Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113024499/em3061sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113024499/em3061Isup2.hkl |
CCDC reference: 969457
In recent decades, coordination polymer solids have emerged as a new class of functional materials and have attracted considerable attention not only for their structural diversity but also for their potential applications in gas storage, molecular magnetism, photoluminescence and catalysis (Eddaoudi et al., 2001; Yoon et al., 2012; Allendorf et al., 2009; Wang et al., 2008). Because the structure of a coordination polymer is the decisive factor in these functionalities, the organic ligands used as structure-directing building units play a vital role. Sulfonate–carboxylate ligands, displaying simultaneously the strong coordination ability of the carboxylate group and the weak coordination ability of the sulfonate group (Kennedy et al., 2006; Evans et al., 1999), have received increasing attention recently (Xiao et al., 2009; Mahmoudkhani & Shimizu, 2007). Some sulfonate–carboxylate ligands, such as 5-sulfoisophthalic acid (Sun et al., 2003; Liu et al., 2010), 2-sulfoterephthalic acid (Horike et al. 2006), 4-sulfobenzoic acid (Zhang & Zhu, 2006) and 4,8-disulfonyl-2,6-naphthalenedicarboxylic acid (Liu et al., 2012), have been used to construct coordination compounds recently. 5-Sulfonobenzene-1,2,4-tricarboxylic acid (H4SBTC), with three carboxylic acid groups and one sulfonic acid group attached to a central benzene ring, is expected to be an effective component in the design of a diverse range of coordination polymers. However, there are no known coordination polymers incorporating H4SBTC, except for two coordination compounds with interesting photoluminescent properties which have been reported in our recent work (Liu et al., 2013), where H4SBTC displays various coordination modes. Further studies of the H4SBTC ligand with other metal ions are needed in order to understand comprehensively the coordination chemistry of this ligand. We report herein the synthesis and crystal structure of the title compound, [K2(H2SBTC)(H2O)2]n, (I), incorporating H4SBTC as the dianionic H2SBTC2- ligand.
KOH (11.2 mg, 0.20 mmol) and 5-sulfonobenzene-1,2,4-tricarboxylic acid (86.7 mg, 0.30 mmol) were mixed in distilled water (10 ml) in a 25 ml Parr Teflon-lined stainless steel vessel. The vessel was sealed and heated to 393 K. The temperature was maintained for 3 d and then the mixture was cooled naturally to obtain a colourless solution. Upon standing and evaporation of the resulting solution under ambient conditions for 10 d, colourless crystals of (I) were obtained. The crystalline product was filtered, washed with distilled water and dried at ambient temperature (yield 51%, based on KOH). IR (KBr pellet, ν, cm-1): 3445, 3128, 2454, 1713, 1606, 1474, 1386, 1327, 1280, 1245, 1206, 1120, 1068, 995, 952, 864, 822, 768, 723, 635, 562, 538, 517, 462.
Crystal data, data collection and structure refinement details are summarized in Table 1. H atoms bonded to C atoms were placed in calculated positions and treated using a riding-model approximation, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C). H atoms bonded to O atoms were located in a difference Fourier map and refined with a restraint of O—H = 0.82 (2) Å and with Uiso(H) = 1.5Ueq(O).
