Literature DB >> 21201259

catena-Poly[[tetra-aqua-zinc(II)]-μ-2,2'-dihydr-oxy-5,5'-diazenediyldibenzoato].

Yu-Hui Tan, Qing-Song Li, Xian-Ping Luo, Xiao-Bing Xie.   

Abstract

In the title compound, [Zn(C(14)H(8)N(2)O(6))(H(2)O)(4)](n), the 2,2'-dihydr-oxy-5,5'-diazenediyldibenzoate ligand acts as a carboxyl-ate bridge, leading to the formation of a polymeric chain running along the [10] direction. The Zn(II) atom is hexa-coordinated in a distorted octa-hedral geometry by six O atoms [Zn-O = 2.055 (4)-2.132 (3) Å] from two carboxylate ligands and four water mol-ecules. The crystal packing is stabilized by inter-molecular O-H⋯O, O-H⋯N and C-H⋯O hydrogen bonds, and two π-π inter-actions. The centroid-centroid distances are 3.803 (16) and 3.804 (17) Å.

Entities:  

Year:  2008        PMID： 21201259      PMCID： PMC2960379          DOI： 10.1107/S1600536807064860

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


Related literature

For related literature, see: Klotz (2005 ▶); Tang, Tan & Cao (2007 ▶); Tang, Tan, Chen & Cao (2007 ▶); Tang, Yang et al. (2007 ▶).

