Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The asymmetric unit of the title coordination polymer, [Gd2(C7H4O5S)2(C2O4)(H2O)6]n or [Gd(2-SB)(ox)0.5(H2O)3]2n (2-SB is 2-sulfonato­benzoate and ox is oxalate), (I), consists of one GdIII ion, one 2-SB anion, three coordinated water mol­ecules and one half of an ox ligand. The ox ligand is located on a crystallographic inversion centre. The GdIII centre shows a distorted tricapped trigonal–prismatic coordination formed by nine O atoms from two 2-SB anions, one ox ligand and three coordinated water mol­ecules. The carboxylate and sulfonate groups of the 2-SB anions adopt μ212 and μ1001 coordination modes to link two GdIII ions, generating a centrosymmetric binuclear [Gd2(2-SB)2(H2O)6]2− subunit. The ox ligand acts as a bridge, linking the binuclear [Gd2(2-SB)2(H2O)6]2− subunits into a one-dimensional chain structure parallel to the b axis. Furthermore, extensive O—H...O hydrogen bonds connect the chains into a three-dimensional supra­molecular architecture.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270111001065/lg3047sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270111001065/lg3047Isup2.hkl
Contains datablock I

CCDC reference: 817036

Comment top

During the past decades, metal–organic coordination polymers (MOCPs) containing lanthanide ions have attracted considerable attention, not only for their novel topologies but also for their potential in the areas of magnetic and fluorescence applications, molecular recognition and photovoltaic conversion (Kido & Okamoto, 2002; Tsukube & Shinoda, 2002; Li et al., 2006; Manna et al., 2006; Zhao et al., 2008; Huang et al., 2009). A key strategy in the construction of MOCPs is to select suitable bi- or multidentate bridging ligands. 2-Sulfonatobenzoate (2-SB) is a prime example of such a ligand for the preparation of MOCPs: its semi-rigidity allows the ligands to accommodate the coordination geometries of different metal centres, and its many O atoms can take part in hydrogen bonds to benefit [leading to] the formation of supramolecular structures. Many transition metal coordination polymers with 2-SB have been prepared and characterized (Li & Yang, 2004; Su et al., 2005; Xiao et al., 2005; Chagas et al., 2008). However, reports of lanthanide coordination compounds with 2-SB are relatively less common: only six lanthanide 2-SB complexes were reported by Li's group, namely, {[Ln2(2-SB)3(phen)3(H2O)2]. nH2O}2 (Ln = Sm, n = 3; Ln = Eu, n = 2; Ln = Tb, n = 2; Ln = Dy, n = 2.5; Ln = Er, Y, n = 4.5) [phen = phenyl?] (Li et al., 2008; Wan et al., 2009). In these compounds, 2-SB works as a bridge and phen as a terminal, and the structures consist of isolated tetranuclear complex molecules, which further assembled into three-dimensional supramolecular architectures through hydrogen-bonding. During our research on coordination polymers containing 2-SB, the oxalate (ox) ligand was selected as a bridge to replace the terminal ligand phen, and the title one-dimensional coordination polymer, (I), was obtained under hydrothermal conditions; this is the first lanthanide metal coordination polymer with 2-SB according to the Cambridge Structural Database (CSD, Version 5.31 of August 2010; Allen, 2002).