The asymmetric unit of (I) consists of two KI cations, one H2SBTC2- ligand, one bridging aqua ligand (O10) and one terminal aqua ligand (O11). As depicted in Fig. 1, atom K1 is eight-coordinated by sulfonate atoms O7 and O9 and carboxylate atom O6 from an H2SBTC2- ligand, by carboxylate atoms O4i and O3iii from two other H2SBTC2- ligands [symmetry codes: (i) -x + 1/2, y + 1/2, -z + 1/2; (iii) x + 1, y, z], sulfonate atom O8ii from a fourth H2SBTC2- ligand [symmetry code: (ii) -x + 1, -y + 1, -z], and water atoms O10 and O10iv [symmetry code: (iv) -x + 3/2, y - 1/2, -z + 1/2]. The K1—O bond lengths vary from 2.6745 (14) to 3.1981 (15) Å (Table 2). The eight-coordination environment for atom K2 (Fig. 1) is completed by carboxylate atom O6 and sulfonate atom O9 from an H2SBTC2- ligand, sulfonate atoms O7v and O8v from an H2SBTC2- ligand [symmetry code: (v) x, y - 1, z], carboxylate atoms O2vi and O5viii from two H2SBTC2- ligands [symmetry codes: (vi) -x, -y, -z; (viii) -x + 1/2, y - 1/2, -z + 1/2], sulfonate atom O9vii of an H2SBTC2- ligand [symmetry code: (vii) -x + 1, -y, -z], and one water O atom (O11). The K2—O bond lengths are comparable with the K1—O bond lengths (Table 2).
Two centrosymmetric sulfonate groups link two K1 and two K2 ions to give a cage-like inorganic unit (Fig. 2). Adjacent inorganic cage units are extended into a one-dimensional chain propagating along the b axis through the K2—O9 bond (Fig. 2), which is further linked by bridging water molecule O10 and the O3—C8—O4 carboxylate bridge to form a two-dimensional layer structure (Fig. 3). The two-dimensional layers are linked by O5—C9—O6 carboxylate groups and benzene rings of H2SBTC2- ligands to generate a three-dimensional framework (Fig. 4). The three-dimensional framework is further reinforced by hydrogen bonds, with O···O distances of 2.3771 (19)–2.958 (3) Å (Table 3).
The solid-state photoluminescent properties of (I) were examined at room temperature. The free H4SBTC molecule exhibits a photoluminescent emission at 460 nm under 348 nm radiation (Liu et al., 2013), which can be assigned to the typical ligand-centred (π–π*) transitions. Compound (I) displays a photoluminescent emission at 460 nm upon excitation at 358 nm (Fig. 5). The emission energy of (I) is very similar to that of the free molecule. Therefore, the luminescence behaviour of (I) can be assigned as the ligand centred π–π* transitions.