Experimental

Crystal data

[Zn(C14H8N2O6)(H2O)4] M = 437.66 Monoclinic, a = 9.510 (2) Å b = 11.255 (3) Å c = 16.214 (4) Å β = 107.019 (3)° V = 1659.5 (7) Å3 Z = 4 Mo Kα radiation μ = 1.54 mm−1 T = 296 (2) K 0.25 × 0.22 × 0.10 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer Absorption correction: multi-scan (; Bruker, 2000 ▶) T min = 0.699, T max = 0.861 10784 measured reflections 3278 independent reflections 3036 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.039 wR(F 2) = 0.098 S = 1.10 3278 reflections 277 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.39 e Å−3 Δρmin = −0.70 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 2000 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807064860/is2258sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807064860/is2258Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn(C14H8N2O6)(H2O)4]F000 = 896
Mr = 437.66Dx = 1.752 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 935 reflections
a = 9.510 (2) Åθ = 1.8–26.0º
b = 11.255 (3) ŵ = 1.54 mm−1
c = 16.214 (4) ÅT = 296 (2) K
β = 107.019 (3)ºBlock, orange
V = 1659.5 (7) Å30.25 × 0.22 × 0.10 mm
Z = 4
Bruker SMART APEX CCD area-detector diffractometer3278 independent reflections
Radiation source: fine-focus sealed tube3036 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.034
T = 296(2) Kθmax = 26.0º
φ and ω scansθmin = 1.8º
Absorption correction: multi-scan(SADABS; Bruker, 2000)h = −11→11
Tmin = 0.699, Tmax = 0.861k = −13→13
10784 measured reflectionsl = −19→19
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.098  w = 1/[σ2(Fo2) + (0.0307P)2 + 1.3308P] where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
3278 reflectionsΔρmax = 0.39 e Å−3
277 parametersΔρmin = −0.70 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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
Zn10.71408 (5)0.64023 (4)0.21196 (3)0.03166 (13)
O60.9487 (4)0.4284 (3)0.2011 (2)0.0620 (11)
O50.7705 (4)0.5388 (3)0.1179 (2)0.0434 (8)
O40.6849 (4)0.5057 (3)−0.0439 (2)0.0511 (9)
H4A0.68730.53590.00250.077*
O31.5187 (4)−0.2597 (3)−0.0536 (2)0.0570 (10)
H3A1.5603−0.2816−0.00420.085*
O21.5791 (3)−0.2637 (2)0.10891 (19)0.0375 (7)
O11.4725 (4)−0.1395 (3)0.17841 (18)0.0508 (8)
O4W0.5362 (4)0.5313 (3)0.2060 (3)0.0535 (9)
O3W0.8865 (4)0.7510 (3)0.2132 (3)0.0501 (8)
O2W0.6659 (4)0.7520 (3)0.3064 (2)0.0493 (9)
O1W0.8398 (4)0.5403 (3)0.3147 (2)0.0431 (8)
N21.0930 (4)0.1421 (3)0.0030 (2)0.0343 (7)
N11.1233 (4)0.1052 (3)−0.0637 (2)0.0334 (8)
C140.8672 (5)0.4557 (4)0.1291 (3)0.0402 (11)
C130.8783 (5)0.3916 (3)0.0511 (3)0.0335 (9)
C120.7874 (5)0.4192 (4)−0.0312 (3)0.0343 (9)
C110.7972 (5)0.3553 (4)−0.1026 (3)0.0414 (10)
H11A0.73670.3751−0.15710.050*
C100.8949 (5)0.2633 (4)−0.0935 (3)0.0372 (9)
H10A0.89890.2196−0.14140.045*
C90.9877 (5)0.2357 (3)−0.0127 (3)0.0316 (9)
C80.9781 (5)0.2998 (4)0.0582 (3)0.0370 (10)
H8A1.04060.28070.11230.044*
C71.2236 (4)0.0099 (3)−0.0537 (3)0.0322 (9)
C61.2416 (5)−0.0349 (4)−0.1298 (3)0.0396 (10)
H6A1.1871−0.0025−0.18220.048*
C51.3378 (6)−0.1259 (4)−0.1296 (3)0.0473 (12)
H5A1.3469−0.1558−0.18120.057*
