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The asymmetric unit of the title compound, [Zn(H2O)6](C6H6NO3S)2, contains one half-cation and one anion; the Zn atom lies on an inversion centre. In the crystal structure, inter­molecular O—H...O and O—H...S hydrogen bonds result in the formation of a supra­molecular network; an intra­molecular C—H...O hydrogen bond is also present.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807056498/at2468sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807056498/at2468Isup2.hkl
Contains datablock I

CCDC reference: 1296854

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.037
  • wR factor = 0.109
  • Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zn1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1AA ... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1BB ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H1B .. S1 .. 3.12 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A .. S1 .. 3.17 Ang. PLAT481_ALERT_4_C Long D...A H-Bond Reported O1 .. S1 .. 3.88 Ang. PLAT481_ALERT_4_C Long D...A H-Bond Reported O3 .. S1 .. 3.92 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 2.44 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

The crystal structure of Hexaaquanickel(II) bis(4-aminobenzenesulfonate), (II), has previously been reported (Zhong et al., 2007). The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with that of (II). We report herein the crystal structure of (I).

In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). The title compound, [Zn(H2O)6](C6H6NO3S)2, contains one half-cation and one anion; the Zn atom lies on an inversion centre, as in (II).

In the crystal structure, intermolecular O—H···O and O—H···S hydrogen bonds (Fig. 2 and Table 2) result in the formation of a supramolecular network structure; an intramolecular C—H···O hydrogen bond is also present, as in (II).

The both compounds, (I) and (II), are isostructural.

Related literature top

For a related structure, see: Zhong et al. (2007). For bond-length data, see: Allen et al. (1987).

Experimental top

Crystals of the title compound were synthesized using hydrothermal method in a 23 ml Teflon-lined Parr bomb, which was then sealed. Europium (III) nitrate pentahydrate (213.9 mg, 0.5 mmol), zine nitrate hexahydrate (148.7 mg, 0.5 mmol), p-aminobenzenesulfonic acid (346.4 mg, 2 mmol), ammonia (0.5 mol/l, 4 ml) and distilled water (8 g) were placed into the bomb and sealed. The bomb was then heated under autogenous pressure up to 453 K over the course of 7 d and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colourless solution was decanted from small colourless crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.

