Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807042912/hb2531sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807042912/hb2531Isup2.hkl |
CCDC reference: 663569
Key indicators
- Single-crystal X-ray study
- T = 98 K
- Mean (C-C) = 0.003 Å
- R factor = 0.024
- wR factor = 0.061
- Data-to-parameter ratio = 14.4
checkCIF/PLATON results
No syntax errors found
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.406 1.000 Tmin(prime) and Tmax expected: 0.662 0.874 RR(prime) = 0.536 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.53
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.87 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P1
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.874 Tmax scaled 0.874 Tmin scaled 0.355 PLAT794_ALERT_5_G Check Predicted Bond Valency for Ag (9) 0.87
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
Ag(PF6) (Aldrich, 0.05 g, 0.20 mmol) was dissolved in CH3CN (20 ml) and layered on top of a CH2Cl2 solution (20 ml) containing 0.041 g (0.20 mmol) of 3-pyridinealdazine (Aldrich). After three days, yellow prisms of (I) were observed at the interface between the two layers; m.p. 579–581 K.
All the H atoms were included in the riding-model approximation, with C–H = 0.95–98 Å, and with Uiso(H) = 1.2 or 1.5Ueq(C).
The structure of the title compound (I) was investigated as part of an on-going study of the structural chemistry of silver salts of the isomeric n-pyridinealdazine, n = 2, 3 and 4, molecules (Broker & Tiekink, 2007a-c).
Compound (I) features an Ag cation in a general position, two half 3-pyridinealdazine molecules, each disposed about a centre of inversion, an hexafluorophosphate anion and an acetonitrile solvent molecule, each in general positions (Fig. 1 & Table 1). The 3-pyridinealdazine molecule is bidentate bridging leading to a zigzag chain with a linear N2 coordination geometry for Ag.
The chains thus formed are linked via weakly bridging acetonitrile molecules with Ag···N5 and N5···Agi of 2.800 (3) and 2.826 (2) Å, respectively, as well as Ag···Agi interactions of 3.2590 (15) Å for (i): -x, 2 - y, -z. The topology of the resulting layer in the ac plane resembles a brick wall (Fig. 2).
The layers stack along the b axis and are interspersed by layers of PF6 anions. Various C—H···N and F interactions consolidate the structure (Fig. 3 & Table 2).
The zigzag topology found for the [Ag(C12H10N4)]n chain in (I) has precedents in the perchlorate, tetrafluoroborate salts (each as acetonitrile solvates) (Kennedy et al., 2005), and the methansulfonate salt (Broker & Tiekink, 2007c).
