The title complex, [Zn(H
2O)
6](C
10H
6O
6S
2), consists of [Zn(H
2O)
6]
2+ cations and naphthalene-1,5-disulfonate anions. The Zn atom is coordinated by six water molecules to form an octahedral geometry [Zn—O = 2.0478 (12)–2.1322 (11) Å]. The cations and anions, which lie on different centers of symmetry, are linked by O—H
O hydrogen bonds into a three-dimensional supramolecular framework.
Supporting information
CCDC reference: 269826
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.002 Å
- R factor = 0.022
- wR factor = 0.062
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Hexaaquazinc(II) naphthalene-1,5-disulfonate'
top
Crystal data top
[Zn(H2O)6](C10H6O6S2) | F(000) = 472 |
Mr = 459.77 | Dx = 1.790 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 7302 reflections |
a = 13.237 (3) Å | θ = 3.1–27.4° |
b = 6.6598 (13) Å | µ = 1.74 mm−1 |
c = 9.6849 (19) Å | T = 295 K |
β = 92.27 (3)° | Plate, colorless |
V = 853.1 (3) Å3 | 0.37 × 0.28 × 0.14 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 1957 independent reflections |
Radiation source: fine-focus sealed tube | 1842 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
Detector resolution: 10 pixels mm-1 | θmax = 27.4°, θmin = 3.1° |
ω scans | h = −17→17 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −8→8 |
Tmin = 0.565, Tmax = 0.792 | l = −12→12 |
8017 measured reflections | |
Refinement top
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.062 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0384P)2 + 0.2395P] where P = (Fo2 + 2Fc2)/3 |
1957 reflections | (Δ/σ)max < 0.001 |
133 parameters | Δρmax = 0.41 e Å−3 |
9 restraints | Δρmin = −0.28 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn1 | 0.5000 | 0.0000 | 0.5000 | 0.01954 (9) | |
S1 | 0.24951 (2) | 0.53337 (5) | 0.41687 (4) | 0.02152 (10) | |
O1w | 0.52601 (8) | −0.27417 (17) | 0.40408 (11) | 0.0306 (2) | |
O2w | 0.58762 (7) | 0.15053 (16) | 0.35165 (10) | 0.0250 (2) | |
O3w | 0.37800 (8) | 0.03589 (16) | 0.36557 (12) | 0.0284 (2) | |
O1 | 0.23867 (8) | 0.73909 (16) | 0.36846 (12) | 0.0320 (2) | |
O2 | 0.30002 (8) | 0.40753 (17) | 0.31660 (11) | 0.0300 (2) | |
O3 | 0.29844 (9) | 0.51844 (16) | 0.55459 (13) | 0.0311 (3) | |
C1 | 0.00512 (11) | 0.1788 (2) | 0.36094 (16) | 0.0300 (3) | |
