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Acta Cryst. (2007). E63, m1640    [ doi:10.1107/S1600536807022581 ]

Bis{tris[[mu]-2-(1H-pyrazol-3-yl-[kappa]N1:[kappa]N2)pyridinato-[kappa]N]trisilver(I)}(2 Ag-Ag)

R. Li

Abstract top

The asymmetric unit of the title complex, [Ag6(C8H6N3)6], contains one half-molecule; the molecule is centrosymmetric. The Ag atoms form two nearly equilateral triangles, with Ag...Ag distances of 3.725 (3), 3.741 (3) and 3.843 (2) Å.

Comment top

The compound, [Ag3(C8H6N3)3]2.2py, (II), (where py is pyridine), first synthesized and characterized by X-ray structure analysis at 295 K (Singh et al., 1997). It was obtained by the reaction of Ag(O3SCF3) with deprotonated 3-(2-pyridyl)pyrazole in methanol. The title complex, [Ag3(C8H6N3)3]2, (I), is obtained by the reaction of AgNO3 with 3-(2-pyridyl)pyrazole in water, under hydrothermal conditions. We herein report its crystal structure.

The asymmetric unit of (I) contains one half molecule (Fig. 1). The bond lengths and angles (Table 1) are within normal ranges (Allen et al., 1987). The Ag2···Ag3 [3.1144 (6) Å] distance is shorter than the corresponding one [3.227 (2) Å] in (II). In the molecule of (I), the silver atoms form two nearly equilateral triangles with Ag1···Ag3A [3.725 (3) Å], Ag1···Ag2 [3.741 (3) Å] and Ag2···Ag3A [3.843 (2) Å] (symmetry code A: -x, 1 - y, -z) distances, they are reported as 3.655, 3.702 and 3.835 Å, respectively, in (II).

Related literature top

For general background, see: Singh et al. (1997); Allen et al. (1987).

Experimental top

The title complex was obtained by the reaction of AgNO3 with 3-(2-pyridyl)pyrazole in the molar ratio of 1:1 mixed with water (15 ml), under hydrothermal conditions at 413 K for 2 d. The colorless crystals were washed by water and acetone, and dried in air (yield: 0.452 g, 50%).

