The title coordination polymer, [Zn(C7H4O6S)(H2O)4]n, comprises octahedral Zn atoms bonded to two carboxylate O atoms of the acid ligands and four water molecules. The zinc(II) ions are bridged by carboxylate moieties, creating a one-dimensional chain structure. The Zn—O bond distances lie in the range 2.074 (3)–2.118 (3) Å. The water molecules are involved in hydrogen bonds.
Supporting information
CCDC reference: 251603
Key indicators
- Single-crystal X-ray study
- T = 213 K
- Mean (C-C) = 0.005 Å
- R factor = 0.030
- wR factor = 0.086
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 28.29
From the CIF: _reflns_number_total 2444
Count of symmetry unique reflns 1491
Completeness (_total/calc) 163.92%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 953
Fraction of Friedel pairs measured 0.639
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
0 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2001).
catena-Poly[[tetraaquazinc(II)]-µ-5-sulfosalicylato-
κ2O:
O']
top
Crystal data top
[Zn(C7H4O6S)(H2O)4] | F(000) = 720 |
Mr = 353.60 | Dx = 1.966 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 2444 reflections |
a = 10.454 (6) Å | θ = 2–28° |
b = 16.192 (6) Å | µ = 2.28 mm−1 |
c = 7.0777 (14) Å | T = 213 K |
β = 94.47 (5)° | Platelett, colourless |
V = 1194.4 (9) Å3 | 0.40 × 0.30 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD diffractometer | 2444 independent reflections |
Radiation source: fine-focus sealed tube | 2424 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω scans | θmax = 28.3°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.445, Tmax = 0.634 | k = −21→18 |
3595 measured reflections | l = −9→9 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.064P)2 + 1.0831P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.086 | (Δ/σ)max = 0.039 |
S = 1.09 | Δρmax = 0.90 e Å−3 |
2444 reflections | Δρmin = −0.72 e Å−3 |
201 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
11 restraints | Extinction coefficient: 0.0101 (9) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 982 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.068 (11) |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.8993 (3) | 0.0641 (2) | 0.9178 (5) | 0.0189 (6) | |
C2 | 1.0251 (4) | 0.05435 (19) | 0.9989 (5) | 0.0199 (6) | |
H2 | 1.0753 | 0.1010 | 1.0320 | 0.025 (7)* | |
C3 | 1.0753 (3) | −0.0241 (2) | 1.0302 (5) | 0.0190 (6) | |
H3 | 1.1603 | −0.0309 | 1.0817 | 0.025 (7)* | |
C4 | 0.9988 (3) | −0.09300 (19) | 0.9848 (5) | 0.0159 (6) | |
C5 | 0.8732 (3) | −0.08435 (19) | 0.9106 (4) | 0.0160 (5) | |
H5 | 0.8222 | −0.1314 | 0.8837 | 0.025 (7)* | |
C6 | 0.8222 (3) | −0.00566 (18) | 0.8759 (5) | 0.0164 (5) | |
C7 | 0.6876 (3) | 0.0028 (2) | 0.7891 (4) | 0.0171 (6) | |
O1 | 0.6162 (3) | 0.21543 (15) | 0.5101 (4) | 0.0251 (5) | |
O2 | 0.3990 (2) | 0.13943 (16) | 0.7324 (3) | 0.0219 (5) | |
O3 | 0.3848 (2) | 0.14829 (15) | 0.2976 (4) | 0.0228 (5) | |
