Literature DB >> 21580908

Bis[μ-2-(3-pyridylmeth-yl)-2H-benzo-triazole]bis-[nitratosilver(I)].

Min Hu1, Song-Tao Ma, Liang-Qi Guo, Guang-Hui Sun, Shao-Ming Fang.   

Abstract

In the title centrosymmetric binuclear Ag(I) complex, [Ag(2)(NO(3))(2)(C(12)H(10)N(4))(2)], each Ag(I) center is coordinated by one pyridine and one benzotriazole N-donor atom of two inversion-related 2-(3-pyridylmeth-yl)-2H-benzotriazole (L) ligands, and an O atom of a coordinated NO(3) (-) anion in a distorted T-shaped geometry. This forms a unique box-like cyclic dimer with an intra-molecular non-bonding Ag⋯Ag separation of 6.327 (2) Å. Weak inter-molecular Ag⋯O(nitrate) inter-actions [2.728 (4) and 2.646 (3) Å] link the binuclear units, forming a two-dimensional network parallel to (100). Inter-molecular C-H⋯O hydrogen-bonding inter-actions, involving the L ligands and the coordinated NO(3) (-) anions, link the sheets, forming a three-dimensional framework.

Entities:  

Year:  2008        PMID： 21580908      PMCID： PMC2959521          DOI： 10.1107/S160053680803479X

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


Related literature

For similar structures, see: Liu et al. (2006 ▶, 2007 ▶); Richardson & Steel (2003 ▶); For the synthesis of ligand L, see: Liu et al. (2008 ▶).