Refinement top

H atoms were positioned geometrically, with C—H = 0.93 Å for aromatic H and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level [symmetry code for unlabelled atoms: -x, 1 - y, -z].
Bis{tris[µ-2-(1H-pyrazol-3-yl-κN1:κN2)pyridinato- κN]trisilver(I)}(2 A g—Ag) top
Crystal data top
[Ag6(C8H6N3)6]F(000) = 1464
Mr = 1512.17Dx = 2.057 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4311 reflections
a = 11.5599 (17) Åθ = 2.5–25.9°
b = 8.5424 (13) ŵ = 2.42 mm−1
c = 25.389 (4) ÅT = 294 K
β = 103.16 (3)°Block, colourless
V = 2441.3 (7) Å30.22 × 0.20 × 0.10 mm
Z = 2
Data collection top
Bruker SMART CCD area-detecter
diffractometer		4272 independent reflections
Radiation source: fine-focus sealed tube3045 reflections with I > 2σ(I)
graphiteRint = 0.034
φ and ω scansθmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −10→13
Tmin = 0.619, Tmax = 0.794k = −10→10
11942 measured reflectionsl = −30→28
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0176P)2 + 0.4151P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
4272 reflectionsΔρmax = 0.32 e Å−3
326 parametersΔρmin = −0.28 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00435 (13)
Crystal data top
[Ag6(C8H6N3)6]V = 2441.3 (7) Å3
Mr = 1512.17Z = 2
Monoclinic, P21/cMo Kα radiation
a = 11.5599 (17) ŵ = 2.42 mm−1
b = 8.5424 (13) ÅT = 294 K
c = 25.389 (4) Å0.22 × 0.20 × 0.10 mm
β = 103.16 (3)°
Data collection top
Bruker SMART CCD area-detecter
diffractometer		4272 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3045 reflections with I > 2σ(I)
Tmin = 0.619, Tmax = 0.794Rint = 0.034
11942 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.056Δρmax = 0.32 e Å−3
S = 1.04Δρmin = −0.28 e Å−3
4272 reflectionsAbsolute structure: ?
326 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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*/Ueq
Ag10.22972 (3)0.51678 (4)0.144579 (13)0.05937 (12)
Ag20.13707 (3)0.75885 (4)0.019264 (12)0.05891 (12)
Ag30.08700 (3)0.50068 (3)−0.069650 (12)0.05764 (11)
C10.4993 (4)0.4002 (5)0.24241 (17)0.0697 (12)
H10.44990.34190.25910.084*
C20.6178 (4)0.3998 (5)0.26535 (17)0.0667 (12)
H20.64820.34380.29690.080*
C30.6911 (4)0.4843 (5)0.24049 (17)0.0623 (11)
H30.77270.48550.25470.075*
C40.6425 (3)0.5671 (4)0.19450 (15)0.0518 (10)
H40.69080.62550.17720.062*
C50.5205 (3)0.5630 (4)0.17397 (15)0.0449 (9)
C60.4638 (3)0.6537 (4)0.12573 (14)0.0450 (9)
C70.5113 (4)0.7506 (5)0.09238 (17)0.0661 (12)
H70.59100.77320.09480.079*
C80.4152 (4)0.8060 (5)0.05497 (17)0.0668 (12)
H80.41920.87420.02690.080*
C90.1409 (4)1.0506 (5)−0.08115 (18)0.0613 (11)
