Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109001590/fa3171sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270109001590/fa3171Isup2.hkl |
CCDC reference: 724195
For related literature, see: Alberti & Constanino (1996); Allen (2002); Cabeza et al. (2002); Clearfield (1998); Groeneman & Atwood (1999); Kong et al. (2006); Prochniak et al. (2008); Sharma & Clearfield (2000); Videnova-Adrabinska (2007); Xiong et al. (2001).
[Sr(C7H5O5S)2(H2O)3]nwas synthesized by dissolving potassium 1-carboxybenzenesulfonate (2.08 mmol) and strontium chloride hexahydrate (1.04 mmol) in distilled water (4 ml). The mixture was sealed in a glass vial and heated at 353 K for 4 h, and then it was cooled slowly, at a rate of 1.25 K h-1, to room temperature. Needle-like crystals suitable for X-ray measurements were retrieved after the cooling process.
The H atoms of the carboxylic acid groups and the water molecules were located in difference Fourier maps and placed at calculated sites. One restraint was used for the O1W—H1W distance. The H atoms of the aromatic ring were placed at calculated positions. All H atoms were refined with isotropic displacement parameters correlated with the anisotropic displacement parameters of the atoms to which they are bonded.
Data collection: CrysAlisPro (Oxford Diffraction, 2007); cell refinement: CrysAlisPro (Oxford Diffraction, 2007); data reduction: CrysAlisPro (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Diamond (Brandenburg, 2007); software used to prepare material for publication: PLATON (Spek 2003) and publCIF (Westrip, 2009).
[Sr(C7H5O5S)2(H2O)3] | F(000) = 1096 |
Mr = 544.01 | Dx = 1.889 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 22.5926 (4) Å | Cell parameters from 6769 reflections |
b = 11.7646 (2) Å | θ = 2.5–32.7° |
c = 7.2025 (11) Å | µ = 3.11 mm−1 |
β = 92.221 (2)° | T = 183 K |
V = 1912.9 (3) Å3 | Needle, colourless |
Z = 4 | 0.22 × 0.07 × 0.05 mm |
Oxford Diffraction MODEL? diffractometer | 5831 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 4046 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 10.4498 pixels mm-1 | θmax = 30.5°, θmin = 2.5° |
ϕ ω scans | h = −32→18 |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2008) | k = −16→16 |
Tmin = 0.548, Tmax = 0.860 | l = −10→10 |
17871 measured reflections |
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.050 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.89 | w = 1/[σ2(Fo2) + (0.0171P)2] where P = (Fo2 + 2Fc2)/3 |
5831 reflections | (Δ/σ)max = 0.004 |
295 parameters | Δρmax = 0.47 e Å−3 |
1 restraint | Δρmin = −0.51 e Å−3 |
[Sr(C7H5O5S)2(H2O)3] | V = 1912.9 (3) Å3 |
Mr = 544.01 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.5926 (4) Å | µ = 3.11 mm−1 |
