Literature DB >> 21583808

Poly[(μ-benzene-1,2,4,5-tetra-carboxyl-ato)tetra-silver(I)].

M Nawaz Tahir, Orhan Atakol, Muhammad Ilyas Tariq.   

Abstract

In the centrosymmetric title compound, [Ag(4)(C(10)H(2)O(8))](n), the benzene ring has irregular bond lengths but remains planar (r.m.s. deviation 0.0002 Å). The Ag-O bond lengths are in the range 2.153 (3)-2.615 (4) Å. The carboxyl-ate groups are oriented at dihedral angles of 26.4 (5) and 74.9 (4)° to the benzene ring. The coordination behaviour of each carboxyl-ate O atom is different: in one carboxylate, the O atoms are coordinated to a single and two Ag atoms; in the other carboxylate, the O atoms are coordinated to two and three Ag atoms. Non-classical inter-molecular C-H⋯O hydrogen bonding is present in the crystal structure. The title compound forms a three-dimensional polymeric network due to the coordination of the Ag atoms.

Entities:  

Year:  2009        PMID： 21583808      PMCID： PMC2977622          DOI： 10.1107/S1600536809015074

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


Related literature

For related structures, see: Jaber et al. (1997 ▶); Tahir et al. (1996 ▶); Ülkü et al. (1996 ▶).

Experimental

Crystal data

[Ag4(C10H2O8)] M = 340.80 Monoclinic, a = 8.328 (1) Å b = 6.317 (1) Å c = 10.945 (2) Å β = 94.36 (2)° V = 574.13 (16) Å3 Z = 4 Mo Kα radiation μ = 6.76 mm−1 T = 296 K 0.30 × 0.10 × 0.08 mm

Data collection

Enraf–Nonius CAD-4 diffractometer Absorption correction: ψ scan (; Fair, 1990 ▶) T min = 0.448, T max = 0.578 1680 measured reflections 1308 independent reflections 1268 reflections with I > 2σ(I) R int = 0.012 3 standard reflections frequency: 120 min intensity decay: 0.1%

