Literature DB >> 22589849

Penta-aqua-(4,6-dihy-droxy-benzene-1,3-disulfonato-κO(1))zinc penta-hydrate.

Zhi-Biao Zhu, Shan Gao, Seik Weng Ng, Edward R T Tiekink.   

Abstract

The Zn(II) atom in the title complex, [Zn(C(6)H(4)O(8)S(2))(H(2)O)(5)]·5H(2)O, is coordinated by five water mol-ecules and an O atom of a 4,6-dihy-droxy-benzene-1,3-disulfonate dianion. The coord-ination geometry is distorted octa-hedral, with the Zn-O(sulfonate) bond relatively long compared to the Zn-O(water) bonds. The coordinated and lattice water mol-ecules inter-act with each other and with the hy-droxy groups and sulfonate ligand through O-H⋯O hydrogen bonds, generating a tightly held three-dimensional network.

Entities:  

Year:  2012        PMID： 22589849      PMCID： PMC3343881          DOI： 10.1107/S1600536812012317

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related structures, see: Xie et al. (2010 ▶); Bakirci et al. (2006 ▶).

Experimental

Crystal data

[Zn(C6H4O8S2)(H2O)5]·5H2O M = 513.74 Triclinic, a = 7.1479 (3) Å b = 11.8929 (5) Å c = 12.2044 (6) Å α = 109.368 (1)° β = 104.690 (1)° γ = 92.953 (1)° V = 936.27 (7) Å3 Z = 2 Mo Kα radiation μ = 1.62 mm−1 T = 293 K 0.21 × 0.17 × 0.14 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.747, T max = 0.820 9270 measured reflections 4257 independent reflections 3883 reflections with I > 2σ(I) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.091 S = 1.06 4257 reflections 310 parameters 32 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.67 e Å−3 Δρmin = −0.35 e Å−3 Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC and Rigaku, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812012317/xu5482sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812012317/xu5482Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn(C6H4O8S2)(H2O)5]·5H2OZ = 2
Mr = 513.74F(000) = 532
Triclinic, P1Dx = 1.822 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.1479 (3) ÅCell parameters from 8162 reflections
b = 11.8929 (5) Åθ = 3.0–27.5°
c = 12.2044 (6) ŵ = 1.62 mm−1
α = 109.368 (1)°T = 293 K
β = 104.690 (1)°Prism, colourless
γ = 92.953 (1)°0.21 × 0.17 × 0.14 mm
V = 936.27 (7) Å3
Rigaku R-AXIS RAPID IP diffractometer4257 independent reflections
Radiation source: fine-focus sealed tube3883 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ω scanθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −8→9
Tmin = 0.747, Tmax = 0.820k = −15→15
9270 measured reflectionsl = −15→15
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0505P)2 + 0.7681P] where P = (Fo2 + 2Fc2)/3
4257 reflections(Δ/σ)max < 0.001
310 parametersΔρmax = 0.67 e Å−3
32 restraintsΔρmin = −0.35 e Å−3