b = 11.7646 (2) Å | T = 183 K |
c = 7.2025 (11) Å | 0.22 × 0.07 × 0.05 mm |
β = 92.221 (2)° |
Oxford Diffraction MODEL? diffractometer | 5831 independent reflections |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2008) | 4046 reflections with I > 2σ(I) |
Tmin = 0.548, Tmax = 0.860 | Rint = 0.041 |
17871 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 1 restraint |
wR(F2) = 0.050 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.89 | Δρmax = 0.47 e Å−3 |
5831 reflections | Δρmin = −0.51 e Å−3 |
295 parameters |
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 | ||
Sr1 | 0.723829 (8) | 0.948791 (16) | 0.80944 (2) | 0.01165 (5) | |
S4 | 0.67395 (2) | 0.87163 (4) | 1.30590 (6) | 0.01227 (10) | |
S4A | 0.81631 (2) | 1.09580 (4) | 0.45855 (6) | 0.01248 (10) | |
O41 | 0.70134 (6) | 0.92676 (12) | 1.15204 (17) | 0.0227 (4) | |
O42 | 0.68274 (6) | 0.93371 (12) | 1.47793 (17) | 0.0182 (3) | |
O43 | 0.68950 (6) | 0.75254 (12) | 1.32334 (19) | 0.0233 (3) | |
O41A | 0.78859 (6) | 1.08528 (11) | 0.63596 (17) | 0.0176 (3) | |
O42A | 0.78397 (6) | 1.17056 (11) | 0.32957 (17) | 0.0173 (3) | |
O43A | 0.82926 (6) | 0.98542 (11) | 0.37769 (17) | 0.0165 (3) | |
O11 | 0.38265 (6) | 0.97413 (12) | 1.18710 (19) | 0.0237 (3) | |
O12 | 0.38918 (6) | 0.81141 (14) | 1.0293 (2) | 0.0306 (4) | |
H12 | 0.3537 (11) | 0.820 (2) | 1.021 (3) | 0.046* | |
O11A | 1.06509 (6) | 1.40545 (12) | 0.61322 (19) | 0.0234 (3) | |
O12A | 1.09079 (6) | 1.23625 (14) | 0.7312 (2) | 0.0291 (4) | |
H12A | 1.1216 (10) | 1.268 (2) | 0.760 (3) | 0.044* | |
O1W | 0.80548 (6) | 0.82010 (13) | 0.6327 (2) | 0.0176 (3) | |
H1W | 0.7935 (9) | 0.7666 (15) | 0.587 (3) | 0.026* | |
H2W | 0.8137 (9) | 0.8623 (19) | 0.539 (3) | 0.026* | |
O2W | 0.72556 (6) | 1.14974 (13) | 0.98569 (19) | 0.0175 (3) | |
H3W | 0.7400 (9) | 1.2060 (19) | 0.935 (3) | 0.026* | |
H4W | 0.7403 (9) | 1.1419 (19) | 1.085 (3) | 0.026* | |
O3W | 0.81809 (6) | 0.92223 (13) | 1.0093 (2) | 0.0237 (4) | |
H5W | 0.8518 (10) | 0.925 (2) | 0.979 (3) | 0.036* | |
H6W | 0.8202 (10) | 0.946 (2) | 1.116 (3) | 0.036* | |
C1 | 0.47671 (8) | 0.88758 (17) | 1.1674 (2) | 0.0148 (4) | |
C2 | 0.50502 (9) | 0.97620 (18) | 1.2594 (3) | 0.0195 (5) | |
H2 | 0.4829 | 1.0411 | 1.2933 | 0.023* | |
C3 | 0.56489 (8) | 0.97197 (17) | 1.3030 (3) | 0.0192 (5) | |
H3 | 0.5841 | 1.0334 | 1.3660 | 0.023* | |
C4 | 0.59664 (8) | 0.87611 (16) | 1.2530 (2) | 0.0123 (4) | |
C5 | 0.56905 (8) | 0.78731 (18) | 1.1595 (3) | 0.0178 (4) | |
H5 | 0.5913 | 0.7226 | 1.1252 | 0.021* | |
C6 | 0.50903 (8) | 0.79276 (18) | 1.1159 (3) | 0.0189 (5) | |
H6 | 0.4899 | 0.7320 | 1.0509 | 0.023* | |
C11 | 0.41181 (9) | 0.89597 (18) | 1.1296 (3) | 0.0177 (4) | |
C1A | 0.99438 (8) | 1.25537 (17) | 0.6029 (2) | 0.0145 (4) | |