H90.22251.0554−0.06720.074*
C100.0920 (4)1.1513 (5)−0.12247 (18)0.0694 (12)
H100.13901.2216−0.13620.083*
C11−0.0289 (4)1.1445 (5)−0.14278 (17)0.0721 (13)
H11−0.06531.2105−0.17080.087*
C12−0.0954 (4)1.0389 (5)−0.12118 (16)0.0621 (11)
H12−0.17731.0346−0.13400.075*
C13−0.0396 (3)0.9396 (4)−0.08040 (14)0.0449 (9)
C14−0.1060 (3)0.8254 (4)−0.05652 (14)0.0457 (9)
C15−0.2251 (3)0.7862 (5)−0.06899 (16)0.0601 (11)
H15−0.28470.8297−0.09590.072*
C16−0.2374 (3)0.6695 (5)−0.03332 (17)0.0622 (12)
H16−0.30830.6196−0.03220.075*
C170.3620 (4)0.6835 (6)−0.0800 (2)0.0778 (14)
H170.39660.6296−0.04850.093*
C180.4308 (5)0.7882 (7)−0.1007 (3)0.0953 (17)
H180.50930.8064−0.08300.114*
C190.3823 (5)0.8637 (6)−0.1472 (3)0.0904 (17)
H190.42790.9328−0.16230.109*
C200.2645 (4)0.8382 (5)−0.1722 (2)0.0720 (13)
H200.22960.8900−0.20410.086*
C210.1997 (3)0.7331 (5)−0.14861 (17)0.0537 (10)
C220.0750 (3)0.6993 (4)−0.17222 (15)0.0475 (9)
C23−0.0011 (4)0.7552 (5)−0.21866 (17)0.0630 (11)
H230.01620.8268−0.24340.076*
C240.1065 (4)0.3171 (5)0.22022 (16)0.0602 (11)
H240.17510.30280.24720.072*
N10.4490 (3)0.4793 (4)0.19730 (13)0.0556 (8)
N20.3454 (2)0.6541 (3)0.10872 (12)0.0486 (8)
N30.3155 (3)0.7482 (4)0.06472 (12)0.0550 (8)
N40.0787 (3)0.9466 (3)−0.05986 (12)0.0502 (8)
N5−0.0509 (3)0.7343 (3)−0.01512 (11)0.0463 (7)
N6−0.1315 (3)0.6389 (4)−0.00049 (12)0.0522 (8)
N70.2489 (3)0.6559 (4)−0.10277 (14)0.0598 (9)
N80.0148 (3)0.5983 (3)−0.14802 (12)0.0497 (8)
N90.0978 (3)0.4114 (4)0.17768 (12)0.0521 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.04537 (19)0.0684 (2)0.0623 (2)−0.01088 (15)0.00801 (15)0.00317 (17)
Ag20.04773 (18)0.0656 (2)0.0541 (2)0.00651 (15)−0.00783 (13)−0.00370 (16)
Ag30.0634 (2)0.0568 (2)0.0507 (2)0.00115 (16)0.00852 (15)0.00713 (15)
C10.064 (3)0.075 (3)0.067 (3)−0.002 (2)0.007 (2)0.021 (2)
C20.062 (3)0.068 (3)0.061 (3)0.003 (2)−0.006 (2)0.012 (2)
C30.047 (2)0.065 (3)0.067 (3)0.003 (2)−0.004 (2)0.000 (2)
C40.048 (2)0.052 (2)0.053 (3)−0.0042 (19)0.0052 (19)−0.005 (2)
C50.040 (2)0.044 (2)0.047 (2)−0.0014 (17)0.0032 (18)−0.0067 (18)
C60.042 (2)0.045 (2)0.043 (2)−0.0031 (17)−0.0003 (18)−0.0042 (18)
C70.050 (2)0.077 (3)0.067 (3)−0.019 (2)0.005 (2)0.017 (2)
C80.063 (3)0.068 (3)0.066 (3)−0.015 (2)0.008 (2)0.021 (2)
C90.056 (3)0.060 (3)0.070 (3)−0.002 (2)0.020 (2)−0.009 (2)
C100.091 (4)0.057 (3)0.069 (3)0.002 (3)0.035 (3)0.006 (2)
C110.091 (4)0.076 (3)0.051 (3)0.016 (3)0.019 (3)0.018 (2)
C120.064 (3)0.074 (3)0.044 (3)0.008 (2)0.003 (2)0.005 (2)
C130.052 (2)0.048 (2)0.035 (2)0.0066 (18)0.0100 (18)−0.0025 (18)
C140.045 (2)0.051 (2)0.038 (2)0.0070 (18)0.0016 (18)−0.0059 (18)