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.
xyzUiso*/Ueq
Zn0.13086 (4)0.18054 (2)0.34895 (2)0.02620 (9)
S10.51381 (7)0.36541 (4)0.60727 (4)0.01787 (11)
S20.58913 (7)0.13241 (4)0.92703 (4)0.01968 (12)
O10.4285 (2)0.24063 (13)0.53364 (13)0.0256 (3)
O20.3656 (2)0.44586 (14)0.60175 (14)0.0260 (3)
O30.6847 (2)0.40513 (15)0.57826 (14)0.0272 (3)
O40.4610 (3)0.04682 (14)0.81323 (15)0.0335 (4)
O50.5033 (2)0.15452 (15)1.02630 (14)0.0277 (3)
O60.7809 (2)0.09405 (16)0.95478 (17)0.0331 (4)
O70.7208 (3)0.57857 (13)0.82673 (14)0.0294 (4)
H70.777 (4)0.637 (2)0.8893 (18)0.044*
O80.7840 (3)0.37304 (15)1.10942 (14)0.0329 (4)
H80.828 (5)0.4422 (15)1.160 (2)0.049*
O1w0.1481 (3)0.34947 (14)0.35174 (15)0.0289 (3)
H110.205 (4)0.401 (2)0.4201 (12)0.043*
H120.178 (4)0.369 (2)0.2982 (17)0.043*
O2w0.3028 (3)0.15031 (17)0.24487 (19)0.0411 (4)
H210.300 (5)0.0797 (13)0.201 (3)0.062*
H220.412 (3)0.191 (2)0.263 (3)0.062*
O3w0.1534 (3)0.03068 (16)0.38332 (19)0.0500 (6)
H310.231 (5)0.030 (3)0.447 (2)0.075*
H320.081 (5)−0.0356 (19)0.347 (3)0.075*
O4w−0.0565 (2)0.22860 (16)0.44222 (16)0.0313 (4)
H41−0.117 (4)0.172 (2)0.450 (3)0.047*
H42−0.136 (3)0.263 (2)0.406 (3)0.047*
O5w−0.1099 (3)0.07189 (19)0.18311 (16)0.0389 (4)
H51−0.214 (3)0.041 (3)0.186 (3)0.058*
H52−0.130 (4)0.084 (3)0.1172 (19)0.058*
O6w0.6621 (3)0.05893 (17)0.44204 (16)0.0330 (4)
H610.623 (4)0.025 (3)0.3672 (10)0.050*
H620.582 (4)0.103 (3)0.467 (2)0.050*
O7w0.3618 (3)0.70069 (16)0.70377 (16)0.0320 (4)
H710.369 (5)0.6284 (12)0.668 (2)0.048*
H720.365 (5)0.712 (2)0.7754 (12)0.048*
O8w0.0699 (3)0.41514 (16)0.71292 (15)0.0320 (4)
H810.142 (3)0.404 (3)0.668 (2)0.048*
H82−0.0465 (17)0.409 (3)0.673 (2)0.048*
O9w1.1390 (3)0.22383 (15)0.98465 (17)0.0345 (4)
H911.236 (3)0.190 (2)0.998 (3)0.052*
H921.037 (2)0.180 (2)0.975 (3)0.052*
O10w0.0671 (5)0.1796 (2)0.7321 (2)0.0718 (8)
H1010.066 (8)0.241 (2)0.714 (4)0.108*
H1020.100 (8)0.197 (4)0.8071 (11)0.108*
C10.5924 (3)0.37148 (18)0.75822 (17)0.0186 (4)
C20.6887 (3)0.47868 (18)0.85336 (19)0.0207 (4)
C30.7494 (3)0.48013 (19)0.97151 (18)0.0231 (4)
H30.81040.55171.03460.028*
C40.7200 (3)0.37540 (19)0.99630 (18)0.0218 (4)
C50.6239 (3)0.26820 (18)0.90129 (18)0.0195 (4)
C60.5610 (3)0.26795 (18)0.78383 (18)0.0200 (4)
H60.49650.19690.72100.024*
U11U22U33U12U13U23
Zn0.02933 (16)0.02089 (14)0.02952 (15)0.00324 (11)0.00921 (11)0.00995 (11)
S10.0216 (2)0.0159 (2)0.0145 (2)0.00053 (18)0.00261 (17)0.00571 (17)
S20.0248 (3)0.0179 (2)0.0185 (2)0.00282 (19)0.00699 (19)0.00866 (18)
O10.0329 (8)0.0185 (7)0.0188 (7)−0.0016 (6)0.0006 (6)0.0041 (6)
O20.0291 (8)0.0240 (7)0.0240 (8)0.0080 (6)0.0039 (6)0.0096 (6)
O30.0283 (8)0.0317 (8)0.0239 (8)−0.0009 (7)0.0094 (6)0.0123 (6)