The asymmetric unit of the title complex contains one GdIII ion, one 2-SB, three coordinated water molecules and one half of an ox ligand, located on an inversion centre. The GdIII centre is coordinated by nine oxygen atoms from two 2-SB, one ox and three coordinated water molecules with tricapped trigonal–prismatic geometry (Fig. 1). The 2-SB adopts µ2-η1: η2 and µ1-η0: η0: η1 modes to link two GdIII ions, generating a centrosymmetric binuclear [Gd2(2-SB)2(H2O)6]2- subunit. The ox forms a bis-µ1-η1: η1 chelating bridge so that the binuclear [Gd2(2-SB)2(H2O)6]2- subunits form chains parallel to the b axis (Fig. 2). In the structure of the previously reported six lanthanide 2-SB complexes (Li et al., 2008, Wan et al., 2009), the 2-SBs adopt µ2-η1: η1 and µ1-η0: η0: η1 modes or µ1-η0: η1 and µ1-η0: η0: η1 modes. In (I), atoms O2ii, O7i, O3W [symmetry codes: (i) -x + 1, -y, -z; (ii) -x + 1, -y + 1, -z] are situated on the tricapped positions of the coordination polyhedron, atoms O2, O5, O6 and O1W, O2W, O1ii are on the top and bottom of the trigonal prism, and the dihedral angle between these two trigonal prisms is 33.7 (1)°, which indicates that the local coordination geometry around the GdIII centre is seriously distorted. The Gd—O bond lengths are in the range 2.368 (3)–2.820 (3) Å, which is similar to reported values (Song et al., 2004). The S—O bond lengths vary from 1.454 (3) to 1.467 (3) Å, and all fall within the typical range of S—O bond distances in the sulfonate anion (Onoda et al., 2001). The similarity in the three S—O bond lengths indicates that the strong conjugation in the sulfonate group is predominant in the structure of the title polymer. In the chain, GdIII ions adopt a zigzag arrangement, in which the Gd···Gd···Gd angles are 104.202 (8)°. The shortest Gd···Gd distance is 4.389 (2) Å, which is shorter than in the previously reported six lanthanide 2-SB complexes (Li et al., 2008, Wan et al., 2009), namely Ln···Ln = 5.454 (3) Å. The short distance of metal centres can improve the magnetic coupling. The variance may be due to the fact that the bulky co-ligand phen has larger steric hindrance than ox in the structure of (I). The Gd···Gd distance separated by the ox ligand is 6.282 (2) Å.

The hydrogen-bonding and ππ stacking interactions play an important role in the structure of (I). The hydrogen-bond geometry is given in Table 2. Within the one-dimensional chain, a carboxylic O atom of ox, acting as hydrogen-bond acceptor, is involved in an intra-chain hydrogen bond via atom H1WB of one coordinated water molecule with graph set C(6) (Bernstein et al., 1995). The sulfonate coordinates to the GdIII ion only through one O atom, and the uncoordinated sulfonate O atoms form four types of inter-chain hydrogen bonds with coordinated water molecules (via H1WA, H2WB, H3WA and H3WB). Within these hydrogen bonds, one type (via H3WB) connects the neighbouring chains into a two-dimensional layer (Fig. 2), with ring [graph set?] R22(12). Furthermore, a carboxylic O atom of 2-SB forms one type of inter-chain hydrogen bond via atom H2WA of one coordinated water molecule with a C(6) chain; this connects the two-dimensional hydrogen-bond-supported layers into a three-dimensional supramolecular architecture (Fig. 3). In addition, three types of hydrogen bond (via H1WA, H3WA and H2WB) exist between the two-dimensional layers, forming hydrogen-bonded rings R22(8) and R12(6) to promote the stability of the structure. There also exist weak inter-chain ππ stacking interactions between the phenyl rings of 2-SBs, with a centroid–centroid separation of 3.982 (8) Å.

Related literature top

For related literature, see: Allen (2002); Bernstein et al. (1995); Chagas et al. (2008); Huang et al. (2009); Kido & Okamoto (2002); Li & Yang (2004); Li et al. (2006, 2008); Manna et al. (2006); Onoda et al. (2001); Song et al. (2004); Su et al. (2005); Tsukube & Shinoda (2002); Wan et al. (2009); Xiao et al. (2005); Zhao et al. (2008).