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.089 S = 1.01 1308 reflections 101 parameters H-atom parameters constrained Δρmax = 1.20 e Å−3 Δρmin = −0.79 e Å−3 Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1993 ▶); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809015074/rk2131sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809015074/rk2131Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag4(C10H2O8)]F(000) = 628
Mr = 340.80Dx = 3.943 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 8.328 (1) Åθ = 11.7–21.0°
b = 6.317 (1) ŵ = 6.76 mm−1
c = 10.945 (2) ÅT = 296 K
β = 94.36 (2)°Needle, pale yellow
V = 574.13 (16) Å30.30 × 0.10 × 0.08 mm
Z = 4
Enraf–Nonius CAD-4 diffractometerRint = 0.012
ω/2θ scansθmax = 28.2°, θmin = 3.7°
Absorption correction: ψ scan (MolEN; Fair, 1990)h = 0→10
Tmin = 0.448, Tmax = 0.578k = 0→8
1680 measured reflectionsl = −14→14
1308 independent reflections3 standard reflections every 120 min
1268 reflections with I > 2σ(I) intensity decay: 0.1%
Refinement on F2Primary atom site location: Patterson
Least-squares matrix: FullSecondary atom site location: Difmap
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.089w = 1/[σ2(Fo2) + (0.0599P)2 + 3.6455P] where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
1308 reflectionsΔρmax = 1.20 e Å−3
101 parametersΔρmin = −0.79 e Å−3
0 restraints
Experimental. The structure was solved by Patterson method using SHELX86. The whole molecule was recognized.
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.s is used for estimating esds involving l.s. planes.
xyzUiso*/Ueq
Ag10.09967 (6)0.44769 (6)0.70351 (4)0.0316 (2)
Ag2−0.15558 (4)0.16471 (6)0.44813 (3)0.0250 (2)
O10.1054 (4)0.2412 (6)0.5218 (3)0.0238 (10)
O20.1422 (4)0.3437 (6)0.3300 (3)0.0264 (10)
O30.3520 (4)0.6473 (6)0.1913 (3)0.0246 (10)
O40.2066 (5)0.8108 (6)0.3346 (3)0.0273 (11)
C10.3498 (5)0.4182 (8)0.4710 (4)0.0169 (11)
C20.4363 (6)0.3358 (7)0.5701 (4)0.0184 (12)
C30.4135 (5)0.5821 (8)0.4012 (4)0.0167 (11)
C40.1874 (5)0.3273 (7)0.4386 (4)0.0191 (12)
C50.3167 (5)0.6850 (8)0.2996 (4)0.0186 (12)
H20.395170.228060.616430.0221*
U11U22U33U12U13U23
Ag10.0447 (3)0.0225 (3)0.0247 (3)−0.0009 (2)−0.0155 (2)−0.0012 (1)
Ag20.0254 (3)0.0282 (3)0.0195 (3)−0.0047 (1)−0.0097 (2)0.0011 (1)
O10.0201 (16)0.0262 (18)0.0240 (17)−0.0079 (13)−0.0045 (13)−0.0005 (14)
O20.0254 (18)0.0292 (19)0.0221 (17)−0.0027 (14)−0.0152 (14)−0.0006 (14)
O30.0222 (17)0.035 (2)0.0156 (16)0.0058 (14)−0.0048 (13)0.0024 (14)
