Literature DB >> 22219756

catena-Poly[[tris[silver(I)-μ-4,4'-bi-pyridine-κN:N']] tris-(perchlorate) di-hydrate].

Xiao-Ming Hu1, Fu-An Li.   

Abstract

In the title compound, {[Ag(3)(C(10)H(8)N(2))(3)](ClO(4))(3)·2H(2)O}(n), one of the Ag(I) ions, one of the 4,4'-bipyridine (bipy) ligands and one of the perchlorate anions are each situated on a twofold rotation axis. Each Ag(I) ion is coordinated by two N atoms from two bridging bipy ligands, forming chains along [101]. π-π inter-actions between the pyridine rings [centroid-centroid distances = 3.638 (8) and 3.688 (8) Å] connect the chains. Inter-molecular O-H⋯O hydrogen bonds link the uncoord-inated water mol-ecules and the perchlorate anions.

Entities:  

Year:  2011        PMID: 22219756      PMCID: PMC3246936          DOI: 10.1107/S1600536811040153

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


Related literature

For background to the network topologies and applications of coordination polymers, see: Du et al. (2007 ▶); Hu et al. (2003 ▶); Lou et al. (2005 ▶); Maspoch et al. (2007 ▶); Ockwig et al. (2005 ▶); Xiao et al. (2006 ▶). For O—H⋯O hydrogen bonds, see: Desiraju (2004 ▶). For π–π inter­actions, see: Zang et al. (2010 ▶).