The results of thermogravimetric analysis are represented by the curve shown in Fig. 6. Compound (I) exhibits three main weight-loss steps. The first step (305–319 K) corresponds to the release of all coordinated water molecules (measured weight loss = 8.88%; theoretical = 8.90%). The second weight loss occurs between 517 and 571 K (measured weight loss = 4.08%) and can be attributed to partial decomposition of the organic ligand. A sharp continuous weight loss occurs at 638 K, which is attributed to further decomposition of the organic ligand.
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: SHELXL97 (Sheldrick, 2008).
[K2(C9H4O9S)(H2O)2] | F(000) = 816 |
Mr = 402.41 | Dx = 1.936 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.4108 (6) Å | Cell parameters from 6780 reflections |
b = 7.1795 (4) Å | θ = 2.4–28.2° |
c = 16.9372 (9) Å | µ = 0.90 mm−1 |
β = 95.774 (1)° | T = 296 K |
V = 1380.52 (13) Å3 | Block, colourless |
Z = 4 | 0.24 × 0.18 × 0.15 mm |
Bruker APEXII area-detector diffractometer | 3411 independent reflections |
Radiation source: fine-focus sealed tube | 3056 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scans | θmax = 28.3°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→14 |
Tmin = 0.813, Tmax = 0.877 | k = −9→9 |
12572 measured reflections | l = −22→22 |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0544P)2 + 0.9006P] where P = (Fo2 + 2Fc2)/3 |
3411 reflections | (Δ/σ)max < 0.001 |
208 parameters | Δρmax = 0.55 e Å−3 |
6 restraints | Δρmin = −0.51 e Å−3 |
[K2(C9H4O9S)(H2O)2] | V = 1380.52 (13) Å3 |
Mr = 402.41 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.4108 (6) Å | µ = 0.90 mm−1 |
b = 7.1795 (4) Å | T = 296 K |
c = 16.9372 (9) Å | 0.24 × 0.18 × 0.15 mm |
β = 95.774 (1)° |
Bruker APEXII area-detector diffractometer | 3411 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3056 reflections with I > 2σ(I) |
Tmin = 0.813, Tmax = 0.877 | Rint = 0.021 |
12572 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 6 restraints |
wR(F2) = 0.094 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 0.55 e Å−3 |
3411 reflections | Δρmin = −0.51 e Å−3 |
208 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 | ||
K1 | 0.63078 (4) | 0.34215 (8) | 0.16439 (3) | 0.04418 (14) | |
K2 | 0.41486 (4) | −0.15869 (5) | 0.08872 (3) | 0.03350 (12) | |
S1 | 0.36844 (3) | 0.36730 (5) | 0.04779 (2) | 0.02366 (11) | |
O1 | −0.03680 (11) | 0.2982 (2) | −0.10471 (7) | 0.0360 (3) | |
O2 | −0.17489 (11) | 0.1925 (2) | −0.03608 (8) | 0.0367 (3) | |
O3 | −0.20614 (11) | 0.1063 (2) | 0.09568 (8) | 0.0416 (4) | |
H3 | −0.191 (3) | 0.139 (4) | 0.0471 (12) | 0.062* | |
O4 | −0.10690 (13) | 0.0685 (3) | 0.21101 (8) | 0.0519 (4) | |