O40.0291 (19)0.033 (2)0.0187 (16)0.0134 (16)−0.0057 (14)0.0017 (14)
C10.0131 (18)0.020 (2)0.0164 (19)−0.0001 (16)−0.0070 (15)0.0001 (16)
C20.017 (2)0.020 (2)0.017 (2)−0.0003 (16)−0.0064 (16)0.0033 (16)
C30.0150 (19)0.021 (2)0.0130 (18)0.0022 (16)−0.0058 (14)0.0001 (16)
C40.016 (2)0.016 (2)0.024 (2)0.0017 (16)−0.0059 (17)−0.0050 (16)
C50.015 (2)0.022 (2)0.018 (2)−0.0005 (16)−0.0046 (16)0.0013 (16)
Ag1—O12.382 (3)O2—C41.224 (5)
Ag1—Ag2i3.0140 (8)O3—C51.265 (5)
Ag1—O2i2.412 (4)O4—C51.293 (6)
Ag1—O2ii2.314 (4)C1—C21.359 (6)
Ag1—O4iii2.233 (4)C1—C31.414 (7)
Ag2—O12.311 (3)C1—C41.487 (6)
Ag2—O3iv2.153 (3)C2—C3vi1.368 (7)
Ag2—O1v2.615 (4)C3—C51.474 (6)
Ag2—O4i2.452 (3)C2—H20.9300
O1—C41.298 (5)
Ag1···C23.334 (5)O1···O4i3.154 (5)
Ag1···C4i3.097 (4)O2···C52.635 (6)
Ag1···Ag1vii3.7449 (9)O2···O33.072 (5)
Ag1···Ag1viii3.7449 (9)O2···O42.999 (5)
Ag1···Ag2viii4.0452 (9)O2···Ag2xii3.666 (4)
Ag1···O1viii4.022 (4)O2···Ag2i3.939 (4)
Ag1···O1i3.495 (4)O3···O23.072 (5)
Ag1···O3i4.061 (3)O3···Ag1i4.061 (3)
Ag1···O3iii3.320 (4)O4···C43.268 (6)
Ag1···C5i3.565 (4)O4···Ag2xiii4.026 (4)
Ag1···Ag2ii3.6134 (9)O4···O22.999 (5)
Ag1···C5iii3.077 (5)O4···Ag1i3.031 (4)
Ag2···O1i3.788 (4)O4···O1i3.155 (5)
Ag2···O4ix4.026 (4)O1···H22.5500
Ag2···C2x3.898 (5)O3···H2xi2.5400
Ag2···Ag1vii4.0452 (9)C2···Ag13.334 (5)
Ag2···C2i3.923 (5)C2···Ag2xiv3.898 (5)
Ag2···C1i3.250 (5)C2···Ag2v3.928 (5)
Ag2···C2v3.928 (5)C2···Ag2i3.923 (5)
Ag2···Ag1xi3.6134 (9)C4···O43.268 (6)
Ag2···C4i3.458 (4)C5···O22.635 (6)
Ag1···H23.0400C5···Ag1i3.565 (4)
Ag2···H2v3.2300H2···Ag13.0400
O1···O22.240 (5)H2···O12.5500
O1···Ag2i3.788 (4)H2···Ag2v3.2300
O1···Ag1vii4.022 (4)H2···O3ii2.5400
O1···Ag1i3.496 (4)
Ag2i—Ag1—O188.36 (9)Ag2—O1—Ag2v88.62 (12)
O1—Ag1—O2i103.99 (12)Ag2v—O1—C4114.3 (3)
O1—Ag1—O2ii92.98 (12)Ag1i—O2—C4112.7 (3)
O1—Ag1—O4iii151.46 (13)Ag1xi—O2—C4122.4 (3)
Ag2i—Ag1—O2i68.57 (9)Ag1i—O2—Ag1xi104.81 (13)
Ag2i—Ag1—O2ii162.28 (9)Ag2xii—O3—C5115.9 (3)
Ag2i—Ag1—O4iii74.22 (9)Ag2i—O4—C5120.3 (3)
O2i—Ag1—O2ii127.86 (12)Ag1xv—O4—C5119.1 (3)
O2i—Ag1—O4iii90.69 (14)Ag1xv—O4—Ag2i119.34 (17)
O2ii—Ag1—O4iii97.10 (13)C2—C1—C3120.9 (4)
O1—Ag2—O3iv154.36 (13)C2—C1—C4117.4 (4)
O1—Ag2—O1v91.37 (12)C3—C1—C4121.7 (4)
Ag1i—Ag2—O180.89 (9)C1—C2—C3vi117.2 (4)
O1—Ag2—O4i82.89 (13)C1—C3—C5121.6 (4)
O1v—Ag2—O3iv98.33 (13)C1—C3—C2vi121.8 (4)
Ag1i—Ag2—O3iv78.00 (10)C2vi—C3—C5116.4 (4)
O3iv—Ag2—O4i120.81 (13)O1—C4—O2125.3 (4)
Ag1i—Ag2—O1v146.75 (8)O1—C4—C1120.8 (4)
O1v—Ag2—O4i88.69 (12)O2—C4—C1114.0 (4)
Ag1i—Ag2—O4i121.88 (9)O3—C5—O4127.9 (4)
Ag1—O1—Ag2109.14 (14)O3—C5—C3118.1 (4)
