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In the title polymeric complex, [K(C7H5O6S)(H2O)3]n, the anions use their sulfonyl and double-bond carbonyl O atoms to link to four K+ cations in a μ4-bonding mode. The compound has a three-dimensional framework which consists of dinuclear [K2O10] fragments linked by sulfonate and carboxylic O atoms from the sulfosalicylate (ssa) ligand. In the three-dimensional network, there are different types of channels along the a, b and c axes. In the crystal structure, classical inter­molecular O—H...O hydrogen bonds also stabilize the three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807020934/hj3040sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807020934/hj3040Isup2.hkl
Contains datablock I

CCDC reference: 650518

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.035
  • wR factor = 0.129
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

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Alert level B PLAT416_ALERT_2_B Short Intra D-H..H-D H3A .. H9A .. 1.14 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT736_ALERT_1_C H...A Calc 2.02(3), Rep 2.021(12) ...... 2.50 su-Ra H7B -O4 1.555 1.545 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.33 Ratio
Alert level G ABSTY01_ALERT_1_G Extra text has been found in the _exptl_absorpt_correction_type field, which should be only a single keyword. A literature citation should be included in the _exptl_absorpt_process_details field. PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 11
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The rational design and synthesis of metal-organic high-dimensional networks are of great interest because of their intriguing structural diversity and their potential applications as functional solid materials (Moulton et al.,2001; Yaghi et al.,2003; Kitagawa et al.,2004). The study of solid-state metal-organic coordination frameworks has concentrated on transition metal complexes, while little attention being paid to the s-block metals, such as Na and K (Braga et al.,1998; Henderson et al., 2003; Sheldrick et al., 2000). Pharmaceuticals, dyes, and pigments typically utilize alkali and alkaline earth cations in preference to transition metals as, in broad terms, the s-block metals have advantages of nontoxicity, cheapness, and often aqueous solubility (Alan et al.,2006). So far most of these materials are formed with N-containing ligands, such as 4,4'-bipyridine and pyrazine(Yaghi et al.,1997; Lloret et al.,1998). The study on ligands containing different coordinating groups is relatively limited(Distler et al.,1998; Hix et al.,2001; Drumel et al.,1995), and we are interested in coordination polymers containing such ligands. It has been demonstrated that the 5-sulfosalicylic acid(Hssa) is a multifunctional ligand(Ma et al., 2005; Gao et al.,2005), which has three potential coordinating groups –OH, –CO2H and –SO3H. Both –CO2H and –SO3H are versatile coordinating groups, that can coordinate to metal in a variety of modes. Until now, the study on the coordination polymers constructed using the Hssa ligand and main group metals with three-dimensional open framework is very rare. In this paper, the first potassium complex with an interesting 3-D framework structure, [K(ssa)(H2O)3](Hssa=5-sulfosalicylic acid) I, was synthesized in aqueous solution and characterizated by single-crystal diffraction.

There is one crystallographically unique potassium ions in the structure (Fig. 1 and Table 1). The K+ ion is 8-coordinated by four water molecules (O7, O8, O9 and O8C, symmetry code C: -x - 1, -y, -z + 2),three sulfonate oxygen atoms (O6, O6D and O5E, symmetry code D: -x, -y, -z + 2; E: x, y - 1, z) and one double-bond carboxylic oxygen atom (O2B, symmetry code B:-x, -y, -z + 1) from four different ssa- anions. The K—O(water) distances and potassium sulfonate oxygen distances range from 2.732 (2) to 3.242 (2) and 2.731 (2) to 2.757 (2) Å, respectively, which are similar to reported values (Kennedy et al.,2004). The potassium carboxylic oxygen distance is 2.668 (2) Å, while the O—K—O bond angles are in the range of 34.55 (3) to 163.77 (4)°.

In compound (I), –SO3H group is deprotonated, but the –CO2H and –OH groups are neutral. The K1 and its symmetry-related ion (K1C, symmetry code C: -x - 1,-y,-z + 2) are linked by two µ2-O from water ligands (O8 and O8C, symmetry code C: -x - 1, -y, -z + 2) to form a dinuclear unit (K2O10), in which the K1···K1C (symmetry code C: -x - 1,-y,-z + 2) distance is 4.3273 (9) Å.

