metal-organic compounds
Tetrakis[μ-1,3-bis(4,5-dihydro-1,3-oxazol-2-yl)benzene-κ2N:N′]trisilver(I) tris(hexafluoridophosphate)
aDepartment of Chemistry, Chung-Yuan Christian University, Jhongli 32023, Taiwan, bDepartment of Creative Fashion Design, Taoyuan Innovation Institute of Technology, Jhongli 32091, Taiwan, cDepartment of Materials Science and Engineering, Vanung University, Jhongli 32061, Taiwan, and dDepartment of Chemistry, Soochow University, Taipei, Taiwan
*Correspondence e-mail: sun@tiit.edu.tw
In the title compound, [Ag3(C12H12N2O2)4](PF6)3, one AgI ion, lying on a twofold rotation axis, is coordinated by four N atoms from four 1,3-bis(4,5-dihydro-1,3-oxazol-2-yl)benzene (L) ligands in a distorted tetrahedral geometry and the other AgI ion is coordinated by two N atoms from two L ligands in a bent arrangement [N—Ag—N = 169.03 (17)°]. Two L ligands adopt a syn conformation, while the other two adopt an anti conformation. They bridge adjacent AgI ions, forming a trinuclear complex. One of the PF6− anions is half-occupied, with the P atom located on a twofold rotation axis. The PF6− anions link the complex molecules via Ag⋯F interactions [2.80 (2) and 2.85 (2) Å] into a polymeric chain along [100].
Related literature
For related structures incorporating the 1,4-bis(4,5-dihydro-2-oxazolyl)benzene ligand, see: Suen et al. (2011); Wang et al. (2008, 2011a,b); Yeh et al. (2011).
Experimental
Crystal data
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Refinement
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Data collection: XSCANS (Siemens, 1995); cell XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Supporting information
10.1107/S1600536812034721/hy2575sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812034721/hy2575Isup2.hkl
An aqueous solution (5.0 ml) of AgPF6 (3.0 mmol) was layered carefully over a methanolic solution (5.0 ml) of 1,3-bis(4,5-dihydro-2-oxazolyl)benzene (4.0 mmol) in a tube and kept it in dark. Colourless crystals were obtained after several weeks. These were washed with methanol and collected in 75.8% yield.
H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 (phenyl) and 0.97 (methylene) Å and with Uiso(H) = 1.2Ueq(C).
Data collection: XSCANS (Siemens, 1995); cell
XSCANS (Siemens, 1995); data reduction: XSCANS (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).[Ag3(C12H12N2O2)4](PF6)3 | F(000) = 3216 |
Mr = 1623.46 | Dx = 1.908 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 36 reflections |
a = 22.7473 (16) Å | θ = 4.8–12.5° |
b = 11.4521 (19) Å | µ = 1.23 mm−1 |
c = 24.1382 (15) Å | T = 298 K |
β = 116.014 (7)° | Plate, colourless |
V = 5651.0 (11) Å3 | 0.60 × 0.40 × 0.30 mm |
Z = 4 |