O5 | 0.28766 (12) | 0.2558 (2) | 0.28376 (7) | 0.0374 (3) | |
H5 | 0.3474 (18) | 0.239 (4) | 0.3156 (14) | 0.056* | |
O6 | 0.40340 (11) | 0.1135 (2) | 0.20402 (8) | 0.0346 (3) | |
O7 | 0.41622 (11) | 0.47421 (18) | 0.11643 (8) | 0.0332 (3) | |
O8 | 0.34166 (12) | 0.4809 (2) | −0.02206 (8) | 0.0400 (3) | |
O9 | 0.43865 (11) | 0.20320 (18) | 0.03397 (8) | 0.0324 (3) | |
O10 | 0.84463 (15) | 0.5745 (3) | 0.19595 (11) | 0.0579 (5) | |
H10A | 0.871 (3) | 0.513 (4) | 0.2340 (16) | 0.087* | |
H10B | 0.904 (2) | 0.610 (5) | 0.174 (2) | 0.087* | |
O11 | 0.63800 (17) | −0.1472 (3) | 0.16637 (12) | 0.0550 (4) | |
H11A | 0.670 (3) | −0.237 (4) | 0.185 (2) | 0.083* | |
H11B | 0.684 (3) | −0.105 (5) | 0.1364 (18) | 0.083* | |
C1 | 0.02142 (13) | 0.2350 (2) | 0.03132 (9) | 0.0197 (3) | |
C2 | 0.00396 (13) | 0.1757 (2) | 0.10903 (9) | 0.0206 (3) | |
C3 | 0.10096 (14) | 0.1725 (2) | 0.16637 (9) | 0.0226 (3) | |
H3A | 0.0894 | 0.1364 | 0.2178 | 0.027* | |
C4 | 0.21371 (13) | 0.2209 (2) | 0.15000 (9) | 0.0206 (3) | |
C5 | 0.23002 (13) | 0.2838 (2) | 0.07363 (9) | 0.0200 (3) | |
C6 | 0.13433 (13) | 0.2908 (2) | 0.01662 (9) | 0.0215 (3) | |
H6 | 0.1458 | 0.3346 | −0.0337 | 0.026* | |
C7 | −0.06914 (14) | 0.2442 (2) | −0.04115 (9) | 0.0228 (3) | |
C8 | −0.10917 (14) | 0.1118 (3) | 0.14150 (10) | 0.0271 (3) | |
C9 | 0.31274 (14) | 0.1926 (2) | 0.21464 (9) | 0.0234 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.0351 (2) | 0.0653 (3) | 0.0320 (2) | 0.0125 (2) | 0.00281 (17) | −0.00328 (19) |
K2 | 0.0313 (2) | 0.0281 (2) | 0.0408 (2) | −0.00191 (14) | 0.00200 (16) | −0.00395 (15) |
S1 | 0.01787 (19) | 0.0253 (2) | 0.0282 (2) | −0.00182 (14) | 0.00390 (15) | 0.00339 (14) |
O1 | 0.0289 (6) | 0.0572 (8) | 0.0201 (6) | −0.0081 (6) | −0.0058 (5) | 0.0079 (5) |
O2 | 0.0185 (6) | 0.0633 (9) | 0.0270 (6) | −0.0040 (6) | −0.0044 (5) | 0.0022 (6) |
O3 | 0.0190 (6) | 0.0747 (10) | 0.0311 (7) | −0.0077 (6) | 0.0024 (5) | 0.0068 (7) |
O4 | 0.0319 (7) | 0.0950 (13) | 0.0293 (7) | −0.0137 (8) | 0.0062 (6) | 0.0144 (8) |
O5 | 0.0280 (6) | 0.0632 (9) | 0.0193 (6) | 0.0116 (6) | −0.0065 (5) | −0.0087 (6) |
O6 | 0.0264 (6) | 0.0488 (8) | 0.0274 (6) | 0.0109 (6) | −0.0033 (5) | −0.0043 (5) |
O7 | 0.0244 (6) | 0.0305 (6) | 0.0439 (7) | −0.0062 (5) | 0.0002 (5) | −0.0055 (5) |
O8 | 0.0303 (7) | 0.0495 (8) | 0.0409 (7) | −0.0022 (6) | 0.0064 (6) | 0.0224 (6) |
O9 | 0.0276 (6) | 0.0319 (6) | 0.0397 (7) | 0.0029 (5) | 0.0134 (5) | 0.0001 (5) |
O10 | 0.0397 (9) | 0.0828 (13) | 0.0506 (10) | −0.0053 (9) | 0.0017 (7) | 0.0169 (9) |
