The title complex, [Ag4(C5F6O4)2(C14H8N2)(C4H8O)2]n, exhibits a one-dimensional chain structure propagated through inversion centres, with two crystallographically independent AgI atoms in the asymmetric unit. One of the Ag atoms has a distorted trigonal-pyramidal coordination, defined by two carboxyl O atoms from two hexafluoroglutarate (HFG2−) anions, one N atom from 4,4′-biphenyldicarbonitrile and one apical O atom of tetrahydrofuran. The other Ag atom is coordinated by two O atoms from two HFG2− anions.
Supporting information
CCDC reference: 263536
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.004 Å
- R factor = 0.025
- wR factor = 0.047
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.70 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C5
PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C1 - C2 ... 1.45 Ang.
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Molecular Structure Corporation, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
catena-Poly[[bis(µ
4-hexafluoroglutarato)bis(tetrahydrofuran)tetrasilver(I)]- µ
2-4,4'-biphenyldicarbonitrile]
top
Crystal data top
[Ag4(C5F6O4)2(C14H8N2)(C4H8O)2] | F(000) = 1212.0 |
Mr = 1256.00 | Dx = 2.345 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -P 2ybc | Cell parameters from 5730 reflections |
a = 5.737 (2) Å | θ = 3.2–27.5° |
b = 18.801 (6) Å | µ = 2.29 mm−1 |
c = 16.518 (6) Å | T = 150 K |
β = 93.368 (4)° | Block, colorless |
V = 1778.6 (11) Å3 | 0.25 × 0.15 × 0.10 mm |
Z = 2 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 3744 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.023 |
ω scans | θmax = 27.5°, θmin = 3.3° |
Absorption correction: multi-scan (Jacobson, 1998) | h = −5→7 |
Tmin = 0.659, Tmax = 0.795 | k = −18→24 |
13771 measured reflections | l = −21→21 |
4068 independent reflections | |
Refinement top
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.025 | w = 1/[σ2(Fo2) + (0.0156P)2 + 1.6769P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.047 | (Δ/σ)max = 0.002 |
S = 1.11 | Δρmax = 0.40 e Å−3 |
3744 reflections | Δρmin = −0.41 e Å−3 |
271 parameters | |
Special details top
Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The
weighted R-factor (wR) and goodness of fit (S) are based
on F2. R-factor (gt) are based on F. The threshold