C2 | 0.10370 (11) | 0.2582 (2) | 0.36075 (15) | 0.0268 (3) | |
C3 | 0.12522 (10) | 0.4347 (2) | 0.42802 (14) | 0.0213 (3) | |
C4 | 0.05013 (10) | 0.5410 (2) | 0.50137 (14) | 0.0202 (3) | |
C5 | 0.06966 (11) | 0.7231 (2) | 0.57393 (15) | 0.0276 (3) | |
H1w1 | 0.4996 (12) | −0.298 (3) | 0.3254 (13) | 0.046* | |
H1w2 | 0.5794 (11) | −0.344 (3) | 0.4166 (19) | 0.046* | |
H2w1 | 0.6215 (12) | 0.248 (2) | 0.3845 (19) | 0.038* | |
H2w2 | 0.6248 (12) | 0.072 (2) | 0.3070 (18) | 0.038* | |
H3w1 | 0.3309 (12) | −0.051 (2) | 0.360 (2) | 0.043* | |
H3w2 | 0.3525 (14) | 0.1510 (16) | 0.350 (2) | 0.043* | |
H1 | −0.0091 | 0.0580 | 0.3161 | 0.036* | |
H2 | 0.1541 | 0.1908 | 0.3151 | 0.032* | |
H5 | 0.1347 | 0.7763 | 0.5770 | 0.033* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.01958 (13) | 0.02069 (13) | 0.01833 (13) | 0.00032 (7) | 0.00048 (9) | 0.00059 (7) |
S1 | 0.01584 (17) | 0.02101 (17) | 0.02777 (19) | −0.00150 (11) | 0.00167 (13) | 0.00153 (12) |
O1w | 0.0319 (5) | 0.0296 (5) | 0.0297 (5) | 0.0079 (4) | −0.0052 (4) | −0.0094 (4) |
O2w | 0.0251 (5) | 0.0260 (5) | 0.0243 (5) | −0.0039 (4) | 0.0058 (4) | −0.0018 (4) |
O3w | 0.0250 (5) | 0.0239 (5) | 0.0357 (6) | −0.0020 (4) | −0.0082 (4) | 0.0042 (4) |
O1 | 0.0252 (5) | 0.0228 (5) | 0.0482 (6) | −0.0022 (4) | 0.0035 (5) | 0.0066 (5) |
O2 | 0.0265 (5) | 0.0277 (5) | 0.0365 (5) | −0.0003 (4) | 0.0100 (4) | −0.0004 (5) |
O3 | 0.0222 (5) | 0.0383 (6) | 0.0325 (6) | −0.0023 (4) | −0.0041 (4) | −0.0006 (4) |
C1 | 0.0276 (7) | 0.0257 (7) | 0.0367 (7) | −0.0055 (6) | 0.0001 (6) | −0.0106 (6) |
C2 | 0.0232 (6) | 0.0251 (7) | 0.0322 (7) | 0.0002 (6) | 0.0035 (5) | −0.0046 (6) |
C3 | 0.0161 (6) | 0.0227 (6) | 0.0252 (6) | −0.0028 (5) | −0.0004 (5) | 0.0018 (5) |
C4 | 0.0171 (6) | 0.0215 (6) | 0.0220 (6) | −0.0027 (5) | −0.0005 (5) | 0.0001 (5) |
C5 | 0.0217 (6) | 0.0271 (7) | 0.0339 (7) | −0.0078 (5) | 0.0002 (6) | −0.0065 (6) |
Geometric parameters (Å, º) top
Zn1—O1w | 2.0835 (11) | O2w—H2w2 | 0.848 (9) |
Zn1—O2w | 2.1322 (11) | O3w—H3w1 | 0.850 (9) |
Zn1—O3w | 2.0478 (12) | O3w—H3w2 | 0.848 (9) |
S1—O1 | 1.4533 (11) | C1—C5ii | 1.362 (2) |
S1—O2 | 1.4643 (11) | C1—C2 | 1.408 (2) |
S1—O3 | 1.4629 (13) | C1—H1 | 0.9300 |
Zn1—O1wi | 2.0835 (11) | C2—C3 | 1.369 (2) |
Zn1—O2wi | 2.1322 (11) | C2—H2 | 0.9300 |
Zn1—O3wi | 2.0478 (12) | C3—C4 | 1.432 (2) |