Experimental

Crystal data

[Ag3(C10H8N2)3](ClO4)3·2H2O M = 1126.54 Monoclinic, a = 21.259 (2) Å b = 15.7647 (17) Å c = 20.949 (3) Å β = 148.768 (5)° V = 3640.4 (9) Å3 Z = 4 Mo Kα radiation μ = 1.90 mm−1 T = 296 K 0.21 × 0.20 × 0.19 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.692, T max = 0.715 7095 measured reflections 3145 independent reflections 2229 reflections with I > 2σ(I) R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.062 wR(F 2) = 0.170 S = 1.01 3145 reflections 254 parameters H-atom parameters constrained Δρmax = 1.87 e Å−3 Δρmin = −1.07 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811040153/hy2472sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811040153/hy2472Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag3(C10H8N2)3](ClO4)3·2H2OF(000) = 2216
Mr = 1126.54Dx = 2.056 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2263 reflections
a = 21.259 (2) Åθ = 3.1–29.0°
b = 15.7647 (17) ŵ = 1.90 mm1
c = 20.949 (3) ÅT = 296 K
β = 148.768 (5)°Block, colorless
V = 3640.4 (9) Å30.21 × 0.20 × 0.19 mm
Z = 4
Bruker APEXII CCD diffractometer3145 independent reflections
Radiation source: fine-focus sealed tube2229 reflections with I > 2σ(I)
graphiteRint = 0.037
φ and ω scansθmax = 25.0°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −25→25
Tmin = 0.692, Tmax = 0.715k = −12→18
7095 measured reflectionsl = −23→24
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.170H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0911P)2] where P = (Fo2 + 2Fc2)/3
3145 reflections(Δ/σ)max = 0.001
254 parametersΔρmax = 1.87 e Å3
0 restraintsΔρmin = −1.07 e Å3
xyzUiso*/Ueq
Ag10.00000.45375 (5)−0.25000.0566 (3)
Ag20.59795 (4)0.05250 (4)0.68999 (4)0.0558 (3)
O10.9612 (11)0.3396 (11)0.2576 (10)0.320 (11)
O21.0878 (12)0.2447 (7)0.3549 (11)0.225 (6)
O30.2999 (8)0.2382 (7)0.1888 (9)0.183 (5)
O40.4471 (17)0.2642 (6)0.3825 (14)0.279 (8)
O50.4822 (10)0.2063 (8)0.3197 (13)0.240 (6)
O60.3993 (6)0.1309 (6)0.3237 (6)0.147 (3)
O1W0.1272 (4)0.2966 (4)0.1401 (5)0.0789 (16)
H1WB0.07980.27510.07130.118*
H1WA0.20000.27880.20160.118*
N10.1878 (5)0.4546 (3)−0.0596 (5)0.0465 (14)
N20.4098 (5)0.0531 (3)0.4983 (5)0.0404 (12)
N3−0.2117 (4)0.0492 (3)−0.1224 (5)0.0410 (13)
C10.2488 (6)0.5264 (4)−0.0009 (6)0.0390 (14)
H10.20810.5774−0.04240.047*
C20.3715 (6)0.5285 (4)0.1205 (6)0.0386 (14)
H20.41150.58030.15820.046*
C30.4347 (5)0.4539 (4)0.1856 (5)0.0318 (13)
C40.3680 (6)0.3788 (4)0.1220 (7)0.0522 (17)
H40.40530.32660.16120.063*
C50.2469 (6)0.3825 (5)0.0010 (6)0.0560 (19)
H50.20440.3319−0.04020.067*
C60.3549 (6)−0.0171 (4)0.4321 (6)0.0480 (16)
H60.3989−0.06750.47060.058*
C70.2379 (5)−0.0197 (4)0.3112 (5)0.0459 (16)