Ag1—O1—C4113.7 (3)O4—C5—C3114.0 (4)
Ag1—O1—Ag2v116.43 (13)C1—C2—H2121.00
Ag2—O1—C4111.9 (3)C3vi—C2—H2121.00
Ag2i—Ag1—O1—Ag2−100.23 (13)O1—Ag2—O1v—C4v113.6 (3)
Ag2i—Ag1—O1—C425.5 (3)O1—Ag2—O4i—C5i125.7 (4)
Ag2i—Ag1—O1—Ag2v161.49 (13)Ag1—O1—C4—O2−132.9 (4)
O2i—Ag1—O1—Ag2−32.80 (17)Ag1—O1—C4—C146.7 (5)
O2i—Ag1—O1—C492.9 (3)Ag2—O1—C4—O2−8.7 (6)
O2i—Ag1—O1—Ag2v−131.09 (14)Ag2—O1—C4—C1170.9 (3)
O2ii—Ag1—O1—Ag297.46 (15)Ag2v—O1—C4—O290.2 (5)
O2ii—Ag1—O1—C4−136.8 (3)Ag2v—O1—C4—C1−90.3 (4)
O2ii—Ag1—O1—Ag2v−0.82 (15)Ag1i—O2—C4—O161.0 (5)
O4iii—Ag1—O1—Ag2−151.8 (2)Ag1i—O2—C4—C1−118.5 (3)
O4iii—Ag1—O1—C4−26.0 (5)Ag1xi—O2—C4—O1−65.4 (6)
O4iii—Ag1—O1—Ag2v110.0 (3)Ag1xi—O2—C4—C1115.1 (4)
O1—Ag1—Ag2i—O4−5.35 (14)Ag2xii—O3—C5—O4−31.4 (7)
O1—Ag1—Ag2i—O1i70.34 (12)Ag2xii—O3—C5—C3151.0 (3)
O1—Ag1—Ag2i—O3iii−124.33 (13)Ag2i—O4—C5—O3176.4 (4)
O2i—Ag1—Ag2i—O4−111.08 (15)Ag2i—O4—C5—C3−5.9 (5)
O4iii—Ag1—Ag2i—O4151.77 (16)Ag1xv—O4—C5—O3−16.2 (7)
O1—Ag1—O2i—C4i−21.4 (3)Ag1xv—O4—C5—C3161.5 (3)
O1—Ag1—O2ii—C4ii162.7 (3)C3—C1—C2—C3vi−0.1 (7)
O1—Ag1—O4iii—C5iii17.6 (5)C4—C1—C2—C3vi179.2 (4)
O3iv—Ag2—O1—Ag1129.8 (3)C2—C1—C3—C5−175.0 (4)
O3iv—Ag2—O1—C43.1 (5)C2—C1—C3—C2vi0.1 (7)
O3iv—Ag2—O1—Ag2v−112.6 (3)C4—C1—C3—C55.7 (7)
O1v—Ag2—O1—Ag1−117.55 (14)C4—C1—C3—C2vi−179.2 (4)
O1v—Ag2—O1—C4115.8 (3)C2—C1—C4—O127.0 (6)
O1v—Ag2—O1—Ag2v0.03 (10)C2—C1—C4—O2−153.5 (4)
Ag1i—Ag2—O1—Ag194.95 (13)C3—C1—C4—O1−153.8 (4)
Ag1i—Ag2—O1—C4−31.8 (3)C3—C1—C4—O225.8 (6)
Ag1i—Ag2—O1—Ag2v−147.47 (8)C1—C2—C3vi—C1vi0.1 (7)
O4i—Ag2—O1—Ag1−29.04 (15)C1—C2—C3vi—C5vi−175.3 (4)
O4i—Ag2—O1—C4−155.7 (3)C1—C3—C5—O3−109.0 (5)
O4i—Ag2—O1—Ag2v88.54 (12)C1—C3—C5—O473.0 (6)
O1—Ag2—O3iv—C5iv8.6 (6)C2vi—C3—C5—O375.6 (6)
O1—Ag2—O1v—Ag1v−110.74 (15)C2vi—C3—C5—O4−102.3 (5)
O1—Ag2—O1v—Ag2v−0.03 (11)
D—H···AD—HH···AD···AD—H···A
C2—H2···O3ii0.93002.54003.422 (6)158.00
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C2—H2⋯O3i0.932.54003.422 (6)158

Symmetry code: (i) .

  1 in total

1.  A short history of SHELX.

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

1.  catena-Poly[bis-(μ(3)-2-methyl-3,5-dinitro-benzoato)disilver(I)].

Authors:  Muhammad Danish; M Nawaz Tahir; Sabiha Ghafoor; Nazir Ahmad; Mehwish Nisa
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-06-18

2.  catena-Poly[bis-(μ(3)-2-methyl-benzoato)disilver(I)].

Authors:  Muhammad Danish; M Nawaz Tahir; Sabiha Ghafoor; Nazir Ahmad; Mehwish Nisa
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-05-07
  2 in total

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