S1—C3 | 1.7786 (14) | C4—C5 | 1.4199 (19) |
O1w—H1w1 | 0.841 (9) | C4—C4ii | 1.435 (3) |
O1w—H1w2 | 0.850 (9) | C5—C1ii | 1.362 (2) |
O2w—H2w1 | 0.842 (9) | C5—H5 | 0.9300 |
| | | |
O1w—Zn1—O1wi | 180 | O3w—Zn1—O2wi | 92.69 (5) |
O1w—Zn1—O2w | 90.44 (5) | O1—S1—C3 | 106.74 (7) |
O1w—Zn1—O2wi | 89.56 (5) | O2—S1—C3 | 106.06 (7) |
O1w—Zn1—O3w | 87.64 (5) | O3—S1—C3 | 107.26 (7) |
O1wi—Zn1—O2w | 89.56 (5) | C1—C2—H2 | 120.1 |
O2w—Zn1—O2wi | 180 | C1ii—C5—C4 | 121.17 (13) |
O2w—Zn1—O3w | 87.31 (4) | C1ii—C5—H5 | 119.4 |
O2w—Zn1—O3wi | 92.69 (5) | C2—C1—H1 | 119.6 |
O3w—Zn1—O3wi | 180 | C2—C3—C4 | 121.70 (12) |
O1—S1—O3 | 113.13 (7) | C2—C3—S1 | 117.64 (11) |
O1—S1—O2 | 111.55 (7) | C3—C2—C1 | 119.82 (13) |
O3—S1—O2 | 111.62 (7) | C3—C2—H2 | 120.1 |
Zn1—O1w—H1w1 | 119.8 (14) | C3—C4—C4ii | 117.54 (15) |
Zn1—O1w—H1w2 | 124.4 (13) | C4—C3—S1 | 120.63 (11) |
Zn1—O2w—H2w1 | 113.7 (13) | C4—C5—H5 | 119.4 |
Zn1—O2w—H2w2 | 113.3 (13) | C5ii—C1—C2 | 120.75 (14) |
Zn1—O3w—H3w1 | 121.2 (14) | C5ii—C1—H1 | 119.6 |
Zn1—O3w—H3w2 | 121.0 (13) | C5—C4—C3 | 123.46 (12) |
O1w—Zn1—O2wi | 89.56 (5) | C5—C4—C4ii | 118.99 (16) |
O1wi—Zn1—O2wi | 90.44 (5) | H1w1—O1w—H1w2 | 110.0 (14) |
O3wi—Zn1—O1wi | 87.64 (4) | H2w1—O2w—H2w2 | 110.8 (13) |
O3w—Zn1—O1wi | 92.36 (4) | H3w1—O3w—H3w2 | 108.5 (13) |
O3wi—Zn1—O2wi | 87.31 (5) | | |
| | | |
S1—C3—C4—C4ii | 176.12 (13) | C1—C2—C3—S1 | −176.99 (12) |
S1—C3—C4—C5 | −2.9 (2) | C1—C2—C3—C4 | 1.0 (2) |
O1—S1—C3—C2 | 126.68 (12) | C2—C3—C4—C4ii | −1.8 (2) |
O1—S1—C3—C4 | −51.38 (13) | C2—C3—C4—C5 | 179.15 (13) |
O2—S1—C3—C2 | 7.61 (13) | C3—C4—C5—C1ii | 178.24 (15) |
O2—S1—C3—C4 | −170.44 (11) | C4ii—C4—C5—C1ii | −0.8 (3) |
O3—S1—C3—C2 | −111.79 (12) | C5ii—C1—C2—C3 | 0.7 (2) |
O3—S1—C3—C4 | 70.15 (13) | | |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2wiii | 0.84 (1) | 2.06 (1) | 2.8900 (17) | 171 (2) |
O1w—H1w2···O3i | 0.85 (1) | 2.00 (1) | 2.8518 (16) | 177 (2) |
O2w—H2w1···O3iv | 0.84 (1) | 1.96 (1) | 2.8019 (16) | 175 (2) |
O2w—H2w2···O2iii | 0.85 (1) | 1.93 (1) | 2.7710 (15) | 172 (2) |
O3w—H3w1···O1v | 0.85 (1) | 1.86 (1) | 2.7043 (16) | 172 (2) |
O3w—H3w2···O2 | 0.85 (1) | 1.87 (1) | 2.7161 (16) | 178 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (iii) −x+1, y−1/2, −z+1/2; (iv) −x+1, −y+1, −z+1; (v) x, y−1, z. |