H70.2051−0.07030.26790.055*
C80.1676 (5)0.0518 (3)0.2521 (5)0.0295 (13)
C90.2230 (6)0.1252 (4)0.3215 (6)0.0461 (16)
H90.17920.17550.28620.055*
C100.3441 (6)0.1232 (4)0.4441 (6)0.0524 (17)
H100.38050.17290.49000.063*
C110.0359 (5)0.0509 (3)0.1213 (5)0.0279 (12)
C12−0.0267 (5)−0.0238 (4)0.0584 (5)0.0318 (13)
H120.0135−0.07540.09710.038*
C13−0.1494 (5)−0.0225 (4)−0.0625 (5)0.0382 (14)
H13−0.1898−0.0737−0.10320.046*
C14−0.1510 (6)0.1215 (4)−0.0627 (6)0.0534 (18)
H14−0.19260.1725−0.10330.064*
C15−0.0293 (5)0.1237 (4)0.0570 (6)0.0490 (17)
H150.00940.17590.09480.059*
Cl11.00000.28764 (14)0.25000.0493 (6)
Cl20.41235 (16)0.21081 (11)0.30907 (16)0.0539 (5)
U11U22U33U12U13U23
Ag10.0280 (4)0.0644 (6)0.0340 (5)0.0000.0197 (4)0.000
Ag20.0251 (3)0.0706 (5)0.0256 (3)0.0006 (2)0.0144 (3)0.0007 (2)
O10.233 (13)0.47 (2)0.132 (8)0.233 (16)0.137 (10)0.076 (12)
O20.310 (15)0.146 (9)0.195 (10)0.143 (9)0.212 (11)0.116 (7)
O30.136 (6)0.223 (12)0.165 (8)0.107 (8)0.125 (7)0.141 (8)
O40.51 (2)0.090 (7)0.279 (15)−0.072 (11)0.343 (19)−0.066 (9)
O50.218 (9)0.225 (13)0.388 (15)0.090 (10)0.277 (12)0.107 (12)
O60.101 (5)0.110 (7)0.090 (5)−0.024 (5)0.060 (5)0.013 (4)
O1W0.069 (3)0.069 (4)0.076 (4)0.002 (3)0.058 (3)0.003 (3)
N10.033 (3)0.048 (4)0.035 (3)0.002 (2)0.025 (3)0.002 (3)
N20.027 (3)0.040 (3)0.032 (3)0.000 (2)0.022 (3)0.003 (2)
N30.017 (2)0.051 (4)0.020 (3)0.001 (2)0.010 (2)0.006 (2)
C10.037 (3)0.034 (3)0.039 (3)−0.001 (3)0.032 (3)−0.003 (3)
C20.042 (3)0.030 (3)0.038 (3)0.001 (3)0.033 (3)−0.001 (3)
C30.027 (3)0.041 (4)0.030 (3)0.000 (2)0.024 (3)0.000 (3)
C40.040 (3)0.031 (4)0.051 (4)0.000 (3)0.033 (3)0.001 (3)
C50.043 (4)0.042 (4)0.043 (4)−0.006 (4)0.030 (4)−0.007 (4)
C60.035 (3)0.043 (4)0.034 (3)0.012 (3)0.024 (3)0.004 (3)
C70.032 (3)0.043 (4)0.027 (3)0.003 (3)0.019 (3)−0.006 (3)
C80.023 (3)0.033 (3)0.023 (3)−0.002 (2)0.018 (3)0.000 (2)
C90.038 (3)0.023 (3)0.039 (4)−0.007 (3)0.027 (3)−0.001 (3)
C100.034 (3)0.037 (4)0.037 (4)−0.009 (3)0.022 (3)−0.006 (3)
C110.022 (3)0.028 (3)0.019 (3)−0.004 (2)0.015 (3)−0.002 (2)
C120.024 (3)0.031 (3)0.029 (3)0.005 (2)0.020 (3)0.003 (3)
C130.026 (3)0.041 (3)0.022 (3)−0.004 (3)0.017 (3)−0.007 (3)
C140.029 (3)0.035 (4)0.027 (3)0.004 (3)0.013 (3)0.010 (3)
C150.036 (3)0.031 (4)0.029 (3)−0.004 (3)0.020 (3)0.005 (3)
Cl10.0637 (15)0.0265 (11)0.0578 (15)0.0000.0520 (14)0.000
Cl20.0567 (11)0.0389 (9)0.0568 (11)0.0052 (8)0.0470 (10)0.0060 (8)
Ag1—N12.149 (6)C3—C41.400 (8)
Ag1—N1i2.149 (6)C3—C3iii1.475 (12)
Ag2—N3ii2.151 (5)C4—C51.378 (10)
Ag2—N22.158 (6)C4—H40.9300
O1—Cl11.27 (3)C5—H50.9300
O2—Cl11.325 (9)C6—C71.353 (8)
O3—Cl21.396 (8)C6—H60.9300
O4—Cl21.295 (10)C7—C81.368 (8)