C2A | 0.94782 (9) | 1.32432 (17) | 0.5418 (3) | 0.0167 (4) | |
H2A | 0.9534 | 1.4041 | 0.5327 | 0.020* | |
C3A | 0.89310 (8) | 1.27683 (17) | 0.4941 (2) | 0.0151 (4) | |
H3A | 0.8610 | 1.3236 | 0.4519 | 0.018* | |
C4A | 0.88594 (8) | 1.16065 (17) | 0.5088 (2) | 0.0129 (4) | |
C5A | 0.93216 (8) | 1.09132 (17) | 0.5695 (3) | 0.0169 (4) | |
H5A | 0.9266 | 1.0114 | 0.5771 | 0.020* | |
C6A | 0.98619 (8) | 1.13871 (17) | 0.6187 (3) | 0.0181 (4) | |
H6A | 1.0178 | 1.0918 | 0.6634 | 0.022* | |
C11A | 1.05274 (8) | 1.30772 (18) | 0.6484 (3) | 0.0167 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr1 | 0.00993 (8) | 0.01402 (9) | 0.01094 (8) | −0.00072 (8) | −0.00040 (6) | 0.00088 (8) |
S4 | 0.0102 (2) | 0.0159 (3) | 0.0107 (2) | 0.0009 (2) | 0.00014 (18) | −0.00015 (19) |
S4A | 0.0125 (2) | 0.0130 (2) | 0.0120 (2) | −0.0017 (2) | 0.00036 (19) | −0.00058 (19) |
O41 | 0.0176 (7) | 0.0370 (10) | 0.0136 (7) | −0.0074 (7) | 0.0027 (6) | 0.0041 (6) |
O42 | 0.0157 (7) | 0.0268 (9) | 0.0116 (6) | 0.0026 (6) | −0.0037 (5) | −0.0043 (6) |
O43 | 0.0183 (8) | 0.0180 (8) | 0.0334 (8) | 0.0067 (6) | −0.0033 (6) | −0.0013 (7) |
O41A | 0.0199 (7) | 0.0202 (8) | 0.0130 (6) | −0.0069 (6) | 0.0050 (6) | −0.0019 (6) |
O42A | 0.0171 (7) | 0.0172 (8) | 0.0171 (7) | 0.0001 (6) | −0.0053 (6) | 0.0014 (6) |
O43A | 0.0184 (7) | 0.0145 (8) | 0.0165 (7) | 0.0004 (6) | 0.0000 (6) | −0.0045 (6) |
O11 | 0.0138 (7) | 0.0290 (9) | 0.0281 (8) | 0.0055 (7) | −0.0013 (6) | −0.0074 (7) |
O12 | 0.0125 (7) | 0.0355 (11) | 0.0433 (10) | 0.0016 (7) | −0.0068 (7) | −0.0168 (8) |
O11A | 0.0184 (7) | 0.0173 (8) | 0.0343 (9) | −0.0056 (6) | 0.0005 (7) | −0.0006 (7) |
O12A | 0.0157 (8) | 0.0272 (10) | 0.0434 (10) | −0.0064 (7) | −0.0109 (7) | 0.0082 (8) |
O1W | 0.0188 (8) | 0.0162 (9) | 0.0178 (7) | −0.0008 (6) | −0.0016 (6) | −0.0007 (6) |
O2W | 0.0170 (7) | 0.0206 (9) | 0.0146 (7) | −0.0051 (6) | −0.0036 (6) | 0.0024 (6) |
O3W | 0.0147 (7) | 0.0397 (11) | 0.0166 (7) | 0.0059 (7) | −0.0022 (6) | −0.0084 (7) |
C1 | 0.0118 (9) | 0.0183 (12) | 0.0142 (9) | 0.0008 (8) | −0.0007 (8) | 0.0011 (8) |
C2 | 0.0153 (10) | 0.0198 (12) | 0.0235 (11) | 0.0056 (9) | 0.0004 (8) | −0.0036 (9) |
C3 | 0.0163 (10) | 0.0193 (12) | 0.0217 (10) | −0.0003 (9) | −0.0029 (8) | −0.0062 (9) |
C4 | 0.0105 (9) | 0.0168 (11) | 0.0096 (9) | −0.0013 (8) | 0.0011 (7) | 0.0022 (8) |
C5 | 0.0165 (10) | 0.0194 (12) | 0.0175 (10) | 0.0034 (9) | 0.0017 (8) | −0.0044 (9) |
C6 | 0.0152 (10) | 0.0208 (12) | 0.0203 (10) | −0.0026 (9) | −0.0021 (9) | −0.0043 (9) |
C11 | 0.0162 (10) | 0.0209 (12) | 0.0159 (10) | −0.0003 (9) | −0.0006 (8) | 0.0015 (9) |
C1A | 0.0120 (9) | 0.0194 (11) | 0.0122 (9) | −0.0026 (9) | 0.0006 (8) | −0.0018 (8) |