Each –SO3 group in the ssa- anion acts as a tridentate ligand linked with three different potassium ions through two sulfonate oxygen atoms, in which one binds to two potassium ions from the dinuclear unit while the other binds to only a single potassium ion. The –CO2H group monodentately coordinate to one potassium ion from the dinuclear unit. Thus, each ssa- anion acting as tetradentate ligand binding to four potassium ions.

As shown in Figs. 2 and 3, the network structure of (I) may be described in terms of a three-dimensional open framework which consists of dinuclear {K2O10} fragments linked by sulfonate(carboxylic) oxygen atoms from the ssa- ligands. The most unusual feature is that in the 3-D network of (I), there exist different types of channels along the a, b and c axes. In fact, there are intercrossing three-dimensional channels in the open framework of compound (I).

In the crystal structure, classical intermolecular O—H···O hydrogen bonds are observed (Table 2),which link –OH, –CO2H and –SO3H in the ssa- ligand and coordinated water molecules and also stabilize the 3-D structure.

Related literature top

For related literature, see: Braga et al. (1998); Distler & Sevov (1998); Drumel et al. (1995); Gao et al. (2005); Henderson et al. (2003); Hix et al. (2001); Kennedy et al. (2004, 2006); Kitagawa et al. (2004); Lloret et al. (1998); Ma et al. (2005); Moulton & Zaworotko (2001); Sheldrick (2000); Yaghi et al. (1997, 2003).

Experimental top

An aqueous solution (10 cm3) of 5-sulfosalicylic acid(0.219 g, 1.0 mmol) was added dropwise to a stirred solution(10 cm3) of KCl(0.091 g, 1.2 mmol) at 70°C for 20 min. Then the solution was adjusted to pH=2.8 by the addition of dilute HCl solution. The resulting colerless solution was allowed to stand in air at room temperature for a week, yielding block colorless crystals(65%). Elemental analysis found(calculated): C 24.01(23.99),H 3.46(3.50), S 3.39(3.36).

Refinement top

The water and hydroxyl H atoms were found in a difference Fourier map and were refined with distance restraints O—H=0.85 (1)Å and H···H=1.39 (1) Å. H atoms bonded to C atoms were treated as riding, with Uiso(H) values equal to 1.2Ueq(C) and C—H distances of 0.93 Å.

Structure description top

The rational design and synthesis of metal-organic high-dimensional networks are of great interest because of their intriguing structural diversity and their potential applications as functional solid materials (Moulton et al.,2001; Yaghi et al.,2003; Kitagawa et al.,2004). The study of solid-state metal-organic coordination frameworks has concentrated on transition metal complexes, while little attention being paid to the s-block metals, such as Na and K (Braga et al.,1998; Henderson et al., 2003; Sheldrick et al., 2000). Pharmaceuticals, dyes, and pigments typically utilize alkali and alkaline earth cations in preference to transition metals as, in broad terms, the s-block metals have advantages of nontoxicity, cheapness, and often aqueous solubility (Alan et al.,2006). So far most of these materials are formed with N-containing ligands, such as 4,4'-bipyridine and pyrazine(Yaghi et al.,1997; Lloret et al.,1998). The study on ligands containing different coordinating groups is relatively limited(Distler et al.,1998; Hix et al.,2001; Drumel et al.,1995), and we are interested in coordination polymers containing such ligands. It has been demonstrated that the 5-sulfosalicylic acid(Hssa) is a multifunctional ligand(Ma et al., 2005; Gao et al.,2005), which has three potential coordinating groups –OH, –CO2H and –SO3H. Both –CO2H and –SO3H are versatile coordinating groups, that can coordinate to metal in a variety of modes. Until now, the study on the coordination polymers constructed using the Hssa ligand and main group metals with three-dimensional open framework is very rare. In this paper, the first potassium complex with an interesting 3-D framework structure, [K(ssa)(H2O)3](Hssa=5-sulfosalicylic acid) I, was synthesized in aqueous solution and characterizated by single-crystal diffraction.

There is one crystallographically unique potassium ions in the structure (Fig. 1 and Table 1). The K+ ion is 8-coordinated by four water molecules (O7, O8, O9 and O8C, symmetry code C: -x - 1, -y, -z + 2),three sulfonate oxygen atoms (O6, O6D and O5E, symmetry code D: -x, -y, -z + 2; E: x, y - 1, z) and one double-bond carboxylic oxygen atom (O2B, symmetry code B:-x, -y, -z + 1) from four different ssa- anions. The K—O(water) distances and potassium sulfonate oxygen distances range from 2.732 (2) to 3.242 (2) and 2.731 (2) to 2.757 (2) Å, respectively, which are similar to reported values (Kennedy et al.,2004). The potassium carboxylic oxygen distance is 2.668 (2) Å, while the O—K—O bond angles are in the range of 34.55 (3) to 163.77 (4)°.