Siemens P4 four-circle diffractometer | 3885 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.020 |
Graphite monochromator | θmax = 25.0°, θmin = 2.0° |
ω scans | h = 0→26 |
Absorption correction: ψ scan (XSCANS; Siemens, 1995) | k = 0→13 |
Tmin = 0.634, Tmax = 0.964 | l = −28→25 |
5107 measured reflections | 3 standard reflections every 297 reflections |
4976 independent reflections | intensity decay: 2.0% |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0628P)2 + 34.3783P] where P = (Fo2 + 2Fc2)/3 |
4976 reflections | (Δ/σ)max < 0.001 |
425 parameters | Δρmax = 1.02 e Å−3 |
0 restraints | Δρmin = −0.81 e Å−3 |
[Ag3(C12H12N2O2)4](PF6)3 | V = 5651.0 (11) Å3 |
Mr = 1623.46 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 22.7473 (16) Å | µ = 1.23 mm−1 |
b = 11.4521 (19) Å | T = 298 K |
c = 24.1382 (15) Å | 0.60 × 0.40 × 0.30 mm |
β = 116.014 (7)° |
Siemens P4 four-circle diffractometer | 3885 reflections with I > 2σ(I) |
Absorption correction: ψ scan (XSCANS; Siemens, 1995) | Rint = 0.020 |
Tmin = 0.634, Tmax = 0.964 | 3 standard reflections every 297 reflections |
5107 measured reflections | intensity decay: 2.0% |
4976 independent reflections |
R[F2 > 2σ(F2)] = 0.050 | 0 restraints |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0628P)2 + 34.3783P] where P = (Fo2 + 2Fc2)/3 |
4976 reflections | Δρmax = 1.02 e Å−3 |
425 parameters | Δρmin = −0.81 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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ag1 | 0.5000 | 0.06276 (6) | 0.2500 | 0.0564 (2) | |
Ag2 | 0.18074 (2) | 0.04964 (5) | 0.26872 (2) | 0.05790 (18) | |
O11 | 0.31412 (19) | −0.1417 (4) | 0.19947 (19) | 0.0637 (11) | |
O31 | 0.3068 (2) | −0.0441 (4) | 0.45572 (19) | 0.0675 (12) | |
O41 | 0.3592 (2) | 0.2537 (5) | 0.08323 (18) | 0.0694 (13) | |
O61 | 0.14979 (18) | 0.1693 (4) | 0.09064 (16) | 0.0532 (9) | |
N11 | 0.4086 (2) | −0.0591 (4) | 0.2133 (2) | 0.0488 (11) | |
N31 | 0.2312 (2) | 0.0070 (4) | 0.3628 (2) | 0.0507 (11) | |
N41 | 0.4514 (2) | 0.1949 (5) | 0.1635 (2) | 0.0558 (12) | |
N61 | 0.1478 (2) | 0.1039 (4) | 0.1765 (2) | 0.0491 (11) | |
C11 | 0.3711 (2) | −0.0898 (5) | 0.2366 (3) | 0.0458 (12) | |
C12 | 0.3785 (3) | −0.0977 (6) | 0.1487 (3) | 0.0580 (15) | |
H12A | 0.4034 | −0.1606 | 0.1423 | 0.070* | |
H12B | 0.3753 | −0.0337 | 0.1212 | 0.070* | |
C13 | 0.3111 (3) | −0.1394 (7) | 0.1382 (3) | 0.0712 (19) | |
H13A | 0.2774 | −0.0860 | 0.1116 | 0.085* | |
H13B | 0.3021 | −0.2166 | 0.1198 | 0.085* | |
C21 | 0.3827 (3) | −0.0752 (5) | 0.3012 (3) | 0.0465 (12) | |
C22 | 0.3315 (3) | −0.0577 (5) | 0.3166 (2) | 0.0457 (12) | |
H22A | 0.2888 | −0.0556 | 0.2856 | 0.055* | |
C23 | 0.3426 (3) | −0.0434 (5) | 0.3773 (2) | 0.0469 (12) | |
