metal-organic compounds
cyclo-Tris[μ-5-(2-pyridyl)pyrazol-1-ido-κ3N1,N5:N2]trisilver(I)
aSchool of Chemistry and Life Science, Maoming University, Maoming 525000, People's Republic of China
*Correspondence e-mail: anz_md@163.com
In the title compound, [Ag3(C8H6N3)3], the contains three silver cations and three depronated 5-(2-pyridyl)pyrazol-1-ide ligands. Each silver cation is chelated by one 5-(2-pyridyl)pyrazol-1-ide ligand, which also acts as a bridging ligand towards the next silver ion via the second pyrazole N atom. In summary, three silver cations and three deprotonated 3-(2-pyridyl)-1H-pyrazole ligands produce a macrocyclic trimeric coordination oligomer that exhibits an almost planar conformation (mean deviation 0.1483 Å). In addition, short non-bonding Ag⋯Ag interactions [3.127 (2) Å] are observed.
Related literature
For coordination compounds with pyridyl-pyrazolide ligands, see: Ward et al. (1998, 2001).
Experimental
Crystal data
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Data collection: SMART (Bruker, 2002); cell SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536809040082/im2146sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809040082/im2146Isup2.hkl
The synthesis of the title compound is performed in 25 ml Teflon-lined stainless steel vessels. Powdered 3-(2-pyridyl)pyrazole (1 mmol) together with silver nitrate (1 mmol) is heated to 170°C in 10 ml of a water/ethanol mixture (1:1) for 24 h. Colorless crystals were obtained after cooling to room temperature.
All hydrogen atoms were positioned geometrically and were refined using a riding model with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).
Deprotonated 3-(2-pyridyl)pyrazole is a potentially tridentate ligands and it's derivatives have been widely used for the construction of supramolecular architectures by their ability of producing coordination compounds (Ward et al. 1998; 2001). As a continuation of these studies, we now report the
of the title complex.As shown in figure 1, the
contains three silver cations and three depronated 5-(2-pyridyl)pyrazol-1-ide ligands. Each silver cation is chelated with one 5-(2-pyridyl)pyrazol-1-ide ligand, which in addition acts as a bridging ligand towards the next silver ion via the second pyrazole nitrogen.In summary, three silver cations and three depronated 5-(2-pyridyl)pyrazol-1-ide ligands produce a macrocyclic trimeric coordination oligomer that exhibits an almost planar conformation. In addition, short non-bonding Ag-Ag interactions (3.127 (2) Å) are observed.
For coordination compounds with pyridyl-pyrazolide ligands, see: Ward et al. (1998, 2001).
Data collection: SMART (Bruker, 2002); cell
SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. A view of the title compound with the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Ag3(C8H6N3)3] | F(000) = 1464 |