Refinement top

H atoms (for H2O) were located in difference syntheses and refined isotropically [O—H = 0.782 (17) and 0.837 (18) Å, Uiso(H) = 0.050 (9) and 0.075 (8) Å2]. The other H atoms were positioned geometrically, with N—H = 0.86 Å (for NH2) and C—H = 0.93 Å for aromatic H, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C,N) for aromatic and amino H atoms, or 1.5Ueq(O) for water molecules' H atoms.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level [symmetry code (A): 3/2 - x,1/2±y, 1/2 - z].
[Figure 2] Fig. 2. A packing diagram of (I). Hydrogen bonds are shown as dashed lines.
Hexaaquazinc(II) bis(4-aminobenzenesulfonate) top
Crystal data top
[Zn(H2O)6](C6H6NO3S)2F(000) = 536
Mr = 517.82Dx = 1.563 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5547 reflections
a = 6.9902 (19) Åθ = 2.1–26.6°
b = 6.2974 (16) ŵ = 1.36 mm1
c = 25.002 (2) ÅT = 273 K
β = 91.449 (2)°Prism, colourless
V = 1100.2 (4) Å30.49 × 0.38 × 0.19 mm
Z = 2
Data collection top
Bruker APEX-II area-detector
diffractometer
2265 independent reflections
Radiation source: fine-focus sealed tube1940 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ϕ and ω scansθmax = 26.8°, θmin = 3.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.552, Tmax = 0.778k = 77
6988 measured reflectionsl = 3131
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0655P)2 + 0.444P]
where P = (Fo2 + 2Fc2)/3
2265 reflections(Δ/σ)max = 0.001
157 parametersΔρmax = 0.39 e Å3
9 restraintsΔρmin = 0.28 e Å3
Crystal data top
[Zn(H2O)6](C6H6NO3S)2V = 1100.2 (4) Å3
Mr = 517.82Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.9902 (19) ŵ = 1.36 mm1
b = 6.2974 (16) ÅT = 273 K
c = 25.002 (2) Å0.49 × 0.38 × 0.19 mm
β = 91.449 (2)°
Data collection top
Bruker APEX-II area-detector
diffractometer
2265 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
1940 reflections with I > 2σ(I)
Tmin = 0.552, Tmax = 0.778Rint = 0.025
6988 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0379 restraints
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.39 e Å3
2265 reflectionsΔρmin = 0.28 e Å3
157 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
Zn10.50000.00000.00000.04348 (17)
S10.01480 (9)0.60833 (10)0.90519 (3)0.04055 (19)
O10.7237 (4)0.1030 (4)0.04800 (11)0.0715 (7)
O20.5086 (3)0.2886 (3)0.03511 (9)0.0527 (5)
O30.3033 (4)0.1032 (4)0.05310 (12)0.0714 (7)
O40.1556 (3)0.5131 (3)0.93092 (9)0.0525 (5)
O50.0143 (3)0.8403 (3)0.90891 (8)0.0518 (5)
O60.1927 (3)0.5160 (3)0.92413 (9)0.0533 (5)
N10.0313 (7)0.3787 (11)0.67178 (14)0.1237 (17)
H1AA0.00480.47090.64730.148*
H1BB0.06840.25340.66310.148*
C10.0126 (5)0.4361 (7)0.72961 (14)0.0676 (9)
C20.0455 (5)0.6320 (7)0.74500 (14)0.0738 (10)
H20.08080.73050.71880.089*
C30.0542 (5)0.6905 (6)0.79837 (13)0.0633 (8)
H30.09340.82620.80790.076*
C40.0037 (4)0.5444 (5)0.83687 (11)0.0447 (6)
C50.0529 (5)0.3427 (5)0.82224 (12)0.0595 (8)
H50.08470.24270.84830.071*
C60.0621 (6)0.2902 (6)0.76880 (13)0.0702 (9)
H60.10200.15510.75910.084*
H1A0.756 (4)0.221 (3)0.0511 (12)0.075 (8)*
H2A0.606 (3)0.347 (5)0.0453 (12)0.053 (9)*
H3A0.271 (5)0.217 (3)0.0619 (15)0.073 (12)*
H1B0.819 (4)0.025 (4)0.0535 (15)0.070 (10)*
H2B0.419 (3)0.347 (5)0.0473 (11)0.050 (9)*
H3B0.219 (4)0.017 (4)0.0598 (15)0.062 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0416 (3)0.0326 (3)0.0562 (3)0.00076 (16)0.00184 (18)0.00150 (17)
S10.0403 (3)0.0304 (3)0.0509 (4)0.0005 (2)0.0026 (2)0.0005 (2)
O10.0702 (15)0.0340 (12)0.1080 (19)0.0050 (11)0.0417 (14)0.0012 (12)
O20.0447 (11)0.0364 (11)0.0771 (14)0.0004 (9)0.0052 (10)0.0139 (9)
O30.0753 (16)0.0350 (12)0.1060 (19)0.0001 (11)0.0465 (14)0.0061 (12)
O40.0560 (12)0.0394 (11)0.0613 (12)0.0057 (8)0.0120 (10)0.0008 (8)
O50.0533 (11)0.0301 (10)0.0722 (13)0.0007 (8)0.0043 (9)0.0018 (9)
O60.0542 (11)0.0388 (11)0.0677 (13)0.0041 (8)0.0178 (10)0.0019 (8)
N10.116 (3)0.193 (5)0.063 (2)0.010 (3)0.011 (2)0.004 (3)
C10.0522 (17)0.094 (3)0.0566 (19)0.0061 (18)0.0016 (14)0.0020 (18)
C20.066 (2)0.097 (3)0.0590 (18)0.007 (2)0.0008 (16)0.0232 (19)
C30.0640 (18)0.060 (2)0.0657 (19)0.0094 (15)0.0040 (15)0.0136 (16)
C40.0394 (13)0.0442 (15)0.0504 (14)0.0004 (11)0.0011 (11)0.0020 (11)
C50.074 (2)0.0495 (18)0.0551 (16)0.0088 (15)0.0006 (14)0.0025 (14)
C60.081 (2)0.072 (2)0.0584 (18)0.0041 (19)0.0054 (16)0.0145 (17)
Geometric parameters (Å, º) top
Zn1—O12.052 (2)O3—H3B0.823 (18)
Zn1—O22.0187 (19)N1—C11.499 (5)
Zn1—O32.042 (2)N1—H1AA0.8600
Zn1—O2i2.0187 (19)N1—H1BB0.8600
Zn1—O3i2.042 (2)C1—C21.358 (6)
Zn1—O1i2.052 (2)C1—C61.381 (6)
S1—O61.463 (2)C2—C31.387 (5)
S1—O51.464 (2)C2—H20.9300
S1—O41.468 (2)C3—C41.371 (4)
S1—C41.758 (3)C3—H30.9300
O1—H1A0.782 (17)C4—C51.382 (4)
O1—H1B0.837 (18)C5—C61.379 (4)
O2—H2A0.806 (17)C5—H50.9300
O2—H2B0.795 (17)C6—H60.9300
O3—H3A0.786 (18)
O1i—Zn1—O1180.0H2A—O2—H2B110 (2)
O1—Zn1—O2i89.06 (9)Zn1—O3—H3A132 (3)
O1—Zn1—O290.94 (9)Zn1—O3—H3B115 (2)
O1—Zn1—O3i88.00 (12)H3A—O3—H3B110 (3)
O1—Zn1—O391.99 (12)C1—N1—H1AA120.0
O2i—Zn1—O2180.0C1—N1—H1BB120.0
O2i—Zn1—O389.02 (10)H1AA—N1—H1BB120.0
O2—Zn1—O390.98 (10)C2—C1—C6118.4 (3)
O3—Zn1—O3i180.0C2—C1—N1121.8 (4)
O2i—Zn1—O1i90.94 (9)C6—C1—N1119.8 (4)
O2i—Zn1—O3i90.98 (10)C1—C2—C3122.3 (3)
O2—Zn1—O3i89.02 (10)C1—C2—H2118.8
O3i—Zn1—O1i91.99 (12)C3—C2—H2118.8
O2i—Zn1—O189.06 (9)C4—C3—C2118.7 (3)
O3i—Zn1—O188.01 (12)C4—C3—H3120.6
O6—S1—O5112.14 (12)C2—C3—H3120.6
O6—S1—O4112.52 (13)C3—C4—C5120.1 (3)
O5—S1—O4112.31 (12)C3—C4—S1120.8 (2)
O6—S1—C4106.39 (13)C5—C4—S1119.2 (2)
O5—S1—C4106.86 (13)C6—C5—C4119.8 (3)
O4—S1—C4106.09 (13)C6—C5—H5120.1
Zn1—O1—H1A125 (2)C4—C5—H5120.1
Zn1—O1—H1B120 (2)C5—C6—C1120.7 (4)
H1A—O1—H1B109 (2)C5—C6—H6119.6
Zn1—O2—H2A124 (2)C1—C6—H6119.6
Zn1—O2—H2B124 (2)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···S1ii0.84 (2)3.12 (2)3.885 (3)153 (3)
O1—H1A···O4iii0.78 (2)1.99 (2)2.763 (3)172 (3)
O1—H1B···O5ii0.84 (2)2.01 (2)2.813 (3)161 (4)
O2—H2A···O4ii0.81 (2)1.97 (2)2.773 (3)179 (3)
O2—H2B···O6iv0.80 (2)1.95 (2)2.746 (3)178 (3)
O3—H3A···S1v0.79 (2)3.17 (2)3.921 (2)162 (3)
O3—H3B···O5iv0.82 (2)1.99 (2)2.797 (3)168 (4)
O3—H3A···O6v0.79 (2)1.99 (2)2.775 (3)174 (4)
C3—H3···O50.932.572.927 (4)103
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x, y+1, z+1; (v) x, y, z+1.

