The title compound crystallizes as centrosymmetric [Zn(μ
2-SO
4)(H
2O)
4]
2 dimers. The six-coordinate geometry of the zinc(II) centre comprises four water molecules and two
cis-located bridging sulfate anions in a distorted octahedral array within which the Zn—O interatomic distances and O—Zn—O interatomic angles fall into the narrow ranges 2.080 (8)–2.125 (7) Å and 83.7 (3)–96.7 (3)°, respectively. Strong O—H
O hydrogen bonds involving seven of the eight water-H atoms link the dimers to form a three-dimensional body-centred network.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (S-O) = 0.008 Å
- R factor = 0.059
- wR factor = 0.157
- Data-to-parameter ratio = 9.6
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
PLATON alerts of the form PLAT_7?? have been detected for an inorganic
structure. These tests are under development for inorganics and
comments are welcomed. It is not necessary to supply a data
validation response form for these alerts at this time.
Alert Level B:
PLAT_736 Alert B H...A Calc 2.35(7), Rep 2.358(14) .... 5.00 s.u-Ratio
H22 -O12 1.555 1.555
Alert Level C:
PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 6
O4 -ZN1 -O11 -S1 -125.00 5.00 1.555 1.555 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(8), Rep 0.82(2) .... 4.00 s.u-Ratio
O1 -H11 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(8), Rep 0.82(2) .... 4.00 s.u-Ratio
O1 -H12 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(6), Rep 0.83(2) .... 3.00 s.u-Ratio
O2 -H22 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(7), Rep 0.82(2) .... 3.50 s.u-Ratio
O3 -H31 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(8), Rep 0.82(2) .... 4.00 s.u-Ratio
O4 -H41 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(5), Rep 0.82(2) .... 2.50 s.u-Ratio
O4 -H42 1.555 1.555
PLAT_736 Alert C H...A Calc 1.95(8), Rep 1.95(3) .... 2.67 s.u-Ratio
H12 -O14 1.555 4.665
PLAT_736 Alert C H...A Calc 1.94(8), Rep 1.94(2) .... 4.00 s.u-Ratio
H31 -O14 1.555 3.566
PLAT_736 Alert C H...A Calc 1.95(6), Rep 1.95(2) .... 3.00 s.u-Ratio
H42 -O12 1.555 1.554
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
10 Alert Level C = Please check
Data collection: STADI4 (Stoe & Cie, 1997); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2001).
zinc(II) sulfate tetrahydrate
top
Crystal data top
[Zn(SO4)(H2O)4]2 | F(000) = 472 |
Mr = 467.05 | Dx = 2.465 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 5.904 (3) Å | Cell parameters from 48 reflections |
b = 13.519 (6) Å | θ = 10.5–16.0° |
c = 7.883 (6) Å | µ = 4.23 mm−1 |
β = 90.26 (6)° | T = 150 K |
V = 629.2 (6) Å3 | Block, colourless |
Z = 2 | 0.09 × 0.08 × 0.03 mm |
Data collection top
Stoe Stadi-4 four-circle diffractometer | 775 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.085 |
Graphite monochromator | θmax = 25.0°, θmin = 3.0° |
ω/θ scans | h = −6→7 |
Absorption correction: numerical (XRED; Stoe & Cie, 1997) | k = 0→16 |
Tmin = 0.724, Tmax = 0.873 | l = −8→9 |
1503 measured reflections | 3 standard reflections every 60 min |
1101 independent reflections | intensity decay: 7.1% |
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)] = 0.059 | Hydrogen site location: see text |
wR(F2) = 0.157 | See text |
S = 1.08 | w = 1/[σ2(Fo2) + (0.056P)2 + 7.905P] where P = (Fo2 + 2Fc2)/3 |
1101 reflections | (Δ/σ)max = 0.008 |
115 parameters | Δρmax = 0.85 e Å−3 |
13 restraints | Δρmin = −1.18 e Å−3 |
Special details top
Experimental. zinc(II) sulfate tetrahydrate |
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 | |
Zn1 | 0.43030 (19) | 0.39673 (9) | 0.28136 (15) | 0.0106 (4) | |