Mr = 756.07 | Dx = 2.036 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 843 reflections |
a = 11.597 (9) Å | θ = 2.9–20.3° |
b = 8.555 (6) Å | µ = 2.39 mm−1 |
c = 25.52 (2) Å | T = 294 K |
β = 103.018 (9)° | Block, colorless |
V = 2467 (3) Å3 | 0.10 × 0.10 × 0.08 mm |
Z = 4 |
Bruker SMART CCD diffractometer | 4294 independent reflections |
Radiation source: fine-focus sealed tube | 2947 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
φ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −13→13 |
Tmin = 0.796, Tmax = 0.832 | k = −9→10 |
12411 measured reflections | l = −30→27 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters not refined |
S = 1.00 | w = 1/[σ2(Fo2) + (0.02P)2] where P = (Fo2 + 2Fc2)/3 |
4294 reflections | (Δ/σ)max = 0.005 |
325 parameters | Δρmax = 0.41 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Ag3(C8H6N3)3] | V = 2467 (3) Å3 |
Mr = 756.07 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.597 (9) Å | µ = 2.39 mm−1 |
b = 8.555 (6) Å | T = 294 K |
c = 25.52 (2) Å | 0.10 × 0.10 × 0.08 mm |
β = 103.018 (9)° |
Bruker SMART CCD diffractometer | 4294 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2947 reflections with I > 2σ(I) |
Tmin = 0.796, Tmax = 0.832 | Rint = 0.041 |
12411 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.064 | H-atom parameters not refined |
S = 1.00 | Δρmax = 0.41 e Å−3 |
4294 reflections | Δρmin = −0.41 e Å−3 |
325 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ag1 | 0.22973 (3) | 0.98307 (4) | 0.144566 (15) | 0.06499 (13) | |
Ag2 | 0.13700 (3) | 0.74112 (4) | 0.019289 (14) | 0.06424 (13) | |
C1 | 0.4980 (4) | 1.0995 (6) | 0.2419 (2) | 0.0747 (15) | |
H1 | 0.4483 | 1.1577 | 0.2584 | 0.090* | |
C2 | 0.6185 (4) | 1.1006 (6) | 0.26491 (19) | 0.0719 (14) | |
H2 | 0.6490 | 1.1581 | 0.2959 | 0.086* | |
C3 | 0.6909 (4) | 1.0148 (5) | 0.24072 (19) | 0.0659 (14) | |
H3 | 0.7720 | 1.0113 | 0.2553 | 0.079* | |
C4 | 0.6424 (4) | 0.9331 (5) | 0.19436 (18) | 0.0580 (12) | |
H4 | 0.6911 | 0.8759 | 0.1771 | 0.070* | |
C5 | 0.5212 (4) | 0.9362 (5) | 0.17348 (17) | 0.0470 (11) | |
C6 | 0.4645 (4) | 0.8456 (5) | 0.12563 (17) | 0.0504 (11) | |
C7 | 0.5111 (4) | 0.7483 (6) | 0.09242 (19) | 0.0708 (14) | |
H7 | 0.5904 | 0.7248 | 0.0949 | 0.085* | |
C8 | 0.4147 (4) | 0.6935 (6) | 0.0548 (2) | 0.0727 (15) | |
H8 | 0.4187 | 0.6258 | 0.0268 | 0.087* | |
C9 | 0.1397 (4) | 0.4507 (6) | −0.0809 (2) | 0.0657 (13) | |
H9 | 0.2208 | 0.4457 | −0.0667 | 0.079* | |
C10 | 0.0916 (5) | 0.3499 (6) | −0.1224 (2) | 0.0731 (14) | |
H10 | 0.1390 | 0.2807 | −0.1362 | 0.088* | |
C11 | −0.0290 (5) | 0.3556 (6) | −0.14265 (19) | 0.0741 (15) | |
H11 | −0.0648 | 0.2889 | −0.1703 | 0.089* | |
C12 | −0.0958 (4) | 0.4609 (5) | −0.12148 (18) | 0.0635 (13) | |
