Literature DB >> 21587457

catena-Poly[[silver(I)-μ-4-aminopyridine] perchlorate]: a 1-D staircase coordination polymer.

Ryan K Golder1, Christopher M Fitchett, Jan L Wikaira, Peter J Steel.   

Abstract

Reaction of 4-amino-pyridine with silver(I) perchlorate leads to a one-dimensional coordination polymer, {[Ag(C(5)H(6)N(2))]ClO(4)}(n), in which the amino-pyridine binds through both N atoms. The perchlorate anion is hydrogen bonded to the amino H atoms and inter-acts weakly with the silver(I) atoms (Ag-O > 2.70 Å), both located on inversion centres, and some aromatic H atoms (O-H > 2.55 ÅA), thereby extending the dimensionality of the assembly. This is the first silver complex in which this ligand acts in a bridging mode.

Entities:  

Year:  2010        PMID: 21587457      PMCID: PMC2983413          DOI: 10.1107/S1600536810037682

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


Related literature

For discrete silver complexes of the same ligand, see: Kristian­sson (2000 ▶); Abu-Youssef et al. (2006 ▶); Liu et al. (2005 ▶); Zhu et al. (2003a ▶,b ▶); Li et al. (2005 ▶); Ma et al. (2004 ▶). For metallosupra­molecular assemblies derived from bridging heterocyclic ligands, see: Steel (2005 ▶). For the use of silver(I) for the self-assembly of both discrete and polymeric aggregates with diverse mol­ecular architectures, see: Fitchett & Steel (2006 ▶); O’Keefe & Steel (2007 ▶). For a review of the use of pyrazine and analogues as bridging ligands for silver(I)-based assemblies, see: Steel & Fitchett (2008 ▶).

Experimental

Crystal data

[Ag(C5H6N2)]ClO4 M = 301.44 Triclinic, a = 5.0720 (2) Å b = 9.0025 (3) Å c = 9.5520 (3) Å α = 93.198 (2)° β = 96.992 (2)° γ = 100.452 (2)° V = 424.37 (3) Å3 Z = 2 Mo Kα radiation μ = 2.67 mm−1 T = 113 K 0.35 × 0.11 × 0.05 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T min = 0.455, T max = 0.878 9107 measured reflections 1740 independent reflections 1591 reflections with I > 2σ(I) R int = 0.046