In compound (I), –SO3H group is deprotonated, but the –CO2H and –OH groups are neutral. The K1 and its symmetry-related ion (K1C, symmetry code C: -x - 1,-y,-z + 2) are linked by two µ2-O from water ligands (O8 and O8C, symmetry code C: -x - 1, -y, -z + 2) to form a dinuclear unit (K2O10), in which the K1···K1C (symmetry code C: -x - 1,-y,-z + 2) distance is 4.3273 (9) Å.

Each –SO3 group in the ssa- anion acts as a tridentate ligand linked with three different potassium ions through two sulfonate oxygen atoms, in which one binds to two potassium ions from the dinuclear unit while the other binds to only a single potassium ion. The –CO2H group monodentately coordinate to one potassium ion from the dinuclear unit. Thus, each ssa- anion acting as tetradentate ligand binding to four potassium ions.

As shown in Figs. 2 and 3, the network structure of (I) may be described in terms of a three-dimensional open framework which consists of dinuclear {K2O10} fragments linked by sulfonate(carboxylic) oxygen atoms from the ssa- ligands. The most unusual feature is that in the 3-D network of (I), there exist different types of channels along the a, b and c axes. In fact, there are intercrossing three-dimensional channels in the open framework of compound (I).

In the crystal structure, classical intermolecular O—H···O hydrogen bonds are observed (Table 2),which link –OH, –CO2H and –SO3H in the ssa- ligand and coordinated water molecules and also stabilize the 3-D structure.

For related literature, see: Braga et al. (1998); Distler & Sevov (1998); Drumel et al. (1995); Gao et al. (2005); Henderson et al. (2003); Hix et al. (2001); Kennedy et al. (2004, 2006); Kitagawa et al. (2004); Lloret et al. (1998); Ma et al. (2005); Moulton & Zaworotko (2001); Sheldrick (2000); Yaghi et al. (1997, 2003).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XPREP (Bruker, 1997); software used to prepare material for publication: SHELXTL (Siemens, 1994).