C150.043 (2)0.077 (3)0.056 (3)0.004 (2)0.0007 (19)0.008 (2)
C160.043 (2)0.073 (3)0.067 (3)−0.006 (2)0.005 (2)0.003 (2)
C170.056 (3)0.090 (3)0.088 (4)−0.004 (3)0.018 (3)−0.012 (3)
C180.063 (3)0.107 (4)0.124 (5)−0.024 (3)0.037 (3)−0.025 (4)
C190.084 (4)0.083 (4)0.122 (5)−0.029 (3)0.057 (4)−0.011 (3)
C200.076 (3)0.062 (3)0.088 (4)−0.015 (2)0.042 (3)−0.007 (2)
C210.055 (2)0.051 (2)0.061 (3)−0.002 (2)0.026 (2)−0.009 (2)
C220.057 (2)0.044 (2)0.045 (2)0.0015 (19)0.020 (2)−0.0020 (18)
C230.084 (3)0.057 (3)0.053 (3)−0.003 (2)0.026 (2)0.006 (2)
C240.062 (3)0.066 (3)0.046 (3)0.007 (2)−0.001 (2)0.006 (2)
N10.0451 (18)0.062 (2)0.056 (2)−0.0043 (16)0.0041 (16)0.0135 (18)
N20.0418 (19)0.0523 (19)0.046 (2)−0.0045 (15)−0.0014 (14)0.0033 (16)
N30.049 (2)0.059 (2)0.050 (2)−0.0078 (17)−0.0045 (15)0.0077 (17)
N40.048 (2)0.0505 (19)0.051 (2)0.0005 (15)0.0079 (16)−0.0045 (15)
N50.0472 (18)0.0476 (18)0.0407 (18)0.0019 (16)0.0034 (14)−0.0006 (15)
N60.0469 (19)0.057 (2)0.048 (2)−0.0035 (16)0.0004 (16)0.0031 (16)
N70.045 (2)0.067 (2)0.069 (2)−0.0060 (17)0.0169 (18)−0.0045 (19)
N80.048 (2)0.0511 (19)0.049 (2)−0.0028 (15)0.0099 (16)0.0069 (16)
N90.049 (2)0.058 (2)0.049 (2)−0.0032 (16)0.0087 (16)0.0051 (17)
Geometric parameters (Å, °) top
Ag1—N92.103 (3)C12—C131.380 (5)
Ag1—N22.132 (3)C12—H120.9300
Ag1—N12.603 (3)C13—N41.350 (4)
Ag2—N32.124 (3)C13—C141.456 (5)
Ag2—N52.160 (3)C14—N51.346 (4)
Ag2—N42.539 (3)C14—C151.382 (5)
Ag2—Ag33.1144 (6)C15—C161.376 (5)
Ag3—N6i2.107 (3)C15—H150.9300
Ag3—N82.144 (3)C16—N61.341 (4)
Ag3—N72.586 (3)C16—H160.9300
C1—N11.343 (5)C17—N71.324 (5)
C1—C21.361 (5)C17—C181.379 (7)
C1—H10.9300C17—H170.9300
C2—C31.371 (6)C18—C191.349 (7)
C2—H20.9300C18—H180.9300
C3—C41.371 (5)C19—C201.382 (6)
C3—H30.9300C19—H190.9300
C4—C51.387 (5)C20—C211.390 (5)
C4—H40.9300C20—H200.9300
C5—N11.330 (5)C21—N71.346 (5)
C5—C61.471 (5)C21—C221.458 (5)
C6—N21.338 (4)C22—N81.342 (4)
C6—C71.384 (5)C22—C231.385 (5)
C7—C81.371 (5)C23—C24i1.359 (5)
C7—H70.9300C23—H230.9300
C8—N31.328 (5)C24—N91.333 (5)
C8—H80.9300C24—C23i1.359 (5)
C9—N41.333 (5)C24—H240.9300
C9—C101.375 (6)N2—N31.356 (4)
C9—H90.9300N5—N61.352 (4)
C10—C111.376 (6)N6—Ag3i2.107 (3)
C10—H100.9300N8—N9i1.350 (4)
C11—C121.377 (6)N9—N8i1.350 (4)
C11—H110.9300
N9—Ag1—N2171.11 (12)C16—C15—C14105.7 (3)
N9—Ag1—N1116.85 (11)C16—C15—H15127.1
N2—Ag1—N169.83 (10)C14—C15—H15127.1
N3—Ag2—N5168.18 (12)N6—C16—C15109.5 (4)
N3—Ag2—N4120.48 (11)N6—C16—H16125.2
N5—Ag2—N471.33 (10)C15—C16—H16125.2
N3—Ag2—Ag3111.15 (9)N7—C17—C18123.2 (5)
N5—Ag2—Ag368.55 (7)N7—C17—H17118.4