Experimental

Crystal data

[Ag2(NO3)2(C12H10N4)2] M = 760.24 Monoclinic, a = 10.472 (2) Å b = 8.6921 (17) Å c = 14.656 (3) Å β = 95.33 (3)° V = 1328.3 (5) Å3 Z = 2 Mo Kα radiation μ = 1.54 mm−1 T = 293 (2) K 0.20 × 0.15 × 0.11 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2008 ▶) T min = 0.749, T max = 0.849 12799 measured reflections 2336 independent reflections 2256 reflections with I > 2σ(I) R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.072 S = 1.11 2335 reflections 190 parameters H-atom parameters constrained Δρmax = 0.96 e Å−3 Δρmin = −0.70 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); 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 and PLATON (Spek, 2003 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680803479X/su2070sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680803479X/su2070Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag2(NO3)2(C12H10N4)2]F(000) = 752
Mr = 760.24Dx = 1.901 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4027 reflections
a = 10.472 (2) Åθ = 2.3–28.0°
b = 8.6921 (17) ŵ = 1.54 mm−1
c = 14.656 (3) ÅT = 293 K
β = 95.33 (3)°Block, yellow
V = 1328.3 (5) Å30.20 × 0.15 × 0.11 mm
Z = 2
Bruker SMART CCD area-detector diffractometer2336 independent reflections
Radiation source: fine-focus sealed tube2256 reflections with I > 2σ(I)
graphiteRint = 0.027
φ and ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)h = −12→12
Tmin = 0.749, Tmax = 0.849k = −10→10
12799 measured reflectionsl = −17→17
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072H-atom parameters constrained
S = 1.11w = 1/[σ2(Fo2) + (0.0212P)2 + 2.3034P] where P = (Fo2 + 2Fc2)/3
2335 reflections(Δ/σ)max < 0.001
190 parametersΔρmax = 0.96 e Å−3
0 restraintsΔρmin = −0.70 e Å−3
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
Ag10.44311 (3)0.21531 (4)0.62448 (2)0.05524 (13)
C10.6409 (3)0.4663 (4)0.5666 (2)0.0383 (8)
H10.60920.51970.61460.046*
C20.7353 (3)0.5350 (4)0.5209 (2)0.0377 (7)
C30.7781 (4)0.4566 (5)0.4484 (3)0.0568 (10)
H30.84120.49900.41550.068*
C40.7268 (5)0.3148 (5)0.4249 (3)0.0656 (12)
H40.75370.26130.37520.079*
C50.6361 (4)0.2536 (4)0.4753 (3)0.0527 (10)
H50.60340.15660.45990.063*
C60.7883 (4)0.6881 (4)0.5539 (2)0.0485 (9)
H610.72020.74830.57690.058*
H620.85380.67150.60430.058*
C70.9795 (3)0.8736 (4)0.4051 (2)0.0407 (8)
C81.0899 (4)0.9289 (5)0.3673 (3)0.0568 (10)
H81.17190.90700.39400.068*
C91.0709 (4)1.0148 (5)0.2908 (3)0.0590 (11)
H91.14171.05390.26460.071*
C100.9472 (4)1.0472 (5)0.2493 (3)0.0590 (11)
H100.93911.10650.19620.071*
C110.8387 (4)0.9950 (5)0.2840 (2)0.0505 (9)
H110.75731.01670.25600.061*
C120.8568 (3)0.9069 (4)0.3639 (2)0.0374 (7)
N10.7703 (3)0.8416 (3)0.41543 (19)0.0398 (7)
N20.8434 (3)0.7743 (3)0.48214 (19)0.0405 (7)
N30.9691 (3)0.7872 (4)0.4807 (2)0.0468 (7)
N40.5926 (3)0.3275 (3)0.5456 (2)0.0416 (7)
N50.4289 (3)0.4142 (4)0.8019 (2)0.0487 (8)
O10.5156 (4)0.4675 (5)0.7624 (2)0.0997 (13)
O20.4036 (3)0.4733 (4)0.8748 (2)0.0705 (8)
O30.3683 (3)0.3011 (4)0.7710 (2)0.0759 (10)
U11U22U33U12U13U23
Ag10.04179 (18)0.0525 (2)0.0734 (2)−0.00689 (13)0.01612 (14)0.00621 (15)
C10.0340 (17)0.044 (2)0.0370 (17)0.0018 (15)0.0035 (14)0.0029 (15)
C20.0400 (18)0.0372 (18)0.0360 (17)−0.0006 (15)0.0036 (14)0.0048 (15)
C30.065 (3)0.051 (2)0.058 (2)−0.007 (2)0.029 (2)−0.0018 (19)
C40.085 (3)0.054 (3)0.063 (3)−0.008 (2)0.031 (2)−0.015 (2)
C50.059 (2)0.040 (2)0.059 (2)−0.0071 (18)0.0048 (19)−0.0036 (18)
C60.060 (2)0.048 (2)0.0391 (19)−0.0129 (18)0.0110 (17)0.0021 (17)
C70.0407 (19)0.0393 (19)0.0431 (19)−0.0094 (15)0.0091 (15)−0.0064 (16)
C80.041 (2)0.066 (3)0.065 (3)−0.0151 (19)0.0127 (18)−0.010 (2)
C90.058 (3)0.064 (3)0.059 (3)−0.025 (2)0.024 (2)−0.008 (2)