For related polymeric silver salts containing the 3-pyridinealdazine ligand, see: Kennedy et al. (2005); Broker & Tiekink (2007c). For related literature, see: Broker & Tiekink (2007a,b).
Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Ag(C12H10N4)]PF6·C2H3N | Z = 2 |
Mr = 504.13 | F(000) = 496 |
Triclinic, P1 | Dx = 1.962 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
a = 7.917 (3) Å | Cell parameters from 3181 reflections |
b = 10.416 (3) Å | θ = 2.7–30.5° |
c = 11.357 (5) Å | µ = 1.35 mm−1 |
α = 75.58 (5)° | T = 98 K |
β = 70.66 (3)° | Prism, yellow |
γ = 81.11 (4)° | 0.30 × 0.20 × 0.10 mm |
V = 853.2 (5) Å3 |
Rigaku AFC12κ/SATURN724 diffractometer | 3508 independent reflections |
Radiation source: fine-focus sealed tube | 3404 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 26.5°, θmin = 2.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −9→9 |
Tmin = 0.406, Tmax = 1.000 | k = −12→13 |
9571 measured reflections | l = −12→14 |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0287P)2 + 0.7535P] where P = (Fo2 + 2Fc2)/3 |
3508 reflections | (Δ/σ)max = 0.002 |
244 parameters | Δρmax = 0.58 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Ag(C12H10N4)]PF6·C2H3N | γ = 81.11 (4)° |
Mr = 504.13 | V = 853.2 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.917 (3) Å | Mo Kα radiation |
b = 10.416 (3) Å | µ = 1.35 mm−1 |
c = 11.357 (5) Å | T = 98 K |
α = 75.58 (5)° | 0.30 × 0.20 × 0.10 mm |
β = 70.66 (3)° |
Rigaku AFC12κ/SATURN724 diffractometer | 3508 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 3404 reflections with I > 2σ(I) |
Tmin = 0.406, Tmax = 1.000 | Rint = 0.019 |
9571 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.58 e Å−3 |
3508 reflections | Δρmin = −0.42 e Å−3 |
244 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 | ||
Ag | 0.19529 (2) | 0.921735 (16) | −0.001479 (15) | 0.02331 (7) | |
P1 | 0.35231 (8) | 0.57251 (5) | 0.27956 (5) | 0.02040 (12) | |
F1 | 0.2394 (2) | 0.68371 (14) | 0.20476 (16) | 0.0373 (4) | |
F2 | 0.4462 (2) | 0.51518 (15) | 0.15379 (14) | 0.0373 (3) | |
F3 | 0.1968 (2) | 0.47507 (15) | 0.32092 (16) | 0.0406 (4) | |
F4 | 0.2591 (2) | 0.63135 (17) | 0.40388 (15) | 0.0432 (4) | |
F5 | 0.46592 (19) | 0.46138 (14) | 0.35278 (14) | 0.0344 (3) | |
F6 | 0.50926 (19) | 0.66944 (14) | 0.23800 (14) | 0.0329 (3) | |
N1 | 0.2938 (2) | 1.03785 (17) | 0.09097 (16) | 0.0170 (3) | |
N2 | 0.4846 (2) | 1.04341 (17) | 0.44581 (16) | 0.0185 (4) | |
