [001] direction, with Sr—O bond lengths in the range of 2.498 (3) to 2.753 (4) Å. Separation between Sr and Sriv (symmetry code iv: -x+1, -y+2, -z+1) is 4.1703 (8) Å (Fig. 1). The polymeric chains are connected via O—H···O and O—H···Br hydrogen bonds interactions in a three-dimensional supramolecular structure (Fig. 2). The O1—H1A···O3 and O1—H1A···Br1 separations are 2.753 Å and 3.603 Å. The O—H···O and O1—H1A···Br1 bond angles are 156 ° and 164°, Table 2.