O40.0508 (11)0.0224 (8)0.0213 (8)−0.0085 (7)0.0031 (7)0.0076 (6)
O50.0330 (8)0.0307 (8)0.0260 (8)0.0064 (7)0.0148 (7)0.0137 (7)
O60.0310 (9)0.0364 (9)0.0463 (10)0.0153 (7)0.0180 (8)0.0262 (8)
O70.0471 (10)0.0156 (7)0.0209 (8)−0.0056 (7)0.0042 (7)0.0064 (6)
O80.0491 (10)0.0268 (8)0.0151 (7)−0.0062 (8)−0.0021 (7)0.0079 (6)
O1w0.0389 (9)0.0205 (7)0.0278 (8)0.0024 (7)0.0081 (7)0.0106 (6)
O2w0.0415 (10)0.0296 (9)0.0476 (11)0.0019 (8)0.0255 (9)−0.0010 (8)
O3w0.0634 (14)0.0237 (9)0.0437 (11)−0.0093 (9)−0.0222 (10)0.0183 (8)
O4w0.0299 (8)0.0332 (9)0.0338 (9)0.0037 (7)0.0129 (7)0.0133 (7)
O5w0.0309 (9)0.0531 (11)0.0280 (9)−0.0082 (8)−0.0014 (7)0.0181 (8)
O6w0.0352 (9)0.0363 (9)0.0273 (8)0.0055 (8)0.0054 (7)0.0137 (7)
O7w0.0383 (9)0.0302 (8)0.0309 (9)0.0087 (7)0.0149 (7)0.0109 (7)
O8w0.0312 (9)0.0354 (9)0.0251 (8)0.0032 (7)0.0056 (7)0.0073 (7)
O9w0.0304 (9)0.0253 (8)0.0401 (10)0.0006 (7)0.0062 (8)0.0053 (7)
O10w0.103 (2)0.0377 (12)0.0521 (14)−0.0216 (13)−0.0148 (14)0.0197 (11)
C10.0211 (9)0.0187 (9)0.0151 (9)0.0011 (8)0.0032 (7)0.0065 (7)
C20.0241 (10)0.0163 (9)0.0209 (10)0.0006 (8)0.0053 (8)0.0070 (8)
C30.0282 (11)0.0184 (9)0.0171 (9)−0.0014 (8)0.0024 (8)0.0030 (7)
C40.0248 (10)0.0231 (10)0.0164 (9)0.0014 (8)0.0033 (8)0.0079 (8)
C50.0233 (10)0.0172 (9)0.0178 (9)0.0011 (8)0.0045 (7)0.0073 (7)
C60.0238 (10)0.0153 (9)0.0175 (9)−0.0010 (8)0.0025 (7)0.0047 (7)
Zn—O12.5415 (15)O3w—H320.833 (10)
Zn—O1w1.9950 (15)O4w—H410.833 (10)
Zn—O2w1.9460 (18)O4w—H420.838 (10)
Zn—O3w1.9671 (17)O5w—H510.831 (10)
Zn—O4w1.9588 (17)O5w—H520.840 (10)
Zn—O5w2.2355 (17)O6w—H610.831 (10)
S1—O31.4528 (16)O6w—H620.836 (10)
S1—O11.4581 (15)O7w—H710.837 (10)
S1—O21.4675 (16)O7w—H720.834 (10)
S1—C11.760 (2)O8w—H810.832 (10)
S2—O51.4475 (16)O8w—H820.838 (10)
S2—O41.4577 (17)O9w—H910.828 (10)
S2—O61.4607 (17)O9w—H920.834 (10)
S2—C51.761 (2)O10w—H1010.832 (10)
O7—C21.355 (2)O10w—H1020.834 (10)
O7—H70.832 (10)C1—C61.388 (3)
O8—C41.350 (2)C1—C21.404 (3)
O8—H80.834 (10)C2—C31.390 (3)
O1w—H110.836 (10)C3—C41.394 (3)
O1w—H120.832 (10)C3—H30.9300
O2w—H210.830 (10)C4—C51.403 (3)
O2w—H220.834 (10)C5—C61.388 (3)
O3w—H310.836 (10)C6—H60.9300
O2w—Zn—O4w171.28 (8)Zn—O2w—H22124 (2)
O2w—Zn—O3w95.37 (10)H21—O2w—H22110.9 (17)
O4w—Zn—O3w92.91 (10)Zn—O3w—H31121 (2)
O2w—Zn—O1w87.93 (8)Zn—O3w—H32128 (2)
O4w—Zn—O1w84.59 (7)H31—O3w—H32109.9 (17)
O3w—Zn—O1w167.14 (8)Zn—O4w—H41114 (2)
O2w—Zn—O5w86.55 (8)Zn—O4w—H42107 (2)
O4w—Zn—O5w91.25 (7)H41—O4w—H42109.4 (16)
O3w—Zn—O5w86.37 (8)Zn—O5w—H51123 (2)
O1w—Zn—O5w106.26 (7)Zn—O5w—H52123 (2)
O2w—Zn—O189.53 (8)H51—O5w—H52109.2 (16)
O4w—Zn—O195.00 (7)H61—O6w—H62110.4 (16)
O3w—Zn—O177.08 (6)H71—O7w—H72109.6 (16)