C24 | 0.4070 (3) | −0.0470 (6) | 0.4234 (3) | 0.0657 (17) | |
H24A | 0.4155 | −0.0356 | 0.4644 | 0.079* | |
C25 | 0.4578 (3) | −0.0674 (6) | 0.4080 (3) | 0.0710 (19) | |
H25A | 0.5003 | −0.0719 | 0.4390 | 0.085* | |
C26 | 0.4465 (3) | −0.0810 (6) | 0.3481 (3) | 0.0639 (17) | |
H26A | 0.4813 | −0.0942 | 0.3384 | 0.077* | |
C31 | 0.2900 (3) | −0.0254 (5) | 0.3960 (2) | 0.0506 (13) | |
C32 | 0.1977 (3) | 0.0162 (6) | 0.4034 (3) | 0.0629 (16) | |
H32A | 0.1619 | −0.0390 | 0.3911 | 0.075* | |
H32B | 0.1809 | 0.0944 | 0.4023 | 0.075* | |
C33 | 0.2505 (4) | −0.0123 (8) | 0.4664 (3) | 0.080 (2) | |
H33A | 0.2603 | 0.0549 | 0.4936 | 0.096* | |
H33B | 0.2374 | −0.0768 | 0.4846 | 0.096* | |
C41 | 0.3914 (3) | 0.2206 (5) | 0.1427 (2) | 0.0464 (12) | |
C42 | 0.4700 (3) | 0.2166 (8) | 0.1130 (3) | 0.081 (2) | |
H42A | 0.4845 | 0.1450 | 0.1013 | 0.098* | |
H42B | 0.5049 | 0.2738 | 0.1252 | 0.098* | |
C43 | 0.4086 (3) | 0.2623 (8) | 0.0603 (3) | 0.080 (2) | |
H43A | 0.4142 | 0.3426 | 0.0508 | 0.096* | |
H43B | 0.3968 | 0.2150 | 0.0237 | 0.096* | |
C51 | 0.3518 (2) | 0.2183 (5) | 0.1772 (2) | 0.0429 (12) | |
C52 | 0.2861 (2) | 0.1886 (5) | 0.1481 (2) | 0.0430 (12) | |
H52A | 0.2663 | 0.1709 | 0.1062 | 0.052* | |
C53 | 0.2499 (2) | 0.1855 (4) | 0.1822 (2) | 0.0407 (11) | |
C54 | 0.2793 (3) | 0.2170 (5) | 0.2441 (2) | 0.0469 (13) | |
H54A | 0.2550 | 0.2162 | 0.2667 | 0.056* | |
C55 | 0.3442 (3) | 0.2492 (5) | 0.2721 (3) | 0.0516 (14) | |
H55A | 0.3635 | 0.2712 | 0.3134 | 0.062* | |
C56 | 0.3809 (3) | 0.2492 (5) | 0.2392 (3) | 0.0495 (13) | |
H56A | 0.4249 | 0.2697 | 0.2584 | 0.059* | |
C61 | 0.1804 (2) | 0.1498 (5) | 0.1510 (2) | 0.0427 (12) | |
C62 | 0.0795 (3) | 0.0839 (7) | 0.1278 (3) | 0.0641 (18) | |
H62A | 0.0479 | 0.1267 | 0.1368 | 0.077* | |
H62B | 0.0684 | 0.0015 | 0.1238 | 0.077* | |
C63 | 0.0821 (3) | 0.1300 (6) | 0.0701 (3) | 0.0555 (14) | |
H63A | 0.0713 | 0.0690 | 0.0393 | 0.067* | |
H63B | 0.0518 | 0.1943 | 0.0527 | 0.067* | |
P1 | 0.5000 | 0.4236 (2) | 0.7500 | 0.0619 (6) | |
F1 | 0.5316 (14) | 0.3242 (15) | 0.7277 (12) | 0.136 (9) | 0.50 |
F2 | 0.4658 (10) | 0.5162 (10) | 0.7741 (9) | 0.102 (4) | 0.50 |
F3 | 0.5624 (8) | 0.503 (2) | 0.7726 (12) | 0.172 (9) | 0.50 |
F4 | 0.4740 (10) | 0.490 (2) | 0.6891 (7) | 0.151 (6) | 0.50 |
F5 | 0.5275 (10) | 0.3615 (19) | 0.8141 (7) | 0.135 (5) | 0.50 |
F6 | 0.4354 (9) | 0.3566 (19) | 0.7311 (13) | 0.156 (8) | 0.50 |
P2 | 0.12182 (9) | 0.19994 (18) | 0.52246 (10) | 0.0733 (5) | |
F7 | 0.0734 (4) | 0.1210 (9) | 0.4738 (4) | 0.231 (5) | |
F8 | 0.0936 (4) | 0.2993 (9) | 0.4800 (5) | 0.241 (6) | |
F9 | 0.1540 (4) | 0.1000 (7) | 0.5635 (6) | 0.266 (7) | |
F10 | 0.0687 (4) | 0.2167 (15) | 0.5419 (5) | 0.290 (8) | |