Experimental top

A mixture of 2-sulfobenzoate (30.6 mg, 0.16 mmol), Gd(NO3)3.6H2O (72.5 mg, 0.16 mmol), oxalate (7.3 mg, 0.08 mmol) and KOH aqueous solution (0.6 ml, 1 M) was added to H2O (10 ml). After stirring, the reaction mixture was sealed in a 23 ml Teflon-lined stainless steel reactor and heated at 393 K for 72 h, then cooled slowly to room temperature. Yellow block-shaped crystals of the title coordination polymer were obtained with a yield of 32% (based on Gd).

Refinement top

The ΔF2/s.u. values of the reflections -1 6 6, 1 1 0 and 1 1 1 are 18.32, 16.90 and 13.35, respectively, and Fo2 << Fc2, which may be caused by an inappropriate beam stop mask file (used in data reduction). They are omitted in the refinement. The H atoms bonded to C atoms were refined in idealized positions using the riding-model approximation, with C—H = 0.93 Å, and Uiso(H) = 1.2Ueq(C). The H atoms of the coordinated water molecules were located in difference maps and refined with an O—H distance restraint of 0.85 (2) Å and H···H distance restraint of 1.34 (2) Å, with Uiso(H) = 1.5Ueq(O).

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear (Rigaku, 2002); data reduction: CrystalClear (Rigaku, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The coordination environment of the GdIII ion in (I), showing the atom-labelling scheme and 50% probability displacement ellipsoids. H atoms have been omitted for clarity. [Symmetry codes: (i) -x + 1, -y, -z; (ii) -x + 1, -y + 1, -z.]
[Figure 2] Fig. 2. Hydrogen bonds in (I) connect neighbouring chains into a two-dimensional layer, viewed towards near (7 -1 -4) plane. Inter-chain hydrogen bonds are denoted by thick, and intra-chain hydrogen bonds by thin, dashed lines. H atoms not bonded to water have been omitted for clarity. [Symmetry codes: (i) -x + 1, -y, -z; (v) -x + 1, -y, -z + 1.]
[Figure 3] Fig. 3. Hydrogen bonds connect the two-dimensional layer into a three-dimensional supramoleculer network in (I), viewed along the c axis. Hydrogen bonds are denoted by dashed lines. H atoms not bonded to water have been omitted for clarity. [Symmetry codes: (iii) x + 1, y, z; (iv) x + 1, y - 1, z.]
catena-Poly[[bis(µ-2-sulfonatobenzoato)bis[triaquagadolinium(III)]]- µ-oxalato] top
Crystal data top
[Gd2(C7H4O5S)2(C2O4)(H2O)6]Z = 1
Mr = 910.94F(000) = 436
Triclinic, P1Dx = 2.429 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.7597 (16) ÅCell parameters from 2008 reflections
b = 8.4998 (17) Åθ = 3.3–25.7°
c = 10.641 (2) ŵ = 5.54 mm1
α = 70.98 (3)°T = 293 K
β = 87.90 (3)°Block, yellow