C2A | 0.0193 (10) | 0.0129 (11) | 0.0179 (10) | −0.0032 (9) | 0.0018 (9) | 0.0010 (8) |
C3A | 0.0114 (9) | 0.0162 (11) | 0.0177 (10) | 0.0015 (8) | 0.0001 (8) | 0.0030 (8) |
C4A | 0.0144 (10) | 0.0161 (11) | 0.0083 (9) | −0.0041 (8) | 0.0033 (8) | −0.0004 (8) |
C5A | 0.0190 (10) | 0.0108 (10) | 0.0206 (10) | −0.0025 (9) | −0.0013 (9) | 0.0027 (8) |
C6A | 0.0153 (10) | 0.0178 (12) | 0.0209 (10) | 0.0024 (9) | −0.0023 (8) | 0.0027 (9) |
C11A | 0.0151 (10) | 0.0204 (12) | 0.0146 (10) | 0.0010 (9) | 0.0024 (8) | −0.0040 (8) |
Sr1—O43i | 2.4956 (14) | O2W—H3W | 0.83 (2) |
Sr1—O41A | 2.5342 (12) | O2W—H4W | 0.78 (2) |
Sr1—O42ii | 2.5343 (13) | O3W—H5W | 0.80 (2) |
Sr1—O3W | 2.5430 (15) | O3W—H6W | 0.82 (2) |
Sr1—O41 | 2.5517 (13) | C1—C2 | 1.379 (3) |
Sr1—O11iii | 2.5719 (13) | C1—C6 | 1.392 (3) |
Sr1—O2W | 2.6829 (15) | C1—C11 | 1.484 (3) |
Sr1—O1W | 2.7382 (14) | C2—C3 | 1.377 (3) |
S4—O41 | 1.4439 (13) | C2—H2 | 0.9500 |
S4—O42 | 1.4454 (13) | C3—C4 | 1.391 (3) |
S4—O43 | 1.4486 (15) | C3—H3 | 0.9500 |
S4—C4 | 1.7739 (18) | C4—C5 | 1.379 (3) |
S4A—O41A | 1.4499 (13) | C5—C6 | 1.382 (3) |
S4A—O42A | 1.4553 (13) | C5—H5 | 0.9500 |
S4A—O43A | 1.4575 (13) | C6—H6 | 0.9500 |
S4A—C4A | 1.7731 (19) | C1A—C2A | 1.386 (3) |
O42—Sr1iv | 2.5343 (13) | C1A—C6A | 1.390 (3) |
O43—Sr1v | 2.4956 (14) | C1A—C11A | 1.481 (3) |
O11—C11 | 1.213 (2) | C2A—C3A | 1.388 (3) |
O11—Sr1iii | 2.5719 (13) | C2A—H2A | 0.9500 |
O12—C11 | 1.320 (2) | C3A—C4A | 1.381 (3) |
O12—H12 | 0.81 (2) | C3A—H3A | 0.9500 |
O11A—C11A | 1.212 (2) | C4A—C5A | 1.382 (3) |
O12A—C11A | 1.327 (2) | C5A—C6A | 1.376 (3) |
O12A—H12A | 0.81 (2) | C5A—H5A | 0.9500 |
O1W—H1W | 0.756 (15) | C6A—H6A | 0.9500 |
O1W—H2W | 0.87 (2) | ||
O43i—Sr1—O41A | 143.85 (4) | H1W—O1W—H2W | 103 (2) |
O43i—Sr1—O42ii | 82.43 (4) | Sr1—O2W—H3W | 119.4 (15) |
O41A—Sr1—O42ii | 77.13 (4) | Sr1—O2W—H4W | 109.1 (17) |
O43i—Sr1—O3W | 96.63 (5) | H3W—O2W—H4W | 110 (2) |
O41A—Sr1—O3W | 82.53 (5) | Sr1—O3W—H5W | 128.5 (16) |
O42ii—Sr1—O3W | 142.45 (4) | Sr1—O3W—H6W | 120.6 (16) |
O43i—Sr1—O41 | 77.93 (4) | H5W—O3W—H6W | 103 (2) |
O41A—Sr1—O41 | 132.96 (4) | C2—C1—C6 | 119.71 (18) |
O42ii—Sr1—O41 | 145.55 (4) | C2—C1—C11 | 118.32 (18) |
O3W—Sr1—O41 | 68.53 (4) | C6—C1—C11 | 121.95 (18) |
O43i—Sr1—O11iii | 92.41 (5) | C3—C2—C1 | 121.01 (19) |
O41A—Sr1—O11iii | 109.84 (4) | C3—C2—H2 | 119.5 |
O42ii—Sr1—O11iii | 74.05 (4) | C1—C2—H2 | 119.5 |
O3W—Sr1—O11iii | 143.22 (5) | C2—C3—C4 | 118.81 (19) |
O41—Sr1—O11iii | 78.76 (4) | C2—C3—H3 | 120.6 |
O43i—Sr1—O2W | 144.71 (4) | C4—C3—H3 | 120.6 |
O41A—Sr1—O2W | 71.15 (4) | C5—C4—C3 | 120.84 (18) |
O42ii—Sr1—O2W | 120.37 (4) | C5—C4—S4 | 120.34 (15) |
O3W—Sr1—O2W | 81.02 (5) | C3—C4—S4 | 118.80 (15) |
O41—Sr1—O2W | 68.39 (4) | C4—C5—C6 | 119.81 (19) |