O4 | 0.4175 (3) | −0.00690 (15) | 0.5146 (4) | 0.0240 (5) | |
O5 | 0.6148 (2) | −0.05955 (14) | 0.7819 (4) | 0.0209 (5) | |
O6 | 0.6541 (2) | 0.07308 (14) | 0.7240 (4) | 0.0201 (5) | |
O7 | 0.8584 (2) | 0.14191 (15) | 0.8876 (4) | 0.0269 (5) | |
H7 | 0.7866 | 0.1413 | 0.8286 | 0.051 (17)* | |
O8 | 0.9648 (3) | −0.25191 (14) | 1.0153 (4) | 0.0200 (4) | |
O9 | 1.1449 (2) | −0.20373 (15) | 0.8518 (3) | 0.0225 (5) | |
O10 | 1.1489 (2) | −0.18956 (15) | 1.1916 (3) | 0.0203 (5) | |
S1 | 1.06835 (7) | −0.19135 (5) | 1.01339 (10) | 0.01541 (17) | |
Zn1 | 0.51628 (3) | 0.105750 (19) | 0.51007 (4) | 0.01690 (13) | |
H1A | 0.612 (6) | 0.241 (4) | 0.612 (9) | 0.042* | |
H1B | 0.617 (6) | 0.241 (4) | 0.418 (8) | 0.036* | |
H2A | 0.322 (2) | 0.155 (3) | 0.711 (6) | 0.027* | |
H2B | 0.434 (4) | 0.174 (3) | 0.811 (6) | 0.034* | |
H3A | 0.310 (2) | 0.160 (3) | 0.328 (6) | 0.023* | |
H3B | 0.413 (4) | 0.186 (3) | 0.235 (7) | 0.046* | |
H4A | 0.403 (6) | −0.036 (3) | 0.417 (4) | 0.042* | |
H4B | 0.450 (4) | −0.037 (2) | 0.602 (4) | 0.021* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0200 (13) | 0.0165 (14) | 0.0200 (14) | 0.0003 (11) | −0.0005 (11) | 0.0005 (12) |
C2 | 0.0205 (13) | 0.0172 (13) | 0.0216 (14) | −0.0021 (12) | −0.0015 (11) | 0.0000 (13) |
C3 | 0.0160 (13) | 0.0224 (16) | 0.0180 (14) | −0.0035 (12) | −0.0025 (11) | 0.0019 (13) |
C4 | 0.0175 (16) | 0.0150 (12) | 0.0152 (16) | 0.0003 (10) | 0.0008 (12) | 0.0001 (11) |
C5 | 0.0161 (12) | 0.0164 (13) | 0.0154 (14) | −0.0019 (10) | 0.0007 (10) | 0.0007 (11) |
C6 | 0.0150 (12) | 0.0162 (13) | 0.0179 (13) | −0.0002 (10) | 0.0007 (10) | 0.0015 (11) |
C7 | 0.0157 (12) | 0.0201 (14) | 0.0155 (14) | 0.0012 (10) | 0.0015 (10) | −0.0006 (11) |
O1 | 0.0390 (13) | 0.0155 (11) | 0.0204 (11) | −0.0052 (10) | −0.0007 (11) | 0.0010 (10) |
O2 | 0.0188 (10) | 0.0246 (12) | 0.0216 (11) | 0.0012 (8) | −0.0023 (9) | −0.0045 (9) |
O3 | 0.0205 (11) | 0.0229 (12) | 0.0251 (12) | 0.0056 (8) | 0.0014 (9) | 0.0079 (9) |
O4 | 0.0313 (13) | 0.0195 (11) | 0.0208 (12) | −0.0025 (9) | −0.0014 (10) | −0.0001 (9) |
O5 | 0.0170 (10) | 0.0203 (11) | 0.0249 (11) | −0.0023 (8) | −0.0002 (8) | 0.0042 (9) |
O6 | 0.0197 (10) | 0.0176 (11) | 0.0223 (11) | 0.0021 (8) | −0.0023 (9) | 0.0021 (9) |
O7 | 0.0257 (11) | 0.0145 (11) | 0.0390 (15) | 0.0003 (8) | −0.0076 (10) | 0.0032 (10) |
O8 | 0.0209 (9) | 0.0162 (11) | 0.0225 (11) | −0.0041 (8) | −0.0011 (8) | −0.0011 (9) |
O9 | 0.0213 (10) | 0.0254 (12) | 0.0210 (11) | −0.0005 (8) | 0.0030 (9) | −0.0041 (9) |
O10 | 0.0200 (10) | 0.0233 (12) | 0.0168 (10) | 0.0006 (8) | −0.0034 (8) | 0.0029 (9) |
S1 | 0.0145 (3) | 0.0156 (4) | 0.0158 (3) | −0.0001 (3) | −0.0009 (2) | 0.0007 (3) |
Zn1 | 0.01680 (17) | 0.01509 (18) | 0.01845 (18) | 0.00086 (16) | −0.00085 (11) | 0.00049 (13) |
Geometric parameters (Å, º) top
C1—O7 | 1.343 (4) | O2—Zn1 | 2.140 (3) |
C1—C2 | 1.402 (5) | O2—H2A | 0.85 (3) |
C1—C6 | 1.406 (4) | O2—H2B | 0.85 (5) |