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.051 S = 1.03 1740 reflections 127 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.57 e Å−3 Δρmin = −0.78 e Å−3 Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810037682/bv2161sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810037682/bv2161Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag(C5H6N2)]ClO4Z = 2
Mr = 301.44F(000) = 292
Triclinic, P1Dx = 2.359 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 5.0720 (2) ÅCell parameters from 6232 reflections
b = 9.0025 (3) Åθ = 3.0–26.4°
c = 9.5520 (3) ŵ = 2.67 mm1
α = 93.198 (2)°T = 113 K
β = 96.992 (2)°Prism, orange
γ = 100.452 (2)°0.35 × 0.11 × 0.05 mm
V = 424.37 (3) Å3
Bruker APEXII CCD diffractometer1740 independent reflections
Radiation source: fine-focus sealed tube1591 reflections with I > 2σ(I)
graphiteRint = 0.046
φ and ω scansθmax = 26.4°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2009)h = −6→6
Tmin = 0.455, Tmax = 0.878k = −11→11
9107 measured reflectionsl = −11→11
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051H atoms treated by a mixture of independent and constrained refinement
S = 1.03w = 1/[σ2(Fo2) + (0.0333P)2 + 0.1489P] where P = (Fo2 + 2Fc2)/3
1740 reflections(Δ/σ)max = 0.017
127 parametersΔρmax = 0.57 e Å3
0 restraintsΔρmin = −0.78 e Å3
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
Ag10.00000.00000.50000.02748 (9)
Ag20.5000−0.50000.00000.02716 (9)
Cl1−0.04375 (9)−0.70217 (6)0.19452 (5)0.02471 (12)
O1−0.0156 (4)−0.81713 (18)0.08849 (17)0.0372 (4)
O20.0718 (4)−0.7384 (2)0.32954 (17)0.0405 (4)
O30.0969 (3)−0.55690 (18)0.16137 (19)0.0338 (4)
O4−0.3233 (3)−0.6953 (2)0.1977 (2)0.0530 (6)
N10.2684 (3)−0.10407 (19)0.38878 (18)0.0212 (3)
C20.3565 (4)−0.2298 (2)0.4306 (2)0.0253 (4)
H2A0.3003−0.27100.51390.030*
C30.5233 (4)−0.3006 (2)0.3584 (2)0.0245 (4)
H3A0.5804−0.38860.39170.029*
C40.6080 (4)−0.2422 (2)0.2358 (2)0.0187 (4)
C50.5244 (4)−0.1101 (2)0.1946 (2)0.0224 (4)
H5A0.5824−0.06470.11340.027*
C60.3576 (4)−0.0467 (2)0.2725 (2)0.0246 (4)
H6A0.30170.04300.24270.030*
N20.7619 (3)−0.3164 (2)0.15325 (19)0.0218 (3)
H2B0.874 (5)−0.362 (3)0.199 (3)0.026*
H2C0.845 (5)−0.259 (3)0.097 (3)0.026*
U11U22U33U12U13U23
Ag10.01995 (12)0.03359 (15)0.02912 (14)0.00871 (9)0.00516 (9)−0.01157 (10)
Ag20.02874 (13)0.02542 (14)0.02684 (14)0.00551 (9)0.00580 (9)−0.00782 (9)
Cl10.0227 (2)0.0299 (3)0.0266 (3)0.01105 (19)0.00968 (18)0.0130 (2)
O10.0491 (10)0.0312 (9)0.0296 (9)0.0013 (7)0.0083 (7)0.0022 (7)
O20.0520 (10)0.0550 (11)0.0238 (8)0.0281 (9)0.0100 (7)0.0138 (8)
O30.0347 (8)0.0259 (8)0.0473 (10)0.0105 (6)0.0211 (7)0.0102 (7)
O40.0238 (9)0.0665 (13)0.0815 (15)0.0196 (8)0.0229 (9)0.0445 (12)
N10.0193 (8)0.0232 (8)0.0211 (8)0.0061 (6)0.0032 (6)−0.0055 (7)
C20.0309 (11)0.0270 (11)0.0197 (10)0.0059 (8)0.0089 (8)0.0023 (8)
C30.0322 (11)0.0224 (10)0.0225 (10)0.0112 (8)0.0075 (8)0.0045 (8)
C40.0167 (9)0.0202 (9)0.0183 (9)0.0031 (7)0.0015 (7)−0.0025 (7)
C50.0276 (10)0.0207 (10)0.0204 (10)0.0058 (8)0.0063 (8)0.0037 (8)
C60.0270 (10)0.0209 (10)0.0269 (11)0.0088 (8)0.0020 (8)0.0000 (8)
N20.0212 (8)0.0233 (9)0.0227 (9)0.0069 (7)0.0072 (7)0.0004 (7)
Ag1—N12.1363 (16)C2—H2A0.9500
Ag1—N1i2.1363 (16)C3—C41.393 (3)
Ag2—N2ii2.2582 (18)C3—H3A0.9500
Ag2—N22.2583 (18)C4—C51.394 (3)
Cl1—O21.4301 (16)C4—N21.399 (3)
Cl1—O41.4344 (16)C5—C61.371 (3)
Cl1—O31.4430 (16)C5—H5A0.9500
Cl1—O11.4454 (17)C6—H6A0.9500
N1—C61.344 (3)N2—H2B0.85 (3)
N1—C21.353 (3)N2—H2C0.86 (3)
C2—C31.373 (3)
N1—Ag1—N1i180.00 (5)C4—C3—H3A120.3
N2ii—Ag2—N2180.0C5—C4—C3117.63 (18)
O2—Cl1—O4109.54 (11)C5—C4—N2120.84 (18)
O2—Cl1—O3109.91 (12)C3—C4—N2121.47 (18)
O4—Cl1—O3108.88 (10)C6—C5—C4119.20 (19)
O2—Cl1—O1108.65 (11)C6—C5—H5A120.4
O4—Cl1—O1110.77 (13)C4—C5—H5A120.4
O3—Cl1—O1109.08 (10)N1—C6—C5123.77 (19)
C6—N1—C2116.76 (17)N1—C6—H6A118.1
C6—N1—Ag1120.93 (13)C5—C6—H6A118.1
C2—N1—Ag1122.31 (13)C4—N2—Ag2111.91 (12)
N1—C2—C3123.15 (19)C4—N2—H2B115.5 (17)
N1—C2—H2A118.4Ag2—N2—H2B104.1 (17)
C3—C2—H2A118.4C4—N2—H2C113.7 (17)
C2—C3—C4119.45 (19)Ag2—N2—H2C101.4 (17)
C2—C3—H3A120.3H2B—N2—H2C109 (2)
D—H···AD—HH···AD···AD—H···A
N2—H2C···O1ii0.86 (3)2.16 (3)2.984 (3)161 (2)
N2—H2B···O3iii0.85 (3)2.29 (3)2.984 (3)139 (2)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
N2—H2C⋯O1i0.86 (3)2.16 (3)2.984 (3)161 (2)
N2—H2B⋯O3ii0.85 (3)2.29 (3)2.984 (3)139 (2)

Symmetry codes: (i) ; (ii) .

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