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The title compound, [Ag(CF3O3S)(C6H6)], has been synthesized and characterized by low-temperature single-crystal X-ray diffraction. The complex is polymeric, with a network of trifluoromethanesulfonate anions bridging the silver cations. The terminal planar benzene ligand is asymmetrically η2-coordinated to the Ag.
Supporting information
CCDC reference: 163893
Data collection: SMART (Bruker, 1998); cell refinement: SAINT+ (Bruker, 1999); data reduction: SAINT+; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXTL (Sheldrick, 1999).
Poly[[{(1,2-
η)-benzene}silver(I)]-µ-trifluoromethanesulfonate-O;O';O'':
O'']
top
Crystal data top
[Ag(CF3O3S)(C6H6)] | F(000) = 1296 |
Mr = 335.05 | Dx = 2.273 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 25.4244 (5) Å | Cell parameters from 8907 reflections |
b = 5.0560 (1) Å | θ = 2.1–28.2° |
c = 18.9045 (4) Å | µ = 2.30 mm−1 |
β = 126.327 (1)° | T = 173 K |
V = 1957.80 (7) Å3 | Needle, colourless |
Z = 8 | 1.25 × 0.14 × 0.08 mm |
Data collection top
CCD area-detector diffractometer | 2420 independent reflections |
Radiation source: fine-focus sealed tube | 2248 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 28.3°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −33→26 |
Tmin = 0.551, Tmax = 0.862 | k = 0→6 |
12969 measured reflections | l = 0→24 |
Refinement top
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)] = 0.023 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.060 | All H-atom parameters refined |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0355P)2 + 3.092P] where P = (Fo2 + 2Fc2)/3 |
2420 reflections | (Δ/σ)max = 0.001 |
160 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ag1 | 0.072605 (7) | 0.13524 (3) | 0.273762 (11) | 0.02681 (7) | |
S2 | 0.04246 (2) | −0.38076 (9) | 0.37505 (3) | 0.02047 (11) | |
O1 | 0.03344 (9) | −0.1054 (3) | 0.34857 (12) | 0.0356 (4) | |
O2 | −0.01754 (7) | −0.5260 (3) | 0.33710 (10) | 0.0306 (3) | |
O3 | 0.09268 (8) | −0.5172 (3) | 0.37540 (10) | 0.0282 (3) | |
F1 | 0.03505 (8) | −0.2388 (4) | 0.50150 (11) | 0.0476 (4) | |
F2 | 0.13151 (7) | −0.2160 (4) | 0.53343 (10) | 0.0473 (4) | |
F3 | 0.09033 (9) | −0.5943 (4) | 0.52767 (10) | 0.0462 (4) | |
C1 | 0.07649 (12) | −0.3576 (5) | 0.49104 (14) | 0.0299 (5) | |
C2 | 0.15398 (12) | −0.1485 (4) | 0.28952 (18) | 0.0308 (5) | |
C3 | 0.15114 (11) | 0.0078 (5) | 0.22694 (16) | 0.0315 (5) | |
C4 | 0.19593 (12) | 0.2129 (5) | 0.25359 (16) | 0.0336 (5) | |
C5 | 0.24312 (11) | 0.2585 (5) | 0.34175 (17) | 0.0318 (5) | |
C6 | 0.24533 (12) | 0.1058 (6) | 0.40433 (17) | 0.0375 (5) | |
C7 | 0.20053 (13) | −0.0958 (5) | 0.37850 (18) | 0.0381 (5) | |
H3 | 0.1217 (14) | −0.031 (6) | 0.171 (2) | 0.033 (7)* | |
H6 | 0.278 (2) | 0.133 (6) | 0.464 (3) | 0.061 (11)* | |
H4 | 0.1946 (15) | 0.313 (6) | 0.210 (2) | 0.043 (8)* | |
H5 | 0.2719 (15) | 0.399 (6) | 0.356 (2) | 0.038 (8)* | |
H7 | 0.2025 (16) | −0.211 (7) | 0.422 (2) | 0.049 (9)* | |
H2 | 0.1284 (16) | −0.296 (7) | 0.273 (2) | 0.041 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.02221 (10) | 0.01980 (10) | 0.03920 (11) | 0.00207 (5) | 0.01862 (8) | 0.00059 (6) |
S2 | 0.0202 (2) | 0.0182 (2) | 0.0191 (2) | −0.00011 (16) | 0.00948 (18) | 0.00121 (16) |
O1 | 0.0358 (9) | 0.0253 (8) | 0.0442 (10) | 0.0060 (6) | 0.0228 (8) | 0.0139 (7) |
O2 | 0.0209 (7) | 0.0297 (8) | 0.0304 (8) | −0.0046 (6) | 0.0093 (6) | −0.0043 (6) |