O1w—Zn—O190.55 (6)H81—O8w—H82110.1 (16)
O5w—Zn—O1162.56 (7)H91—O9w—H92110.9 (17)
O3—S1—O1113.06 (10)H101—O10w—H102111.0 (18)
O3—S1—O2112.15 (10)C6—C1—C2119.17 (18)
O1—S1—O2110.90 (9)C6—C1—S1119.49 (15)
O3—S1—C1107.07 (9)C2—C1—S1121.33 (15)
O1—S1—C1106.27 (9)O7—C2—C3121.69 (18)
O2—S1—C1106.94 (9)O7—C2—C1118.50 (18)
O5—S2—O4112.66 (10)C3—C2—C1119.81 (18)
O5—S2—O6112.17 (10)C2—C3—C4120.69 (19)
O4—S2—O6110.50 (11)C2—C3—H3119.7
O5—S2—C5108.45 (10)C4—C3—H3119.7
O4—S2—C5105.67 (10)O8—C4—C3121.99 (19)
O6—S2—C5107.00 (10)O8—C4—C5118.46 (18)
S1—O1—Zn123.46 (9)C3—C4—C5119.53 (18)
C2—O7—H7111 (2)C6—C5—C4119.40 (18)
C4—O8—H8111 (2)C6—C5—S2119.21 (15)
Zn—O1w—H11114 (2)C4—C5—S2121.34 (15)
Zn—O1w—H12123 (2)C1—C6—C5121.38 (18)
H11—O1w—H12110.0 (16)C1—C6—H6119.3
Zn—O2w—H21118 (2)C5—C6—H6119.3
O3—S1—O1—Zn−99.48 (12)O7—C2—C3—C4−178.1 (2)
O2—S1—O1—Zn27.48 (13)C1—C2—C3—C41.6 (3)
C1—S1—O1—Zn143.35 (10)C2—C3—C4—O8177.4 (2)
O2w—Zn—O1—S199.04 (12)C2—C3—C4—C5−1.5 (3)
O4w—Zn—O1—S1−73.50 (12)O8—C4—C5—C6−178.5 (2)
O3w—Zn—O1—S1−165.34 (14)C3—C4—C5—C60.5 (3)
O1w—Zn—O1—S111.11 (12)O8—C4—C5—S2−0.8 (3)
O5w—Zn—O1—S1175.93 (17)C3—C4—C5—S2178.15 (17)
O3—S1—C1—C6−122.53 (17)O5—S2—C5—C6−131.59 (17)
O1—S1—C1—C6−1.4 (2)O4—S2—C5—C6−10.6 (2)
O2—S1—C1—C6117.08 (18)O6—S2—C5—C6107.21 (18)
O3—S1—C1—C256.62 (19)O5—S2—C5—C450.8 (2)
O1—S1—C1—C2177.71 (17)O4—S2—C5—C4171.81 (18)
O2—S1—C1—C2−63.77 (19)O6—S2—C5—C4−70.4 (2)
C6—C1—C2—O7179.0 (2)C2—C1—C6—C5−0.4 (3)
S1—C1—C2—O7−0.1 (3)S1—C1—C6—C5178.79 (16)
C6—C1—C2—C3−0.6 (3)C4—C5—C6—C10.4 (3)
S1—C1—C2—C3−179.75 (17)S2—C5—C6—C1−177.26 (16)
D—H···AD—HH···AD···AD—H···A
O7—H7···O9wi0.83 (1)1.79 (1)2.612 (2)170 (3)
O8—H8···O8wii0.83 (1)1.84 (1)2.664 (2)172 (3)
O1w—H11···O20.84 (1)2.09 (2)2.852 (2)151 (3)
O1w—H12···O7iii0.83 (1)2.09 (1)2.923 (2)175 (3)
O2w—H21···O6iv0.83 (1)2.22 (1)3.021 (3)162 (3)
O2w—H22···O7wiii0.83 (1)1.88 (1)2.710 (3)171 (4)
O3w—H31···O6wiv0.84 (1)2.01 (2)2.765 (2)149 (3)
O3w—H32···O10wv0.83 (1)1.79 (1)2.618 (3)178 (5)
O4w—H41···O6wvi0.83 (1)1.98 (1)2.774 (2)160 (3)
O4w—H42···O7wvii0.84 (1)1.99 (1)2.802 (3)164 (3)
O5w—H51···O4v0.83 (1)2.00 (1)2.833 (3)176 (4)
O5w—H52···O6viii0.84 (1)1.97 (1)2.802 (3)170 (3)
O6w—H62···O10.84 (1)2.08 (1)2.903 (2)168 (3)
O6w—H61···O4iv0.83 (1)1.99 (1)2.821 (2)176 (3)
O7w—H71···O20.84 (1)2.05 (1)2.874 (2)170 (3)
O7w—H72···O5ii0.83 (1)2.33 (2)3.034 (2)143 (3)
O8w—H81···O20.83 (1)2.07 (2)2.854 (2)157 (3)
O8w—H82···O3vi0.84 (1)1.96 (1)2.799 (2)176 (3)
O9w—H91···O5ix0.83 (1)1.95 (1)2.747 (2)162 (3)
O9w—H92···O60.83 (1)1.97 (1)2.795 (2)173 (3)
O10w—H101···O8w0.83 (1)2.07 (2)2.887 (3)167 (4)
O10w—H102···O9wvi0.83 (1)2.03 (1)2.851 (3)171 (5)
Table 1