Figures top
[Figure 1] Fig. 1. View of the asymmetric unit of (I) with the atom labeling scheme. Displacement ellipsoids are drawn at the 35% probability level and H atoms are drawn as spheres of arbitrary radii.The symmetry codes are those used in Table 1.
[Figure 2] Fig. 2. Ball-stick views of compound (I) showing different channels along the a axis. The H atoms of the coordinated water are omitted for clarity.
[Figure 3] Fig. 3. Ball-stick views of compound (I) showing different channels along the b axis. The H atoms of the coordinated water are omitted for clarity.
poly[triaqua(µ4-5-sulfosalicylato)potassium(I)] top
Crystal data top
[K(C7H5O6S)(H2O)3]V = 594.44 (3) Å3
Mr = 310.32Z = 2
Triclinic, P1F(000) = 320
Hall symbol: -P 1Dx = 1.734 Mg m3
a = 7.2648 (2) ÅMo Kα radiation, λ = 0.71070 Å
b = 7.2760 (2) ŵ = 0.66 mm1
c = 11.9225 (4) ÅT = 223 K
α = 87.394 (2)°Block, colourless
β = 81.907 (2)°0.60 × 0.38 × 0.30 mm
γ = 72.313 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
2149 independent reflections
Radiation source: fine-focus sealed tube2002 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 25.4°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.693, Tmax = 0.827k = 88
5725 measured reflectionsl = 1314
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.112P)2]
where P = (Fo2 + 2Fc2)/3
2149 reflections(Δ/σ)max = 0.014
188 parametersΔρmax = 0.57 e Å3
11 restraintsΔρmin = 0.66 e Å3
Crystal data top
[K(C7H5O6S)(H2O)3]γ = 72.313 (2)°
Mr = 310.32V = 594.44 (3) Å3
Triclinic, P1Z = 2
a = 7.2648 (2) ÅMo Kα radiation
b = 7.2760 (2) ŵ = 0.66 mm1
c = 11.9225 (4) ÅT = 223 K
α = 87.394 (2)°0.60 × 0.38 × 0.30 mm
β = 81.907 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
2149 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2002 reflections with I > 2σ(I)
Tmin = 0.693, Tmax = 0.827Rint = 0.017
5725 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03511 restraints
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 0.57 e Å3
2149 reflectionsΔρmin = 0.66 e Å3
188 parameters
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
K10.21738 (6)0.07091 (6)0.89768 (4)0.0259 (2)
S10.00136 (7)0.35575 (6)0.84164 (4)0.0204 (2)
O10.2733 (2)0.2594 (3)0.41097 (13)0.0375 (4)
H1B0.178 (3)0.218 (4)0.3606 (17)0.045*
O20.0876 (2)0.1545 (2)0.32035 (12)0.0336 (4)
O30.3188 (2)0.1565 (2)0.42516 (13)0.0344 (4)
H3A0.388 (3)0.135 (3)0.3612 (12)0.041*
O40.2022 (2)0.3544 (2)0.81377 (12)0.0277 (4)
O50.1288 (2)0.5369 (2)0.88906 (12)0.0303 (4)
O60.0158 (2)0.1913 (2)0.91284 (12)0.0286 (4)
O70.2490 (3)0.2851 (2)0.86574 (14)0.0408 (4)
H7B0.244 (5)0.390 (3)0.8412 (19)0.061*
H7A0.201 (4)0.271 (4)0.9349 (11)0.061*
O80.5126 (2)0.2531 (2)0.96902 (14)0.0377 (4)
H8A0.519 (4)0.341 (3)1.0167 (18)0.045*
H8B0.613 (3)0.301 (3)0.933 (2)0.045*
O90.5442 (2)0.0411 (2)0.77160 (13)0.0309 (4)
H9B0.614 (3)0.108 (3)0.8055 (16)0.037*
H9A0.523 (4)0.071 (3)0.7020 (9)0.037*
C10.2767 (3)0.3642 (3)0.70429 (18)0.0281 (5)
H1A0.36830.40600.76900.034*
C20.3391 (3)0.3402 (3)0.60464 (18)0.0311 (5)
H2A0.47290.36470.60130.037*