O3 | 0.0303 (8) | 0.0280 (8) | 0.0309 (8) | −0.0008 (6) | 0.0207 (7) | −0.0036 (6) |
F1 | 0.0489 (9) | 0.0588 (11) | 0.0467 (9) | 0.0037 (8) | 0.0345 (8) | −0.0112 (8) |
F2 | 0.0322 (8) | 0.0589 (10) | 0.0339 (8) | −0.0131 (7) | 0.0103 (6) | −0.0205 (7) |
F3 | 0.0489 (9) | 0.0529 (9) | 0.0319 (7) | 0.0098 (8) | 0.0213 (7) | 0.0194 (7) |
C1 | 0.0281 (11) | 0.0362 (13) | 0.0230 (10) | −0.0003 (8) | 0.0138 (9) | −0.0034 (8) |
C2 | 0.0255 (10) | 0.0205 (10) | 0.0486 (13) | 0.0008 (8) | 0.0231 (10) | −0.0033 (9) |
C3 | 0.0265 (10) | 0.0321 (12) | 0.0303 (11) | −0.0005 (9) | 0.0138 (9) | −0.0082 (9) |
C4 | 0.0362 (12) | 0.0325 (12) | 0.0355 (12) | −0.0017 (10) | 0.0231 (10) | 0.0013 (10) |
C5 | 0.0251 (10) | 0.0300 (12) | 0.0428 (13) | −0.0044 (9) | 0.0214 (10) | −0.0072 (9) |
C6 | 0.0262 (11) | 0.0496 (15) | 0.0289 (11) | −0.0006 (10) | 0.0120 (10) | −0.0062 (10) |
C7 | 0.0355 (13) | 0.0391 (13) | 0.0421 (13) | 0.0060 (10) | 0.0242 (11) | 0.0116 (11) |
Geometric parameters (Å, º) top
Ag1—C2 | 2.387 (2) | F2—C1 | 1.335 (3) |
Ag1—O2i | 2.4103 (16) | F3—C1 | 1.322 (3) |
Ag1—O3ii | 2.4247 (15) | C2—C3 | 1.388 (4) |
Ag1—O1 | 2.4779 (18) | C2—C7 | 1.394 (4) |
Ag1—O1iii | 2.5904 (17) | C2—H2 | 0.92 (3) |
Ag1—C3 | 2.698 (2) | C3—C4 | 1.395 (3) |
Ag1—Ag1iii | 3.2415 (3) | C3—H3 | 0.89 (3) |
S2—O2 | 1.4438 (16) | C4—C5 | 1.379 (3) |
S2—O3 | 1.4478 (16) | C4—H4 | 0.94 (3) |
S2—O1 | 1.4512 (16) | C5—C6 | 1.386 (4) |
S2—C1 | 1.823 (2) | C5—H5 | 0.94 (3) |
O1—Ag1iii | 2.5904 (17) | C6—C7 | 1.384 (4) |
O2—Ag1iv | 2.4103 (16) | C6—H6 | 0.93 (4) |
O3—Ag1v | 2.4247 (15) | C7—H7 | 0.99 (3) |
F1—C1 | 1.325 (3) | | |
| | | |
C2—Ag1—O2i | 123.34 (8) | S2—O3—Ag1v | 124.79 (9) |
C2—Ag1—O3ii | 125.22 (7) | F3—C1—F1 | 108.7 (2) |
O2i—Ag1—O3ii | 85.14 (6) | F3—C1—F2 | 108.2 (2) |
C2—Ag1—O1 | 104.21 (7) | F1—C1—F2 | 108.08 (19) |
O2i—Ag1—O1 | 128.49 (6) | F3—C1—S2 | 111.17 (16) |
O3ii—Ag1—O1 | 82.57 (6) | F1—C1—S2 | 110.84 (16) |
C2—Ag1—O1iii | 101.30 (7) | F2—C1—S2 | 109.77 (16) |
O2i—Ag1—O1iii | 78.24 (6) | C3—C2—C7 | 119.9 (2) |
O3ii—Ag1—O1iii | 131.84 (5) | C3—C2—Ag1 | 87.02 (14) |
O1—Ag1—O1iii | 73.82 (8) | C7—C2—Ag1 | 95.12 (16) |
C2—Ag1—C3 | 30.92 (8) | C3—C2—H2 | 120.5 (19) |
O2i—Ag1—C3 | 92.64 (7) | C7—C2—H2 | 119.3 (19) |
O3ii—Ag1—C3 | 125.72 (6) | Ag1—C2—H2 | 93 (2) |
O1—Ag1—C3 | 134.08 (7) | C2—C3—C4 | 119.7 (2) |
O1iii—Ag1—C3 | 100.14 (6) | C2—C3—Ag1 | 62.06 (12) |
C2—Ag1—Ag1iii | 142.69 (5) | C4—C3—Ag1 | 107.96 (16) |
O2i—Ag1—Ag1iii | 77.26 (4) | C2—C3—H3 | 118 (2) |
O3ii—Ag1—Ag1iii | 83.70 (4) | C4—C3—H3 | 122 (2) |
O1—Ag1—Ag1iii | 51.79 (4) | Ag1—C3—H3 | 100.6 (19) |
O1iii—Ag1—Ag1iii | 48.73 (4) | C5—C4—C3 | 120.0 (2) |
C3—Ag1—Ag1iii | 148.41 (5) | C5—C4—H4 | 121 (2) |
O2—S2—O3 | 115.43 (10) | C3—C4—H4 | 119 (2) |
O2—S2—O1 | 114.34 (10) | C4—C5—C6 | 120.3 (2) |
O3—S2—O1 | 114.67 (10) | C4—C5—H5 | 116.2 (19) |
O2—S2—C1 | 103.84 (10) | C6—C5—H5 | 123.4 (19) |
O3—S2—C1 | 103.67 (10) | C7—C6—C5 | 120.0 (2) |
O1—S2—C1 | 102.63 (11) | C7—C6—H6 | 119 (2) |
S2—O1—Ag1 | 129.28 (11) | C5—C6—H6 | 121 (2) |
S2—O1—Ag1iii | 128.81 (11) | C6—C7—C2 | 120.0 (2) |
Ag1—O1—Ag1iii | 79.48 (5) | C6—C7—H7 | 121 (2) |
S2—O2—Ag1iv | 133.79 (10) | C2—C7—H7 | 119 (2) |
Symmetry codes: (i) −x, y+1, −z+1/2; (ii) x, y+1, z; (iii) −x, y, −z+1/2; (iv) −x, y−1, −z+1/2; (v) x, y−1, z. |
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