expression of F2 > 2.0 σ(F2) is used only for calculating
R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ag1 | 0.14531 (3) | 0.36656 (1) | 0.52899 (1) | 0.02074 (6) | |
Ag2 | −0.21763 (3) | 0.47580 (1) | 0.55857 (1) | 0.02028 (6) | |
F1 | 0.2934 (3) | 0.49447 (8) | 0.80268 (9) | 0.0287 (3) | |
F2 | 0.6096 (2) | 0.49830 (8) | 0.7362 (1) | 0.0269 (3) | |
F3 | 0.1590 (2) | 0.62219 (8) | 0.74880 (9) | 0.0225 (3) | |
F4 | 0.5150 (3) | 0.62023 (8) | 0.80215 (8) | 0.0245 (3) | |
F5 | 0.4417 (3) | 0.71047 (7) | 0.67759 (9) | 0.0242 (3) | |
F6 | 0.6946 (2) | 0.62704 (8) | 0.65825 (9) | 0.0226 (3) | |
O1 | 0.3457 (3) | 0.43461 (9) | 0.6241 (1) | 0.0203 (4) | |
O2 | 0.0418 (3) | 0.50577 (9) | 0.6507 (1) | 0.0202 (4) | |
O3 | 0.1471 (3) | 0.65412 (9) | 0.5655 (1) | 0.0212 (4) | |
O4 | 0.4221 (3) | 0.57173 (8) | 0.54231 (9) | 0.0173 (3) | |
O5 | −0.0024 (3) | 0.3010 (1) | 0.6485 (1) | 0.0268 (4) | |
N1 | 0.3859 (4) | 0.2655 (1) | 0.5085 (1) | 0.0283 (5) | |
C1 | 0.5003 (5) | 0.2174 (1) | 0.5042 (2) | 0.0229 (5) | |
C2 | 0.6495 (5) | 0.1551 (1) | 0.5004 (2) | 0.0228 (5) | |
C3 | 0.8566 (5) | 0.1523 (2) | 0.5477 (2) | 0.0387 (8) | |
C4 | 0.9924 (5) | 0.0914 (2) | 0.5471 (2) | 0.0393 (8) | |
C5 | 0.9275 (5) | 0.0330 (1) | 0.4995 (2) | 0.0209 (5) | |
C6 | 0.7214 (6) | 0.0380 (2) | 0.4518 (2) | 0.0376 (8) | |
C7 | 0.5832 (6) | 0.0980 (2) | 0.4523 (2) | 0.0362 (7) | |
C8 | 0.2439 (4) | 0.4819 (1) | 0.6607 (1) | 0.0154 (5) | |
C9 | 0.3830 (4) | 0.5180 (1) | 0.7329 (1) | 0.0176 (5) | |
C10 | 0.3769 (4) | 0.6001 (1) | 0.7361 (1) | 0.0174 (5) | |
C11 | 0.4637 (4) | 0.6402 (1) | 0.6619 (1) | 0.0167 (5) | |
C12 | 0.3286 (4) | 0.6213 (1) | 0.5811 (1) | 0.0150 (5) | |
C13 | −0.2162 (5) | 0.3169 (2) | 0.6852 (2) | 0.0299 (6) | |
C14 | −0.1449 (6) | 0.3453 (2) | 0.7673 (2) | 0.0373 (7) | |
C15 | 0.0685 (6) | 0.3005 (2) | 0.7922 (2) | 0.0408 (8) | |
C16 | 0.1618 (5) | 0.2784 (2) | 0.7128 (2) | 0.0372 (7) | |
H1 | 0.9052 | 0.1918 | 0.5803 | 0.0464* | |
H2 | 1.1335 | 0.0896 | 0.5801 | 0.0471* | |
H3 | 0.6742 | −0.0009 | 0.4178 | 0.0451* | |
H4 | 0.4418 | 0.1000 | 0.4194 | 0.0435* | |
H5 | −0.3030 | 0.3515 | 0.6543 | 0.0359* | |
H6 | −0.3076 | 0.2751 | 0.6895 | 0.0359* | |
H7 | −0.1059 | 0.3943 | 0.7648 | 0.0448* | |
H8 | −0.2651 | 0.3388 | 0.8037 | 0.0448* | |
H9 | 0.1807 | 0.3278 | 0.8232 | 0.0489* | |
H10 | 0.0258 | 0.2601 | 0.8225 | 0.0489* | |
H11 | 0.1790 | 0.2281 | 0.7113 | 0.0447* | |
H12 | 0.3090 | 0.3002 | 0.7066 | 0.0447* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.0205 (1) | 0.0205 (1) | 0.0207 (1) | 0.00320 (8) | −0.00269 (7) | −0.00345 (7) |
Ag2 | 0.0173 (1) | 0.0225 (1) | 0.02031 (9) | 0.00244 (8) | −0.00499 (7) | −0.00609 (7) |
F1 | 0.0364 (9) | 0.0319 (9) | 0.0172 (7) | −0.0051 (7) | −0.0024 (6) | 0.0045 (6) |
F2 | 0.0152 (7) | 0.0255 (8) | 0.0387 (9) | 0.0071 (6) | −0.0087 (6) | −0.0034 (7) |
F3 | 0.0173 (7) | 0.0270 (8) | 0.0236 (8) | 0.0043 (6) | 0.0039 (6) | −0.0074 (6) |
F4 | 0.0267 (8) | 0.0290 (8) | 0.0169 (7) | −0.0042 (6) | −0.0070 (6) | −0.0073 (6) |
F5 | 0.0298 (8) | 0.0150 (7) | 0.0274 (8) | −0.0022 (6) | −0.0022 (6) | −0.0074 (6) |
F6 | 0.0106 (7) | 0.0315 (8) | 0.0255 (8) | −0.0010 (6) | −0.0006 (6) | −0.0060 (6) |
O1 | 0.0197 (9) | 0.0157 (8) | 0.0253 (9) | 0.0029 (7) | −0.0005 (7) | −0.0038 (7) |
O2 | 0.0133 (9) | 0.0241 (9) | 0.0229 (9) | 0.0017 (7) | −0.0025 (7) | −0.0070 (7) |
O3 | 0.0172 (9) | 0.0214 (9) | 0.0246 (9) | 0.0040 (7) | −0.0033 (7) | −0.0046 (7) |
O4 | 0.0183 (9) | 0.0163 (8) | 0.0170 (8) | 0.0014 (7) | −0.0009 (7) | −0.0044 (6) |
O5 | 0.0170 (9) | 0.031 (1) | 0.033 (1) | 0.0041 (8) | 0.0022 (8) | 0.0091 (8) |
N1 | 0.026 (1) | 0.024 (1) | 0.035 (1) | 0.005 (1) | 0.0064 (10) | 0.0009 (10) |
C1 | 0.027 (1) | 0.019 (1) | 0.024 (1) | 0.000 (1) | 0.007 (1) | 0.002 (1) |
C2 | 0.029 (1) | 0.017 (1) | 0.023 (1) | 0.004 (1) | 0.010 (1) | 0.0027 (10) |
C3 | 0.031 (2) | 0.027 (2) | 0.057 (2) | 0.006 (1) | −0.005 (1) | −0.019 (1) |
C4 | 0.029 (2) | 0.030 (2) | 0.058 (2) | 0.010 (1) | −0.010 (1) | −0.017 (1) |
C5 | 0.026 (1) | 0.016 (1) | 0.020 (1) | 0.003 (1) | 0.005 (1) | −0.0005 (9) |
C6 | 0.055 (2) | 0.024 (1) | 0.032 (2) | 0.015 (1) | −0.018 (1) | −0.011 (1) |
C7 | 0.044 (2) | 0.027 (2) | 0.035 (2) | 0.013 (1) | −0.018 (1) | −0.005 (1) |
C8 | 0.016 (1) | 0.014 (1) | 0.016 (1) | −0.0026 (9) | −0.0003 (9) | 0.0024 (9) |
C9 | 0.014 (1) | 0.020 (1) | 0.018 (1) | 0.0022 (10) | −0.0017 (9) | 0.0000 (9) |
C10 | 0.013 (1) | 0.023 (1) | 0.016 (1) | 0.0016 (10) | −0.0025 (9) | −0.0069 (9) |
C11 | 0.015 (1) | 0.015 (1) | 0.021 (1) | −0.0005 (9) | −0.0006 (9) | −0.0058 (9) |
C12 | 0.015 (1) | 0.013 (1) | 0.017 (1) | −0.0029 (9) | 0.0007 (9) | −0.0002 (9) |
C13 | 0.014 (1) | 0.031 (1) | 0.045 (2) | 0.004 (1) | 0.006 (1) | 0.017 (1) |
C14 | 0.040 (2) | 0.024 (1) | 0.049 (2) | 0.006 (1) | 0.013 (1) | 0.004 (1) |
C15 | 0.045 (2) | 0.037 (2) | 0.038 (2) | 0.002 (1) | −0.011 (1) | −0.001 (1) |
C16 | 0.020 (1) | 0.045 (2) | 0.047 (2) | 0.012 (1) | 0.001 (1) | 0.021 (1) |
Geometric parameters (Å, º) top
Ag1—O1 | 2.284 (2) | C3—H1 | 0.950 |
Ag1—O3i | 2.257 (2) | C4—C5 | 1.389 (4) |
Ag1—O5 | 2.516 (2) | C4—H2 | 0.950 |
Ag1—N1 | 2.385 (2) | C5—C5ii | 1.494 (5) |
Ag2—O2 | 2.141 (2) | C5—C6 | 1.385 (4) |
Ag2—O4i | 2.173 (2) | C6—C7 | 1.380 (4) |
F1—C9 | 1.363 (3) | C6—H3 | 0.950 |
F2—C9 | 1.350 (3) | C7—H4 | 0.950 |
F3—C10 | 1.345 (3) | C8—C9 | 1.551 (3) |
F4—C10 | 1.364 (3) | C9—C10 | 1.546 (4) |
F5—C11 | 1.353 (3) | C10—C11 | 1.545 (3) |
F6—C11 | 1.352 (3) | C11—C12 | 1.546 (3) |
O1—C8 | 1.240 (3) | C13—C14 | 1.492 (4) |
O2—C8 | 1.245 (3) | C13—H5 | 0.950 |
O3—C12 | 1.224 (3) | C13—H6 | 0.950 |
O4—C12 | 1.268 (3) | C14—C15 | 1.523 (4) |
O5—C13 | 1.431 (3) | C14—H7 | 0.950 |
O5—C16 | 1.441 (4) | C14—H8 | 0.950 |
N1—C1 | 1.122 (3) | C15—C16 | 1.503 (5) |
C1—C2 | 1.454 (4) | C15—H9 | 0.950 |
C2—C3 | 1.384 (4) | C15—H10 | 0.950 |
C2—C7 | 1.376 (4) | C16—H11 | 0.950 |
C3—C4 | 1.385 (4) | C16—H12 | 0.950 |
| | | |
Ag1···O5 | 2.516 (2) | F5···C15vi | 3.293 (4) |
Ag1···O4iii | 3.039 (2) | F5···N1iii | 3.315 (3) |
Ag1···F6iii | 3.280 (2) | F5···C1iii | 3.329 (3) |
Ag2···O4iv | 2.744 (2) | F5···C13viii | 3.340 (3) |
Ag2···O1iv | 2.893 (2) | F5···C15viii | 3.443 (4) |
Ag2···F2iv | 3.180 (2) | F6···O2vii | 3.035 (2) |
Ag2···F6iv | 3.339 (2) | F6···O3vii | 3.133 (2) |
F1···C7v | 3.379 (3) | F6···N1iii | 3.426 (3) |
F1···C6v | 3.428 (3) | O1···O4iii | 3.127 (2) |
F1···C4vi | 3.556 (4) | O1···C13vii | 3.455 (3) |
F2···O2vii | 2.928 (2) | O3···N1iii | 3.368 (3) |
F2···C14vii | 3.231 (3) | O3···C1iii | 3.395 (3) |
F3···F6iv | 2.979 (2) | O4···O4iii | 3.190 (3) |
F3···C3vi | 3.415 (4) | O4···N1iii | 3.375 (3) |
F3···C16viii | 3.543 (4) | O5···C3iv | 3.329 (4) |
F3···C4vi | 3.577 (4) | N1···C12iii | 3.112 (3) |
F4···C3vi | 3.417 (4) | N1···C11iii | 3.478 (3) |
F4···C2vi | 3.509 (3) | C1···C12iii | 3.508 (3) |