C30.2040 (3)0.2791 (3)0.50731 (17)0.0264 (5)
C40.0053 (3)0.2436 (3)0.51325 (16)0.0222 (4)
C50.0560 (3)0.2686 (3)0.61575 (16)0.0209 (4)
H5A0.18940.24530.62000.025*
C60.0788 (3)0.3274 (3)0.71112 (16)0.0210 (4)
C70.1370 (3)0.1813 (3)0.41096 (17)0.0240 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0292 (3)0.0247 (3)0.0241 (3)0.0091 (2)0.0019 (2)0.0032 (2)
S10.0232 (3)0.0198 (3)0.0183 (3)0.0071 (2)0.0006 (2)0.0029 (2)
O10.0273 (9)0.0596 (11)0.0249 (8)0.0089 (8)0.0084 (6)0.0059 (7)
O20.0330 (9)0.0487 (9)0.0183 (8)0.0118 (7)0.0009 (6)0.0043 (7)
O30.0260 (9)0.0536 (10)0.0241 (8)0.0148 (8)0.0033 (6)0.0075 (7)
O40.0246 (8)0.0335 (8)0.0270 (8)0.0116 (6)0.0023 (6)0.0065 (6)
O50.0364 (9)0.0249 (7)0.0257 (8)0.0039 (6)0.0005 (6)0.0083 (6)
O60.0372 (9)0.0274 (7)0.0241 (8)0.0137 (6)0.0057 (6)0.0012 (6)
O70.0563 (11)0.0404 (9)0.0337 (9)0.0304 (8)0.0058 (8)0.0100 (7)
O80.0310 (9)0.0449 (9)0.0326 (9)0.0036 (7)0.0041 (7)0.0067 (7)
O90.0297 (8)0.0392 (9)0.0249 (8)0.0140 (7)0.0028 (6)0.0047 (7)
C10.0237 (11)0.0316 (11)0.0245 (11)0.0045 (9)0.0032 (8)0.0017 (9)
C20.0195 (10)0.0409 (12)0.0297 (11)0.0052 (9)0.0017 (8)0.0001 (9)
C30.0290 (11)0.0275 (10)0.0224 (10)0.0069 (9)0.0066 (8)0.0010 (8)
C40.0245 (10)0.0212 (9)0.0190 (10)0.0054 (8)0.0008 (8)0.0008 (8)
C50.0190 (10)0.0221 (9)0.0218 (10)0.0070 (8)0.0018 (7)0.0007 (7)
C60.0258 (10)0.0182 (9)0.0189 (10)0.0065 (8)0.0026 (8)0.0027 (7)
C70.0262 (10)0.0244 (10)0.0205 (10)0.0077 (8)0.0001 (8)0.0001 (8)
Geometric parameters (Å, º) top
K1—O2i2.6686 (15)O3—H3A0.845 (10)
K1—O5ii2.7315 (14)O5—K1v2.7315 (14)
K1—O82.7345 (16)O6—K1iv2.9556 (14)
K1—O62.7604 (15)O7—H7B0.843 (10)
K1—O92.9338 (16)O7—H7A0.847 (10)
K1—O8iii2.9394 (18)O8—K1iii2.9394 (18)
K1—O6iv2.9556 (14)O8—H8A0.862 (10)
K1—O73.2456 (19)O8—H8B0.870 (10)
K1—K1iii4.3258 (9)O9—H9B0.859 (10)
K1—K1iv4.6230 (9)O9—H9A0.847 (9)
K1—H7A3.03 (3)C1—C21.366 (3)
S1—O51.4465 (14)C1—C61.394 (3)
S1—O61.4569 (14)C1—H1A0.9400
S1—O41.4662 (15)C2—C31.403 (3)
S1—C61.7683 (19)C2—H2A0.9400
O1—C31.347 (3)C3—C41.398 (3)
O1—H1B0.840 (10)C4—C51.395 (3)
O2—C71.227 (3)C4—C71.474 (3)
O2—K1i2.6686 (15)C5—C61.382 (3)
O3—C71.311 (3)C5—H5A0.9400
O2i—K1—O5ii75.99 (5)O6iv—K1—H7A40.9 (2)
O2i—K1—O8123.24 (5)O7—K1—H7A15.0 (2)
O5ii—K1—O8142.02 (5)K1iii—K1—H7A136.3 (2)
O2i—K1—O695.58 (5)K1iv—K1—H7A45.4 (4)
O5ii—K1—O6136.33 (5)O5—S1—O6112.44 (9)
O8—K1—O678.32 (5)O5—S1—O4113.18 (9)
O2i—K1—O969.64 (4)O6—S1—O4110.93 (9)
O5ii—K1—O988.56 (5)O5—S1—C6106.78 (9)
O8—K1—O971.83 (5)O6—S1—C6107.43 (8)
O6—K1—O9129.16 (4)O4—S1—C6105.60 (8)
O2i—K1—O8iii121.94 (5)C3—O1—H1B108.0 (19)
O5ii—K1—O8iii61.99 (5)C7—O2—K1i143.75 (14)
O8—K1—O8iii80.71 (5)C7—O3—H3A108.3 (18)
O6—K1—O8iii142.48 (5)S1—O5—K1v148.50 (9)
O9—K1—O8iii71.07 (4)S1—O6—K1131.03 (8)
O2i—K1—O6iv125.55 (5)S1—O6—K1iv120.92 (8)
O5ii—K1—O6iv78.51 (4)K1—O6—K1iv107.90 (4)
O8—K1—O6iv106.27 (5)K1—O7—H7B97 (2)
O6—K1—O6iv72.10 (4)K1—O7—H7A68 (2)
O9—K1—O6iv155.59 (5)H7B—O7—H7A110.3 (16)
O8iii—K1—O6iv84.56 (4)K1—O8—K1iii99.29 (5)
O2i—K1—O769.99 (4)K1—O8—H8A131.3 (16)
O5ii—K1—O767.47 (4)K1iii—O8—H8A98 (2)