Selected bond lengths (Å)

Zn—O12.5415 (15)
Zn—O1w1.9950 (15)
Zn—O2w1.9460 (18)
Zn—O3w1.9671 (17)
Zn—O4w1.9588 (17)
Zn—O5w2.2355 (17)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O7—H7⋯O9wi0.83 (1)1.79 (1)2.612 (2)170 (3)
O8—H8⋯O8wii0.83 (1)1.84 (1)2.664 (2)172 (3)
O1w—H11⋯O20.84 (1)2.09 (2)2.852 (2)151 (3)
O1w—H12⋯O7iii0.83 (1)2.09 (1)2.923 (2)175 (3)
O2w—H21⋯O6iv0.83 (1)2.22 (1)3.021 (3)162 (3)
O2w—H22⋯O7wiii0.83 (1)1.88 (1)2.710 (3)171 (4)
O3w—H31⋯O6wiv0.84 (1)2.01 (2)2.765 (2)149 (3)
O3w—H32⋯O10wv0.83 (1)1.79 (1)2.618 (3)178 (5)
O4w—H41⋯O6wvi0.83 (1)1.98 (1)2.774 (2)160 (3)
O4w—H42⋯O7wvii0.84 (1)1.99 (1)2.802 (3)164 (3)
O5w—H51⋯O4v0.83 (1)2.00 (1)2.833 (3)176 (4)
O5w—H52⋯O6viii0.84 (1)1.97 (1)2.802 (3)170 (3)
O6w—H62⋯O10.84 (1)2.08 (1)2.903 (2)168 (3)
O6w—H61⋯O4iv0.83 (1)1.99 (1)2.821 (2)176 (3)
O7w—H71⋯O20.84 (1)2.05 (1)2.874 (2)170 (3)
O7w—H72⋯O5ii0.83 (1)2.33 (2)3.034 (2)143 (3)
O8w—H81⋯O20.83 (1)2.07 (2)2.854 (2)157 (3)
O8w—H82⋯O3vi0.84 (1)1.96 (1)2.799 (2)176 (3)
O9w—H91⋯O5ix0.83 (1)1.95 (1)2.747 (2)162 (3)
O9w—H92⋯O60.83 (1)1.97 (1)2.795 (2)173 (3)
O10w—H101⋯O8w0.83 (1)2.07 (2)2.887 (3)167 (4)
O10w—H102⋯O9wvi0.83 (1)2.03 (1)2.851 (3)171 (5)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

  3 in total

1.  Dynamically self-assembling metalloenzyme models based on calixarenes.

Authors:  Hüseyin Bakirci; Apurba L Koner; Michael H Dickman; Ulrich Kortz; Werner M Nau
Journal:  Angew Chem Int Ed Engl       Date:  2006-11-13       Impact factor: 15.336

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Penta-aqua-(acetonitrile-κN)zinc(II) 4,6-dihydroxy-benzene-1,3-disulfonate trihydrate.

Authors:  Bu-Yun Xie; Wei Huang; Ying Zhang; Rui-Qing Yang; Yong-Rong Xie
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-02-27
  3 in total

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