Literature DB >> 21587368

Poly[(μ(2)-2,2'-bipyridine-κN:N')bis-(μ(3)-2,2,2-trifluoro-acetato-κO:O:O')disilver(I)].

Hadi D Arman, Tyler Miller, Edward R T Tiekink.   

Abstract

In the title salt, [Ag(2)(CF(3)CO(2))(2)(C(10)H(8)N(2))](n), which may also be regarded as a coordination polymer if long Ag⋯O inter-actions are considered, each of the N atoms of the somewhat twisted 2,2'-bipyridine mol-ecule [N-C-C-N = -27.5 (4)°] binds to an Ag atom, and each of the carboxyl-ate ligands is tridentate, linking to three Ag atoms. The bidentate carboxyl-ate O atoms bridge the same two Ag atoms, resulting in the formation of Ag(2)O(2) rings. These rings are bridged by the 2,2'-bipyridine ligands, forming a chain along the b axis. The chains are linked into double chains via the remaining Ag-O bonds and Ag⋯Ag contacts. As a consequence of the Ag⋯Ag contacts, the NO(4) donor set about each Ag atom is heavily distorted. Finally, the chains are linked into a three-dimensional network by a combination of C-H⋯O and C-H⋯F inter-actions.

Entities:  

Year:  2010        PMID： 21587368      PMCID： PMC2983243          DOI： 10.1107/S1600536810035282

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


Related literature

For structural diversity in the supra­molecular structures of silver salts, see: Kundu et al. (2010 ▶). For a related Ag salt, see: Arman et al. (2010 ▶).

Experimental

Crystal data

[Ag2(C2F3O2)2(C10H8N2)] M = 597.96 Monoclinic, a = 24.597 (6) Å b = 6.8474 (14) Å c = 21.253 (5) Å β = 116.029 (4)° V = 3216.5 (13) Å3 Z = 8 Mo Kα radiation μ = 2.53 mm−1 T = 98 K 0.31 × 0.29 × 0.20 mm