O8—K1—O7146.52 (5)K1—O8—H8B122.5 (15)
O6—K1—O769.40 (4)K1iii—O8—H8B81.3 (19)
O9—K1—O7136.88 (4)H8A—O8—H8B104.8 (14)
O8iii—K1—O7120.54 (4)K1—O9—H9B109.1 (16)
O6iv—K1—O755.87 (4)K1—O9—H9A120.1 (17)
O2i—K1—K1iii134.91 (4)H9B—O9—H9A107.3 (14)
O5ii—K1—K1iii100.32 (4)C2—C1—C6120.72 (19)
O8—K1—K1iii42.11 (4)C2—C1—H1A119.6
O6—K1—K1iii114.26 (4)C6—C1—H1A119.6
O9—K1—K1iii65.32 (3)C1—C2—C3120.2 (2)
O8iii—K1—K1iii38.60 (3)C1—C2—H2A119.9
O6iv—K1—K1iii96.46 (3)C3—C2—H2A119.9
O7—K1—K1iii150.75 (3)O1—C3—C4122.78 (18)
O2i—K1—K1iv115.45 (4)O1—C3—C2117.81 (18)
O5ii—K1—K1iv107.73 (4)C4—C3—C2119.40 (18)
O8—K1—K1iv93.33 (4)C5—C4—C3119.68 (17)
O6—K1—K1iv37.47 (3)C5—C4—C7120.71 (17)
O9—K1—K1iv163.58 (3)C3—C4—C7119.62 (17)
O8iii—K1—K1iv114.39 (4)C6—C5—C4120.24 (18)
O6iv—K1—K1iv34.62 (3)C6—C5—H5A119.9
O7—K1—K1iv55.33 (3)C4—C5—H5A119.9
K1iii—K1—K1iv108.502 (17)C5—C6—C1119.76 (18)
O2i—K1—H7A84.9 (2)C5—C6—S1120.37 (15)
O5ii—K1—H7A68.1 (5)C1—C6—S1119.87 (15)
O8—K1—H7A138.7 (4)O2—C7—O3123.26 (19)
O6—K1—H7A68.5 (5)O2—C7—C4122.08 (18)
O9—K1—H7A149.2 (3)O3—C7—C4114.66 (17)
O8iii—K1—H7A111.5 (4)
O6—S1—O5—K1v159.19 (15)O8iii—K1—O8—K1iii0.0
O4—S1—O5—K1v32.5 (2)O6iv—K1—O8—K1iii81.50 (5)
C6—S1—O5—K1v83.23 (18)O7—K1—O8—K1iii133.31 (7)
O5—S1—O6—K199.55 (11)K1iv—K1—O8—K1iii114.18 (4)
O4—S1—O6—K1132.59 (10)C6—C1—C2—C30.4 (3)
C6—S1—O6—K117.64 (13)C1—C2—C3—O1179.40 (19)
O5—S1—O6—K1iv85.42 (11)C1—C2—C3—C40.2 (3)
O4—S1—O6—K1iv42.44 (11)O1—C3—C4—C5179.45 (17)
C6—S1—O6—K1iv157.38 (8)C2—C3—C4—C50.3 (3)
O2i—K1—O6—S149.90 (12)O1—C3—C4—C70.2 (3)
O5ii—K1—O6—S1125.43 (11)C2—C3—C4—C7179.40 (19)
O8—K1—O6—S172.93 (12)C3—C4—C5—C60.2 (3)
O9—K1—O6—S118.31 (14)C7—C4—C5—C6179.90 (17)
O8iii—K1—O6—S1130.24 (10)C4—C5—C6—C10.8 (3)
O6iv—K1—O6—S1175.52 (15)C4—C5—C6—S1179.07 (13)
O7—K1—O6—S1116.07 (12)C2—C1—C6—C50.9 (3)
K1iii—K1—O6—S195.39 (11)C2—C1—C6—S1178.97 (16)
K1iv—K1—O6—S1175.52 (15)O5—S1—C6—C5134.71 (15)
O2i—K1—O6—K1iv125.61 (5)O6—S1—C6—C5104.47 (16)
O5ii—K1—O6—K1iv50.09 (8)O4—S1—C6—C513.98 (18)
O8—K1—O6—K1iv111.55 (6)O5—S1—C6—C145.39 (18)
O9—K1—O6—K1iv166.17 (5)O6—S1—C6—C175.43 (17)
O8iii—K1—O6—K1iv54.24 (9)O4—S1—C6—C1166.12 (15)
O6iv—K1—O6—K1iv0.0K1i—O2—C7—O35.6 (4)
O7—K1—O6—K1iv59.44 (5)K1i—O2—C7—C4174.65 (14)
K1iii—K1—O6—K1iv89.09 (5)C5—C4—C7—O2178.52 (18)
O2i—K1—O8—K1iii122.25 (5)C3—C4—C7—O21.8 (3)
O5ii—K1—O8—K1iii10.60 (10)C5—C4—C7—O31.2 (3)
O6—K1—O8—K1iii148.71 (5)C3—C4—C7—O3178.45 (17)
O9—K1—O8—K1iii73.01 (5)
Symmetry codes: (i) x, y, z+1; (ii) x, y1, z; (iii) x1, y, z+2; (iv) x, y, z+2; (v) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O20.84 (1)1.84 (2)2.586 (2)147 (3)
O3—H3A···O9i0.85 (1)1.84 (1)2.674 (2)170 (2)
O7—H7A···O6iv0.85 (1)2.09 (1)2.917 (2)164 (3)
O7—H7B···O4ii0.84 (1)2.02 (1)2.852 (2)168 (2)
O8—H8A···O5vi0.86 (1)2.55 (3)2.926 (2)108 (2)
O8—H8A···O7iv0.86 (1)2.50 (2)2.997 (2)118 (2)
O8—H8B···O4vii0.87 (1)2.04 (1)2.879 (2)163 (2)
O9—H9A···O3i0.85 (1)1.95 (2)2.674 (2)144 (2)
O9—H9B···O7vii0.86 (1)1.91 (1)2.763 (2)172 (2)
Symmetry codes: (i) x, y, z+1; (ii) x, y1, z; (iv) x, y, z+2; (vi) x1, y+1, z+2; (vii) x1, y, z.