N3 | 0.1510 (2) | 0.79723 (18) | −0.11309 (17) | 0.0198 (4) | |
N4 | 0.0213 (2) | 0.97670 (19) | −0.44279 (17) | 0.0219 (4) | |
N5 | −0.1325 (3) | 0.84620 (19) | 0.17805 (19) | 0.0257 (4) | |
C1 | 0.3153 (3) | 1.1678 (2) | 0.0438 (2) | 0.0198 (4) | |
H1 | 0.2888 | 1.2083 | −0.0335 | 0.024* | |
C2 | 0.3746 (3) | 1.2454 (2) | 0.1027 (2) | 0.0205 (4) | |
H2 | 0.3873 | 1.3373 | 0.0663 | 0.025* | |
C3 | 0.4149 (3) | 1.1887 (2) | 0.2139 (2) | 0.0186 (4) | |
H3 | 0.4535 | 1.2406 | 0.2568 | 0.022* | |
C4 | 0.3977 (3) | 1.0527 (2) | 0.26239 (19) | 0.0154 (4) | |
C5 | 0.3354 (3) | 0.9823 (2) | 0.19818 (19) | 0.0168 (4) | |
H5 | 0.3218 | 0.8901 | 0.2322 | 0.020* | |
C6 | 0.4383 (3) | 0.9820 (2) | 0.37887 (19) | 0.0168 (4) | |
H6 | 0.4301 | 0.8885 | 0.4054 | 0.020* | |
C7 | 0.1646 (3) | 0.6635 (2) | −0.0804 (2) | 0.0246 (5) | |
H7 | 0.1888 | 0.6218 | −0.0025 | 0.030* | |
C8 | 0.1449 (3) | 0.5847 (2) | −0.1553 (2) | 0.0269 (5) | |
H8 | 0.1562 | 0.4906 | −0.1294 | 0.032* | |
C9 | 0.1085 (3) | 0.6436 (2) | −0.2681 (2) | 0.0246 (5) | |
H9 | 0.0950 | 0.5910 | −0.3213 | 0.030* | |
C10 | 0.0921 (3) | 0.7817 (2) | −0.3023 (2) | 0.0201 (4) | |
C11 | 0.1164 (3) | 0.8541 (2) | −0.2224 (2) | 0.0192 (4) | |
H11 | 0.1079 | 0.9484 | −0.2468 | 0.023* | |
C12 | 0.0484 (3) | 0.8502 (2) | −0.4185 (2) | 0.0221 (4) | |
H12 | 0.0402 | 0.8008 | −0.4761 | 0.027* | |
C13 | −0.1674 (3) | 0.7765 (2) | 0.2742 (2) | 0.0204 (4) | |
C14 | −0.2150 (3) | 0.6882 (2) | 0.3989 (2) | 0.0267 (5) | |
H14A | −0.2694 | 0.7407 | 0.4647 | 0.040* | |
H14B | −0.1068 | 0.6364 | 0.4137 | 0.040* | |
H14C | −0.3009 | 0.6278 | 0.4027 | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag | 0.02641 (11) | 0.02883 (11) | 0.02023 (10) | −0.00394 (7) | −0.01124 (7) | −0.00841 (7) |
P1 | 0.0219 (3) | 0.0189 (3) | 0.0211 (3) | −0.0042 (2) | −0.0069 (2) | −0.0036 (2) |
F1 | 0.0384 (8) | 0.0276 (7) | 0.0514 (10) | 0.0002 (6) | −0.0285 (7) | 0.0002 (7) |
F2 | 0.0498 (9) | 0.0342 (8) | 0.0282 (8) | −0.0041 (7) | −0.0077 (7) | −0.0122 (6) |
F3 | 0.0327 (8) | 0.0354 (8) | 0.0526 (10) | −0.0166 (6) | −0.0124 (7) | −0.0001 (7) |
F4 | 0.0445 (9) | 0.0501 (10) | 0.0345 (9) | 0.0053 (7) | −0.0059 (7) | −0.0223 (7) |
F5 | 0.0321 (8) | 0.0320 (8) | 0.0303 (8) | 0.0008 (6) | −0.0093 (6) | 0.0064 (6) |
F6 | 0.0310 (8) | 0.0290 (7) | 0.0415 (8) | −0.0117 (6) | −0.0157 (6) | −0.0002 (6) |
N1 | 0.0176 (9) | 0.0201 (9) | 0.0137 (8) | −0.0017 (7) | −0.0056 (7) | −0.0030 (7) |
N2 | 0.0208 (9) | 0.0203 (9) | 0.0146 (8) | −0.0032 (7) | −0.0075 (7) | −0.0004 (7) |