F11 | 0.1701 (3) | 0.2775 (6) | 0.5752 (3) | 0.156 (3) | |
F12 | 0.1760 (4) | 0.1934 (12) | 0.5037 (4) | 0.248 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0330 (3) | 0.0662 (4) | 0.0635 (4) | 0.000 | 0.0150 (3) | 0.000 |
Ag2 | 0.0457 (3) | 0.0879 (4) | 0.0438 (3) | 0.0038 (2) | 0.0231 (2) | 0.0128 (2) |
O11 | 0.045 (2) | 0.090 (3) | 0.059 (2) | −0.027 (2) | 0.0255 (19) | −0.016 (2) |
O31 | 0.082 (3) | 0.080 (3) | 0.041 (2) | 0.009 (2) | 0.028 (2) | 0.010 (2) |
O41 | 0.056 (2) | 0.114 (4) | 0.048 (2) | 0.017 (3) | 0.031 (2) | 0.018 (2) |
O61 | 0.042 (2) | 0.075 (3) | 0.042 (2) | 0.0003 (19) | 0.0179 (16) | 0.0088 (19) |
N11 | 0.035 (2) | 0.057 (3) | 0.057 (3) | −0.008 (2) | 0.023 (2) | −0.003 (2) |
N31 | 0.054 (3) | 0.059 (3) | 0.042 (2) | −0.003 (2) | 0.024 (2) | 0.004 (2) |
N41 | 0.039 (3) | 0.080 (4) | 0.056 (3) | 0.005 (2) | 0.029 (2) | 0.011 (2) |
N61 | 0.035 (2) | 0.074 (3) | 0.043 (2) | 0.004 (2) | 0.0216 (19) | 0.007 (2) |
C11 | 0.036 (3) | 0.043 (3) | 0.056 (3) | 0.000 (2) | 0.017 (2) | 0.000 (2) |
C12 | 0.048 (3) | 0.067 (4) | 0.063 (4) | −0.009 (3) | 0.029 (3) | −0.009 (3) |
C13 | 0.063 (4) | 0.096 (5) | 0.057 (4) | −0.026 (4) | 0.029 (3) | −0.019 (4) |
C21 | 0.039 (3) | 0.046 (3) | 0.053 (3) | −0.006 (2) | 0.018 (2) | 0.001 (2) |
C22 | 0.040 (3) | 0.045 (3) | 0.044 (3) | −0.003 (2) | 0.011 (2) | 0.003 (2) |
C23 | 0.043 (3) | 0.046 (3) | 0.045 (3) | −0.003 (2) | 0.013 (2) | 0.005 (2) |
C24 | 0.066 (4) | 0.074 (4) | 0.041 (3) | −0.009 (3) | 0.008 (3) | 0.005 (3) |
C25 | 0.045 (3) | 0.087 (5) | 0.059 (4) | −0.003 (3) | 0.001 (3) | 0.011 (3) |
C26 | 0.037 (3) | 0.075 (4) | 0.069 (4) | −0.003 (3) | 0.014 (3) | 0.008 (3) |
C31 | 0.065 (4) | 0.047 (3) | 0.038 (3) | −0.005 (3) | 0.021 (3) | 0.002 (2) |
C32 | 0.076 (4) | 0.064 (4) | 0.064 (4) | 0.001 (3) | 0.045 (3) | 0.005 (3) |
C33 | 0.087 (5) | 0.112 (6) | 0.050 (4) | −0.007 (5) | 0.039 (4) | −0.001 (4) |
C41 | 0.047 (3) | 0.051 (3) | 0.046 (3) | 0.000 (2) | 0.024 (2) | 0.001 (2) |
C42 | 0.065 (4) | 0.126 (7) | 0.074 (4) | 0.016 (4) | 0.050 (4) | 0.027 (4) |
C43 | 0.069 (4) | 0.128 (7) | 0.061 (4) | 0.005 (4) | 0.046 (4) | 0.011 (4) |
C51 | 0.039 (3) | 0.048 (3) | 0.045 (3) | 0.007 (2) | 0.021 (2) | 0.005 (2) |
C52 | 0.042 (3) | 0.050 (3) | 0.041 (3) | 0.006 (2) | 0.021 (2) | 0.004 (2) |
C53 | 0.035 (3) | 0.045 (3) | 0.044 (3) | 0.007 (2) | 0.019 (2) | 0.004 (2) |
C54 | 0.045 (3) | 0.059 (3) | 0.045 (3) | 0.010 (3) | 0.027 (2) | 0.005 (2) |
C55 | 0.049 (3) | 0.065 (4) | 0.044 (3) | −0.001 (3) | 0.023 (3) | −0.006 (3) |
C56 | 0.039 (3) | 0.060 (4) | 0.050 (3) | 0.003 (3) | 0.020 (2) | 0.000 (3) |
C61 | 0.040 (3) | 0.047 (3) | 0.043 (3) | 0.008 (2) | 0.021 (2) | 0.004 (2) |
C62 | 0.035 (3) | 0.109 (5) | 0.047 (3) | −0.011 (3) | 0.017 (2) | 0.005 (3) |