Experimental details

Crystal data
Chemical formula[K(C7H5O6S)(H2O)3]
Mr310.32
Crystal system, space groupTriclinic, P1
Temperature (K)223
a, b, c (Å)7.2648 (2), 7.2760 (2), 11.9225 (4)
α, β, γ (°)87.394 (2), 81.907 (2), 72.313 (2)
V3)594.44 (3)
Z2
Radiation typeMo Kα
µ (mm1)0.66
Crystal size (mm)0.60 × 0.38 × 0.30
Data collection
DiffractometerSiemens SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.693, 0.827
No. of measured, independent and
observed [I > 2σ(I)] reflections
5725, 2149, 2002
Rint0.017
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.129, 1.01
No. of reflections2149
No. of parameters188
No. of restraints11
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.57, 0.66

Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XPREP (Bruker, 1997), SHELXTL (Siemens, 1994).

Selected geometric parameters (Å, º) top
K1—O2i2.6686 (15)K1—O92.9338 (16)
K1—O5ii2.7315 (14)K1—O8iii2.9394 (18)
K1—O82.7345 (16)K1—O6iv2.9556 (14)
K1—O62.7604 (15)K1—O73.2456 (19)
O2i—K1—O5ii75.99 (5)O6—K1—O9129.16 (4)
O2i—K1—O8123.24 (5)O5ii—K1—O8iii61.99 (5)
O5ii—K1—O8142.02 (5)O6—K1—O8iii142.48 (5)
O5ii—K1—O6136.33 (5)O2i—K1—O6iv125.55 (5)
O8—K1—O678.32 (5)O6—K1—O6iv72.10 (4)
O2i—K1—O969.64 (4)
Symmetry codes: (i) x, y, z+1; (ii) x, y1, z; (iii) x1, y, z+2; (iv) x, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O20.840 (10)1.839 (18)2.586 (2)147 (3)
O3—H3A···O9i0.845 (10)1.838 (11)2.674 (2)170 (2)
O7—H7A···O6iv0.847 (10)2.092 (13)2.917 (2)164 (3)
O7—H7B···O4ii0.843 (10)2.021 (12)2.852 (2)168 (2)
O8—H8A···O5v0.862 (10)2.55 (3)2.926 (2)108 (2)
O8—H8A···O7iv0.862 (10)2.50 (2)2.997 (2)117.9 (18)
O8—H8B···O4vi0.870 (10)2.037 (11)2.879 (2)163 (2)
O9—H9A···O3i0.847 (9)1.945 (16)2.674 (2)144 (2)
O9—H9B···O7vi0.859 (10)1.910 (11)2.763 (2)172 (2)
Symmetry codes: (i) x, y, z+1; (ii) x, y1, z; (iv) x, y, z+2; (v) x1, y+1, z+2; (vi) x1, y, z.
 

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