O11iii—Sr1—O2W | 71.41 (4) | C4—C5—H5 | 120.1 |
O43i—Sr1—O1W | 73.14 (4) | C6—C5—H5 | 120.1 |
O41A—Sr1—O1W | 73.08 (4) | C5—C6—C1 | 119.81 (19) |
O42ii—Sr1—O1W | 75.65 (4) | C5—C6—H6 | 120.1 |
O3W—Sr1—O1W | 68.32 (4) | C1—C6—H6 | 120.1 |
O41—Sr1—O1W | 123.81 (5) | O11—C11—O12 | 123.62 (18) |
O11iii—Sr1—O1W | 147.86 (4) | O11—C11—C1 | 122.23 (19) |
O2W—Sr1—O1W | 135.19 (4) | O12—C11—C1 | 114.15 (18) |
O41—S4—O42 | 112.47 (8) | C2A—C1A—C6A | 120.13 (18) |
O41—S4—O43 | 113.04 (8) | C2A—C1A—C11A | 119.02 (18) |
O42—S4—O43 | 112.92 (8) | C6A—C1A—C11A | 120.85 (18) |
O41—S4—C4 | 105.64 (8) | C1A—C2A—C3A | 120.05 (19) |
O42—S4—C4 | 105.69 (8) | C1A—C2A—H2A | 120.0 |
O43—S4—C4 | 106.31 (9) | C3A—C2A—H2A | 120.0 |
O41A—S4A—O42A | 113.00 (8) | C4A—C3A—C2A | 119.03 (18) |
O41A—S4A—O43A | 112.11 (8) | C4A—C3A—H3A | 120.5 |
O42A—S4A—O43A | 112.77 (8) | C2A—C3A—H3A | 120.5 |
O41A—S4A—C4A | 105.48 (8) | C3A—C4A—C5A | 121.27 (18) |
O42A—S4A—C4A | 106.85 (9) | C3A—C4A—S4A | 121.05 (15) |
O43A—S4A—C4A | 105.95 (8) | C5A—C4A—S4A | 117.64 (15) |
S4—O41—Sr1 | 153.52 (9) | C6A—C5A—C4A | 119.61 (19) |
S4—O42—Sr1iv | 151.19 (8) | C6A—C5A—H5A | 120.2 |
S4—O43—Sr1v | 171.54 (9) | C4A—C5A—H5A | 120.2 |
S4A—O41A—Sr1 | 139.99 (8) | C5A—C6A—C1A | 119.90 (18) |
C11—O11—Sr1iii | 142.27 (13) | C5A—C6A—H6A | 120.0 |
C11—O12—H12 | 107.8 (18) | C1A—C6A—H6A | 120.0 |
C11A—O12A—H12A | 110.7 (18) | O11A—C11A—O12A | 122.99 (19) |
Sr1—O1W—H1W | 115.3 (17) | O11A—C11A—C1A | 123.94 (19) |
Sr1—O1W—H2W | 102.5 (14) | O12A—C11A—C1A | 113.07 (18) |
O42—S4—O41—Sr1 | −173.89 (17) | O43—S4—C4—C3 | 153.37 (14) |
O43—S4—O41—Sr1 | 56.8 (2) | C3—C4—C5—C6 | −0.5 (3) |
C4—S4—O41—Sr1 | −59.1 (2) | S4—C4—C5—C6 | −178.72 (14) |
O43i—Sr1—O41—S4 | −18.63 (19) | C4—C5—C6—C1 | −0.3 (3) |
O41A—Sr1—O41—S4 | −176.95 (17) | C2—C1—C6—C5 | 0.9 (3) |
O42ii—Sr1—O41—S4 | 38.0 (2) | C11—C1—C6—C5 | −177.89 (18) |
O3W—Sr1—O41—S4 | −120.8 (2) | Sr1iii—O11—C11—O12 | 0.3 (4) |
O11iii—Sr1—O41—S4 | 76.32 (19) | Sr1iii—O11—C11—C1 | −179.54 (13) |
O2W—Sr1—O41—S4 | 150.6 (2) | C2—C1—C11—O11 | −4.8 (3) |
O1W—Sr1—O41—S4 | −78.6 (2) | C6—C1—C11—O11 | 173.98 (19) |
O41—S4—O42—Sr1iv | −117.33 (16) | C2—C1—C11—O12 | 175.32 (17) |
O43—S4—O42—Sr1iv | 12.06 (19) | C6—C1—C11—O12 | −5.9 (3) |
C4—S4—O42—Sr1iv | 127.88 (16) | C6A—C1A—C2A—C3A | −0.8 (3) |
O42A—S4A—O41A—Sr1 | 101.03 (13) | C11A—C1A—C2A—C3A | 178.47 (16) |
O43A—S4A—O41A—Sr1 | −27.75 (15) | C1A—C2A—C3A—C4A | 0.1 (3) |
C4A—S4A—O41A—Sr1 | −142.60 (12) | C2A—C3A—C4A—C5A | −0.2 (3) |
O43i—Sr1—O41A—S4A | 19.92 (17) | C2A—C3A—C4A—S4A | 177.50 (13) |
O42ii—Sr1—O41A—S4A | −37.27 (12) | O41A—S4A—C4A—C3A | −94.88 (15) |
O3W—Sr1—O41A—S4A | 110.95 (13) | O42A—S4A—C4A—C3A | 25.62 (17) |
O41—Sr1—O41A—S4A | 162.16 (11) | O43A—S4A—C4A—C3A | 146.09 (14) |