C63 | 0.041 (3) | 0.071 (4) | 0.049 (3) | 0.004 (3) | 0.015 (2) | 0.006 (3) |
P1 | 0.0493 (12) | 0.0745 (16) | 0.0784 (16) | 0.000 | 0.0431 (12) | 0.000 |
F1 | 0.21 (3) | 0.091 (9) | 0.20 (2) | 0.038 (14) | 0.18 (2) | 0.011 (13) |
F2 | 0.124 (13) | 0.075 (6) | 0.157 (12) | 0.029 (8) | 0.108 (11) | 0.014 (8) |
F3 | 0.071 (9) | 0.21 (2) | 0.23 (2) | −0.047 (10) | 0.064 (13) | −0.034 (19) |
F4 | 0.142 (13) | 0.225 (18) | 0.118 (11) | 0.074 (14) | 0.086 (11) | 0.076 (12) |
F5 | 0.157 (13) | 0.161 (15) | 0.105 (9) | 0.074 (12) | 0.074 (9) | 0.066 (10) |
F6 | 0.101 (11) | 0.142 (19) | 0.25 (3) | −0.054 (11) | 0.101 (15) | −0.039 (16) |
P2 | 0.0472 (9) | 0.0794 (13) | 0.0804 (12) | 0.0067 (9) | 0.0161 (9) | −0.0022 (10) |
F7 | 0.147 (7) | 0.200 (9) | 0.208 (9) | −0.008 (6) | −0.048 (6) | −0.083 (7) |
F8 | 0.140 (6) | 0.246 (11) | 0.283 (12) | 0.054 (7) | 0.043 (7) | 0.168 (10) |
F9 | 0.118 (6) | 0.153 (7) | 0.368 (14) | −0.043 (5) | −0.041 (7) | 0.137 (8) |
F10 | 0.091 (5) | 0.61 (2) | 0.194 (8) | 0.005 (9) | 0.086 (6) | −0.080 (12) |
F11 | 0.110 (5) | 0.137 (5) | 0.166 (6) | −0.005 (4) | 0.010 (4) | −0.052 (5) |
F12 | 0.139 (6) | 0.457 (18) | 0.165 (7) | 0.096 (9) | 0.082 (6) | −0.042 (9) |
Ag1—N11 | 2.331 (4) | C32—H32A | 0.9700 |
Ag1—N41 | 2.418 (5) | C32—H32B | 0.9700 |
Ag2—N31 | 2.104 (5) | C33—H33A | 0.9700 |
Ag2—N61 | 2.106 (4) | C33—H33B | 0.9700 |
O11—C11 | 1.348 (6) | C41—C51 | 1.472 (7) |
O11—C13 | 1.450 (7) | C42—C43 | 1.511 (10) |
O31—C31 | 1.335 (7) | C42—H42A | 0.9700 |
O31—C33 | 1.460 (8) | C42—H42B | 0.9700 |
O41—C41 | 1.348 (7) | C43—H43A | 0.9700 |
O41—C43 | 1.457 (7) | C43—H43B | 0.9700 |
O61—C61 | 1.329 (6) | C51—C52 | 1.387 (7) |
O61—C63 | 1.467 (7) | C51—C56 | 1.391 (7) |
N11—C11 | 1.260 (7) | C52—C53 | 1.396 (7) |
N11—C12 | 1.469 (7) | C52—H52A | 0.9300 |
N31—C31 | 1.276 (8) | C53—C54 | 1.391 (7) |
N31—C32 | 1.485 (7) | C53—C61 | 1.479 (7) |
N41—C41 | 1.264 (7) | C54—C55 | 1.378 (8) |
N41—C42 | 1.478 (7) | C54—H54A | 0.9300 |
N61—C61 | 1.269 (7) | C55—C56 | 1.382 (7) |
N61—C62 | 1.498 (7) | C55—H55A | 0.9300 |
C11—C21 | 1.474 (8) | C56—H56A | 0.9300 |
C12—C13 | 1.517 (8) | C62—C63 | 1.515 (8) |
C12—H12A | 0.9700 | C62—H62A | 0.9700 |
C12—H12B | 0.9700 | C62—H62B | 0.9700 |
C13—H13A | 0.9700 | C63—H63A | 0.9700 |
C13—H13B | 0.9700 | C63—H63B | 0.9700 |
C21—C22 | 1.384 (8) | P1—F4 | 1.527 (12) |
C21—C26 | 1.396 (8) | P1—F6 | 1.539 (16) |
C22—C23 | 1.383 (8) | P1—F1 | 1.562 (13) |
C22—H22A | 0.9300 | P1—F5 | 1.564 (11) |
C23—C24 | 1.398 (8) | P1—F3 | 1.566 (16) |
C23—C31 | 1.469 (8) | P1—F2 | 1.570 (11) |
C24—C25 | 1.380 (10) | P2—F8 | 1.476 (8) |
C24—H24A | 0.9300 | P2—F9 | 1.481 (7) |
C25—C26 | 1.363 (10) | P2—F12 | 1.488 (8) |