γ = 70.32 (3)°0.26 × 0.15 × 0.09 mm
V = 622.7 (2) Å3
Data collection top
Rigaku Saturn 724 CCD area-detector
diffractometer
2308 independent reflections
Radiation source: fine-focus sealed tube2290 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ω scansθmax = 25.7°, θmin = 3.3°
Absorption correction: numerical
(RAPID-AUTO; Rigaku, 1998)
h = 99
Tmin = 0.20, Tmax = 0.47k = 109
4598 measured reflectionsl = 1212
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)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.050H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0186P)2 + 1.4132P]
where P = (Fo2 + 2Fc2)/3
2308 reflections(Δ/σ)max = 0.001
199 parametersΔρmax = 0.79 e Å3
9 restraintsΔρmin = 0.85 e Å3
Crystal data top
[Gd2(C7H4O5S)2(C2O4)(H2O)6]γ = 70.32 (3)°
Mr = 910.94V = 622.7 (2) Å3
Triclinic, P1Z = 1
a = 7.7597 (16) ÅMo Kα radiation
b = 8.4998 (17) ŵ = 5.54 mm1
c = 10.641 (2) ÅT = 293 K
α = 70.98 (3)°0.26 × 0.15 × 0.09 mm
β = 87.90 (3)°
Data collection top
Rigaku Saturn 724 CCD area-detector
diffractometer
2308 independent reflections
Absorption correction: numerical
(RAPID-AUTO; Rigaku, 1998)
2290 reflections with I > 2σ(I)
Tmin = 0.20, Tmax = 0.47Rint = 0.034
4598 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0219 restraints
wR(F2) = 0.050H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.79 e Å3
2308 reflectionsΔρmin = 0.85 e Å3
199 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
Gd10.66614 (2)0.22407 (2)0.109705 (15)0.01674 (7)
S10.28821 (12)0.19343 (12)0.30992 (9)0.02198 (19)
O30.1660 (4)0.2985 (4)0.1893 (3)0.0335 (6)
O40.2243 (4)0.0586 (4)0.4002 (3)0.0355 (7)
O20.4356 (3)0.4811 (3)0.1272 (3)0.0226 (5)
O50.4775 (3)0.1175 (3)0.2785 (3)0.0239 (5)
O60.4167 (3)0.2256 (3)0.0225 (3)0.0220 (5)
C60.2501 (8)0.4105 (7)0.5982 (5)0.0520 (14)
H60.23780.37550.68950.062*
C10.4154 (5)0.0836 (4)0.0341 (3)0.0181 (7)
C30.2906 (5)0.5137 (5)0.3255 (4)0.0242 (8)
C80.2862 (5)0.3444 (5)0.3935 (4)0.0242 (8)
C20.3201 (5)0.5788 (5)0.1808 (4)0.0205 (7)
C40.2708 (7)0.6300 (6)0.3961 (4)0.0407 (11)
H40.27080.74410.35160.049*
C70.2674 (7)0.2938 (6)0.5296 (4)0.0379 (10)
H70.26630.18030.57510.045*
C50.2511 (9)0.5780 (7)0.5315 (5)0.0539 (14)
H50.23860.65680.57760.065*
O1W0.8132 (4)0.4267 (3)0.1107 (3)0.0323 (7)
H1WA0.924 (3)0.405 (6)0.131 (5)0.048*
H1WB0.763 (5)0.536 (3)0.082 (5)0.048*
O2W0.9997 (4)0.0655 (4)0.1193 (3)0.0293 (6)
H2WA1.060 (6)0.041 (3)0.124 (5)0.044*
H2WB1.066 (6)0.124 (5)0.080 (5)0.044*
O3W0.8250 (4)0.1000 (4)0.3335 (3)0.0341 (7)
H3WA0.941 (3)0.065 (7)0.347 (5)0.051*
H3WB0.789 (6)0.057 (7)0.409 (3)0.051*