Data collection

Rigaku AFC12/SATURN724 diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.619, T max = 1.000 10231 measured reflections 3662 independent reflections 3469 reflections with I > 2σ(I) R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.031 wR(F 2) = 0.091 S = 1.09 3661 reflections 253 parameters H-atom parameters constrained Δρmax = 0.66 e Å−3 Δρmin = −0.65 e Å−3 Data collection: CrystalClear (Molecular Structure Corporation & Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810035282/hb5622sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810035282/hb5622Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag2(C2F3O2)2(C10H8N2)]F(000) = 2288
Mr = 597.96Dx = 2.470 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 8570 reflections
a = 24.597 (6) Åθ = 1.8–40.5°
b = 6.8474 (14) ŵ = 2.53 mm−1
c = 21.253 (5) ÅT = 98 K
β = 116.029 (4)°Block, colourless
V = 3216.5 (13) Å30.31 × 0.29 × 0.20 mm
Z = 8
Rigaku AFC12K/SATURN724 diffractometer3662 independent reflections
Radiation source: fine-focus sealed tube3469 reflections with I > 2σ(I)
graphiteRint = 0.037
ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −25→31
Tmin = 0.619, Tmax = 1.000k = −8→8
10231 measured reflectionsl = −27→27
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.09w = 1/[σ2(Fo2) + (0.0473P)2 + 8.2186P] where P = (Fo2 + 2Fc2)/3
3661 reflections(Δ/σ)max < 0.001
253 parametersΔρmax = 0.66 e Å−3
0 restraintsΔρmin = −0.65 e Å−3
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 s.u.'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
Ag10.270544 (11)0.27690 (4)0.078818 (12)0.01708 (10)
Ag20.239869 (12)0.73275 (4)0.063674 (12)0.01661 (10)
F10.05870 (11)0.2464 (3)0.01451 (13)0.0250 (5)
F20.04349 (10)0.0721 (4)−0.07648 (10)0.0313 (5)
F30.07622 (10)−0.0612 (3)0.02507 (11)0.0243 (4)
F40.45993 (11)0.7568 (3)0.16884 (13)0.0287 (5)
F50.45617 (9)0.9732 (3)0.09408 (11)0.0298 (5)
F60.43891 (9)1.0540 (3)0.18104 (11)0.0296 (5)
O10.18662 (10)0.1008 (3)0.06300 (11)0.0186 (5)
O20.15108 (12)0.2233 (3)−0.04584 (13)0.0207 (5)
O30.32741 (11)0.9056 (3)0.11732 (12)0.0189 (5)
O40.35046 (13)0.7790 (4)0.03384 (13)0.0234 (5)
N10.32454 (12)0.4507 (4)0.18047 (13)0.0148 (5)
N20.20388 (13)0.5665 (4)0.13321 (13)0.0161 (5)
C10.38483 (15)0.4390 (5)0.20200 (16)0.0179 (6)
H10.39910.40090.16890.021*
C20.42676 (14)0.4794 (5)0.26943 (17)0.0187 (6)
H20.46880.46680.28260.022*
C30.40639 (15)0.5387 (5)0.31752 (16)0.0185 (6)
H30.43430.56820.36430.022*
C40.34421 (15)0.5545 (4)0.29617 (15)0.0166 (6)
H40.32910.59510.32830.020*
C50.30455 (14)0.5100 (4)0.22711 (16)0.0156 (6)
C60.23773 (14)0.5279 (4)0.20229 (16)0.0147 (6)
C70.21148 (15)0.5069 (4)0.24806 (15)0.0160 (6)
H70.23610.48260.29640.019*
C80.14863 (16)0.5217 (5)0.22253 (18)0.0205 (6)
H80.13000.50920.25310.025*
C90.11430 (15)0.5549 (5)0.15166 (18)0.0193 (6)
H90.07150.56250.13250.023*
C100.14338 (15)0.5769 (4)0.10896 (17)0.0182 (6)
H100.11950.60040.06040.022*
C110.14613 (14)0.1417 (4)0.00329 (15)0.0156 (6)
C120.08041 (15)0.0970 (5)−0.00906 (16)0.0174 (6)
C130.36199 (14)0.8644 (4)0.09028 (15)0.0149 (6)
C140.42956 (15)0.9154 (5)0.13331 (16)0.0174 (6)
U11U22U33U12U13U23