O11 | 0.0513 (11) | 0.0572 (11) | 0.0553 (11) | −0.0060 (8) | −0.0011 (8) | 0.0028 (8) |
C1 | 0.0168 (7) | 0.0230 (7) | 0.0184 (7) | 0.0008 (5) | −0.0021 (5) | −0.0016 (5) |
C2 | 0.0162 (7) | 0.0261 (7) | 0.0193 (7) | −0.0008 (5) | 0.0012 (5) | −0.0020 (5) |
C3 | 0.0200 (7) | 0.0312 (8) | 0.0163 (7) | −0.0005 (6) | 0.0007 (5) | −0.0002 (6) |
C4 | 0.0181 (7) | 0.0253 (7) | 0.0177 (7) | 0.0000 (6) | −0.0019 (5) | −0.0020 (5) |
C5 | 0.0165 (7) | 0.0228 (7) | 0.0208 (7) | −0.0021 (5) | 0.0016 (5) | −0.0008 (5) |
C6 | 0.0208 (7) | 0.0261 (7) | 0.0174 (7) | −0.0013 (6) | 0.0007 (5) | 0.0024 (5) |
C7 | 0.0200 (7) | 0.0268 (7) | 0.0203 (7) | 0.0014 (6) | −0.0041 (5) | −0.0017 (6) |
C8 | 0.0201 (7) | 0.0364 (9) | 0.0255 (8) | −0.0008 (6) | 0.0056 (6) | −0.0007 (6) |
C9 | 0.0208 (7) | 0.0288 (7) | 0.0198 (7) | −0.0006 (6) | −0.0026 (6) | −0.0008 (6) |
K1—O7 | 2.6745 (14) | O4—C8 | 1.215 (2) |
K1—O4i | 2.6990 (16) | O4—K1viii | 2.6990 (16) |
K1—O8ii | 2.7708 (13) | O5—C9 | 1.313 (2) |
K1—O3iii | 2.8496 (16) | O5—K2i | 3.3744 (14) |
K1—O10 | 2.960 (2) | O5—H5 | 0.835 (17) |
K1—O10iv | 3.039 (2) | O6—C9 | 1.210 (2) |
K1—O9 | 3.1156 (15) | O7—K2x | 2.6768 (14) |
K1—O6 | 3.1981 (15) | O8—K1ii | 2.7708 (13) |
K2—O7v | 2.6768 (14) | O8—K2x | 3.2558 (17) |
K2—O11 | 2.747 (2) | O9—K2vii | 2.8130 (13) |
K2—O6 | 2.7749 (14) | O10—K1xi | 3.039 (2) |
K2—O9 | 2.7811 (14) | O10—H10A | 0.815 (18) |
K2—O2vi | 2.8037 (13) | O10—H10B | 0.842 (18) |
K2—O9vii | 2.8130 (13) | O11—H11A | 0.788 (18) |
K2—O8v | 3.2558 (17) | O11—H11B | 0.823 (18) |
K2—O5viii | 3.3744 (14) | C1—C6 | 1.395 (2) |
S1—O8 | 1.4440 (13) | C1—C2 | 1.416 (2) |
S1—O7 | 1.4527 (13) | C1—C7 | 1.524 (2) |
S1—O9 | 1.4570 (13) | C2—C3 | 1.397 (2) |
S1—C5 | 1.7845 (15) | C2—C8 | 1.524 (2) |
O1—C7 | 1.235 (2) | C3—C4 | 1.387 (2) |
O2—C7 | 1.274 (2) | C3—H3A | 0.9300 |
O2—K2vi | 2.8037 (13) | C4—C5 | 1.400 (2) |
O3—C8 | 1.287 (2) | C4—C9 | 1.506 (2) |
O3—K1ix | 2.8496 (16) | C5—C6 | 1.384 (2) |
O3—H3 | 0.890 (17) | C6—H6 | 0.9300 |
O7—K1—O4i | 82.11 (4) | O9—S1—C5 | 106.41 (7) |
O7—K1—O8ii | 75.74 (4) | C7—O2—K2vi | 154.89 (11) |
O4i—K1—O8ii | 115.68 (6) | C8—O3—K1ix | 107.01 (11) |
O7—K1—O3iii | 134.59 (4) | C8—O3—H3 | 108 (2) |
O4i—K1—O3iii | 142.99 (5) | K1ix—O3—H3 | 114.7 (19) |
O8ii—K1—O3iii | 77.36 (4) | C8—O4—K1viii | 156.56 (16) |
O7—K1—O10 | 124.61 (5) | C9—O5—K2i | 149.09 (10) |
O4i—K1—O10 | 70.47 (6) | C9—O5—H5 | 106.8 (19) |
O8ii—K1—O10 | 74.63 (5) | K2i—O5—H5 | 100.4 (19) |
O3iii—K1—O10 | 81.27 (5) | C9—O6—K2 | 122.48 (11) |
O7—K1—O10iv | 118.08 (5) | C9—O6—K1 | 120.93 (12) |