H12 | −0.1774 | 0.4655 | −0.1344 | 0.076* | |
C13 | −0.0391 (4) | 0.5615 (5) | −0.08009 (16) | 0.0476 (11) | |
C14 | −0.1064 (4) | 0.6755 (5) | −0.05658 (16) | 0.0484 (11) | |
C15 | −0.2255 (4) | 0.7133 (6) | −0.06914 (19) | 0.0658 (14) | |
H15 | −0.2846 | 0.6698 | −0.0959 | 0.079* | |
C16 | −0.2375 (4) | 0.8301 (6) | −0.03316 (19) | 0.0653 (14) | |
H16 | −0.3081 | 0.8796 | −0.0318 | 0.078* | |
N1 | 0.4493 (3) | 1.0192 (4) | 0.19734 (15) | 0.0632 (11) | |
N2 | 0.3451 (3) | 0.8464 (4) | 0.10893 (14) | 0.0544 (10) | |
N3 | 0.3148 (3) | 0.7521 (4) | 0.06469 (15) | 0.0619 (10) | |
N4 | 0.0777 (3) | 0.5539 (4) | −0.05982 (14) | 0.0555 (10) | |
N5 | −0.0503 (3) | 0.7659 (4) | −0.01505 (14) | 0.0518 (9) | |
N6 | −0.1319 (3) | 0.8612 (4) | −0.00053 (14) | 0.0552 (10) | |
Ag3 | −0.08697 (3) | 1.00054 (4) | 0.069660 (14) | 0.06312 (13) | |
N7 | −0.2477 (3) | 1.1562 (4) | 0.10333 (16) | 0.0636 (11) | |
N8 | −0.0152 (3) | 1.0984 (4) | 0.14786 (13) | 0.0522 (9) | |
C17 | −0.3626 (5) | 1.1848 (6) | 0.0800 (2) | 0.0807 (16) | |
H17 | −0.3968 | 1.1320 | 0.0484 | 0.097* | |
C21 | −0.1995 (4) | 1.2328 (5) | 0.1486 (2) | 0.0568 (12) | |
C22 | −0.0746 (4) | 1.1992 (5) | 0.17237 (18) | 0.0531 (12) | |
N9 | 0.0977 (3) | 1.0881 (4) | 0.17771 (14) | 0.0565 (10) | |
C18 | −0.4303 (5) | 1.2879 (8) | 0.1008 (3) | 0.101 (2) | |
H18 | −0.5090 | 1.3046 | 0.0836 | 0.122* | |
C20 | −0.2641 (5) | 1.3382 (6) | 0.1718 (2) | 0.0766 (15) | |
H20 | −0.2292 | 1.3894 | 0.2035 | 0.092* | |
C23 | 0.0005 (4) | 1.2554 (5) | 0.21894 (19) | 0.0638 (13) | |
H23 | −0.0174 | 1.3265 | 0.2435 | 0.077* | |
C24 | 0.1063 (4) | 1.1833 (6) | 0.22055 (19) | 0.0667 (13) | |
H24 | 0.1745 | 1.1978 | 0.2474 | 0.080* | |
C19 | −0.3813 (6) | 1.3662 (7) | 0.1470 (3) | 0.099 (2) | |
H19 | −0.4260 | 1.4372 | 0.1617 | 0.118* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0523 (2) | 0.0727 (3) | 0.0678 (3) | 0.01114 (19) | 0.00901 (18) | −0.0029 (2) |
Ag2 | 0.0542 (2) | 0.0702 (3) | 0.0589 (2) | −0.00637 (19) | −0.00713 (17) | 0.0037 (2) |
C1 | 0.076 (4) | 0.073 (4) | 0.075 (4) | 0.002 (3) | 0.016 (3) | −0.020 (3) |
C2 | 0.072 (4) | 0.073 (4) | 0.060 (3) | −0.002 (3) | −0.009 (3) | −0.011 (3) |
C3 | 0.051 (3) | 0.066 (3) | 0.069 (4) | 0.001 (3) | −0.010 (3) | 0.000 (3) |
C4 | 0.052 (3) | 0.059 (3) | 0.059 (3) | 0.005 (2) | 0.005 (2) | 0.003 (3) |
C5 | 0.043 (3) | 0.046 (3) | 0.049 (3) | 0.004 (2) | 0.004 (2) | 0.006 (2) |
C6 | 0.046 (3) | 0.052 (3) | 0.049 (3) | 0.009 (2) | 0.001 (2) | 0.002 (2) |
C7 | 0.052 (3) | 0.085 (4) | 0.072 (3) | 0.018 (3) | 0.007 (3) | −0.017 (3) |
C8 | 0.068 (3) | 0.076 (4) | 0.069 (4) | 0.014 (3) | 0.005 (3) | −0.019 (3) |
C9 | 0.064 (3) | 0.065 (4) | 0.071 (4) | −0.001 (3) | 0.022 (3) | 0.005 (3) |
C10 | 0.094 (4) | 0.058 (4) | 0.075 (4) | 0.004 (3) | 0.035 (3) | −0.001 (3) |