C25—H25A | 0.9300 | P2—F10 | 1.490 (7) |
C26—H26A | 0.9300 | P2—F7 | 1.509 (7) |
C32—C33 | 1.504 (10) | P2—F11 | 1.546 (6) |
N11—Ag1—N11i | 106.5 (2) | O61—C63—C62 | 104.7 (4) |
N11—Ag1—N41i | 134.17 (16) | O61—C63—H63A | 110.8 |
N11i—Ag1—N41i | 93.01 (17) | C62—C63—H63A | 110.8 |
N11—Ag1—N41 | 93.01 (17) | O61—C63—H63B | 110.8 |
N11i—Ag1—N41 | 134.17 (16) | C62—C63—H63B | 110.8 |
N41i—Ag1—N41 | 102.5 (3) | H63A—C63—H63B | 108.9 |
N31—Ag2—N61 | 169.03 (17) | F4ii—P1—F4 | 120 (2) |
C11—O11—C13 | 105.7 (4) | F4ii—P1—F6 | 116.9 (11) |
C31—O31—C33 | 107.0 (5) | F4—P1—F6 | 92.7 (16) |
C41—O41—C43 | 105.9 (5) | F4ii—P1—F6ii | 92.7 (16) |
C61—O61—C63 | 106.7 (4) | F4—P1—F6ii | 116.9 (11) |
C11—N11—C12 | 107.2 (4) | F6—P1—F6ii | 120.2 (18) |
C11—N11—Ag1 | 131.5 (4) | F4ii—P1—F1ii | 94.4 (10) |
C12—N11—Ag1 | 120.5 (3) | F6ii—P1—F1ii | 93.3 (12) |
C31—N31—C32 | 107.7 (5) | F4ii—P1—F1 | 130.8 (17) |
C31—N31—Ag2 | 132.2 (4) | F4—P1—F1 | 94.4 (10) |
C32—N31—Ag2 | 120.1 (4) | F6—P1—F1 | 93.3 (12) |
C41—N41—C42 | 106.4 (5) | F1ii—P1—F1 | 86.4 (13) |
C41—N41—Ag1 | 119.6 (4) | F4ii—P1—F5ii | 177.0 (16) |
C42—N41—Ag1 | 129.0 (4) | F4—P1—F5ii | 57.1 (9) |
C61—N61—C62 | 107.9 (4) | F6—P1—F5ii | 64.2 (9) |
C61—N61—Ag2 | 128.5 (4) | F6ii—P1—F5ii | 89.0 (10) |
C62—N61—Ag2 | 123.4 (3) | F1ii—P1—F5ii | 88.0 (11) |
N11—C11—O11 | 118.0 (5) | F1—P1—F5ii | 51.1 (9) |
N11—C11—C21 | 126.8 (5) | F4ii—P1—F5 | 57.1 (9) |
O11—C11—C21 | 115.2 (5) | F4—P1—F5 | 177.0 (17) |
N11—C12—C13 | 103.9 (5) | F6—P1—F5 | 89.0 (10) |
N11—C12—H12A | 111.0 | F6ii—P1—F5 | 64.2 (9) |
C13—C12—H12A | 111.0 | F1ii—P1—F5 | 51.1 (9) |
N11—C12—H12B | 111.0 | F1—P1—F5 | 88.0 (11) |
C13—C12—H12B | 111.0 | F5ii—P1—F5 | 125.9 (18) |
H12A—C12—H12B | 109.0 | F4ii—P1—F3 | 57.7 (9) |
O11—C13—C12 | 104.0 (5) | F4—P1—F3 | 87.4 (11) |
O11—C13—H13A | 111.0 | F6—P1—F3 | 173.3 (12) |
C12—C13—H13A | 111.0 | F6ii—P1—F3 | 65.4 (11) |
O11—C13—H13B | 111.0 | F1ii—P1—F3 | 141.7 (17) |
C12—C13—H13B | 111.0 | F1—P1—F3 | 93.3 (12) |
H13A—C13—H13B | 109.0 | F5ii—P1—F3 | 121.0 (10) |
C22—C21—C26 | 119.2 (6) | F5—P1—F3 | 90.6 (16) |
C22—C21—C11 | 121.3 (5) | F4ii—P1—F3ii | 87.4 (11) |
C26—C21—C11 | 119.5 (5) | F4—P1—F3ii | 57.7 (9) |
C23—C22—C21 | 121.1 (5) | F6—P1—F3ii | 65.4 (11) |
C23—C22—H22A | 119.4 | F6ii—P1—F3ii | 173.3 (12) |
C21—C22—H22A | 119.4 | F1ii—P1—F3ii | 93.3 (12) |
C22—C23—C24 | 118.8 (6) | F1—P1—F3ii | 141.7 (17) |
C22—C23—C31 | 123.2 (5) | F5ii—P1—F3ii | 90.6 (16) |
C24—C23—C31 | 118.0 (5) | F5—P1—F3ii | 121.0 (10) |
C25—C24—C23 | 119.9 (6) | F3—P1—F3ii | 109.4 (18) |
C25—C24—H24A | 120.0 | F4ii—P1—F2 | 49.6 (8) |
C23—C24—H24A | 120.0 | F4—P1—F2 | 88.4 (9) |
C26—C25—C24 | 121.0 (6) | F6—P1—F2 | 83.2 (11) |