O10.2318 (4)0.7378 (3)0.1138 (3)0.0289 (6)
O70.2925 (3)0.0631 (3)0.0929 (3)0.0234 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.01559 (10)0.01520 (10)0.02063 (11)0.00513 (7)0.00239 (7)0.00778 (7)
S10.0204 (4)0.0256 (5)0.0225 (4)0.0113 (4)0.0050 (3)0.0081 (4)
O30.0213 (14)0.0469 (17)0.0302 (15)0.0113 (13)0.0019 (11)0.0101 (13)
O40.0445 (18)0.0367 (16)0.0357 (16)0.0272 (15)0.0173 (13)0.0133 (13)
O20.0193 (13)0.0212 (13)0.0273 (13)0.0040 (11)0.0077 (10)0.0117 (11)
O50.0215 (13)0.0213 (13)0.0263 (13)0.0066 (11)0.0040 (10)0.0053 (11)
O60.0234 (13)0.0151 (12)0.0291 (13)0.0062 (10)0.0015 (10)0.0092 (10)
C60.091 (4)0.043 (3)0.021 (2)0.021 (3)0.009 (2)0.011 (2)
C10.0200 (17)0.0149 (16)0.0188 (16)0.0064 (15)0.0021 (13)0.0045 (13)
C30.0254 (19)0.0210 (18)0.0225 (19)0.0034 (15)0.0049 (15)0.0076 (15)
C80.0270 (19)0.0244 (19)0.0211 (18)0.0079 (16)0.0035 (14)0.0087 (15)
C20.0188 (17)0.0199 (17)0.0219 (17)0.0054 (14)0.0013 (13)0.0068 (14)
C40.065 (3)0.025 (2)0.032 (2)0.013 (2)0.011 (2)0.0107 (18)
C70.059 (3)0.028 (2)0.025 (2)0.016 (2)0.0085 (19)0.0051 (17)
C50.096 (4)0.038 (3)0.031 (3)0.020 (3)0.012 (3)0.020 (2)
O1W0.0195 (13)0.0161 (13)0.0554 (19)0.0040 (11)0.0114 (13)0.0050 (13)
O2W0.0211 (14)0.0263 (14)0.0389 (16)0.0032 (11)0.0050 (11)0.0143 (13)
O3W0.0291 (15)0.0485 (18)0.0226 (14)0.0186 (14)0.0010 (11)0.0033 (13)
O10.0321 (15)0.0197 (13)0.0226 (13)0.0008 (11)0.0062 (11)0.0018 (11)
O70.0204 (13)0.0176 (12)0.0320 (14)0.0037 (10)0.0047 (10)0.0100 (11)
Geometric parameters (Å, º) top
Gd1—O1W2.368 (3)C1—O71.248 (4)
Gd1—O22.370 (3)C1—C1i1.554 (7)
Gd1—O52.415 (3)C3—C41.392 (6)
Gd1—O7i2.418 (2)C3—C81.396 (5)
Gd1—O62.429 (2)C3—C21.495 (5)
Gd1—O1ii2.433 (3)C8—C71.388 (5)
Gd1—O3W2.451 (3)C2—O11.260 (4)
Gd1—O2W2.471 (3)C2—Gd1ii3.015 (4)
Gd1—O2ii2.820 (3)C4—C51.382 (6)
Gd1—C2ii3.015 (4)C4—H40.9300
S1—O41.454 (3)C7—H70.9300
S1—O31.454 (3)C5—H50.9300
S1—O51.467 (3)O1W—H1WA0.840 (19)
S1—C81.779 (4)O1W—H1WB0.831 (19)
O2—C21.260 (4)O2W—H2WA0.855 (19)
O2—Gd1ii2.820 (3)O2W—H2WB0.842 (19)
O6—C11.255 (4)O3W—H3WA0.851 (19)
C6—C51.371 (7)O3W—H3WB0.846 (19)
C6—C71.383 (7)O1—Gd1ii2.433 (3)
C6—H60.9300O7—Gd1i2.418 (2)
O1W—Gd1—O272.97 (9)O3—S1—O5111.38 (16)
O1W—Gd1—O5125.62 (10)O4—S1—C8107.18 (17)
O2—Gd1—O574.39 (9)O3—S1—C8105.74 (18)
O1W—Gd1—O7i145.33 (9)O5—S1—C8107.58 (17)
O2—Gd1—O7i141.66 (9)C2—O2—Gd1158.4 (2)
O5—Gd1—O7i78.34 (9)C2—O2—Gd1ii86.4 (2)
O1W—Gd1—O6136.48 (9)Gd1—O2—Gd1ii115.17 (10)
O2—Gd1—O681.26 (9)S1—O5—Gd1133.99 (15)
O5—Gd1—O677.70 (9)C1—O6—Gd1120.0 (2)
O7i—Gd1—O666.86 (9)C5—C6—C7119.9 (4)
O1W—Gd1—O1ii84.13 (11)C5—C6—H6120.0
O2—Gd1—O1ii113.26 (9)C7—C6—H6120.0