N4—Ag2—Ag384.36 (7)C18—C17—H17118.4
N6i—Ag3—N8166.69 (12)C19—C18—C17118.8 (5)
N6i—Ag3—N7120.62 (11)C19—C18—H18120.6
N8—Ag3—N769.91 (11)C17—C18—H18120.6
N6i—Ag3—Ag279.55 (9)C18—C19—C20119.8 (5)
N8—Ag3—Ag2111.48 (8)C18—C19—H19120.1
N7—Ag3—Ag281.01 (7)C20—C19—H19120.1
N1—C1—C2124.4 (4)C19—C20—C21118.4 (5)
N1—C1—H1117.8C19—C20—H20120.8
C2—C1—H1117.8C21—C20—H20120.8
C1—C2—C3117.9 (4)N7—C21—C20121.7 (4)
C1—C2—H2121.0N7—C21—C22116.3 (3)
C3—C2—H2121.0C20—C21—C22122.0 (4)
C2—C3—C4119.2 (4)N8—C22—C23108.4 (3)
C2—C3—H3120.4N8—C22—C21120.4 (3)
C4—C3—H3120.4C23—C22—C21131.2 (4)
C3—C4—C5119.4 (4)C24i—C23—C22105.0 (4)
C3—C4—H4120.3C24i—C23—H23127.5
C5—C4—H4120.3C22—C23—H23127.5
N1—C5—C4121.9 (3)N9—C24—C23i110.5 (4)
N1—C5—C6116.7 (3)N9—C24—H24124.8
C4—C5—C6121.4 (3)C23i—C24—H24124.8
N2—C6—C7108.7 (3)C5—N1—C1117.2 (3)
N2—C6—C5119.9 (3)C5—N1—Ag1109.7 (2)
C7—C6—C5131.4 (3)C1—N1—Ag1133.0 (3)
C8—C7—C6105.0 (3)C6—N2—N3108.5 (3)
C8—C7—H7127.5C6—N2—Ag1123.8 (2)
C6—C7—H7127.5N3—N2—Ag1127.7 (2)
N3—C8—C7110.1 (4)C8—N3—N2107.7 (3)
N3—C8—H8125.0C8—N3—Ag2131.3 (3)
C7—C8—H8125.0N2—N3—Ag2120.5 (2)
N4—C9—C10124.1 (4)C9—N4—C13117.7 (3)
N4—C9—H9118.0C9—N4—Ag2132.2 (3)
C10—C9—H9118.0C13—N4—Ag2110.0 (2)
C9—C10—C11117.8 (4)C14—N5—N6109.3 (3)
C9—C10—H10121.1C14—N5—Ag2120.9 (2)
C11—C10—H10121.1N6—N5—Ag2129.8 (2)
C10—C11—C12119.3 (4)C16—N6—N5107.5 (3)
C10—C11—H11120.3C16—N6—Ag3i130.4 (3)
C12—C11—H11120.3N5—N6—Ag3i121.5 (2)
C11—C12—C13119.6 (4)C17—N7—C21118.1 (4)
C11—C12—H12120.2C17—N7—Ag3131.7 (3)
C13—C12—H12120.2C21—N7—Ag3109.7 (2)
N4—C13—C12121.5 (4)C22—N8—N9i108.6 (3)
N4—C13—C14116.9 (3)C22—N8—Ag3122.8 (2)
C12—C13—C14121.6 (4)N9i—N8—Ag3128.0 (2)
N5—C14—C15108.0 (3)C24—N9—N8i107.5 (3)
N5—C14—C13120.8 (3)C24—N9—Ag1130.9 (3)
C15—C14—C13131.2 (3)N8i—N9—Ag1119.9 (2)
N3—Ag2—Ag3—N6i61.47 (13)Ag1—N2—N3—C8−177.3 (3)
N5—Ag2—Ag3—N6i−105.85 (11)C6—N2—N3—Ag2172.3 (2)
N4—Ag2—Ag3—N6i−177.98 (11)Ag1—N2—N3—Ag2−4.7 (4)
N3—Ag2—Ag3—N8−126.29 (13)N5—Ag2—N3—C8169.4 (5)
N5—Ag2—Ag3—N866.39 (12)N4—Ag2—N3—C8−12.9 (4)
N4—Ag2—Ag3—N8−5.75 (11)Ag3—Ag2—N3—C883.1 (4)
N3—Ag2—Ag3—N7−62.14 (12)N5—Ag2—N3—N2−1.2 (8)
N5—Ag2—Ag3—N7130.54 (12)N4—Ag2—N3—N2176.5 (2)
N4—Ag2—Ag3—N758.41 (11)Ag3—Ag2—N3—N2−87.5 (3)
N1—C1—C2—C3−0.7 (7)C10—C9—N4—C130.3 (6)
C1—C2—C3—C41.0 (6)C10—C9—N4—Ag2−175.4 (3)
C2—C3—C4—C5−0.3 (6)C12—C13—N4—C9−1.5 (5)
C3—C4—C5—N1−0.8 (6)C14—C13—N4—C9−179.9 (3)
C3—C4—C5—C6178.1 (3)C12—C13—N4—Ag2175.0 (3)
N1—C5—C6—N22.6 (5)C14—C13—N4—Ag2−3.3 (4)
C4—C5—C6—N2−176.3 (3)N3—Ag2—N4—C9−0.4 (4)
N1—C5—C6—C7−179.7 (4)N5—Ag2—N4—C9179.1 (4)
C4—C5—C6—C71.3 (6)Ag3—Ag2—N4—C9−111.7 (3)
N2—C6—C7—C8−0.5 (5)N3—Ag2—N4—C13−176.3 (2)