N3 | 0.0189 (9) | 0.0240 (9) | 0.0175 (9) | −0.0042 (7) | −0.0057 (7) | −0.0045 (7) |
N4 | 0.0173 (9) | 0.0346 (11) | 0.0155 (9) | −0.0034 (7) | −0.0039 (7) | −0.0090 (8) |
N5 | 0.0295 (11) | 0.0251 (10) | 0.0236 (10) | −0.0050 (8) | −0.0094 (8) | −0.0035 (8) |
C1 | 0.0200 (10) | 0.0226 (10) | 0.0160 (10) | −0.0041 (8) | −0.0057 (8) | −0.0007 (8) |
C2 | 0.0219 (11) | 0.0187 (10) | 0.0188 (10) | −0.0027 (8) | −0.0048 (8) | −0.0012 (8) |
C3 | 0.0154 (10) | 0.0204 (10) | 0.0203 (10) | −0.0034 (8) | −0.0044 (8) | −0.0054 (8) |
C4 | 0.0121 (9) | 0.0202 (10) | 0.0136 (9) | −0.0002 (7) | −0.0030 (7) | −0.0047 (8) |
C5 | 0.0168 (10) | 0.0163 (9) | 0.0166 (10) | −0.0004 (7) | −0.0046 (8) | −0.0033 (8) |
C6 | 0.0157 (10) | 0.0187 (10) | 0.0156 (10) | −0.0014 (7) | −0.0047 (8) | −0.0030 (8) |
C7 | 0.0206 (11) | 0.0275 (11) | 0.0251 (11) | −0.0037 (9) | −0.0079 (9) | −0.0021 (9) |
C8 | 0.0240 (12) | 0.0243 (11) | 0.0330 (13) | −0.0006 (9) | −0.0094 (10) | −0.0071 (10) |
C9 | 0.0189 (11) | 0.0286 (11) | 0.0313 (12) | −0.0019 (8) | −0.0073 (9) | −0.0157 (10) |
C10 | 0.0123 (10) | 0.0293 (11) | 0.0187 (10) | −0.0030 (8) | −0.0020 (8) | −0.0081 (9) |
C11 | 0.0147 (10) | 0.0241 (10) | 0.0187 (10) | −0.0040 (8) | −0.0032 (8) | −0.0056 (8) |
C12 | 0.0168 (10) | 0.0333 (12) | 0.0191 (10) | −0.0023 (8) | −0.0041 (8) | −0.0123 (9) |
C13 | 0.0195 (10) | 0.0216 (10) | 0.0225 (11) | −0.0014 (8) | −0.0080 (8) | −0.0070 (9) |
C14 | 0.0327 (13) | 0.0262 (12) | 0.0196 (11) | −0.0036 (9) | −0.0085 (9) | −0.0005 (9) |
Ag—N1 | 2.1538 (19) | C2—H2 | 0.9500 |
Ag—N3 | 2.160 (2) | C3—C4 | 1.397 (3) |
Ag—N5 | 2.800 (2) | C3—H3 | 0.9500 |
Ag—Agi | 3.2590 (15) | C4—C5 | 1.389 (3) |
P1—F4 | 1.5858 (17) | C4—C6 | 1.455 (3) |
P1—F3 | 1.5914 (16) | C5—H5 | 0.9500 |
P1—F2 | 1.5917 (17) | C6—H6 | 0.9500 |
P1—F5 | 1.5919 (16) | C7—C8 | 1.377 (3) |
P1—F6 | 1.5964 (16) | C7—H7 | 0.9500 |
P1—F1 | 1.5984 (16) | C8—C9 | 1.377 (3) |
N1—C5 | 1.335 (3) | C8—H8 | 0.9500 |
N1—C1 | 1.341 (3) | C9—C10 | 1.391 (3) |
N2—C6 | 1.273 (3) | C9—H9 | 0.9500 |
N2—N2ii | 1.403 (3) | C10—C11 | 1.389 (3) |
N3—C11 | 1.333 (3) | C10—C12 | 1.459 (3) |
N3—C7 | 1.346 (3) | C11—H11 | 0.9500 |
N4—C12 | 1.276 (3) | C12—H12 | 0.9500 |
N4—N4iii | 1.401 (4) | C13—C14 | 1.448 (3) |
N5—C13 | 1.124 (3) | C14—H14A | 0.9800 |
C1—C2 | 1.384 (3) | C14—H14B | 0.9800 |
C1—H1 | 0.9500 | C14—H14C | 0.9800 |
C2—C3 | 1.372 (3) | ||
N1—Ag—N3 | 168.86 (7) | C2—C3—H3 | 120.9 |
N1—Ag—N5 | 103.25 (7) | C4—C3—H3 | 120.9 |
N3—Ag—N5 | 86.67 (7) | C5—C4—C3 | 118.59 (19) |
N1—Ag—Agi | 101.63 (6) | C5—C4—C6 | 118.50 (18) |