Ag10.01380 (15)0.02195 (15)0.01404 (15)−0.00357 (9)0.00477 (11)−0.00392 (8)
Ag20.01414 (15)0.02253 (15)0.01274 (15)−0.00263 (8)0.00552 (11)0.00048 (8)
F10.0216 (12)0.0243 (10)0.0344 (12)0.0023 (8)0.0171 (10)−0.0020 (8)
F20.0195 (10)0.0516 (14)0.0162 (10)−0.0099 (10)0.0017 (8)−0.0047 (9)
F30.0235 (10)0.0207 (9)0.0324 (11)−0.0027 (8)0.0158 (9)0.0038 (8)
F40.0181 (11)0.0223 (10)0.0330 (13)0.0050 (8)−0.0005 (10)0.0093 (8)
F50.0195 (10)0.0442 (13)0.0257 (11)−0.0064 (10)0.0100 (9)0.0057 (9)
F60.0182 (10)0.0323 (11)0.0288 (11)−0.0015 (8)0.0017 (9)−0.0153 (9)
O10.0154 (11)0.0236 (11)0.0126 (10)−0.0014 (9)0.0024 (9)−0.0004 (8)
O20.0187 (13)0.0276 (12)0.0190 (12)0.0018 (9)0.0112 (11)0.0058 (9)
O30.0144 (11)0.0240 (11)0.0180 (10)−0.0016 (9)0.0068 (9)−0.0030 (9)
O40.0192 (13)0.0307 (13)0.0158 (12)0.0028 (10)0.0035 (11)−0.0065 (9)
N10.0164 (12)0.0141 (11)0.0121 (11)−0.0021 (10)0.0045 (10)−0.0019 (9)
N20.0171 (13)0.0170 (12)0.0133 (12)0.0010 (10)0.0058 (10)0.0029 (9)
C10.0185 (15)0.0191 (14)0.0156 (14)−0.0022 (12)0.0070 (13)−0.0038 (11)
C20.0140 (14)0.0221 (15)0.0185 (15)−0.0027 (13)0.0058 (12)−0.0019 (12)
C30.0196 (16)0.0204 (14)0.0112 (13)0.0010 (12)0.0027 (12)−0.0015 (11)
C40.0206 (16)0.0149 (13)0.0117 (13)0.0010 (11)0.0048 (12)−0.0013 (11)
C50.0196 (15)0.0117 (13)0.0163 (14)−0.0001 (12)0.0086 (12)0.0012 (10)
C60.0174 (14)0.0102 (12)0.0173 (14)0.0011 (11)0.0083 (12)−0.0011 (10)
C70.0243 (16)0.0141 (13)0.0110 (13)0.0007 (13)0.0091 (12)0.0022 (10)
C80.0291 (18)0.0154 (14)0.0245 (16)−0.0005 (13)0.0185 (15)−0.0012 (12)
C90.0162 (15)0.0160 (13)0.0268 (16)−0.0010 (12)0.0105 (13)−0.0021 (12)
C100.0175 (15)0.0162 (14)0.0185 (14)−0.0010 (12)0.0057 (13)0.0018 (11)
C110.0137 (14)0.0162 (13)0.0138 (13)−0.0009 (12)0.0031 (11)−0.0016 (11)
C120.0154 (15)0.0203 (15)0.0155 (14)−0.0012 (12)0.0059 (12)−0.0027 (11)
C130.0119 (14)0.0150 (13)0.0142 (13)0.0000 (11)0.0024 (11)0.0008 (11)
C140.0152 (15)0.0184 (14)0.0171 (14)0.0006 (12)0.0057 (12)0.0008 (11)
Ag1—O12.284 (2)O4—Ag2iii2.280 (3)
Ag1—N12.309 (3)N1—C51.348 (4)
Ag1—O2i2.323 (3)N1—C11.349 (4)
Ag1—O3ii2.844 (2)N2—C101.346 (4)
Ag1—O22.993 (3)N2—C61.359 (4)
Ag1—Ag1i3.0675 (9)C1—C21.377 (4)
Ag1—Ag23.1941 (7)C1—H10.9500
Ag2—O32.276 (2)C2—C31.382 (4)
Ag2—O4iii2.280 (3)C2—H20.9500
Ag2—N22.326 (3)C3—C41.396 (5)
Ag2—O1iv2.837 (2)C3—H30.9500
Ag2—O43.069 (3)C4—C51.394 (4)
Ag2—Ag2iii2.9687 (8)C4—H40.9500
F1—C121.348 (4)C5—C61.495 (4)
F2—C121.328 (4)C6—C71.391 (4)
F3—C121.333 (4)C7—C81.400 (5)
F4—C141.346 (4)C7—H70.9500
F5—C141.326 (4)C8—C91.385 (5)
F6—C141.333 (4)C8—H80.9500
O1—C111.254 (4)C9—C101.388 (4)
O2—C111.237 (4)C9—H90.9500
O2—Ag1i2.322 (3)C10—H100.9500
O3—C131.250 (4)C11—C121.550 (4)
O4—C131.250 (4)C13—C141.545 (4)
O1—Ag1—N1121.42 (9)C5—C4—C3119.1 (3)
O1—Ag1—O2i140.48 (9)C5—C4—H4120.5
N1—Ag1—O2i94.01 (9)C3—C4—H4120.5
O1—Ag1—Ag1i86.13 (5)N1—C5—C4121.9 (3)
N1—Ag1—Ag1i149.60 (7)N1—C5—C6117.7 (3)
O2i—Ag1—Ag1i65.77 (7)C4—C5—C6120.4 (3)
O1—Ag1—Ag2110.04 (6)N2—C6—C7121.6 (3)
N1—Ag1—Ag266.67 (7)N2—C6—C5117.0 (3)
O2i—Ag1—Ag299.26 (6)C7—C6—C5121.4 (3)
Ag1i—Ag1—Ag293.284 (12)C6—C7—C8119.6 (3)
O3—Ag2—O4iii143.51 (9)C6—C7—H7120.2
O3—Ag2—N2118.43 (9)C8—C7—H7120.2
O4iii—Ag2—N293.99 (10)C9—C8—C7118.4 (3)