C11 | 0.094 (4) | 0.068 (4) | 0.060 (4) | −0.012 (3) | 0.017 (3) | −0.016 (3) |
C12 | 0.067 (3) | 0.070 (4) | 0.051 (3) | −0.008 (3) | 0.007 (3) | −0.009 (3) |
C13 | 0.053 (3) | 0.052 (3) | 0.038 (3) | −0.007 (2) | 0.010 (2) | 0.003 (2) |
C14 | 0.047 (3) | 0.055 (3) | 0.037 (3) | −0.007 (2) | −0.003 (2) | 0.005 (2) |
C15 | 0.053 (3) | 0.079 (4) | 0.059 (3) | −0.003 (3) | −0.001 (2) | −0.007 (3) |
C16 | 0.052 (3) | 0.072 (4) | 0.066 (4) | 0.005 (3) | 0.001 (3) | 0.004 (3) |
N1 | 0.052 (2) | 0.071 (3) | 0.060 (3) | 0.006 (2) | 0.000 (2) | −0.011 (2) |
N2 | 0.046 (2) | 0.056 (2) | 0.057 (2) | 0.0048 (18) | 0.0026 (18) | −0.007 (2) |
N3 | 0.059 (2) | 0.062 (3) | 0.059 (3) | 0.008 (2) | 0.002 (2) | −0.007 (2) |
N4 | 0.054 (2) | 0.056 (3) | 0.056 (2) | 0.0006 (19) | 0.012 (2) | −0.001 (2) |
N5 | 0.052 (2) | 0.052 (2) | 0.048 (2) | −0.002 (2) | 0.0045 (18) | −0.0009 (19) |
N6 | 0.053 (2) | 0.059 (3) | 0.049 (2) | 0.003 (2) | 0.0016 (19) | −0.0032 (19) |
Ag3 | 0.0699 (3) | 0.0608 (3) | 0.0563 (2) | −0.00182 (19) | 0.00949 (19) | −0.00739 (19) |
N7 | 0.055 (3) | 0.067 (3) | 0.071 (3) | 0.008 (2) | 0.018 (2) | 0.006 (2) |
N8 | 0.048 (2) | 0.055 (2) | 0.052 (2) | 0.0061 (18) | 0.0074 (19) | −0.0068 (19) |
C17 | 0.066 (4) | 0.082 (4) | 0.093 (4) | 0.004 (3) | 0.014 (3) | 0.010 (3) |
C21 | 0.061 (3) | 0.049 (3) | 0.069 (3) | 0.001 (2) | 0.034 (3) | 0.009 (3) |
C22 | 0.061 (3) | 0.049 (3) | 0.055 (3) | 0.001 (2) | 0.025 (3) | 0.003 (2) |
N9 | 0.054 (2) | 0.059 (2) | 0.055 (2) | 0.0018 (19) | 0.009 (2) | −0.007 (2) |
C18 | 0.061 (4) | 0.106 (5) | 0.144 (7) | 0.024 (4) | 0.039 (4) | 0.022 (5) |
C20 | 0.090 (4) | 0.066 (4) | 0.082 (4) | 0.016 (3) | 0.038 (3) | 0.007 (3) |
C23 | 0.081 (3) | 0.058 (3) | 0.058 (3) | 0.006 (3) | 0.026 (3) | −0.003 (3) |
C24 | 0.074 (4) | 0.067 (3) | 0.055 (3) | −0.009 (3) | 0.006 (3) | −0.007 (3) |
C19 | 0.092 (5) | 0.093 (5) | 0.125 (6) | 0.033 (4) | 0.053 (4) | 0.016 (4) |
Ag1—N9 | 2.110 (4) | C13—N4 | 1.338 (5) |
Ag1—N2 | 2.129 (4) | C13—C14 | 1.460 (6) |
Ag1—N1 | 2.617 (4) | C14—N5 | 1.354 (5) |
Ag2—N3 | 2.127 (4) | C14—C15 | 1.384 (6) |
Ag2—N5 | 2.162 (4) | C15—C16 | 1.385 (6) |
Ag2—N4 | 2.547 (4) | C15—H15 | 0.9300 |
Ag2—Ag3i | 3.1274 (17) | C16—N6 | 1.343 (5) |
C1—N1 | 1.340 (5) | C16—H16 | 0.9300 |
C1—C2 | 1.389 (6) | N2—N3 | 1.368 (4) |
C1—H1 | 0.9300 | N5—N6 | 1.361 (4) |
C2—C3 | 1.363 (6) | N6—Ag3 | 2.117 (4) |
C2—H2 | 0.9300 | Ag3—N8 | 2.151 (4) |
C3—C4 | 1.380 (6) | Ag3—N7 | 2.590 (4) |
C3—H3 | 0.9300 | Ag3—Ag2i | 3.1274 (17) |
C4—C5 | 1.387 (5) | N7—C21 | 1.337 (5) |
C4—H4 | 0.9300 | N7—C17 | 1.354 (6) |
C5—N1 | 1.341 (5) | N8—C22 | 1.343 (5) |
C5—C6 | 1.470 (5) | N8—N9 | 1.362 (4) |
C6—N2 | 1.354 (5) | C17—C18 | 1.365 (7) |
C6—C7 | 1.382 (6) | C17—H17 | 0.9300 |
C7—C8 | 1.381 (6) | C21—C20 | 1.387 (6) |
C7—H7 | 0.9300 | C21—C22 | 1.467 (6) |