Experimental details

Crystal data
Chemical formula[Zn(H2O)6](C6H6NO3S)2
Mr517.82
Crystal system, space groupMonoclinic, P21/n
Temperature (K)273
a, b, c (Å)6.9902 (19), 6.2974 (16), 25.002 (2)
β (°) 91.449 (2)
V3)1100.2 (4)
Z2
Radiation typeMo Kα
µ (mm1)1.36
Crystal size (mm)0.49 × 0.38 × 0.19
Data collection
DiffractometerBruker APEX-II area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.552, 0.778
No. of measured, independent and
observed [I > 2σ(I)] reflections
6988, 2265, 1940
Rint0.025
(sin θ/λ)max1)0.633
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.109, 1.04
No. of reflections2265
No. of parameters157
No. of restraints9
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.39, 0.28

Computer programs: APEX2 (Bruker, 2005), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996).

Selected geometric parameters (Å, º) top
Zn1—O12.052 (2)Zn1—O32.042 (2)
Zn1—O22.0187 (19)
O1i—Zn1—O1180.0O2i—Zn1—O2180.0
O1—Zn1—O2i89.06 (9)O2i—Zn1—O389.02 (10)
O1—Zn1—O290.94 (9)O2—Zn1—O390.98 (10)
O1—Zn1—O3i88.00 (12)O3—Zn1—O3i180.0
O1—Zn1—O391.99 (12)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···S1ii0.837 (18)3.12 (2)3.885 (3)153 (3)
O1—H1A···O4iii0.782 (17)1.986 (18)2.763 (3)172 (3)
O1—H1B···O5ii0.837 (18)2.01 (2)2.813 (3)161 (4)
O2—H2A···O4ii0.806 (17)1.967 (18)2.773 (3)179 (3)
O2—H2B···O6iv0.795 (17)1.951 (17)2.746 (3)178 (3)
O3—H3A···S1v0.786 (18)3.17 (2)3.921 (2)162 (3)
O3—H3B···O5iv0.823 (18)1.99 (2)2.797 (3)168 (4)
O3—H3A···O6v0.786 (18)1.992 (18)2.775 (3)174 (4)
C3—H3···O50.932.572.927 (4)103
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x, y+1, z+1; (v) x, y, z+1.
 

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