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The title compound, [Ag(C5H6N2)2]ClO4, is a mononuclear silver(I) complex. The Ag atom, lying on a twofold rotation axis, is bicoordinated in a distorted linear configuration by two N atoms from two symmetry-related 2-amino­pyridine ligands. The perchlorate ion is disordered across a crystallographic mirror plane. The cations and anions are arranged as alternating layers along the a axis and are interlinked by weak N—H...O interactions in addition to the electrostatic interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804022780/ci6443sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804022780/ci6443Isup2.hkl
Contains datablock I

CCDC reference: 252776

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.011 Å
  • Disorder in solvent or counterion
  • R factor = 0.055
  • wR factor = 0.174
  • Data-to-parameter ratio = 11.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O2 PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O2' PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for O2' PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for O3 PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for O3' PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for O2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 38.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O3 PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O3' PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A .. O1 .. 2.65 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Bis(2-aminopyridine-κN1)silver(I) perchlorate top
Crystal data top
[Ag(C5H6N2)2]ClO4F(000) = 1568
Mr = 395.56Dx = 1.940 Mg m3
Orthorhombic, CmcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2bc 2Cell parameters from 1237 reflections
a = 12.720 (4) Åθ = 2.5–25°
b = 9.810 (3) ŵ = 1.70 mm1
c = 21.710 (7) ÅT = 298 K
V = 2709.0 (15) Å3Prism, colourless
Z = 80.22 × 0.15 × 0.13 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
1241 independent reflections
Radiation source: fine-focus sealed tube964 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
φ and ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 915
Tmin = 0.706, Tmax = 0.809k = 1111
5599 measured reflectionsl = 2525
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.055H-atom parameters constrained
wR(F2) = 0.174 w = 1/[σ2(Fo2) + (0.1098P)2 + 2.440P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
1241 reflectionsΔρmax = 1.13 e Å3
112 parametersΔρmin = 0.75 e Å3
29 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0065 (8)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ag10.15153 (5)0.00000.50000.0887 (5)
Cl10.00000.33614 (18)0.60297 (8)0.0552 (6)
N10.1489 (3)0.0955 (5)0.4121 (2)0.0623 (13)
N20.1512 (4)0.3121 (6)0.4534 (2)0.0730 (15)
H2A0.15520.27770.48980.088*
H2B0.15000.39910.44870.088*
C10.1469 (4)0.2293 (6)0.4036 (3)0.0541 (13)
C20.1409 (4)0.2844 (6)0.3452 (3)0.0630 (16)