C8—N3 | 1.338 (5) | C22—C23 | 1.391 (6) |
C8—H8 | 0.9300 | N9—C24 | 1.349 (5) |
C9—N4 | 1.326 (5) | C18—C19 | 1.365 (8) |
C9—C10 | 1.383 (6) | C18—H18 | 0.9300 |
C9—H9 | 0.9300 | C20—C19 | 1.385 (7) |
C10—C11 | 1.378 (6) | C20—H20 | 0.9300 |
C10—H10 | 0.9300 | C23—C24 | 1.365 (6) |
C11—C12 | 1.376 (6) | C23—H23 | 0.9300 |
C11—H11 | 0.9300 | C24—H24 | 0.9300 |
C12—C13 | 1.406 (6) | C19—H19 | 0.9300 |
C12—H12 | 0.9300 | ||
N9—Ag1—N2 | 171.09 (14) | C5—N1—C1 | 118.1 (4) |
N9—Ag1—N1 | 116.95 (14) | C5—N1—Ag1 | 109.6 (3) |
N2—Ag1—N1 | 69.66 (13) | C1—N1—Ag1 | 132.3 (3) |
N3—Ag2—N5 | 168.08 (14) | C6—N2—N3 | 108.1 (3) |
N3—Ag2—N4 | 120.99 (13) | C6—N2—Ag1 | 124.4 (3) |
N5—Ag2—N4 | 70.93 (13) | N3—N2—Ag1 | 127.4 (3) |
N3—Ag2—Ag3i | 111.26 (10) | C8—N3—N2 | 107.7 (4) |
N5—Ag2—Ag3i | 68.36 (9) | C8—N3—Ag2 | 130.9 (3) |
N4—Ag2—Ag3i | 84.05 (10) | N2—N3—Ag2 | 120.9 (3) |
N1—C1—C2 | 123.6 (5) | C9—N4—C13 | 118.0 (4) |
N1—C1—H1 | 118.2 | C9—N4—Ag2 | 131.7 (3) |
C2—C1—H1 | 118.2 | C13—N4—Ag2 | 110.2 (3) |
C3—C2—C1 | 118.0 (4) | C14—N5—N6 | 108.3 (3) |
C3—C2—H2 | 121.0 | C14—N5—Ag2 | 121.5 (3) |
C1—C2—H2 | 121.0 | N6—N5—Ag2 | 130.1 (3) |
C2—C3—C4 | 119.1 (4) | C16—N6—N5 | 107.8 (4) |
C2—C3—H3 | 120.4 | C16—N6—Ag3 | 130.7 (3) |
C4—C3—H3 | 120.4 | N5—N6—Ag3 | 120.9 (3) |
C3—C4—C5 | 120.1 (4) | N6—Ag3—N8 | 166.96 (13) |
C3—C4—H4 | 119.9 | N6—Ag3—N7 | 120.80 (14) |
C5—C4—H4 | 119.9 | N8—Ag3—N7 | 69.45 (14) |
N1—C5—C4 | 121.0 (4) | N6—Ag3—Ag2i | 79.27 (11) |
N1—C5—C6 | 116.7 (4) | N8—Ag3—Ag2i | 111.59 (10) |
C4—C5—C6 | 122.3 (4) | N7—Ag3—Ag2i | 81.24 (9) |
N2—C6—C7 | 108.9 (4) | C21—N7—C17 | 118.1 (4) |
N2—C6—C5 | 119.5 (4) | C21—N7—Ag3 | 110.3 (3) |
C7—C6—C5 | 131.5 (4) | C17—N7—Ag3 | 131.1 (4) |
C8—C7—C6 | 105.3 (4) | C22—N8—N9 | 108.1 (4) |
C8—C7—H7 | 127.4 | C22—N8—Ag3 | 123.4 (3) |
C6—C7—H7 | 127.4 | N9—N8—Ag3 | 128.0 (3) |
N3—C8—C7 | 110.0 (4) | C18—C17—N7 | 122.7 (5) |
N3—C8—H8 | 125.0 | C18—C17—H17 | 118.6 |
C7—C8—H8 | 125.0 | N7—C17—H17 | 118.6 |
N4—C9—C10 | 124.3 (5) | N7—C21—C20 | 121.7 (5) |
N4—C9—H9 | 117.8 | N7—C21—C22 | 116.3 (4) |
C10—C9—H9 | 117.8 | C20—C21—C22 | 122.0 (5) |
C9—C10—C11 | 117.8 (5) | N8—C22—C23 | 109.4 (4) |
C9—C10—H10 | 121.1 | N8—C22—C21 | 119.7 (4) |
C11—C10—H10 | 121.1 | C23—C22—C21 | 130.9 (4) |
C12—C11—C10 | 119.3 (5) | C24—N9—N8 | 107.5 (3) |
C12—C11—H11 | 120.3 | C24—N9—Ag1 | 130.9 (3) |
C10—C11—H11 | 120.3 | N8—N9—Ag1 | 119.8 (3) |
C11—C12—C13 | 119.1 (5) | C17—C18—C19 | 119.3 (6) |
C11—C12—H12 | 120.5 | C17—C18—H18 | 120.3 |
C13—C12—H12 | 120.5 | C19—C18—H18 | 120.4 |
N4—C13—C12 | 121.5 (4) | C21—C20—C19 | 119.2 (5) |
N4—C13—C14 | 117.5 (4) | C21—C20—H20 | 120.4 |
C12—C13—C14 | 121.0 (4) | C19—C20—H20 | 120.4 |
N5—C14—C15 | 109.0 (4) | C24—C23—C22 | 104.8 (4) |
N5—C14—C13 | 119.8 (4) | C24—C23—H23 | 127.6 |
C15—C14—C13 | 131.2 (4) | C22—C23—H23 | 127.6 |