C26—C25—H25A | 119.5 | F6ii—P1—F2 | 142.3 (15) |
C24—C25—H25A | 119.5 | F1ii—P1—F2 | 89.3 (8) |
C25—C26—C21 | 119.9 (6) | F1—P1—F2 | 175.7 (8) |
C25—C26—H26A | 120.0 | F5ii—P1—F2 | 128.7 (14) |
C21—C26—H26A | 120.0 | F5—P1—F2 | 89.3 (8) |
N31—C31—O31 | 116.8 (5) | F3—P1—F2 | 90.1 (9) |
N31—C31—C23 | 128.2 (5) | F4ii—P1—F2ii | 88.4 (9) |
O31—C31—C23 | 115.0 (5) | F4—P1—F2ii | 49.6 (8) |
N31—C32—C33 | 103.9 (5) | F6—P1—F2ii | 142.3 (15) |
N31—C32—H32A | 111.0 | F6ii—P1—F2ii | 83.2 (11) |
C33—C32—H32A | 111.0 | F1ii—P1—F2ii | 175.7 (8) |
N31—C32—H32B | 111.0 | F1—P1—F2ii | 89.3 (8) |
C33—C32—H32B | 111.0 | F5ii—P1—F2ii | 89.3 (8) |
H32A—C32—H32B | 109.0 | F5—P1—F2ii | 128.7 (14) |
O31—C33—C32 | 104.3 (5) | F3ii—P1—F2ii | 90.1 (9) |
O31—C33—H33A | 110.9 | F2—P1—F2ii | 95.1 (9) |
C32—C33—H33A | 110.9 | F6ii—F1—F5ii | 133 (2) |
O31—C33—H33B | 110.9 | F6ii—F1—P1 | 69.6 (14) |
C32—C33—H33B | 110.9 | F5ii—F1—P1 | 64.5 (9) |
H33A—C33—H33B | 108.9 | F3ii—F2—F4ii | 132.4 (16) |
N41—C41—O41 | 118.5 (5) | F3ii—F2—P1 | 70.6 (13) |
N41—C41—C51 | 126.3 (5) | F4ii—F2—P1 | 63.5 (8) |
O41—C41—C51 | 115.2 (5) | F2ii—F3—F4ii | 116.2 (18) |
N41—C42—C43 | 105.0 (5) | F2ii—F3—P1 | 70.9 (11) |
N41—C42—H42A | 110.8 | F4ii—F3—P1 | 59.8 (8) |
C43—C42—H42A | 110.8 | F2ii—F3—F6ii | 96 (2) |
N41—C42—H42B | 110.8 | F4ii—F3—F6ii | 89 (2) |
C43—C42—H42B | 110.8 | P1—F3—F6ii | 56.5 (9) |
H42A—C42—H42B | 108.8 | F2ii—F4—F5ii | 104.8 (12) |
O41—C43—C42 | 103.9 (5) | F2ii—F4—F3ii | 105.1 (17) |
O41—C43—H43A | 111.0 | F5ii—F4—F3ii | 97.0 (18) |
C42—C43—H43A | 111.0 | F2ii—F4—P1 | 66.9 (8) |
O41—C43—H43B | 111.0 | F5ii—F4—P1 | 62.7 (7) |
C42—C43—H43B | 111.0 | F3ii—F4—P1 | 62.5 (8) |
H43A—C43—H43B | 109.0 | F1ii—F5—F4ii | 106.5 (13) |
C52—C51—C56 | 120.5 (5) | F1ii—F5—P1 | 64.4 (8) |
C52—C51—C41 | 120.6 (5) | F4ii—F5—P1 | 60.2 (7) |
C56—C51—C41 | 118.9 (5) | F1ii—F5—F6ii | 97.1 (15) |
C51—C52—C53 | 119.3 (5) | F4ii—F5—F6ii | 90.2 (15) |
C51—C52—H52A | 120.3 | P1—F5—F6ii | 57.2 (7) |
C53—C52—H52A | 120.3 | F1ii—F6—P1 | 72.1 (15) |
C54—C53—C52 | 119.8 (5) | F1ii—F6—F5ii | 107 (2) |
C54—C53—C61 | 121.4 (4) | P1—F6—F5ii | 58.6 (7) |
C52—C53—C61 | 118.8 (5) | F1ii—F6—F3ii | 113 (3) |
C55—C54—C53 | 120.3 (5) | P1—F6—F3ii | 58.1 (8) |
C55—C54—H54A | 119.9 | F5ii—F6—F3ii | 84.0 (17) |
C53—C54—H54A | 119.9 | F8—P2—F9 | 175.8 (7) |
C54—C55—C56 | 120.3 (5) | F8—P2—F12 | 89.7 (6) |
C54—C55—H55A | 119.8 | F9—P2—F12 | 86.1 (7) |
C56—C55—H55A | 119.8 | F8—P2—F10 | 87.3 (7) |
C55—C56—C51 | 119.7 (5) | F9—P2—F10 | 96.8 (8) |
C55—C56—H56A | 120.1 | F12—P2—F10 | 175.4 (9) |
C51—C56—H56A | 120.1 | F8—P2—F7 | 88.6 (6) |
N61—C61—O61 | 117.7 (5) | F9—P2—F7 | 92.0 (6) |
N61—C61—C53 | 126.2 (5) | F12—P2—F7 | 98.8 (6) |