O5—Gd1—O1ii149.37 (10)O7—C1—O6127.0 (3)
O7i—Gd1—O1ii79.11 (9)O7—C1—C1i117.2 (4)
O6—Gd1—O1ii74.51 (10)O6—C1—C1i115.8 (4)
O1W—Gd1—O3W76.45 (10)C4—C3—C8118.8 (3)
O2—Gd1—O3W100.30 (11)C4—C3—C2117.0 (3)
O5—Gd1—O3W68.12 (9)C8—C3—C2124.3 (3)
O7i—Gd1—O3W93.85 (10)C7—C8—C3119.8 (4)
O6—Gd1—O3W143.70 (9)C7—C8—S1117.8 (3)
O1ii—Gd1—O3W134.03 (10)C3—C8—S1122.3 (3)
O1W—Gd1—O2W73.36 (10)O2—C2—O1120.2 (3)
O2—Gd1—O2W145.70 (9)O2—C2—C3121.5 (3)
O5—Gd1—O2W122.03 (10)O1—C2—C3118.2 (3)
O7i—Gd1—O2W72.37 (9)O2—C2—Gd1ii68.98 (19)
O6—Gd1—O2W129.33 (9)O1—C2—Gd1ii51.22 (18)
O1ii—Gd1—O2W69.29 (10)C3—C2—Gd1ii169.4 (3)
O3W—Gd1—O2W65.35 (10)C5—C4—C3120.8 (4)
O1W—Gd1—O2ii69.10 (9)C5—C4—H4119.6
O2—Gd1—O2ii64.83 (10)C3—C4—H4119.6
O5—Gd1—O2ii129.63 (8)C6—C7—C8120.6 (4)
O7i—Gd1—O2ii117.65 (8)C6—C7—H7119.7
O6—Gd1—O2ii68.33 (8)C8—C7—H7119.7
O1ii—Gd1—O2ii48.45 (8)C6—C5—C4120.2 (4)
O3W—Gd1—O2ii145.11 (9)C6—C5—H5119.9
O2W—Gd1—O2ii108.28 (9)C4—C5—H5119.9
O1W—Gd1—C2ii75.22 (11)Gd1—O1W—H1WA128 (3)
O2—Gd1—C2ii89.47 (10)Gd1—O1W—H1WB125 (3)
O5—Gd1—C2ii145.75 (9)H1WA—O1W—H1WB107 (3)
O7i—Gd1—C2ii98.55 (10)Gd1—O2W—H2WA131 (3)
O6—Gd1—C2ii70.00 (9)Gd1—O2W—H2WB118 (3)
O1ii—Gd1—C2ii23.81 (9)H2WA—O2W—H2WB105 (3)
O3W—Gd1—C2ii145.72 (9)Gd1—O3W—H3WA123 (3)
O2W—Gd1—C2ii88.19 (10)Gd1—O3W—H3WB131 (3)
O2ii—Gd1—C2ii24.64 (9)H3WA—O3W—H3WB105 (3)
O4—S1—O3112.83 (18)C2—O1—Gd1ii105.0 (2)
O4—S1—O5111.72 (17)C1—O7—Gd1i119.9 (2)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3iii0.84 (2)1.82 (2)2.636 (4)165 (4)
O1W—H1WB···O6ii0.83 (2)1.94 (2)2.750 (4)163 (4)
O2W—H2WA···O1iv0.86 (2)1.94 (2)2.779 (4)168 (4)
O2W—H2WB···O3iii0.84 (2)2.47 (4)2.983 (4)120 (4)
O3W—H3WA···O4iii0.85 (2)2.27 (3)3.080 (4)160 (5)
O3W—H3WB···O4v0.85 (2)1.96 (2)2.787 (4)164 (4)
Symmetry codes: (ii) x+1, y+1, z; (iii) x+1, y, z; (iv) x+1, y1, z; (v) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[Gd2(C7H4O5S)2(C2O4)(H2O)6]
Mr910.94
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.7597 (16), 8.4998 (17), 10.641 (2)
α, β, γ (°)70.98 (3), 87.90 (3), 70.32 (3)
V3)622.7 (2)
Z1
Radiation typeMo Kα
µ (mm1)5.54
Crystal size (mm)0.26 × 0.15 × 0.09
Data collection
DiffractometerRigaku Saturn 724 CCD area-detector
diffractometer
Absorption correctionNumerical
(RAPID-AUTO; Rigaku, 1998)
Tmin, Tmax0.20, 0.47
No. of measured, independent and
observed [I > 2σ(I)] reflections
4598, 2308, 2290
Rint0.034
(sin θ/λ)max1)0.609
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.050, 1.04
No. of reflections2308
No. of parameters199
No. of restraints9
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.79, 0.85