C2—C3 | 1.386 (5) | O3—Zn1 | 2.074 (3) |
C2—H2 | 0.9400 | O3—H3A | 0.85 (3) |
C3—C4 | 1.395 (4) | O3—H3B | 0.82 (5) |
C3—H3 | 0.9400 | O4—Zn1 | 2.098 (3) |
C4—C5 | 1.383 (4) | O4—H4A | 0.84 (4) |
C4—S1 | 1.756 (3) | O4—H4B | 0.84 (3) |
C5—C6 | 1.396 (4) | O5—Zn1i | 2.118 (3) |
C5—H5 | 0.9400 | O6—Zn1 | 2.076 (3) |
C6—C7 | 1.497 (4) | O7—H7 | 0.8300 |
C7—O5 | 1.264 (4) | O8—S1 | 1.461 (2) |
C7—O6 | 1.267 (4) | O9—S1 | 1.460 (3) |
O1—Zn1 | 2.061 (3) | O10—S1 | 1.461 (2) |
O1—H1A | 0.84 (7) | Zn1—O5ii | 2.118 (3) |
O1—H1B | 0.77 (6) | | |
| | | |
O7—C1—C2 | 116.6 (3) | H3A—O3—H3B | 110 (3) |
O7—C1—C6 | 123.4 (3) | Zn1—O4—H4A | 122 (4) |
C2—C1—C6 | 120.0 (3) | Zn1—O4—H4B | 110 (3) |
C3—C2—C1 | 120.0 (3) | H4A—O4—H4B | 109 (3) |
C3—C2—H2 | 120.0 | C7—O5—Zn1i | 125.4 (2) |
C1—C2—H2 | 120.0 | C7—O6—Zn1 | 130.6 (2) |
C2—C3—C4 | 119.5 (3) | C1—O7—H7 | 109.5 |
C2—C3—H3 | 120.2 | O9—S1—O10 | 111.41 (14) |
C4—C3—H3 | 120.2 | O9—S1—O8 | 111.52 (15) |
C5—C4—C3 | 121.1 (3) | O10—S1—O8 | 112.47 (15) |
C5—C4—S1 | 120.5 (3) | O9—S1—C4 | 106.37 (16) |
C3—C4—S1 | 118.3 (2) | O10—S1—C4 | 106.67 (15) |
C4—C5—C6 | 119.8 (3) | O8—S1—C4 | 108.02 (15) |
C4—C5—H5 | 120.1 | O1—Zn1—O3 | 91.22 (11) |
C6—C5—H5 | 120.1 | O1—Zn1—O6 | 84.06 (11) |
C5—C6—C1 | 119.4 (3) | O3—Zn1—O6 | 175.22 (10) |
C5—C6—C7 | 119.3 (3) | O1—Zn1—O4 | 178.75 (12) |
C1—C6—C7 | 121.2 (3) | O3—Zn1—O4 | 90.03 (10) |
O5—C7—O6 | 123.7 (3) | O6—Zn1—O4 | 94.69 (10) |
O5—C7—C6 | 119.2 (3) | O1—Zn1—O5ii | 91.59 (11) |
O6—C7—C6 | 117.2 (3) | O3—Zn1—O5ii | 84.19 (10) |
Zn1—O1—H1A | 111 (4) | O6—Zn1—O5ii | 96.61 (9) |
Zn1—O1—H1B | 120 (4) | O4—Zn1—O5ii | 88.51 (10) |
H1A—O1—H1B | 119 (5) | O1—Zn1—O2 | 95.74 (11) |
Zn1—O2—H2A | 122 (3) | O3—Zn1—O2 | 93.61 (10) |
Zn1—O2—H2B | 114 (3) | O6—Zn1—O2 | 86.19 (10) |
H2A—O2—H2B | 106 (3) | O4—Zn1—O2 | 84.21 (10) |
Zn1—O3—H3A | 118 (3) | O5ii—Zn1—O2 | 172.39 (9) |
Zn1—O3—H3B | 113 (4) | | |
| | | |
O7—C1—C2—C3 | −178.5 (3) | C1—C6—C7—O6 | 12.4 (5) |
C6—C1—C2—C3 | 2.8 (5) | O6—C7—O5—Zn1i | −101.6 (3) |
C1—C2—C3—C4 | −1.6 (6) | C6—C7—O5—Zn1i | 79.5 (3) |
C2—C3—C4—C5 | −0.6 (5) | O5—C7—O6—Zn1 | −25.9 (5) |
C2—C3—C4—S1 | 176.3 (3) | C6—C7—O6—Zn1 | 153.1 (2) |
C3—C4—C5—C6 | 1.5 (5) | C5—C4—S1—O9 | 99.4 (3) |
S1—C4—C5—C6 | −175.3 (3) | C3—C4—S1—O9 | −77.5 (3) |
C4—C5—C6—C1 | −0.3 (5) | C5—C4—S1—O10 | −141.5 (3) |
C4—C5—C6—C7 | 177.8 (3) | C3—C4—S1—O10 | 41.5 (3) |
O7—C1—C6—C5 | 179.5 (3) | C5—C4—S1—O8 | −20.4 (3) |
C2—C1—C6—C5 | −1.8 (5) | C3—C4—S1—O8 | 162.6 (3) |
O7—C1—C6—C7 | 1.4 (5) | C7—O6—Zn1—O1 | −161.4 (3) |
C2—C1—C6—C7 | −179.9 (3) | C7—O6—Zn1—O4 | 18.6 (3) |
C5—C6—C7—O5 | 13.3 (4) | C7—O6—Zn1—O5ii | −70.5 (3) |
C1—C6—C7—O5 | −168.6 (3) | C7—O6—Zn1—O2 | 102.4 (3) |
C5—C6—C7—O6 | −165.7 (3) | | |
Symmetry codes: (i) x, −y, z+1/2; (ii) x, −y, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7···O6 | 0.83 | 1.88 | 2.600 (4) | 145 |
O4—H4B···O5 | 0.84 (3) | 2.09 (4) | 2.820 (4) | 145 (3) |