O61—C61—C53 | 116.1 (4) | F10—P2—F7 | 84.6 (6) |
N61—C62—C63 | 103.0 (4) | F8—P2—F11 | 93.7 (6) |
N61—C62—H62A | 111.2 | F9—P2—F11 | 85.9 (5) |
C63—C62—H62A | 111.2 | F12—P2—F11 | 84.0 (5) |
N61—C62—H62B | 111.2 | F10—P2—F11 | 92.8 (6) |
C63—C62—H62B | 111.2 | F7—P2—F11 | 176.4 (6) |
H62A—C62—H62B | 109.1 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1, y, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Ag3(C12H12N2O2)4](PF6)3 |
Mr | 1623.46 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 22.7473 (16), 11.4521 (19), 24.1382 (15) |
β (°) | 116.014 (7) |
V (Å3) | 5651.0 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.23 |
Crystal size (mm) | 0.60 × 0.40 × 0.30 |
Data collection | |
Diffractometer | Siemens P4 four-circle diffractometer |
Absorption correction | ψ scan (XSCANS; Siemens, 1995) |
Tmin, Tmax | 0.634, 0.964 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5107, 4976, 3885 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.137, 1.01 |
No. of reflections | 4976 |
No. of parameters | 425 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0628P)2 + 34.3783P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.02, −0.81 |
Computer programs: XSCANS (Siemens, 1995), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).
Acknowledgements
We are grateful to the National Science Council of the Republic of China and the Taoyuan Innovation Institute of Technology for support.
References
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Siemens (1995). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Google Scholar
Suen, M.-C., Yeh, C.-W., Lin, S.-C. & Hsu, Y.-F. (2011). Acta Cryst. E67, m1099. Web of Science CSD CrossRef IUCr Journals Google Scholar
Wang, Y.-H., Lee, H.-T. & Suen, M.-C. (2008). Polyhedron, 27, 1177–1184. Web of Science CSD CrossRef Google Scholar
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Several Ag(I), Cd(II) and Cu(II) complexes containing 1,4-bis(4,5-dihydro-2-oxazolyl)benzene ligands have been reported, which show various dimensional structures (Suen et al., 2011; Wang et al., 2008, 2011a,b; Yeh et al., 2011). In the title trinuclear complex, one AgI ion, lying on a twofold axis, is coordinated by four N atoms from four 1,3-bis(4,5-dihydro-2-oxazolyl)benzene (L) ligands in a distorted tetrahedral geometry and the other two are each coordinated by two N atoms from two L ligands in a bent linear arrangement (Fig. 1, Table 1). The Ag···Ag separation in the trimer is 7.473 (1) Å. The L ligands show both syn and anti conformations. The PF6- anions link the trinuclear cationic complexes via Ag···F interactions [2.80 (2) and 2.85 (2) Å], forming one-dimensional beaded polymeric chains along [100] (Fig. 2).