S1 | 0.3058 (4) | 0.39213 (19) | 0.6765 (3) | 0.0092 (6) | |
O11 | 0.2461 (11) | 0.4269 (5) | 0.5047 (9) | 0.0114 (15) | |
O12 | 0.4980 (12) | 0.4499 (5) | 0.7438 (9) | 0.0140 (16) | |
O13 | 0.3669 (12) | 0.2875 (5) | 0.6757 (9) | 0.0124 (16) | |
O14 | 0.1080 (11) | 0.4078 (5) | 0.7876 (9) | 0.0115 (15) | |
O1 | 0.3173 (12) | 0.2508 (5) | 0.2833 (9) | 0.0139 (16) | |
H11 | 0.249 (17) | 0.236 (7) | 0.196 (9) | 0.021* | |
H12 | 0.404 (15) | 0.205 (5) | 0.305 (13) | 0.021* | |
O2 | 0.7276 (12) | 0.3591 (5) | 0.4138 (9) | 0.0135 (16) | |
H21 | 0.817 (15) | 0.314 (6) | 0.430 (10) | 0.020* | |
H22 | 0.673 (17) | 0.378 (7) | 0.506 (6) | 0.020* | |
O3 | 0.1325 (13) | 0.4221 (5) | 0.1464 (9) | 0.0145 (16) | |
H31 | 0.064 (18) | 0.474 (4) | 0.159 (11) | 0.022* | |
H32 | 0.159 (19) | 0.415 (7) | 0.045 (3) | 0.022* | |
O4 | 0.6135 (13) | 0.3754 (5) | 0.0582 (9) | 0.0149 (17) | |
H41 | 0.683 (18) | 0.323 (5) | 0.058 (12) | 0.022* | |
H42 | 0.584 (19) | 0.391 (8) | −0.040 (5) | 0.022* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0099 (6) | 0.0093 (6) | 0.0127 (6) | −0.0006 (5) | −0.0004 (4) | −0.0006 (5) |
S1 | 0.0096 (12) | 0.0069 (12) | 0.0112 (13) | −0.0002 (10) | −0.0017 (9) | 0.0006 (11) |
O11 | 0.011 (4) | 0.014 (4) | 0.009 (4) | −0.003 (3) | 0.001 (3) | −0.007 (3) |
O12 | 0.020 (4) | 0.006 (3) | 0.016 (4) | −0.004 (3) | −0.008 (3) | 0.002 (3) |
O13 | 0.013 (4) | 0.009 (4) | 0.015 (4) | −0.002 (3) | 0.001 (3) | 0.000 (3) |
O14 | 0.010 (3) | 0.008 (3) | 0.016 (4) | 0.000 (3) | 0.002 (3) | −0.003 (3) |
O1 | 0.014 (4) | 0.012 (4) | 0.016 (4) | 0.006 (3) | −0.007 (3) | 0.002 (3) |
O2 | 0.016 (4) | 0.014 (4) | 0.011 (4) | 0.006 (3) | 0.000 (3) | −0.002 (3) |
O3 | 0.020 (4) | 0.013 (4) | 0.011 (4) | 0.006 (3) | 0.000 (3) | 0.001 (3) |
O4 | 0.020 (4) | 0.013 (4) | 0.011 (4) | 0.008 (3) | 0.002 (3) | 0.000 (3) |
Geometric parameters (Å, º) top
Zn1—O1 | 2.083 (8) | Zn1—O12i | 2.125 (7) |
Zn1—O2 | 2.101 (7) | S1—O11 | 1.475 (7) |
Zn1—O3 | 2.080 (8) | S1—O12 | 1.475 (7) |
Zn1—O4 | 2.089 (7) | S1—O13 | 1.460 (7) |
Zn1—O11 | 2.113 (7) | S1—O14 | 1.479 (7) |
| | | |
O1—Zn1—O2 | 91.9 (3) | O4—Zn1—O12i | 87.2 (3) |
O1—Zn1—O3 | 83.7 (3) | O4—Zn1—O11 | 176.8 (3) |
O1—Zn1—O4 | 92.4 (3) | O11—Zn1—O12i | 89.6 (3) |
O1—Zn1—O11 | 90.6 (3) | O11—S1—O12 | 110.0 (4) |
O1—Zn1—O12i | 171.3 (3) | O11—S1—O13 | 111.3 (4) |
O2—Zn1—O3 | 175.5 (3) | O11—S1—O14 | 108.2 (4) |
O2—Zn1—O4 | 87.2 (3) | O12—S1—O14 | 108.6 (4) |
O2—Zn1—O11 | 93.7 (3) | O12—S1—O13 | 109.0 (4) |
O2—Zn1—O12i | 96.7 (3) | O13—S1—O14 | 109.7 (4) |
O3—Zn1—O4 | 91.8 (3) | Zn1—O11—S1 | 125.6 (4) |
O3—Zn1—O11 | 87.6 (3) | Zn1i—O12—S1 | 129.5 (4) |
O3—Zn1—O12i | 87.7 (3) | | |
| | | |
O13—S1—O11—Zn1 | −45.7 (6) | O2—Zn1—O11—S1 | −19.1 (5) |
O12—S1—O11—Zn1 | 75.2 (6) | O12i—Zn1—O11—S1 | −115.8 (5) |
O14—S1—O11—Zn1 | −166.2 (4) | O13—S1—O12—Zn1i | 160.7 (5) |
O3—Zn1—O11—S1 | 156.5 (5) | O11—S1—O12—Zn1i | 38.5 (7) |
O1—Zn1—O11—S1 | 72.9 (5) | O14—S1—O12—Zn1i | −79.8 (6) |
O4—Zn1—O11—S1 | −125 (5) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···O13ii | 0.82 (2) | 2.29 (10) | 2.835 (10) | 125 (10) |
O1—H12···O14iii | 0.82 (2) | 1.95 (3) | 2.746 (10) | 163 (10) |
O2—H22···O12 | 0.83 (2) | 2.36 (1) | 3.185 (10) | 172 (8) |
O3—H31···O14iv | 0.82 (2) | 1.94 (2) | 2.753 (10) | 174 (10) |
O3—H32···O14v | 0.82 (2) | 2.05 (4) | 2.838 (10) | 160 (11) |
O4—H41···O13iii | 0.82 (2) | 2.06 (4) | 2.817 (10) | 153 (9) |
O4—H42···O12v | 0.82 (2) | 1.95 (2) | 2.758 (10) | 170 (10) |
Symmetry codes: (ii) x−1/2, −y+1/2, z−1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x, −y+1, −z+1; (v) x, y, z−1. |