O11iii—Sr1—O41A—S4A | −104.81 (12) | O41A—S4A—C4A—C5A | 82.86 (16) |
O2W—Sr1—O41A—S4A | −166.03 (14) | O42A—S4A—C4A—C5A | −156.64 (14) |
O1W—Sr1—O41A—S4A | 41.41 (12) | O43A—S4A—C4A—C5A | −36.17 (16) |
C6—C1—C2—C3 | −0.6 (3) | C3A—C4A—C5A—C6A | 0.9 (3) |
C11—C1—C2—C3 | 178.21 (18) | S4A—C4A—C5A—C6A | −176.86 (14) |
C1—C2—C3—C4 | −0.2 (3) | C4A—C5A—C6A—C1A | −1.6 (3) |
C2—C3—C4—C5 | 0.8 (3) | C2A—C1A—C6A—C5A | 1.5 (3) |
C2—C3—C4—S4 | 179.02 (15) | C11A—C1A—C6A—C5A | −177.74 (17) |
O41—S4—C4—C5 | 91.97 (16) | C2A—C1A—C11A—O11A | −10.1 (3) |
O42—S4—C4—C5 | −148.63 (15) | C6A—C1A—C11A—O11A | 169.23 (18) |
O43—S4—C4—C5 | −28.39 (17) | C2A—C1A—C11A—O12A | 170.43 (17) |
O41—S4—C4—C3 | −86.28 (16) | C6A—C1A—C11A—O12A | −10.3 (3) |
O42—S4—C4—C3 | 33.12 (17) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, y, z−1; (iii) −x+1, −y+2, −z+2; (iv) x, y, z+1; (v) x, −y+3/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O12A—H12A···O1Wvi | 0.81 (2) | 1.89 (2) | 2.692 (2) | 168 (3) |
O12—H12···O2Wiii | 0.81 (2) | 1.82 (2) | 2.630 (2) | 175 (3) |
O1W—H1W···O3Wi | 0.76 (2) | 2.36 (2) | 3.003 (2) | 143 (2) |
O1W—H2W···O43A | 0.87 (2) | 1.90 (2) | 2.743 (2) | 165 (2) |
O2W—H3W···O42Avii | 0.83 (2) | 1.93 (2) | 2.7550 (19) | 172 (2) |
O2W—H4W···O42Aiv | 0.78 (2) | 2.01 (2) | 2.7717 (19) | 163 (2) |
O3W—H5W···O11Aviii | 0.80 (2) | 2.03 (2) | 2.8220 (19) | 170 (2) |
O3W—H6W···O43Aiv | 0.82 (2) | 1.94 (2) | 2.7579 (19) | 174 (2) |
C5A—H5A···O11Aviii | 0.95 | 2.56 | 3.162 (3) | 122 |
C2A—H2A···O11Aix | 0.95 | 2.50 | 3.378 (3) | 153 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) −x+1, −y+2, −z+2; (iv) x, y, z+1; (vi) −x+2, y+1/2, −z+3/2; (vii) x, −y+5/2, z+1/2; (viii) −x+2, y−1/2, −z+3/2; (ix) −x+2, −y+3, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Sr(C7H5O5S)2(H2O)3] |
Mr | 544.01 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 183 |
a, b, c (Å) | 22.5926 (4), 11.7646 (2), 7.2025 (11) |
β (°) | 92.221 (2) |
V (Å3) | 1912.9 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.11 |
Crystal size (mm) | 0.22 × 0.07 × 0.05 |
Data collection | |
Diffractometer | Oxford Diffraction MODEL? diffractometer |
Absorption correction | Multi-scan (CrysAlis RED; Oxford Diffraction, 2008) |
Tmin, Tmax | 0.548, 0.860 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17871, 5831, 4046 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.714 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.050, 0.89 |
No. of reflections | 5831 |
No. of parameters | 295 |
No. of restraints | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.47, −0.51 |
Computer programs: CrysAlisPro (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), Diamond (Brandenburg, 2007), PLATON (Spek 2003) and publCIF (Westrip, 2009).