C41.4210 (5)−0.1727 (4)−0.0517 (3)0.0372 (10)
C31.4032 (4)−0.1293 (4)0.0259 (2)0.0301 (8)
C21.3051 (5)−0.0383 (3)0.0244 (3)0.0316 (9)
H2A1.2936−0.00930.07580.038*
C11.4901 (5)−0.1794 (4)0.1108 (3)0.0321 (9)
H1WA0.872 (6)0.496 (5)0.283 (4)0.062 (18)*
H3WA0.872 (7)0.779 (5)0.170 (4)0.05 (2)*
H4WA0.507 (9)0.504 (6)0.159 (5)0.09 (3)*
H2WA0.597 (7)0.802 (5)0.260 (4)0.073 (19)*
H3WB0.921 (7)0.796 (6)0.250 (5)0.07 (2)*
H4WB0.545 (7)0.488 (5)0.253 (4)0.066 (19)*
H1WB0.895 (8)0.580 (6)0.359 (4)0.08 (2)*
H2WB0.619 (8)0.703 (6)0.330 (5)0.09 (3)*
U11U22U33U12U13U23
Zn10.0368 (2)0.0289 (2)0.0260 (2)0.0034 (2)0.00388 (19)0.0022 (2)
O60.076 (2)0.070 (2)0.0266 (18)0.045 (2)−0.0057 (17)−0.0064 (16)
O50.0494 (18)0.0396 (16)0.0341 (18)0.0196 (14)0.0009 (13)−0.0061 (13)
O40.056 (2)0.0503 (18)0.0372 (19)0.0296 (16)−0.0021 (15)−0.0070 (15)
O30.076 (2)0.062 (2)0.0339 (19)0.0451 (19)0.0164 (18)0.0057 (16)
O20.0453 (16)0.0341 (14)0.0297 (16)0.0143 (13)0.0057 (13)0.0039 (12)
O10.068 (2)0.0524 (16)0.0286 (15)0.0272 (18)0.0085 (16)0.0010 (16)
O4W0.051 (2)0.059 (2)0.039 (2)−0.0120 (16)−0.0032 (17)0.0131 (19)
O3W0.060 (2)0.055 (2)0.030 (2)−0.0195 (17)0.0066 (17)0.001 (2)
O2W0.061 (2)0.051 (2)0.034 (2)0.0169 (18)0.0105 (16)0.0009 (15)
O1W0.0504 (19)0.0440 (17)0.0321 (19)0.0105 (15)0.0077 (14)0.0042 (14)
N20.0380 (17)0.0340 (15)0.0279 (17)0.0107 (16)0.0052 (14)0.0014 (16)
N10.0393 (18)0.0326 (17)0.0265 (18)0.0100 (14)0.0070 (15)0.0019 (13)
C140.044 (2)0.037 (2)0.036 (3)0.0115 (19)0.0051 (19)−0.0071 (19)
C130.039 (2)0.0294 (19)0.026 (2)0.0077 (17)−0.0003 (18)−0.0018 (15)
C120.032 (2)0.034 (2)0.032 (2)0.0076 (18)0.0013 (16)0.0019 (18)
C110.042 (2)0.048 (2)0.027 (2)0.014 (2)−0.0004 (18)0.000 (2)
C100.047 (2)0.039 (2)0.023 (2)0.0071 (19)0.0049 (17)−0.0056 (17)
C90.035 (2)0.0302 (19)0.028 (2)0.0089 (16)0.0061 (17)−0.0002 (16)
C80.043 (2)0.037 (2)0.026 (2)0.0108 (19)0.0030 (18)−0.0017 (18)
C70.035 (2)0.0308 (19)0.029 (2)0.0071 (16)0.0067 (17)0.0030 (17)
C60.047 (3)0.040 (2)0.026 (2)0.015 (2)0.0027 (18)0.0056 (18)
C50.068 (3)0.049 (2)0.023 (2)0.020 (3)0.009 (2)−0.001 (2)
C40.046 (2)0.034 (2)0.031 (2)0.0162 (18)0.0108 (19)0.0018 (17)
C30.035 (2)0.0271 (17)0.0262 (19)0.0065 (17)0.0064 (16)0.0032 (17)
C20.035 (2)0.0306 (19)0.029 (2)0.0051 (17)0.0088 (17)−0.0001 (17)
C10.036 (2)0.0322 (19)0.026 (2)0.0039 (17)0.0059 (17)−0.0014 (16)
Zn1—O3W2.055 (4)N2—N11.267 (5)
Zn1—O4W2.069 (4)N2—C91.425 (5)
Zn1—O1W2.075 (3)N1—C71.413 (5)
Zn1—O2i2.086 (3)C14—C131.487 (6)
Zn1—O52.097 (3)C13—C81.385 (6)
Zn1—O2W2.132 (3)C13—C121.396 (6)
O6—C141.236 (6)C12—C111.389 (6)
O5—C141.286 (5)C11—C101.370 (6)
O4—C121.350 (5)C11—H11A0.9300
O4—H4A0.8200C10—C91.383 (6)
O3—C41.356 (5)C10—H10A0.9300
O3—H3A0.8200C9—C81.383 (6)
O2—C11.278 (5)C8—H8A0.9300
O2—Zn1ii2.086 (3)C7—C21.387 (6)
O1—C11.240 (5)C7—C61.389 (6)
O4W—H4WA0.80 (8)C6—C51.372 (6)
O4W—H4WB0.88 (7)C6—H6A0.9300
O3W—H3WA0.74 (6)C5—C41.382 (6)
O3W—H3WB0.78 (7)C5—H5A0.9300
O2W—H2WA1.02 (7)C4—C31.406 (6)
O2W—H2WB0.87 (7)C3—C21.381 (5)
O1W—H1WA0.83 (6)C3—C11.493 (5)
O1W—H1WB0.88 (7)C2—H2A0.9300
O3W—Zn1—O4W177.75 (16)C12—C13—C14121.8 (4)
O3W—Zn1—O1W92.90 (16)O4—C12—C11117.9 (4)