H20.13820.37850.34010.076*
C30.1387 (5)0.2020 (8)0.2957 (3)0.0771 (19)
H30.13420.23850.25630.093*
C40.1433 (5)0.0626 (9)0.3041 (4)0.085 (2)
H40.14330.00300.27080.103*
C50.1477 (4)0.0164 (7)0.3625 (5)0.076 (2)
H50.15000.07750.36840.091*
O10.00000.2173 (6)0.5667 (3)0.097 (2)
O20.00000.4518 (10)0.5659 (5)0.076 (3)0.50
O30.0901 (11)0.3432 (15)0.6404 (7)0.137 (5)0.50
O2'0.00000.299 (2)0.6642 (4)0.114 (5)0.50
O3'0.0983 (10)0.3912 (18)0.5895 (8)0.149 (5)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0885 (7)0.0870 (8)0.0906 (7)0.0000.0000.0454 (4)
Cl10.0653 (12)0.0495 (11)0.0507 (10)0.0000.0000.0041 (8)
N10.059 (3)0.057 (3)0.071 (3)0.003 (2)0.010 (2)0.016 (3)
N20.093 (4)0.066 (3)0.061 (3)0.010 (3)0.005 (2)0.005 (3)
C10.044 (3)0.059 (3)0.060 (3)0.003 (2)0.006 (2)0.011 (3)
C20.064 (4)0.062 (4)0.062 (3)0.003 (3)0.003 (2)0.017 (3)
C30.080 (4)0.094 (5)0.057 (4)0.006 (4)0.001 (3)0.012 (4)
C40.089 (5)0.084 (5)0.083 (5)0.012 (4)0.010 (3)0.010 (4)
C50.074 (4)0.059 (4)0.095 (6)0.011 (3)0.016 (3)0.008 (4)
O10.156 (7)0.048 (4)0.087 (4)0.0000.0000.002 (3)
O20.119 (8)0.039 (5)0.070 (6)0.0000.0000.014 (5)
O30.133 (8)0.136 (9)0.142 (8)0.016 (7)0.061 (7)0.004 (7)
O2'0.138 (10)0.143 (10)0.062 (6)0.0000.0000.003 (7)
O3'0.144 (8)0.157 (9)0.147 (9)0.057 (8)0.025 (7)0.023 (8)
Geometric parameters (Å, º) top
Ag1—N12.126 (5)N2—C11.352 (8)
Ag1—N1i2.126 (5)N2—H2A0.86
Cl1—O2'1.378 (9)N2—H2B0.86
Cl1—O21.390 (8)C1—C21.381 (8)
Cl1—O3'ii1.394 (9)C2—C31.345 (9)
Cl1—O3'1.394 (9)C2—H20.93
Cl1—O11.407 (6)C3—C41.381 (12)
Cl1—O31.407 (8)C3—H30.93
Cl1—O3ii1.407 (8)C4—C51.346 (13)
N1—C11.326 (8)C4—H40.93
N1—C51.329 (10)C5—H50.93
N1—Ag1—N1i178.2 (2)C1—N1—C5117.7 (6)
O2'—Cl1—O2140.7 (10)C1—N1—Ag1124.2 (4)
O2'—Cl1—O3'ii107.8 (8)C5—N1—Ag1118.1 (4)
O2—Cl1—O3'ii64.0 (8)C1—N2—H2A120.0
O2'—Cl1—O3'107.8 (8)C1—N2—H2B120.0
O2—Cl1—O3'64.0 (8)H2A—N2—H2B120.0
O3'ii—Cl1—O3'127.7 (17)N1—C1—N2118.9 (5)
O2'—Cl1—O1108.7 (9)N1—C1—C2121.1 (6)
O2—Cl1—O1110.7 (6)N2—C1—C2120.0 (5)
O3'ii—Cl1—O1101.7 (7)C3—C2—C1119.9 (6)
O3'—Cl1—O1101.7 (7)C3—C2—H2120.0
O2'—Cl1—O357.0 (8)C1—C2—H2120.0
O2—Cl1—O3107.1 (7)C2—C3—C4119.3 (7)
O3'ii—Cl1—O3146.5 (9)C2—C3—H3120.4
O3'—Cl1—O351.1 (8)C4—C3—H3120.4
O1—Cl1—O3111.3 (7)C5—C4—C3117.4 (8)
O2'—Cl1—O3ii57.0 (8)C5—C4—H4121.3
O2—Cl1—O3ii107.1 (7)C3—C4—H4121.3
O3'ii—Cl1—O3ii51.1 (8)N1—C5—C4124.5 (7)
O3'—Cl1—O3ii146.5 (9)N1—C5—H5117.7
O1—Cl1—O3ii111.3 (7)C4—C5—H5117.7
O3—Cl1—O3ii109.1 (16)
C5—N1—C1—N2178.1 (5)C1—C2—C3—C40.4 (9)
Ag1—N1—C1—N22.9 (7)C2—C3—C4—C51.2 (10)
C5—N1—C1—C21.7 (7)C1—N1—C5—C40.8 (9)
Ag1—N1—C1—C2177.2 (4)Ag1—N1—C5—C4178.2 (5)
N1—C1—C2—C31.2 (8)C3—C4—C5—N10.7 (10)
N2—C1—C2—C3178.7 (5)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···O30.862.543.128 (16)126
N2—H2A···O10.862.653.259 (8)128
N2—H2B···O3iii0.862.313.130 (17)159
N2—H2B···O2iv0.862.433.041 (9)129
Symmetry codes: (iii) x, y+1, z+1; (iv) x, y+1, z+1.
 

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