O4i—K1—O10iv | 77.34 (6) | K2—O6—K1 | 96.73 (4) |
O8ii—K1—O10iv | 163.26 (5) | S1—O7—K1 | 108.31 (7) |
O3iii—K1—O10iv | 85.94 (5) | S1—O7—K2x | 112.63 (7) |
O10—K1—O10iv | 101.88 (3) | K1—O7—K2x | 113.03 (5) |
O7—K1—O9 | 48.76 (4) | S1—O8—K1ii | 159.82 (8) |
O4i—K1—O9 | 128.90 (4) | S1—O8—K2x | 87.46 (7) |
O8ii—K1—O9 | 70.33 (4) | K1ii—O8—K2x | 95.27 (4) |
O3iii—K1—O9 | 87.82 (4) | S1—O9—K2 | 128.91 (7) |
O10—K1—O9 | 144.79 (4) | S1—O9—K2vii | 126.00 (7) |
O10iv—K1—O9 | 110.65 (5) | K2—O9—K2vii | 103.03 (4) |
O7—K1—O6 | 60.56 (4) | S1—O9—K1 | 89.21 (6) |
O4i—K1—O6 | 89.84 (5) | K2—O9—K1 | 98.51 (4) |
O8ii—K1—O6 | 125.70 (4) | K2vii—O9—K1 | 97.59 (4) |
O3iii—K1—O6 | 110.95 (4) | K1—O10—K1xi | 120.46 (6) |
O10—K1—O6 | 157.36 (5) | K1—O10—H10A | 94 (3) |
O10iv—K1—O6 | 61.66 (4) | K1xi—O10—H10A | 74 (3) |
O9—K1—O6 | 57.08 (3) | K1—O10—H10B | 141 (3) |
O7v—K2—O11 | 87.52 (5) | K1xi—O10—H10B | 98 (3) |
O7v—K2—O6 | 124.73 (4) | H10A—O10—H10B | 105 (3) |
O11—K2—O6 | 75.47 (5) | K2—O11—H11A | 122 (3) |
O7v—K2—O9 | 168.30 (4) | K2—O11—H11B | 109 (3) |
O11—K2—O9 | 90.85 (5) | H11A—O11—H11B | 104 (4) |
O6—K2—O9 | 65.79 (4) | C6—C1—C2 | 118.09 (13) |
O7v—K2—O2vi | 87.63 (4) | C6—C1—C7 | 114.04 (13) |
O11—K2—O2vi | 169.56 (5) | C2—C1—C7 | 127.87 (13) |
O6—K2—O2vi | 99.85 (4) | C3—C2—C1 | 118.37 (13) |
O9—K2—O2vi | 95.73 (4) | C3—C2—C8 | 112.62 (13) |
O7v—K2—O9vii | 91.39 (4) | C1—C2—C8 | 129.00 (14) |
O11—K2—O9vii | 76.47 (5) | C4—C3—C2 | 122.86 (14) |
O6—K2—O9vii | 132.33 (4) | C4—C3—H3A | 118.6 |
O9—K2—O9vii | 76.97 (4) | C2—C3—H3A | 118.6 |
O2vi—K2—O9vii | 112.90 (4) | C3—C4—C5 | 118.53 (13) |
O7v—K2—O8v | 46.77 (4) | C3—C4—C9 | 117.65 (13) |
O11—K2—O8v | 118.12 (5) | C5—C4—C9 | 123.74 (13) |
O6—K2—O8v | 159.68 (4) | C6—C5—C4 | 119.17 (13) |
O9—K2—O8v | 125.33 (4) | C6—C5—S1 | 118.20 (11) |
O2vi—K2—O8v | 64.03 (4) | C4—C5—S1 | 122.55 (11) |
O9vii—K2—O8v | 67.73 (4) | C5—C6—C1 | 122.89 (14) |
O7v—K2—O5viii | 72.59 (4) | C5—C6—H6 | 118.6 |
O11—K2—O5viii | 111.13 (5) | C1—C6—H6 | 118.6 |
O6—K2—O5viii | 66.04 (4) | O1—C7—O2 | 121.23 (14) |
O9—K2—O5viii | 118.66 (4) | O1—C7—C1 | 118.53 (14) |
O2vi—K2—O5viii | 58.53 (3) | O2—C7—C1 | 120.22 (14) |
O9vii—K2—O5viii | 161.48 (4) | O4—C8—O3 | 120.63 (16) |
O8v—K2—O5viii | 94.11 (4) | O4—C8—C2 | 119.37 (15) |
O8—S1—O7 | 112.88 (9) | O3—C8—C2 | 120.00 (14) |
O8—S1—O9 | 113.54 (9) | O6—C9—O5 | 124.13 (15) |
O7—S1—O9 | 112.81 (8) | O6—C9—C4 | 123.08 (14) |
O8—S1—C5 | 105.72 (7) | O5—C9—C4 | 112.73 (13) |