O5—Cl21.30 (3)C7—H70.9300
O6—Cl21.379 (8)C8—C91.383 (8)
O1W—H1WB0.8500C8—C111.492 (8)
O1W—H1WA0.8500C9—C101.385 (9)
N1—C11.323 (8)C9—H90.9300
N1—C51.324 (9)C10—H100.9300
N2—C61.320 (8)C11—C151.364 (8)
N2—C101.323 (8)C11—C121.377 (8)
N3—C131.328 (8)C12—C131.386 (7)
N3—C141.329 (8)C12—H120.9300
C1—C21.389 (9)C13—H130.9300
C1—H10.9300C14—C151.374 (8)
C2—C31.383 (8)C14—H140.9300
C2—H20.9300C15—H150.9300
N1—Ag1—N1i179.3 (3)C9—C8—C11120.8 (5)
N3ii—Ag2—N2176.36 (19)C8—C9—C10119.5 (6)
H1WB—O1W—H1WA115.0C8—C9—H9120.3
C1—N1—C5118.1 (6)C10—C9—H9120.3
C1—N1—Ag1121.3 (4)N2—C10—C9122.4 (6)
C5—N1—Ag1120.5 (5)N2—C10—H10118.8
C6—N2—C10117.6 (6)C9—C10—H10118.8
C6—N2—Ag2121.2 (4)C15—C11—C12116.1 (6)
C10—N2—Ag2121.1 (4)C15—C11—C8122.1 (5)
C13—N3—C14117.3 (5)C12—C11—C8121.7 (5)
C13—N3—Ag2iv123.0 (4)C11—C12—C13120.3 (6)
C14—N3—Ag2iv119.7 (4)C11—C12—H12119.9
N1—C1—C2122.4 (6)C13—C12—H12119.9
N1—C1—H1118.8N3—C13—C12122.5 (6)
C2—C1—H1118.8N3—C13—H13118.7
C3—C2—C1120.4 (6)C12—C13—H13118.7
C3—C2—H2119.8N3—C14—C15122.5 (6)
C1—C2—H2119.8N3—C14—H14118.8
C2—C3—C4116.2 (6)C15—C14—H14118.8
C2—C3—C3iii121.7 (4)C11—C15—C14121.2 (6)
C4—C3—C3iii122.1 (4)C11—C15—H15119.4
C5—C4—C3119.6 (6)C14—C15—H15119.4
C5—C4—H4120.2O1v—Cl1—O199.3 (17)
C3—C4—H4120.2O1v—Cl1—O2v105.5 (7)
N1—C5—C4123.3 (6)O1—Cl1—O2v113.2 (9)
N1—C5—H5118.4O1v—Cl1—O2113.2 (9)
C4—C5—H5118.4O1—Cl1—O2105.5 (7)
N2—C6—C7123.4 (6)O2v—Cl1—O2118.6 (12)
N2—C6—H6118.3O4—Cl2—O5115.0 (10)
C7—C6—H6118.3O4—Cl2—O6110.4 (7)
C6—C7—C8120.5 (6)O5—Cl2—O6109.2 (6)
C6—C7—H7119.8O4—Cl2—O3107.5 (9)
C8—C7—H7119.8O5—Cl2—O3105.6 (7)
C7—C8—C9116.7 (6)O6—Cl2—O3108.9 (5)
C7—C8—C11122.5 (5)
C5—N1—C1—C20.5 (10)C6—N2—C10—C9−2.1 (10)
Ag1—N1—C1—C2−177.1 (4)Ag2—N2—C10—C9−179.5 (5)
N1—C1—C2—C3−0.8 (9)C8—C9—C10—N2−0.1 (10)
C1—C2—C3—C40.2 (9)C7—C8—C11—C15−169.4 (6)
C1—C2—C3—C3iii179.6 (6)C9—C8—C11—C1514.1 (9)
C2—C3—C4—C50.8 (10)C7—C8—C11—C1210.0 (9)
C3iii—C3—C4—C5−178.7 (7)C9—C8—C11—C12−166.5 (5)
C1—N1—C5—C40.5 (11)C15—C11—C12—C13−1.4 (8)
Ag1—N1—C5—C4178.1 (6)C8—C11—C12—C13179.1 (5)
C3—C4—C5—N1−1.1 (11)C14—N3—C13—C121.3 (9)
C10—N2—C6—C74.0 (10)Ag2iv—N3—C13—C12179.9 (4)
Ag2—N2—C6—C7−178.7 (5)C11—C12—C13—N3−0.1 (9)
N2—C6—C7—C8−3.6 (11)C13—N3—C14—C15−1.0 (10)
C6—C7—C8—C91.2 (9)Ag2iv—N3—C14—C15−179.7 (5)
C6—C7—C8—C11−175.4 (6)C12—C11—C15—C141.7 (9)
C7—C8—C9—C100.5 (9)C8—C11—C15—C14−178.8 (6)
C11—C8—C9—C10177.2 (6)N3—C14—C15—C11−0.5 (11)
D—H···AD—HH···AD···AD—H···A
O1W—H1WB···O4vi0.852.213.060 (15)173
O1W—H1WA···O30.852.442.99 (3)123
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O1W—H1WB⋯O4i0.852.213.060 (15)173
O1W—H1WA⋯O30.852.442.99 (3)123

Symmetry code: (i) .

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