O4W—Zn1—O1W89.28 (15)O4—C12—C13121.6 (4)
O3W—Zn1—O2i89.72 (15)C11—C12—C13120.5 (4)
O4W—Zn1—O2i88.10 (14)C10—C11—C12120.7 (4)
O1W—Zn1—O2i177.36 (13)C10—C11—H11A119.7
O3W—Zn1—O587.93 (16)C12—C11—H11A119.7
O4W—Zn1—O591.35 (16)C11—C10—C9119.8 (4)
O1W—Zn1—O594.52 (13)C11—C10—H10A120.1
O2i—Zn1—O585.89 (11)C9—C10—H10A120.1
O3W—Zn1—O2W88.49 (17)C8—C9—C10119.4 (4)
O4W—Zn1—O2W92.21 (18)C8—C9—N2116.8 (4)
O1W—Zn1—O2W86.44 (15)C10—C9—N2123.8 (4)
O2i—Zn1—O2W93.32 (13)C9—C8—C13122.0 (4)
O5—Zn1—O2W176.33 (15)C9—C8—H8A119.0
C14—O5—Zn1128.2 (3)C13—C8—H8A119.0
C12—O4—H4A109.5C2—C7—C6119.2 (4)
C4—O3—H3A109.5C2—C7—N1125.4 (4)
C1—O2—Zn1ii128.5 (3)C6—C7—N1115.4 (3)
Zn1—O4W—H4WA109 (6)C5—C6—C7121.6 (4)
Zn1—O4W—H4WB114 (4)C5—C6—H6A119.2
H4WA—O4W—H4WB122 (6)C7—C6—H6A119.2
Zn1—O3W—H3WA109 (5)C6—C5—C4119.3 (4)
Zn1—O3W—H3WB125 (5)C6—C5—H5A120.3
H3WA—O3W—H3WB111 (7)C4—C5—H5A120.3
Zn1—O2W—H2WA91 (3)O3—C4—C5117.9 (4)
Zn1—O2W—H2WB101 (5)O3—C4—C3122.2 (4)
H2WA—O2W—H2WB112 (5)C5—C4—C3119.9 (4)
Zn1—O1W—H1WA93 (4)C2—C3—C4120.0 (3)
Zn1—O1W—H1WB117 (4)C2—C3—C1119.0 (4)
H1WA—O1W—H1WB125 (6)C4—C3—C1121.0 (4)
N1—N2—C9114.4 (3)C3—C2—C7120.0 (4)
N2—N1—C7117.7 (3)C3—C2—H2A120.0
O6—C14—O5122.6 (4)C7—C2—H2A120.0
O6—C14—C13120.1 (4)O1—C1—O2123.5 (4)
O5—C14—C13117.3 (4)O1—C1—C3119.8 (4)
C8—C13—C12117.6 (4)O2—C1—C3116.7 (4)
C8—C13—C14120.6 (4)
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O60.84 (6)1.86 (6)2.677 (5)168 (6)
O1W—H1WB···N2iii0.88 (7)2.32 (6)3.058 (5)143 (6)
O2W—H2WA···O1i1.01 (6)1.63 (6)2.636 (5)170 (6)
O2W—H2WB···O3iv0.87 (7)2.44 (8)2.997 (5)123 (6)
O3W—H3WA···N1v0.74 (6)2.17 (6)2.893 (5)164 (5)
O3W—H3WB···O6iii0.78 (8)1.95 (7)2.664 (5)152 (7)
O4W—H4WA···O4vi0.79 (7)2.20 (8)2.875 (6)144 (8)
O4W—H4WB···O1iii0.89 (6)1.85 (6)2.703 (5)160 (6)
O3—H3A···O20.821.802.528 (4)147
O4—H4A···O50.821.812.537 (4)148
C2—H2A···O1Wvii0.932.533.405 (6)157
Zn1—O3W2.055 (4)
Zn1—O4W2.069 (4)
Zn1—O1W2.075 (3)
Zn1—O2i2.086 (3)
Zn1—O52.097 (3)
Zn1—O2W2.132 (3)
O3W—Zn1—O4W177.75 (16)
O3W—Zn1—O1W92.90 (16)
O4W—Zn1—O1W89.28 (15)
O3W—Zn1—O2i89.72 (15)
O4W—Zn1—O2i88.10 (14)
O1W—Zn1—O2i177.36 (13)
O3W—Zn1—O587.93 (16)
O4W—Zn1—O591.35 (16)
O1W—Zn1—O594.52 (13)
O2i—Zn1—O585.89 (11)
O3W—Zn1—O2W88.49 (17)
O4W—Zn1—O2W92.21 (18)
O1W—Zn1—O2W86.44 (15)
O2i—Zn1—O2W93.32 (13)
O5—Zn1—O2W176.33 (15)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1WA⋯O60.84 (6)1.86 (6)2.677 (5)168 (6)
O1W—H1WB⋯N2ii0.88 (7)2.32 (6)3.058 (5)143 (6)
O2W—H2WA⋯O1i1.01 (6)1.63 (6)2.636 (5)170 (6)
O2W—H2WB⋯O3iii0.87 (7)2.44 (8)2.997 (5)123 (6)
O3W—H3WA⋯N1iv0.74 (6)2.17 (6)2.893 (5)164 (5)
O3W—H3WB⋯O6ii0.78 (8)1.95 (7)2.664 (5)152 (7)
O4W—H4WA⋯O4v0.79 (7)2.20 (8)2.875 (6)144 (8)
O4W—H4WB⋯O1ii0.89 (6)1.85 (6)2.703 (5)160 (6)
O3—H3A⋯O20.821.802.528 (4)147
O4—H4A⋯O50.821.812.537 (4)148
C2—H2A⋯O1Wvi0.932.533.405 (6)157

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

  1 in total

Review 1.  Colonic targeting of aminosalicylates for the treatment of ulcerative colitis.

Authors:  U Klotz
Journal:  Dig Liver Dis       Date:  2005-03-02       Impact factor: 4.088
  1 in total

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