Computer programs: CrystalClear (Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2004), SHELXL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Gd1—O1W2.368 (3)Gd1—O3W2.451 (3)
Gd1—O22.370 (3)Gd1—O2W2.471 (3)
Gd1—O52.415 (3)Gd1—O2ii2.820 (3)
Gd1—O7i2.418 (2)S1—O41.454 (3)
Gd1—O62.429 (2)S1—O31.454 (3)
Gd1—O1ii2.433 (3)S1—O51.467 (3)
O1W—Gd1—O272.97 (9)O7i—Gd1—O3W93.85 (10)
O1W—Gd1—O5125.62 (10)O6—Gd1—O3W143.70 (9)
O2—Gd1—O574.39 (9)O1ii—Gd1—O3W134.03 (10)
O1W—Gd1—O7i145.33 (9)O1W—Gd1—O2W73.36 (10)
O2—Gd1—O7i141.66 (9)O2—Gd1—O2W145.70 (9)
O5—Gd1—O7i78.34 (9)O5—Gd1—O2W122.03 (10)
O1W—Gd1—O6136.48 (9)O7i—Gd1—O2W72.37 (9)
O2—Gd1—O681.26 (9)O6—Gd1—O2W129.33 (9)
O5—Gd1—O677.70 (9)O1ii—Gd1—O2W69.29 (10)
O7i—Gd1—O666.86 (9)O3W—Gd1—O2W65.35 (10)
O1W—Gd1—O1ii84.13 (11)O1W—Gd1—O2ii69.10 (9)
O2—Gd1—O1ii113.26 (9)O2—Gd1—O2ii64.83 (10)
O5—Gd1—O1ii149.37 (10)O5—Gd1—O2ii129.63 (8)
O7i—Gd1—O1ii79.11 (9)O7i—Gd1—O2ii117.65 (8)
O6—Gd1—O1ii74.51 (10)O6—Gd1—O2ii68.33 (8)
O1W—Gd1—O3W76.45 (10)O1ii—Gd1—O2ii48.45 (8)
O2—Gd1—O3W100.30 (11)O3W—Gd1—O2ii145.11 (9)
O5—Gd1—O3W68.12 (9)O2W—Gd1—O2ii108.28 (9)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O3iii0.840 (19)1.82 (2)2.636 (4)165 (4)
O1W—H1WB···O6ii0.831 (19)1.94 (2)2.750 (4)163 (4)
O2W—H2WA···O1iv0.855 (19)1.94 (2)2.779 (4)168 (4)
O2W—H2WB···O3iii0.842 (19)2.47 (4)2.983 (4)120 (4)
O3W—H3WA···O4iii0.851 (19)2.27 (3)3.080 (4)160 (5)
O3W—H3WB···O4v0.846 (19)1.96 (2)2.787 (4)164 (4)
Symmetry codes: (ii) x+1, y+1, z; (iii) x+1, y, z; (iv) x+1, y1, z; (v) x+1, y, z+1.
 

Subscribe to Acta Crystallographica Section C: Structural Chemistry

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds