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The title compound, [Zn(H2O)6][H3NC10H5(SO3)2]2·4H2O (Zn site symmetry \overline{1}), is isostructural with its nickel(II) and cobalt(II) analogues. An extensive network of N—H...O and O—H...O hydrogen bonds involving the ammonio group, water mol­ecules, and sulfonate O atoms helps to establish the packing. One of the uncoordinated water mol­ecules is disordered over at least two sites (modelled over two positions with site occupancy ratio ca 2:1).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807036938/hb2484sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807036938/hb2484Isup2.hkl
Contains datablock I

CCDC reference: 660047

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.002 Å
  • H-atom completeness 89%
  • Disorder in solvent or counterion
  • R factor = 0.038
  • wR factor = 0.107
  • Data-to-parameter ratio = 22.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT214_ALERT_2_B Atom O11B (Anion/Solvent) ADP max/min Ratio 6.00 prola
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 5 PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 10.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O11A PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O11B PLAT430_ALERT_2_C Short Inter D...A Contact O6 .. O11B .. 2.89 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O11A .. O11A .. 2.89 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 H2 O
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C20 H36 N2 O22 S4 Zn1 Atom count from the _atom_site data: C20 H32 N2 O22 S4 Zn1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_sum C20 H36 N2 O22 S4 Zn TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 20.00 20.00 0.00 H 36.00 32.00 4.00 N 2.00 2.00 0.00 O 22.00 22.00 0.00 S 4.00 4.00 0.00 Zn 1.00 1.00 0.00 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 8
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

As part of our ongoing studies of salts of 3-aminonaphthalene-1,5-sulfonate with divalent transition metals, we now report the structure of the title compound, (I), which is isostructural with its nickel(II) (Gunderman, Kabell et al., 1997) and cobalt(II) analogues (Genther et al., 2007). Compound (I) consists of centrosymmetic hexaaquazinc(II) cations, 3-ammonionaphthalene-1,5-disulfonate anions, and water molecules of crystallization (Fig. 1). Owing to the protonation of the amine group, each anion carries a single negative charge and the salt has the same 1:2 stoichiometry as would be observed with a monosulfonate anion. The cations reside on centers of inversion and display very regular octahedral geometry with maximum deviation from ideal 90° bond angles of just under 5°. This feature is very similar to what is found in the zinc naphthalene-1,5-disulfonate compound without the amine functionality (Huo et al., 2005).

The crystal packing (Fig. 2) is typical for transition metal arene- and naphthalenesulfonates (Chen et al., 2002; Gunderman, Dubey & Squattrito, 1997), consisting of alternating layers of hexaaquametal cations and sulfonate anions parallel to the ac plane, with the anions positioned so that the charged groups (i.e., NH3+ and SO3_) line the surface of the layer. The anions are positioned so that all the rings are parallel with contacts between adjacent rings of ca 3.7 Å. Neighboring rows of anions running along the a axis have the ammonio groups inverted. The water molecules of crystallization are located in between the cations in close association with the charged groups and coordinated water molecules so as to participate in hydrogen bonding interactions. One of the two crystallographically independent water molecules is disordered over at least two positions.

The layers are held together by a series of strong O—H···O and N—H···O hydrogen bonds involving water and ammonio donors and sulfonate and water acceptors (Table 2).

Related literature top

Compound (I) is isostructural with its nickel(II) (Gunderman, Kabell et al., 1997) and cobalt(II) (Genther et al., 2007) analogues. For background, see: Chen et al. (2002); Gunderman, Dubey & Squattrito (1997); Huo et al. (2005).

Experimental top

The title compound was prepared by direct reaction of Zn(NO3)2·6H2O and disodium 3-aminonaphthalene-1,5-disulfonate (1:2 stoichiometry) in aqueous solution. Following approximately one hour of heating, during which most of the reactants dissolved, the resulting solution was gravity filtered and set out in open air. Upon evaporation of the water, many small colorless, needles of (I) were recovered.

Refinement top

The O11 atom, corresponding to one water of crystallization, was found to be disordered and was refined on split positions ca 0.5 Å apart with occupancy factors constrained to sum to 1. Final occupancies were roughly 63% (O11A) and 37% (O11B). The B site has a significantly prolate displacement ellipsoid, but further splitting of the position could not be successfully modeled. The H atoms attached to the disordered water molecule could not be located. All other H atoms were located in difference maps and positionally refined either freely or with distance restraints of O—H = 0.82 (2) Å, and with Uiso(H) = 1.2Ueq(N,C) or Uiso(H) = 1.5Ueq(O).

Structure description top

As part of our ongoing studies of salts of 3-aminonaphthalene-1,5-sulfonate with divalent transition metals, we now report the structure of the title compound, (I), which is isostructural with its nickel(II) (Gunderman, Kabell et al., 1997) and cobalt(II) analogues (Genther et al., 2007). Compound (I) consists of centrosymmetic hexaaquazinc(II) cations, 3-ammonionaphthalene-1,5-disulfonate anions, and water molecules of crystallization (Fig. 1). Owing to the protonation of the amine group, each anion carries a single negative charge and the salt has the same 1:2 stoichiometry as would be observed with a monosulfonate anion. The cations reside on centers of inversion and display very regular octahedral geometry with maximum deviation from ideal 90° bond angles of just under 5°. This feature is very similar to what is found in the zinc naphthalene-1,5-disulfonate compound without the amine functionality (Huo et al., 2005).

The crystal packing (Fig. 2) is typical for transition metal arene- and naphthalenesulfonates (Chen et al., 2002; Gunderman, Dubey & Squattrito, 1997), consisting of alternating layers of hexaaquametal cations and sulfonate anions parallel to the ac plane, with the anions positioned so that the charged groups (i.e., NH3+ and SO3_) line the surface of the layer. The anions are positioned so that all the rings are parallel with contacts between adjacent rings of ca 3.7 Å. Neighboring rows of anions running along the a axis have the ammonio groups inverted. The water molecules of crystallization are located in between the cations in close association with the charged groups and coordinated water molecules so as to participate in hydrogen bonding interactions. One of the two crystallographically independent water molecules is disordered over at least two positions.

The layers are held together by a series of strong O—H···O and N—H···O hydrogen bonds involving water and ammonio donors and sulfonate and water acceptors (Table 2).

Compound (I) is isostructural with its nickel(II) (Gunderman, Kabell et al., 1997) and cobalt(II) (Genther et al., 2007) analogues. For background, see: Chen et al. (2002); Gunderman, Dubey & Squattrito (1997); Huo et al. (2005).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with atom labels and 50% probability displacement ellipsoids for non-H atoms. Symmetry-equivalent water molecules (marked 'i') are included to show the full coordination sphere of the zinc cation. [symmetry operation (i): -x, -y, -z]
[Figure 2] Fig. 2. The packing of (I), viewed down the a axis, showing layers connected by O—H···O and N—H···O hydrogen bonds (dashed lines). H atoms not involved in hydrogen bonding have been omitted.
Hexaaquazinc(II) 3-ammonionaphthalene-1,5-disulfonate tetrahydrate top
Crystal data top
[Zn(H2O)6](C10H8NO6S2)2·4H2OZ = 1
Mr = 850.12F(000) = 440
Triclinic, P1Dx = 1.778 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 5.4294 (2) ÅCell parameters from 6586 reflections
b = 12.7411 (5) Åθ = 3.0–34.4°
c = 12.9537 (6) ŵ = 1.13 mm1
α = 114.497 (1)°T = 273 K
β = 101.563 (1)°Pyramidal, colourless
γ = 90.889 (1)°0.25 × 0.22 × 0.10 mm
V = 793.97 (6) Å3
Data collection top
Bruker SMART 6000 CCD area-detector
diffractometer
6235 independent reflections
Radiation source: fine-focus sealed tube5724 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ω scansθmax = 34.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)
h = 88
Tmin = 0.757, Tmax = 0.890k = 2019
17231 measured reflectionsl = 2020
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)] = 0.038Hydrogen site location: difference Fourier map
wR(F2) = 0.107H atoms treated by a mixture of independent and constrained refinement
S = 0.94 w = 1/[σ2(Fo2) + (0.0664P)2 + 0.8611P]
where P = (Fo2 + 2Fc2)/3
6235 reflections(Δ/σ)max = 0.004
281 parametersΔρmax = 1.21 e Å3
8 restraintsΔρmin = 1.03 e Å3
Crystal data top
[Zn(H2O)6](C10H8NO6S2)2·4H2Oγ = 90.889 (1)°
Mr = 850.12V = 793.97 (6) Å3
Triclinic, P1Z = 1
a = 5.4294 (2) ÅMo Kα radiation
b = 12.7411 (5) ŵ = 1.13 mm1
c = 12.9537 (6) ÅT = 273 K
α = 114.497 (1)°0.25 × 0.22 × 0.10 mm
β = 101.563 (1)°
Data collection top
Bruker SMART 6000 CCD area-detector
diffractometer
6235 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)
5724 reflections with I > 2σ(I)
Tmin = 0.757, Tmax = 0.890Rint = 0.026
17231 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0388 restraints
wR(F2) = 0.107H atoms treated by a mixture of independent and constrained refinement
S = 0.94Δρmax = 1.21 e Å3
6235 reflectionsΔρmin = 1.03 e Å3
281 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*/UeqOcc. (<1)
Zn10.00000.00000.00000.01329 (6)
O70.2667 (2)0.12300 (10)0.00440 (10)0.01655 (19)
H90.347 (5)0.168 (2)0.0698 (16)0.025*
H100.227 (5)0.154 (2)0.037 (2)0.025*
O80.0542 (2)0.10549 (11)0.16894 (10)0.0191 (2)
H110.166 (4)0.148 (2)0.181 (2)0.029*
H120.062 (4)0.148 (2)0.220 (2)0.029*
O90.3033 (2)0.05209 (12)0.08378 (12)0.0214 (2)
H130.433 (4)0.066 (2)0.060 (2)0.032*
H140.275 (6)0.090 (2)0.119 (2)0.032*
S10.53398 (6)0.32440 (3)0.32236 (3)0.01257 (7)
O10.5772 (2)0.25319 (10)0.20550 (10)0.0174 (2)
O20.3014 (2)0.28147 (10)0.33812 (10)0.0182 (2)
O30.7536 (2)0.34056 (10)0.41396 (11)0.0197 (2)
S20.01825 (7)0.76440 (3)0.20463 (3)0.01679 (8)
O40.2443 (2)0.80350 (13)0.18042 (14)0.0272 (3)
O50.2114 (2)0.75525 (12)0.12018 (12)0.0237 (2)
O60.0005 (3)0.83525 (11)0.32527 (11)0.0236 (2)
N10.8696 (3)0.75553 (12)0.48044 (12)0.0181 (2)
H60.931 (5)0.779 (2)0.441 (2)0.022*
H70.975 (5)0.731 (2)0.523 (2)0.022*
H80.810 (5)0.811 (2)0.524 (2)0.022*
C10.4944 (3)0.46453 (12)0.32637 (12)0.0129 (2)
C20.6842 (3)0.55153 (12)0.39906 (12)0.0140 (2)
H10.823 (5)0.537 (2)0.442 (2)0.017*
C30.6666 (3)0.66315 (12)0.40379 (12)0.0143 (2)
C40.4673 (3)0.68879 (12)0.33900 (13)0.0150 (2)
H20.453 (5)0.762 (2)0.342 (2)0.018*
C50.0526 (3)0.62251 (13)0.19425 (13)0.0149 (2)
C60.1367 (3)0.53564 (14)0.12033 (14)0.0182 (3)
H30.266 (5)0.556 (2)0.080 (2)0.022*
C70.1215 (3)0.42251 (14)0.11220 (14)0.0185 (3)
H40.257 (5)0.358 (2)0.055 (2)0.022*
C80.0801 (3)0.39811 (13)0.17860 (13)0.0159 (2)
H50.083 (5)0.321 (2)0.171 (2)0.019*
C90.2798 (3)0.48562 (12)0.25578 (12)0.0129 (2)
C100.2676 (3)0.60071 (12)0.26362 (12)0.0133 (2)
O100.2280 (5)0.04341 (18)0.3472 (2)0.0540 (5)
H150.171 (8)0.028 (2)0.338 (4)0.081*
H160.233 (9)0.036 (4)0.273 (2)0.081*
O11A0.5941 (15)0.9487 (4)0.5787 (5)0.091 (3)0.628 (15)
O11B0.687 (2)0.9475 (6)0.5944 (16)0.136 (7)0.372 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.01269 (10)0.01336 (11)0.01533 (11)0.00281 (7)0.00337 (8)0.00746 (8)
O70.0166 (5)0.0175 (5)0.0169 (5)0.0004 (4)0.0012 (4)0.0099 (4)
O80.0162 (5)0.0202 (5)0.0175 (5)0.0044 (4)0.0030 (4)0.0050 (4)
O90.0170 (5)0.0293 (6)0.0305 (6)0.0088 (4)0.0090 (4)0.0230 (5)
S10.01214 (13)0.01096 (13)0.01408 (14)0.00084 (10)0.00037 (10)0.00599 (11)
O10.0180 (5)0.0148 (5)0.0174 (5)0.0041 (4)0.0042 (4)0.0047 (4)
O20.0168 (5)0.0185 (5)0.0206 (5)0.0025 (4)0.0037 (4)0.0100 (4)
O30.0171 (5)0.0174 (5)0.0226 (5)0.0008 (4)0.0061 (4)0.0115 (4)
S20.01698 (15)0.01829 (16)0.02169 (16)0.00366 (12)0.00445 (12)0.01480 (13)
O40.0202 (5)0.0358 (7)0.0423 (7)0.0043 (5)0.0094 (5)0.0318 (6)
O50.0200 (5)0.0283 (6)0.0302 (6)0.0056 (4)0.0014 (5)0.0215 (5)
O60.0353 (7)0.0156 (5)0.0235 (5)0.0048 (5)0.0084 (5)0.0111 (4)
N10.0224 (6)0.0141 (5)0.0156 (5)0.0039 (4)0.0032 (4)0.0079 (4)
C10.0130 (5)0.0115 (5)0.0139 (5)0.0017 (4)0.0019 (4)0.0057 (4)
C20.0143 (5)0.0123 (5)0.0145 (5)0.0003 (4)0.0000 (4)0.0065 (4)
C30.0164 (6)0.0120 (5)0.0133 (5)0.0010 (4)0.0005 (4)0.0057 (4)
C40.0175 (6)0.0120 (5)0.0158 (6)0.0008 (4)0.0019 (5)0.0072 (4)
C50.0148 (6)0.0163 (6)0.0164 (6)0.0034 (4)0.0029 (5)0.0099 (5)
C60.0156 (6)0.0206 (6)0.0197 (6)0.0019 (5)0.0002 (5)0.0116 (5)
C70.0160 (6)0.0178 (6)0.0197 (6)0.0003 (5)0.0010 (5)0.0083 (5)
C80.0139 (5)0.0143 (6)0.0184 (6)0.0010 (4)0.0008 (5)0.0072 (5)
C90.0129 (5)0.0127 (5)0.0135 (5)0.0022 (4)0.0024 (4)0.0061 (4)
C100.0141 (5)0.0133 (5)0.0138 (5)0.0021 (4)0.0025 (4)0.0074 (4)
O100.0723 (15)0.0376 (10)0.0527 (12)0.0136 (9)0.0136 (11)0.0199 (9)
O11A0.117 (5)0.042 (2)0.057 (3)0.039 (3)0.040 (3)0.0083 (18)
O11B0.103 (7)0.018 (3)0.253 (15)0.019 (3)0.150 (9)0.023 (5)
Geometric parameters (Å, º) top
Zn1—O92.0605 (12)N1—H70.86 (3)
Zn1—O9i2.0605 (12)N1—H80.82 (3)
Zn1—O72.0925 (11)C1—C21.3739 (19)
Zn1—O7i2.0926 (11)C1—C91.4328 (19)
Zn1—O82.1244 (12)C2—C31.404 (2)
Zn1—O8i2.1244 (12)C2—H10.91 (2)
O7—H90.823 (17)C3—C41.363 (2)
O7—H100.794 (17)C4—C101.420 (2)
O8—H110.817 (17)C4—H20.92 (2)
O8—H120.811 (17)C5—C61.375 (2)
O9—H130.814 (17)C5—C101.4297 (19)
O9—H140.812 (17)C6—C71.406 (2)
S1—O31.4471 (11)C6—H30.89 (3)
S1—O21.4526 (12)C7—C81.375 (2)
S1—O11.4764 (12)C7—H41.01 (3)
S1—C11.7820 (14)C8—C91.422 (2)
S2—O51.4520 (13)C8—H50.94 (2)
S2—O41.4554 (13)C9—C101.431 (2)
S2—O61.4694 (14)O10—H150.93 (4)
S2—C51.7721 (15)O10—H160.92 (3)
N1—C31.4621 (19)O11A—O11B0.510 (15)
N1—H60.80 (3)
O9—Zn1—O9i180.0C3—N1—H7110.0 (17)
O9—Zn1—O794.77 (5)H6—N1—H7115 (3)
O9i—Zn1—O785.24 (5)C3—N1—H8109.7 (18)
O9—Zn1—O7i85.24 (5)H6—N1—H8106 (3)
O9i—Zn1—O7i94.76 (5)H7—N1—H8108 (2)
O7—Zn1—O7i180.0C2—C1—C9121.35 (13)
O9—Zn1—O8i93.93 (5)C2—C1—S1116.45 (10)
O9i—Zn1—O8i86.07 (5)C9—C1—S1122.18 (10)
O7—Zn1—O8i93.91 (5)C1—C2—C3119.06 (13)
O7i—Zn1—O8i86.09 (5)C1—C2—H1121.1 (15)
O9—Zn1—O886.07 (5)C3—C2—H1119.8 (15)
O9i—Zn1—O893.93 (5)C4—C3—C2122.40 (13)
O7—Zn1—O886.08 (5)C4—C3—N1118.54 (13)
O7i—Zn1—O893.92 (5)C2—C3—N1119.06 (13)
O8i—Zn1—O8180.0C3—C4—C10119.75 (13)
Zn1—O7—H9115.4 (19)C3—C4—H2123.3 (15)
Zn1—O7—H10118 (2)C10—C4—H2116.9 (15)
H9—O7—H10113 (3)C6—C5—C10121.47 (13)
Zn1—O8—H11124 (2)C6—C5—S2117.93 (11)
Zn1—O8—H12121 (2)C10—C5—S2120.57 (11)
H11—O8—H1299 (3)C5—C6—C7119.90 (14)
Zn1—O9—H13122 (2)C5—C6—H3116.4 (17)
Zn1—O9—H14118 (2)C7—C6—H3123.7 (17)
H13—O9—H14113 (3)C8—C7—C6120.54 (14)
O3—S1—O2114.10 (7)C8—C7—H4119.9 (15)
O3—S1—O1112.15 (7)C6—C7—H4119.6 (15)
O2—S1—O1111.45 (7)C7—C8—C9121.15 (14)
O3—S1—C1105.83 (7)C7—C8—H5118.2 (15)
O2—S1—C1107.51 (7)C9—C8—H5120.7 (15)
O1—S1—C1105.11 (7)C8—C9—C10118.74 (13)
O5—S2—O4113.19 (8)C8—C9—C1123.30 (13)
O5—S2—O6112.69 (8)C10—C9—C1117.96 (12)
O4—S2—O6111.13 (9)C4—C10—C5122.34 (13)
O5—S2—C5106.45 (7)C4—C10—C9119.47 (13)
O4—S2—C5107.12 (8)C5—C10—C9118.19 (13)
O6—S2—C5105.70 (7)H15—O10—H1697 (4)
C3—N1—H6108.6 (19)
O3—S1—C1—C27.97 (13)S2—C5—C6—C7177.90 (12)
O2—S1—C1—C2130.29 (12)C5—C6—C7—C80.7 (2)
O1—S1—C1—C2110.88 (12)C6—C7—C8—C90.9 (2)
O3—S1—C1—C9173.49 (12)C7—C8—C9—C100.1 (2)
O2—S1—C1—C951.18 (13)C7—C8—C9—C1179.69 (14)
O1—S1—C1—C967.66 (13)C2—C1—C9—C8179.43 (14)
C9—C1—C2—C30.1 (2)S1—C1—C9—C81.0 (2)
S1—C1—C2—C3178.47 (11)C2—C1—C9—C100.4 (2)
C1—C2—C3—C40.2 (2)S1—C1—C9—C10178.83 (11)
C1—C2—C3—N1179.51 (13)C3—C4—C10—C5179.46 (14)
C2—C3—C4—C100.2 (2)C3—C4—C10—C90.7 (2)
N1—C3—C4—C10179.88 (14)C6—C5—C10—C4178.88 (15)
O5—S2—C5—C64.21 (15)S2—C5—C10—C43.0 (2)
O4—S2—C5—C6125.58 (13)C6—C5—C10—C91.0 (2)
O6—S2—C5—C6115.84 (13)S2—C5—C10—C9177.09 (11)
O5—S2—C5—C10177.62 (12)C8—C9—C10—C4179.08 (13)
O4—S2—C5—C1056.25 (14)C1—C9—C10—C40.7 (2)
O6—S2—C5—C1062.33 (13)C8—C9—C10—C50.8 (2)
C10—C5—C6—C70.3 (2)C1—C9—C10—C5179.38 (12)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H9···O1i0.82 (2)1.82 (2)2.6360 (16)169 (3)
O7—H10···O5ii0.79 (2)1.87 (2)2.6452 (16)166 (3)
O8—H11···O1iii0.82 (2)1.93 (2)2.7439 (16)177 (3)
O8—H12···O20.81 (2)1.97 (2)2.7662 (17)166 (3)
O9—H13···O7iv0.81 (2)1.99 (2)2.8015 (17)172 (3)
O9—H14···O4ii0.81 (2)1.87 (2)2.6660 (17)169 (3)
N1—H6···O6iv0.80 (3)2.01 (3)2.7966 (19)166 (3)
N1—H7···O3v0.86 (3)1.97 (3)2.8107 (18)166 (2)
N1—H8···O11A0.82 (3)2.08 (3)2.863 (6)160 (3)
O10—H15···O6ii0.93 (4)1.95 (2)2.876 (2)171 (4)
O10—H16···O80.92 (3)2.24 (3)3.036 (3)144 (4)
Symmetry codes: (i) x, y, z; (ii) x, y1, z; (iii) x1, y, z; (iv) x+1, y, z; (v) x+2, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Zn(H2O)6](C10H8NO6S2)2·4H2O
Mr850.12
Crystal system, space groupTriclinic, P1
Temperature (K)273
a, b, c (Å)5.4294 (2), 12.7411 (5), 12.9537 (6)
α, β, γ (°)114.497 (1), 101.563 (1), 90.889 (1)
V3)793.97 (6)
Z1
Radiation typeMo Kα
µ (mm1)1.13
Crystal size (mm)0.25 × 0.22 × 0.10
Data collection
DiffractometerBruker SMART 6000 CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2004)
Tmin, Tmax0.757, 0.890
No. of measured, independent and
observed [I > 2σ(I)] reflections
17231, 6235, 5724
Rint0.026
(sin θ/λ)max1)0.797
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.107, 0.94
No. of reflections6235
No. of parameters281
No. of restraints8
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.21, 1.03

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXTL (Sheldrick, 2001), SHELXTL and local programs.

Selected bond lengths (Å) top
Zn1—O92.0605 (12)Zn1—O82.1244 (12)
Zn1—O72.0925 (11)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H9···O1i0.823 (17)1.824 (17)2.6360 (16)169 (3)
O7—H10···O5ii0.794 (17)1.868 (18)2.6452 (16)166 (3)
O8—H11···O1iii0.816 (17)1.928 (17)2.7439 (16)177 (3)
O8—H12···O20.811 (17)1.971 (18)2.7662 (17)166 (3)
O9—H13···O7iv0.814 (17)1.994 (18)2.8015 (17)172 (3)
O9—H14···O4ii0.812 (17)1.865 (18)2.6660 (17)169 (3)
N1—H6···O6iv0.80 (3)2.01 (3)2.7966 (19)166 (3)
N1—H7···O3v0.86 (3)1.97 (3)2.8107 (18)166 (2)
N1—H8···O11A0.82 (3)2.08 (3)2.863 (6)160 (3)
O10—H15···O6ii0.93 (4)1.95 (2)2.876 (2)171 (4)
O10—H16···O80.92 (3)2.24 (3)3.036 (3)144 (4)
Symmetry codes: (i) x, y, z; (ii) x, y1, z; (iii) x1, y, z; (iv) x+1, y, z; (v) x+2, y+1, z+1.
 

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