Sr1—O43i | 2.4956 (14) | S4—O41 | 1.4439 (13) |
Sr1—O41A | 2.5342 (12) | S4—O42 | 1.4454 (13) |
Sr1—O42ii | 2.5343 (13) | S4—O43 | 1.4486 (15) |
Sr1—O3W | 2.5430 (15) | S4—C4 | 1.7739 (18) |
Sr1—O41 | 2.5517 (13) | S4A—O41A | 1.4499 (13) |
Sr1—O11iii | 2.5719 (13) | S4A—O42A | 1.4553 (13) |
Sr1—O2W | 2.6829 (15) | S4A—O43A | 1.4575 (13) |
Sr1—O1W | 2.7382 (14) | S4A—C4A | 1.7731 (19) |
O43i—Sr1—O41A | 143.85 (4) | O42ii—Sr1—O41 | 145.55 (4) |
O43i—Sr1—O42ii | 82.43 (4) | O43i—Sr1—O11iii | 92.41 (5) |
O41A—Sr1—O42ii | 77.13 (4) | O41A—Sr1—O11iii | 109.84 (4) |
O43i—Sr1—O41 | 77.93 (4) | O42ii—Sr1—O11iii | 74.05 (4) |
O41A—Sr1—O41 | 132.96 (4) | O41—Sr1—O11iii | 78.76 (4) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, y, z−1; (iii) −x+1, −y+2, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O12A—H12A···O1Wiv | 0.81 (2) | 1.89 (2) | 2.692 (2) | 168 (3) |
O12—H12···O2Wiii | 0.81 (2) | 1.82 (2) | 2.630 (2) | 175 (3) |
O1W—H1W···O3Wi | 0.756 (15) | 2.362 (18) | 3.003 (2) | 143 (2) |
O1W—H2W···O43A | 0.87 (2) | 1.90 (2) | 2.743 (2) | 165 (2) |
O2W—H3W···O42Av | 0.83 (2) | 1.93 (2) | 2.7550 (19) | 172 (2) |
O2W—H4W···O42Avi | 0.78 (2) | 2.01 (2) | 2.7717 (19) | 163 (2) |
O3W—H5W···O11Avii | 0.80 (2) | 2.03 (2) | 2.8220 (19) | 170 (2) |
O3W—H6W···O43Avi | 0.82 (2) | 1.94 (2) | 2.7579 (19) | 174 (2) |
C5A—H5A···O11Avii | 0.95 | 2.56 | 3.162 (3) | 122 |
C2A—H2A···O11Aviii | 0.95 | 2.50 | 3.378 (3) | 153 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) −x+1, −y+2, −z+2; (iv) −x+2, y+1/2, −z+3/2; (v) x, −y+5/2, z+1/2; (vi) x, y, z+1; (vii) −x+2, y−1/2, −z+3/2; (viii) −x+2, −y+3, −z+1. |
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Hybrid inorganic-organic layered compounds are of interest for their potential applications in chemical separation, gas sorption, sensing and catalysis (Clearfield, 1998; Alberti & Constanino, 1996; Kong et al., 2006; Sharma & Clearfield, 2000; Cabeza et al., 2002). The aromatic dicarboxylic acids with endo-positioned functional groups, and especially terephthalic acid, are broadly exploited as bridging ligands and organic linkers in order to form coordination polymers. Moreover, by controlling the geometry of the entities between the metal ions one can regulate the organization within layers and obtain different structures. In this context, the monosubstituted sulfonic analogues of terephthalic acid merit special attention. The ligand 4-sulfobenzoic acid has the potential to bind metal ions with variable coordination modes (from η1µ1 to η10µ9), which can lead to high-dimensional networks and structurally diverse compounds (Videnova-Adrabinska, 2007; Prochniak et al., 2008). The lack of symmetry in the organic linker is a useful attribute of the ligand since this may lead to structural variation in the interlayer region. However, most of the 28 4-sulfobenzoate compounds retrieved from the Cambridge Structural Database (Version 5.29; Allen, 2002), contain chelating auxiliary ligands, obviating higher-dimensional aggregation of the ions. Only two compounds, catena-[(µ4-benzene-1,4-disulfonato)-bis(µ4-4-sulfobenzoato)-bis(µ2-aqua)-aqua-dieuropium(III)] and catena-[(µ4-benzene-1,4-disulfonato)-bis(µ4-4-sulfobenzoato)-bis(µ2-aqua)-aqua-digadolinium(III)], were found to have a layered structure, but they incorporate an additional 1,4-disulfonate ligand (Xiong et al., 2001). We report here the crystal structure of [Sr(4-sb)2(H2O)3]n, (I), where 4-sb is 4-carboxybenzenesulfonate.