C100.081 (3)0.052 (2)0.045 (2)−0.021 (2)0.017 (2)0.0025 (19)
C110.054 (2)0.053 (2)0.045 (2)−0.0077 (18)0.0065 (17)0.0038 (18)
C120.0389 (18)0.0356 (18)0.0387 (18)−0.0084 (14)0.0088 (14)−0.0068 (15)
N10.0361 (15)0.0445 (16)0.0394 (15)−0.0103 (13)0.0063 (12)0.0011 (13)
N20.0413 (16)0.0413 (16)0.0397 (15)−0.0092 (13)0.0086 (13)0.0008 (13)
N30.0400 (17)0.0509 (18)0.0495 (18)−0.0052 (14)0.0038 (13)0.0006 (15)
N40.0363 (15)0.0405 (16)0.0475 (17)−0.0034 (13)0.0008 (13)0.0040 (14)
N50.0404 (17)0.0463 (18)0.060 (2)−0.0007 (15)0.0081 (15)−0.0028 (16)
O10.091 (3)0.124 (3)0.089 (2)−0.053 (2)0.038 (2)−0.001 (2)
O20.0648 (19)0.067 (2)0.081 (2)−0.0013 (15)0.0153 (16)−0.0275 (17)
O30.080 (2)0.071 (2)0.081 (2)−0.0322 (18)0.0301 (17)−0.0311 (17)
Ag1—N42.253 (3)C7—N31.351 (5)
Ag1—N1i2.311 (3)C7—C121.399 (5)
Ag1—O32.468 (3)C7—C81.412 (5)
Ag1—O1ii2.728 (4)C8—C91.345 (6)
Ag1—O2ii2.646 (3)C8—H80.9300
C1—N41.333 (4)C9—C101.408 (6)
C1—C21.381 (5)C9—H90.9300
C1—H10.9300C10—C111.365 (5)
C2—C31.372 (5)C10—H100.9300
C2—C61.504 (5)C11—C121.397 (5)
C3—C41.376 (6)C11—H110.9300
C3—H30.9300C12—N11.356 (4)
C4—C51.364 (6)N1—N21.321 (4)
C4—H40.9300N1—Ag1i2.311 (3)
C5—N41.329 (5)N2—N31.324 (4)
C5—H50.9300N5—O11.214 (4)
C6—N21.454 (4)N5—O31.234 (4)
C6—H610.9700N5—O21.236 (4)
C6—H620.9700
N4—Ag1—N1i131.66 (10)C9—C8—H8121.5
N4—Ag1—O3127.43 (11)C7—C8—H8121.5
N1i—Ag1—O384.66 (11)C8—C9—C10122.0 (4)
N4—C1—C2123.6 (3)C8—C9—H9119.0
N4—C1—H1118.2C10—C9—H9119.0
C2—C1—H1118.2C11—C10—C9122.4 (4)
C3—C2—C1117.4 (3)C11—C10—H10118.8
C3—C2—C6123.4 (3)C9—C10—H10118.8
C1—C2—C6119.1 (3)C10—C11—C12116.2 (4)
C2—C3—C4119.4 (4)C10—C11—H11121.9
C2—C3—H3120.3C12—C11—H11121.9
C4—C3—H3120.3N1—C12—C11130.6 (3)
C5—C4—C3119.3 (4)N1—C12—C7107.9 (3)
C5—C4—H4120.4C11—C12—C7121.5 (3)
C3—C4—H4120.4N2—N1—C12103.1 (3)
N4—C5—C4122.5 (4)N2—N1—Ag1i125.0 (2)
N4—C5—H5118.8C12—N1—Ag1i129.0 (2)
C4—C5—H5118.8N1—N2—N3117.4 (3)
N2—C6—C2112.5 (3)N1—N2—C6121.5 (3)
N2—C6—H61109.1N3—N2—C6121.1 (3)
C2—C6—H61109.1N2—N3—C7102.5 (3)
N2—C6—H62109.1C5—N4—C1117.8 (3)
C2—C6—H62109.1C5—N4—Ag1119.5 (2)
H61—C6—H62107.8C1—N4—Ag1122.6 (2)
N3—C7—C12109.2 (3)O1—N5—O3120.7 (4)
N3—C7—C8130.0 (4)O1—N5—O2119.0 (4)
C12—C7—C8120.9 (3)O3—N5—O2120.3 (3)
C9—C8—C7116.9 (4)N5—O3—Ag1111.5 (2)
N4—C1—C2—C32.0 (5)C12—N1—N2—N3−0.2 (4)
N4—C1—C2—C6−176.4 (3)Ag1i—N1—N2—N3161.7 (2)
C1—C2—C3—C4−0.4 (6)C12—N1—N2—C6−179.6 (3)
C6—C2—C3—C4177.9 (4)Ag1i—N1—N2—C6−17.7 (4)
C2—C3—C4—C5−1.2 (7)C2—C6—N2—N174.0 (4)
C3—C4—C5—N41.6 (7)C2—C6—N2—N3−105.4 (4)
C3—C2—C6—N225.6 (5)N1—N2—N3—C70.5 (4)
C1—C2—C6—N2−156.1 (3)C6—N2—N3—C7179.9 (3)
N3—C7—C8—C9−179.3 (4)C12—C7—N3—N2−0.7 (4)
C12—C7—C8—C90.3 (6)C8—C7—N3—N2179.0 (4)
C7—C8—C9—C10−0.7 (6)C4—C5—N4—C1−0.1 (6)
C8—C9—C10—C110.5 (7)C4—C5—N4—Ag1−179.8 (3)
C9—C10—C11—C120.2 (6)C2—C1—N4—C5−1.7 (5)
C10—C11—C12—N1178.7 (4)C2—C1—N4—Ag1177.9 (2)
C10—C11—C12—C7−0.6 (5)N1i—Ag1—N4—C5−68.9 (3)
N3—C7—C12—N10.6 (4)O3—Ag1—N4—C5169.5 (3)
C8—C7—C12—N1−179.0 (3)N1i—Ag1—N4—C1111.5 (3)
N3—C7—C12—C11−179.9 (3)O3—Ag1—N4—C1−10.1 (3)
C8—C7—C12—C110.4 (5)O1—N5—O3—Ag1−1.8 (5)
C11—C12—N1—N2−179.6 (4)O2—N5—O3—Ag1179.5 (3)
C7—C12—N1—N2−0.3 (4)N4—Ag1—O3—N5−3.8 (3)
C11—C12—N1—Ag1i19.5 (5)N1i—Ag1—O3—N5−144.1 (3)
C7—C12—N1—Ag1i−161.1 (2)
D—H···AD—HH···AD···AD—H···A
C5—H5···O2iii0.932.593.365 (3)141
C6—H61···O2iv0.972.483.416 (5)161
Ag1—N42.253 (3)
Ag1—N1i2.311 (3)
Ag1—O32.468 (3)
Ag1—O1ii2.728 (4)
Ag1—O2ii2.646 (3)
N4—Ag1—N1i131.66 (10)
N4—Ag1—O3127.43 (11)
N1i—Ag1—O384.66 (11)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C5—H5⋯O2iii0.932.593.365 (3)141
C6—H61⋯O2iv0.972.483.416 (5)161

Symmetry codes: (iii) ; (iv) .

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