O7—S1—C5 | 104.56 (7) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (iv) −x+3/2, y−1/2, −z+1/2; (v) x, y−1, z; (vi) −x, −y, −z; (vii) −x+1, −y, −z; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x−1, y, z; (x) x, y+1, z; (xi) −x+3/2, y+1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2 | 0.89 (2) | 1.49 (2) | 2.3771 (19) | 176 (3) |
O5—H5···O1xii | 0.84 (2) | 1.81 (2) | 2.6400 (18) | 172 (3) |
O10—H10A···O11xi | 0.82 (2) | 2.05 (2) | 2.814 (3) | 155 (3) |
O10—H10B···O1ii | 0.84 (2) | 2.12 (2) | 2.952 (2) | 172 (3) |
O11—H11A···O4viii | 0.79 (2) | 2.42 (3) | 2.958 (3) | 127 (3) |
O11—H11B···O3iii | 0.82 (2) | 2.13 (2) | 2.888 (2) | 154 (4) |
Symmetry codes: (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (viii) −x+1/2, y−1/2, −z+1/2; (xi) −x+3/2, y+1/2, −z+1/2; (xii) x+1/2, −y+1/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [K2(C9H4O9S)(H2O)2] |
Mr | 402.41 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 296 |
a, b, c (Å) | 11.4108 (6), 7.1795 (4), 16.9372 (9) |
β (°) | 95.774 (1) |
V (Å3) | 1380.52 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.90 |
Crystal size (mm) | 0.24 × 0.18 × 0.15 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.813, 0.877 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12572, 3411, 3056 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.666 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.094, 1.00 |
No. of reflections | 3411 |
No. of parameters | 208 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.55, −0.51 |
Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005).
K1—O7 | 2.6745 (14) | K2—O7v | 2.6768 (14) |
K1—O4i | 2.6990 (16) | K2—O11 | 2.747 (2) |
K1—O8ii | 2.7708 (13) | K2—O6 | 2.7749 (14) |
K1—O3iii | 2.8496 (16) | K2—O9 | 2.7811 (14) |
K1—O10 | 2.960 (2) | K2—O2vi | 2.8037 (13) |
K1—O10iv | 3.039 (2) | K2—O9vii | 2.8130 (13) |
K1—O9 | 3.1156 (15) | K2—O8v | 3.2558 (17) |
K1—O6 | 3.1981 (15) | K2—O5viii | 3.3744 (14) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (iv) −x+3/2, y−1/2, −z+1/2; (v) x, y−1, z; (vi) −x, −y, −z; (vii) −x+1, −y, −z; (viii) −x+1/2, y−1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O2 | 0.890 (17) | 1.489 (18) | 2.3771 (19) | 176 (3) |
O5—H5···O1ix | 0.835 (17) | 1.811 (18) | 2.6400 (18) | 172 (3) |
O10—H10A···O11x | 0.815 (18) | 2.05 (2) | 2.814 (3) | 155 (3) |
O10—H10B···O1ii | 0.842 (18) | 2.116 (19) | 2.952 (2) | 172 (3) |
O11—H11A···O4viii | 0.788 (18) | 2.42 (3) | 2.958 (3) | 127 (3) |
O11—H11B···O3iii | 0.823 (18) | 2.13 (2) | 2.888 (2) | 154 (4) |
Symmetry codes: (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x+1/2, −y+1/2, z+1/2; (x) −x+3/2, y+1/2, −z+1/2. |