The asymmetric unit consists of one Sr ion, two independent monodeprotonated 4-carboxybenzenesulfonate anions and three water molecules. The coordination environment of the metal center consists of four sulfonate and one carboxylic acid groups, from five different acid monoanions (one of which is symmetry unique), and three water molecules. The SrO8 coordination polyhedron is strongly deformed and intermediate between an antiprism (sap) with a face symbol [38.42] (see https://rcsr.anu.edu.au) and a bisdisphenoid (bds; [312]) (Fig. 1). The coordination bonds range between 2.496 (1) and 2.738 (1) Å (Table 1). One of the acid monoanions mediates the arrangement of the metal ions into a thick monolayer, while the second independent anion serves to cross-link the monolayers. The sulfonate site of the first monoanion bridges, in µ3 fashion, the strontium ions along the c axis in order to form coordination ribbons. The Sr1—O41 and Sr1—O42ii bonds bridge the metal centers into a C(4) chain, and the third Sr—O43i bond interweaves two c-glide chains into a ribbon [symmetry codes: (i) x, -y + 3/2, z - 1/2; (ii) x, y, z - 1]. An R2,4(8) [should the numbers be sub/superscripts as with hydrogen-boonding motifs?] ring motif is generated along the ribbon (Videnova-Adrabinska, 2007). The aromatic rings are arrayed on both sides of the ribbons. The distal carboxylic acid groups serve to link neighboring inversion-related ribbons via the Sr—O11iii bond [symmetry code: (iii) -x + 1, -y + 2, -z + 2], in order to form an undulating monolayer with a hydrophobic interior and hydrophilic surfaces (Fig. 2). The two-dimensional network of the monolayer is girded with smaller ring motifs [R2,4(8)] along the ribbons and larger motifs [R2,4(18)] between the ribbons, where the aqua ligands and the benzene rings reside. (For a topological description of the motifs see Videnova-Adrabinska, 2007.) The aromatic rings of the µ4 ligands play the role of linkers between the ribbons and are arranged in the interior of the monolayer with offset face-to-face (OFF) interactions.
The second independent acid anion (atom labels ending with A) is bonded to strontium in a monodentate fashion (Sr—O41A) and arranged outward from both sides of the monolayer (Fig. 3). The aromatic portions of the A ligands protrude into the interlayer regions and are organized into stacks along the c axis. The rings along the stack are c-glide-related, with a distance of 3.735 (1) Å between their centers of gravity. The aqua ligands serve to complete the coordination sphere of the strontium ion and to stabilize the monolayer structure. A carboxylic acid–water hydrogen bond [O12—H12···O2Wiii; symmetry codes as in Table 2] stabilizes the interior of the monolayer. Four more hydrogen-bonds [O1W—H2W···O43A, O2W—H3W···O42Av, O2W—H4W···O42Avi and O3W—H6W···O43Avi; O···O = 2.743 (2)–2.7717 (19) Å], established between the water molecules and the sulfonate O atoms of the A ligands, contribute to the layer folding. The distal carboxylic acid groups of the A ligands are used to connect the monolayers via hydrogen-bond interactions (Fig. 4). Two relatively strong hydrogen-bonds, O12A—H12A···O1Wiv and O3W—H5W···O11Avii, formed between the carboxylic acid groups of one layer and the aqua ligands of the next layer, cross-link the monolayers. There are no aromatic interactions between the stacks of adjacent monolayers. Interlayer interactions (C2A—H2A···O11Aviii and C5A—H5A···O11Avii; Table 2) are established between the aromatic rings and the carbonyl O atoms. The crystal packing involves segregation of hydrophilic and hydrophobic regions alternating along the crystallographic a axis. The hydrophilic regions contain the metal ions and the functional groups of the ligands. All coordination and hydrogen bonds occur here. However, the hydrophobic regions on opposite sides of the hydrophilic region are different: the benzene rings (the organic linkers) on one side are organized with intralayer OFF interactions and on the other side with interlayer FF interactions.
Finally, it seems useful to compare this polymeric structure with that of [Sr(terephthalate)(H2O)4] (Groeneman & Atwood, 1999). Only one of the end-positioned functional groups of the terephthalate dianion serves as a ligand and bridges the strontium ions with a µ2-mode in order to form coordination strands. The second carboxylate site bears a negative charge and the ribbons are held together by numerous water–carboxylate hydrogen bonds and π–π interactions. Hence, this compound exhibits a one-dimensional coordination network instead of a monolayer structure.