C5—C6—C7—C8−178.4 (4)N5—Ag2—N4—C133.2 (2)
C6—C7—C8—N30.3 (5)Ag3—Ag2—N4—C1372.4 (2)
N4—C9—C10—C110.4 (6)C15—C14—N5—N6−0.5 (4)
C9—C10—C11—C120.2 (6)C13—C14—N5—N6−179.9 (3)
C10—C11—C12—C13−1.4 (6)C15—C14—N5—Ag2−178.6 (2)
C11—C12—C13—N42.1 (6)C13—C14—N5—Ag22.0 (4)
C11—C12—C13—C14−179.6 (4)N3—Ag2—N5—C14175.2 (5)
N4—C13—C14—N51.4 (5)N4—Ag2—N5—C14−2.7 (2)
C12—C13—C14—N5−177.0 (3)Ag3—Ag2—N5—C14−93.9 (3)
N4—C13—C14—C15−177.9 (4)N3—Ag2—N5—N6−2.5 (8)
C12—C13—C14—C153.8 (6)N4—Ag2—N5—N6179.6 (3)
N5—C14—C15—C160.2 (4)Ag3—Ag2—N5—N688.4 (3)
C13—C14—C15—C16179.5 (4)C15—C16—N6—N5−0.5 (4)
C14—C15—C16—N60.2 (5)C15—C16—N6—Ag3i170.5 (3)
N7—C17—C18—C19−1.8 (8)C14—N5—N6—C160.6 (4)
C17—C18—C19—C201.7 (8)Ag2—N5—N6—C16178.5 (2)
C18—C19—C20—C21−0.6 (7)C14—N5—N6—Ag3i−171.4 (2)
C19—C20—C21—N7−0.5 (6)Ag2—N5—N6—Ag3i6.5 (4)
C19—C20—C21—C22179.9 (4)C18—C17—N7—C210.7 (7)
N7—C21—C22—N81.1 (5)C18—C17—N7—Ag3−170.4 (4)
C20—C21—C22—N8−179.3 (4)C20—C21—N7—C170.5 (6)
N7—C21—C22—C23−179.0 (4)C22—C21—N7—C17−179.9 (3)
C20—C21—C22—C230.6 (6)C20—C21—N7—Ag3173.5 (3)
N8—C22—C23—C24i−0.1 (4)C22—C21—N7—Ag3−7.0 (4)
C21—C22—C23—C24i−180.0 (4)N6i—Ag3—N7—C17−9.6 (4)
C4—C5—N1—C11.1 (6)N8—Ag3—N7—C17179.4 (4)
C6—C5—N1—C1−177.8 (3)Ag2—Ag3—N7—C1762.5 (4)
C4—C5—N1—Ag1178.7 (3)N6i—Ag3—N7—C21178.7 (2)
C6—C5—N1—Ag1−0.3 (4)N8—Ag3—N7—C217.8 (2)
C2—C1—N1—C5−0.4 (6)Ag2—Ag3—N7—C21−109.1 (2)
C2—C1—N1—Ag1−177.2 (3)C23—C22—N8—N9i−0.2 (4)
N9—Ag1—N1—C5−174.8 (2)C21—C22—N8—N9i179.7 (3)
N2—Ag1—N1—C5−1.2 (2)C23—C22—N8—Ag3−172.4 (2)
N9—Ag1—N1—C12.2 (4)C21—C22—N8—Ag37.5 (5)
N2—Ag1—N1—C1175.8 (4)N6i—Ag3—N8—C22−152.0 (5)
C7—C6—N2—N30.5 (4)N7—Ag3—N8—C22−7.9 (3)
C5—C6—N2—N3178.7 (3)Ag2—Ag3—N8—C2263.2 (3)
C7—C6—N2—Ag1177.7 (3)N6i—Ag3—N8—N9i37.4 (7)
C5—C6—N2—Ag1−4.2 (5)N7—Ag3—N8—N9i−178.5 (3)
N1—Ag1—N2—C62.8 (3)Ag2—Ag3—N8—N9i−107.4 (3)
N1—Ag1—N2—N3179.4 (3)C23i—C24—N9—N8i0.4 (4)
C7—C8—N3—N20.0 (5)C23i—C24—N9—Ag1−164.0 (3)
C7—C8—N3—Ag2−171.5 (3)N1—Ag1—N9—C24−5.3 (4)
C6—N2—N3—C8−0.3 (4)N1—Ag1—N9—N8i−168.1 (2)
Symmetry codes: (i) −x, −y+1, −z.
Table 1
Selected geometric parameters (Å) top
Ag1—N92.103 (3)Ag2—N42.539 (3)
Ag1—N22.132 (3)Ag2—Ag33.1144 (6)
Ag1—N12.603 (3)Ag3—N6i2.107 (3)
Ag2—N32.124 (3)Ag3—N82.144 (3)
Ag2—N52.160 (3)Ag3—N72.586 (3)
Symmetry codes: (i) −x, −y+1, −z.
references
References top

Allen, F. H., Kennard, O., Watson, D. G., Brammer, L., Orpen, A. G. & Taylor, R. (1987). J. Chem. Soc. Perkin Trans. 2, pp. S1–19.

Bruker (1998). SMART, SAINT and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Singh, K., Long, J. R. & Stavropoulos, P. (1997). J. Am. Chem. Soc. 119, 2942–2943.