F4···C16vi | 3.520 (4) | C6···C6ix | 3.393 (6) |
F5···C16vi | 3.098 (3) | C6···C7ix | 3.525 (4) |
F5···C14viii | 3.214 (3) | | |
| | | |
O1—Ag1—O3i | 153.64 (6) | F2—C9—C10 | 107.3 (2) |
O1—Ag1—O5 | 85.03 (6) | C8—C9—C10 | 116.8 (2) |
O1—Ag1—N1 | 105.78 (7) | F3—C10—F4 | 106.9 (2) |
O3i—Ag1—O5 | 100.80 (6) | F3—C10—C9 | 109.7 (2) |
O3i—Ag1—N1 | 100.23 (7) | F3—C10—C11 | 108.6 (2) |
O5—Ag1—N1 | 86.88 (7) | F4—C10—C9 | 106.9 (2) |
O2—Ag2—O4i | 167.13 (6) | F4—C10—C11 | 107.4 (2) |
Ag1—O1—C8 | 120.3 (1) | C9—C10—C11 | 116.8 (2) |
Ag2—O2—C8 | 127.1 (2) | F5—C11—F6 | 106.9 (2) |
Ag1i—O3—C12 | 130.3 (2) | F5—C11—C10 | 106.7 (2) |
Ag2i—O4—C12 | 117.7 (1) | F5—C11—C12 | 110.0 (2) |
Ag1—O5—C13 | 124.5 (2) | F6—C11—C10 | 108.0 (2) |
Ag1—O5—C16 | 119.1 (2) | F6—C11—C12 | 111.2 (2) |
C13—O5—C16 | 106.8 (2) | C10—C11—C12 | 113.8 (2) |
Ag1—N1—C1 | 175.5 (2) | O3—C12—O4 | 130.1 (2) |
N1—C1—C2 | 178.8 (3) | O3—C12—C11 | 116.3 (2) |
C1—C2—C3 | 119.6 (2) | O4—C12—C11 | 113.6 (2) |
C1—C2—C7 | 120.6 (2) | O5—C13—C14 | 105.2 (2) |
C3—C2—C7 | 119.7 (3) | O5—C13—H5 | 110.5 |
C2—C3—C4 | 119.5 (3) | O5—C13—H6 | 110.5 |
C2—C3—H1 | 120.3 | C14—C13—H5 | 110.5 |
C4—C3—H1 | 120.3 | C14—C13—H6 | 110.5 |
C3—C4—C5 | 121.7 (3) | H5—C13—H6 | 109.5 |
C3—C4—H2 | 119.2 | C13—C14—C15 | 102.8 (2) |
C5—C4—H2 | 119.1 | C13—C14—H7 | 111.1 |
C4—C5—C5ii | 121.3 (3) | C13—C14—H8 | 111.1 |
C4—C5—C6 | 117.4 (2) | C15—C14—H7 | 111.1 |
C5ii—C5—C6 | 121.2 (3) | C15—C14—H8 | 111.1 |
C5—C6—C7 | 121.5 (3) | H7—C14—H8 | 109.5 |
C5—C6—H3 | 119.2 | C14—C15—C16 | 103.8 (3) |
C7—C6—H3 | 119.2 | C14—C15—H9 | 110.9 |
C2—C7—C6 | 120.2 (3) | C14—C15—H10 | 110.9 |
C2—C7—H4 | 119.9 | C16—C15—H9 | 110.9 |
C6—C7—H4 | 119.9 | C16—C15—H10 | 110.9 |
O1—C8—O2 | 130.9 (2) | H9—C15—H10 | 109.5 |
O1—C8—C9 | 116.9 (2) | O5—C16—C15 | 108.0 (2) |
O2—C8—C9 | 112.2 (2) | O5—C16—H11 | 109.8 |
F1—C9—F2 | 106.7 (2) | O5—C16—H12 | 109.8 |
F1—C9—C8 | 107.8 (2) | C15—C16—H11 | 109.8 |
F1—C9—C10 | 106.5 (2) | C15—C16—H12 | 109.8 |
F2—C9—C8 | 111.2 (2) | H11—C16—H12 | 109.5 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+2, −y, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z; (v) x, −y+1/2, z+1/2; (vi) −x+1, y+1/2, −z+3/2; (vii) x+1, y, z; (viii) −x, y+1/2, −z+3/2; (ix) −x+1, −y, −z+1. |