C14—C15—C16 | 105.0 (4) | N9—C24—C23 | 110.3 (4) |
C14—C15—H15 | 127.5 | N9—C24—H24 | 124.9 |
C16—C15—H15 | 127.5 | C23—C24—H24 | 124.9 |
N6—C16—C15 | 109.9 (4) | C18—C19—C20 | 119.0 (6) |
N6—C16—H16 | 125.1 | C18—C19—H19 | 120.5 |
C15—C16—H16 | 125.1 | C20—C19—H19 | 120.5 |
Symmetry code: (i) −x, −y+2, −z. |
Experimental details
Crystal data | |
Chemical formula | [Ag3(C8H6N3)3] |
Mr | 756.07 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 294 |
a, b, c (Å) | 11.597 (9), 8.555 (6), 25.52 (2) |
β (°) | 103.018 (9) |
V (Å3) | 2467 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.39 |
Crystal size (mm) | 0.10 × 0.10 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.796, 0.832 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12411, 4294, 2947 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.064, 1.00 |
No. of reflections | 4294 |
No. of parameters | 325 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.41, −0.41 |
Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2003), SHELXTL (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008).
Acknowledgements
The authors acknowledge financial support from the program for Talent Introduction in Guangdong Higher Education Institutions and the Scientific Research Start-up Funds of Talent Introduction in Maoming University.
References
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2002). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2003). SAINT-Plus. Bruker AXS Inc, Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Ward, M. D., Fleming, J. S., Psillakis, E., Jeffery, J. C. & McCleverty, J. A. (1998). Acta Cryst. C54, 609–612. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Ward, M. D., McCleverty, J. A. & Jeffery, J. C. (2001). Coord. Chem. Rev. 222, 251–272. Web of Science CrossRef CAS Google Scholar
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Deprotonated 3-(2-pyridyl)pyrazole is a potentially tridentate ligands and it's derivatives have been widely used for the construction of supramolecular architectures by their ability of producing coordination compounds (Ward et al. 1998; 2001). As a continuation of these studies, we now report the crystal structure of the title complex.
As shown in figure 1, the asymmetric unit contains three silver cations and three depronated 5-(2-pyridyl)pyrazol-1-ide ligands. Each silver cation is chelated with one 5-(2-pyridyl)pyrazol-1-ide ligand, which in addition acts as a bridging ligand towards the next silver ion via the second pyrazole nitrogen.
In summary, three silver cations and three depronated 5-(2-pyridyl)pyrazol-1-ide ligands produce a macrocyclic trimeric coordination oligomer that exhibits an almost planar conformation. In addition, short non-bonding Ag-Ag interactions (3.127 (2) Å) are observed.