O3—Ag2—Ag2iii85.12 (6)C9—C8—H8120.8
O4iii—Ag2—Ag2iii70.16 (7)C7—C8—H8120.8
N2—Ag2—Ag2iii151.77 (7)C8—C9—C10119.1 (3)
O3—Ag2—Ag1109.14 (6)C8—C9—H9120.5
O4iii—Ag2—Ag198.63 (6)C10—C9—H9120.5
N2—Ag2—Ag166.22 (7)N2—C10—C9123.0 (3)
Ag2iii—Ag2—Ag192.459 (12)N2—C10—H10118.5
C11—O1—Ag1107.24 (19)C9—C10—H10118.5
C11—O2—Ag1i131.1 (2)O2—C11—O1128.8 (3)
C13—O3—Ag2109.72 (19)O2—C11—C12115.3 (3)
C13—O4—Ag2iii127.5 (2)O1—C11—C12115.7 (3)
C5—N1—C1118.0 (3)F2—C12—F3107.7 (3)
C5—N1—Ag1126.7 (2)F2—C12—F1107.7 (3)
C1—N1—Ag1112.5 (2)F3—C12—F1106.1 (2)
C10—N2—C6118.3 (3)F2—C12—C11112.1 (2)
C10—N2—Ag2113.3 (2)F3—C12—C11113.1 (3)
C6—N2—Ag2123.9 (2)F1—C12—C11109.9 (3)
N1—C1—C2123.4 (3)O4—C13—O3129.3 (3)
N1—C1—H1118.3O4—C13—C14114.0 (3)
C2—C1—H1118.3O3—C13—C14116.7 (3)
C1—C2—C3118.7 (3)F5—C14—F6107.3 (3)
C1—C2—H2120.7F5—C14—F4106.7 (3)
C3—C2—H2120.7F6—C14—F4106.2 (3)
C2—C3—C4118.9 (3)F5—C14—C13113.3 (3)
C2—C3—H3120.5F6—C14—C13113.1 (3)
C4—C3—H3120.5F4—C14—C13109.7 (3)
O1—Ag1—Ag2—O3159.39 (8)C1—C2—C3—C40.3 (5)
N1—Ag1—Ag2—O342.84 (9)C2—C3—C4—C50.1 (5)
O2i—Ag1—Ag2—O3−47.55 (9)C1—N1—C5—C4−1.4 (4)
Ag1i—Ag1—Ag2—O3−113.53 (6)Ag1—N1—C5—C4158.2 (2)
O1—Ag1—Ag2—O4iii−44.62 (9)C1—N1—C5—C6178.3 (3)
N1—Ag1—Ag2—O4iii−161.18 (10)Ag1—N1—C5—C6−22.1 (4)
O2i—Ag1—Ag2—O4iii108.43 (9)C3—C4—C5—N10.5 (5)
Ag1i—Ag1—Ag2—O4iii42.45 (7)C3—C4—C5—C6−179.2 (3)
O1—Ag1—Ag2—N245.95 (9)C10—N2—C6—C7−2.5 (4)
N1—Ag1—Ag2—N2−70.61 (11)Ag2—N2—C6—C7152.2 (2)
O2i—Ag1—Ag2—N2−161.00 (10)C10—N2—C6—C5177.8 (3)
Ag1i—Ag1—Ag2—N2133.03 (8)Ag2—N2—C6—C5−27.5 (4)
O1—Ag1—Ag2—Ag2iii−114.92 (6)N1—C5—C6—N2−27.5 (4)
N1—Ag1—Ag2—Ag2iii128.52 (7)C4—C5—C6—N2152.2 (3)
O2i—Ag1—Ag2—Ag2iii38.13 (7)N1—C5—C6—C7152.8 (3)
Ag1i—Ag1—Ag2—Ag2iii−27.845 (17)C4—C5—C6—C7−27.5 (4)
N1—Ag1—O1—C11132.75 (19)N2—C6—C7—C81.3 (4)
O2i—Ag1—O1—C11−76.9 (2)C5—C6—C7—C8−179.0 (3)
Ag1i—Ag1—O1—C11−33.61 (19)C6—C7—C8—C90.7 (5)
Ag2—Ag1—O1—C1158.5 (2)C7—C8—C9—C10−1.5 (5)
O4iii—Ag2—O3—C13−78.8 (2)C6—N2—C10—C91.7 (5)
N2—Ag2—O3—C13131.3 (2)Ag2—N2—C10—C9−155.6 (3)
Ag2iii—Ag2—O3—C13−32.30 (19)C8—C9—C10—N20.3 (5)
Ag1—Ag2—O3—C1358.6 (2)Ag1i—O2—C11—O131.3 (5)
O1—Ag1—N1—C5−20.2 (3)Ag1i—O2—C11—C12−153.5 (2)
O2i—Ag1—N1—C5178.2 (2)Ag1—O1—C11—O215.3 (4)
Ag1i—Ag1—N1—C5132.1 (2)Ag1—O1—C11—C12−159.9 (2)
Ag2—Ag1—N1—C579.9 (2)O2—C11—C12—F227.9 (4)
O1—Ag1—N1—C1140.4 (2)O1—C11—C12—F2−156.2 (3)
O2i—Ag1—N1—C1−21.3 (2)O2—C11—C12—F3149.9 (3)
Ag1i—Ag1—N1—C1−67.4 (3)O1—C11—C12—F3−34.2 (4)
Ag2—Ag1—N1—C1−119.6 (2)O2—C11—C12—F1−91.8 (3)
O3—Ag2—N2—C10140.1 (2)O1—C11—C12—F184.1 (3)
O4iii—Ag2—N2—C10−22.5 (2)Ag2iii—O4—C13—O326.8 (5)
Ag2iii—Ag2—N2—C10−76.4 (3)Ag2iii—O4—C13—C14−156.6 (2)
Ag1—Ag2—N2—C10−120.2 (2)Ag2—O3—C13—O415.0 (4)
O3—Ag2—N2—C6−15.7 (3)Ag2—O3—C13—C14−161.6 (2)
O4iii—Ag2—N2—C6−178.3 (2)O4—C13—C14—F538.5 (4)
Ag2iii—Ag2—N2—C6127.8 (2)O3—C13—C14—F5−144.4 (3)
Ag1—Ag2—N2—C684.0 (2)O4—C13—C14—F6160.9 (3)
C5—N1—C1—C21.8 (5)O3—C13—C14—F6−22.0 (4)
Ag1—N1—C1—C2−160.6 (3)O4—C13—C14—F4−80.7 (3)
N1—C1—C2—C3−1.3 (5)O3—C13—C14—F496.5 (3)
D—H···AD—HH···AD···AD—H···A
C4—H4···O1v0.952.503.410 (4)159
C8—H8···O3vi0.952.583.287 (4)132
C1—H1···F6ii0.952.543.072 (4)116
C2—H2···F4vii0.952.553.145 (4)121
C10—H10···F3iv0.952.523.076 (4)117
Table 1

Selected bond lengths (Å)

Ag1—O12.284 (2)
Ag1—N12.309 (3)
Ag1—O2i2.323 (3)
Ag1—O3ii2.844 (2)
Ag1—O22.993 (3)
Ag1⋯Ag1i3.0675 (9)
Ag1⋯Ag23.1941 (7)
Ag2—O32.276 (2)
Ag2—O4iii2.280 (3)
Ag2—N22.326 (3)
Ag2—O1iv2.837 (2)
Ag2—O43.069 (3)
Ag2⋯Ag2iii2.9687 (8)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C4—H4⋯O1v0.952.503.410 (4)159
C8—H8⋯O3vi0.952.583.287 (4)132
C1—H1⋯F6ii0.952.543.072 (4)116
C2—H2⋯F4vii0.952.553.145 (4)121
C10—H10⋯F3iv0.952.523.076 (4)117

Symmetry codes: (ii) ; (iv) ; (v) ; (vi) ; (vii) .

  2 in total

1.  A short history of SHELX.

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

2.  Poly[[bis-[μ(2)-N,N'-bis-(2-pyridyl-meth-yl)oxalamide-κN,O:N',O'][μ(2)-N,N'-bis-(2-pyridyl-meth-yl)oxalamide-κN:N']disilver(I)] bis-(trifluoro-methane-sulfonate)].

Authors:  Hadi D Arman; Tyler Miller; Pavel Poplaukhin; Edward R T Tiekink
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-08-28
  2 in total

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