N3—Ag—Agi | 88.15 (6) | C3—C4—C6 | 122.90 (19) |
N5—Ag—Agi | 54.97 (5) | N1—C5—C4 | 123.18 (19) |
F4—P1—F3 | 90.61 (10) | N1—C5—H5 | 118.4 |
F4—P1—F2 | 179.32 (9) | C4—C5—H5 | 118.4 |
F3—P1—F2 | 89.86 (10) | N2—C6—C4 | 121.01 (19) |
F4—P1—F5 | 91.01 (10) | N2—C6—H6 | 119.5 |
F3—P1—F5 | 90.18 (9) | C4—C6—H6 | 119.5 |
F2—P1—F5 | 89.48 (9) | N3—C7—C8 | 122.6 (2) |
F4—P1—F6 | 89.61 (10) | N3—C7—H7 | 118.7 |
F3—P1—F6 | 179.63 (9) | C8—C7—H7 | 118.7 |
F2—P1—F6 | 89.93 (9) | C9—C8—C7 | 119.5 (2) |
F5—P1—F6 | 89.52 (9) | C9—C8—H8 | 120.3 |
F4—P1—F1 | 89.54 (10) | C7—C8—H8 | 120.3 |
F3—P1—F1 | 89.92 (9) | C8—C9—C10 | 118.5 (2) |
F2—P1—F1 | 89.98 (10) | C8—C9—H9 | 120.7 |
F5—P1—F1 | 179.44 (10) | C10—C9—H9 | 120.7 |
F6—P1—F1 | 90.38 (9) | C11—C10—C9 | 118.6 (2) |
C5—N1—C1 | 117.55 (18) | C11—C10—C12 | 120.2 (2) |
C5—N1—Ag | 120.78 (14) | C9—C10—C12 | 121.2 (2) |
C1—N1—Ag | 121.66 (14) | N3—C11—C10 | 123.0 (2) |
C6—N2—N2ii | 111.5 (2) | N3—C11—H11 | 118.5 |
C11—N3—C7 | 117.88 (19) | C10—C11—H11 | 118.5 |
C11—N3—Ag | 119.05 (15) | N4—C12—C10 | 119.9 (2) |
C7—N3—Ag | 123.00 (15) | N4—C12—H12 | 120.1 |
C12—N4—N4iii | 111.3 (2) | C10—C12—H12 | 120.1 |
C13—N5—Ag | 132.65 (18) | N5—C13—C14 | 179.0 (3) |
N1—C1—C2 | 122.9 (2) | C13—C14—H14A | 109.5 |
N1—C1—H1 | 118.6 | C13—C14—H14B | 109.5 |
C2—C1—H1 | 118.6 | H14A—C14—H14B | 109.5 |
C3—C2—C1 | 119.6 (2) | C13—C14—H14C | 109.5 |
C3—C2—H2 | 120.2 | H14A—C14—H14C | 109.5 |
C1—C2—H2 | 120.2 | H14B—C14—H14C | 109.5 |
C2—C3—C4 | 118.2 (2) | ||
N3—Ag—N1—C5 | −88.2 (4) | C1—N1—C5—C4 | 0.6 (3) |
N5—Ag—N1—C5 | 64.29 (16) | Ag—N1—C5—C4 | −179.35 (15) |
Agi—Ag—N1—C5 | 120.67 (15) | C3—C4—C5—N1 | 1.1 (3) |
N3—Ag—N1—C1 | 91.9 (4) | C6—C4—C5—N1 | 179.73 (18) |
N5—Ag—N1—C1 | −115.62 (17) | N2ii—N2—C6—C4 | 179.41 (19) |
Agi—Ag—N1—C1 | −59.24 (16) | C5—C4—C6—N2 | −175.40 (19) |
N1—Ag—N3—C11 | −95.7 (4) | C3—C4—C6—N2 | 3.1 (3) |
N5—Ag—N3—C11 | 111.04 (16) | C11—N3—C7—C8 | 0.2 (3) |
Agi—Ag—N3—C11 | 56.03 (15) | Ag—N3—C7—C8 | −176.72 (17) |
N1—Ag—N3—C7 | 81.2 (4) | N3—C7—C8—C9 | −0.4 (3) |
N5—Ag—N3—C7 | −72.03 (18) | C7—C8—C9—C10 | −0.3 (3) |
Agi—Ag—N3—C7 | −127.04 (17) | C8—C9—C10—C11 | 1.2 (3) |
N1—Ag—N5—C13 | −69.2 (2) | C8—C9—C10—C12 | −178.1 (2) |
N3—Ag—N5—C13 | 105.7 (2) | C7—N3—C11—C10 | 0.7 (3) |
Agi—Ag—N5—C13 | −164.3 (2) | Ag—N3—C11—C10 | 177.80 (15) |
C5—N1—C1—C2 | −1.4 (3) | C9—C10—C11—N3 | −1.4 (3) |
Ag—N1—C1—C2 | 178.55 (16) | C12—C10—C11—N3 | 177.89 (19) |
N1—C1—C2—C3 | 0.4 (3) | N4iii—N4—C12—C10 | −179.1 (2) |
C1—C2—C3—C4 | 1.3 (3) | C11—C10—C12—N4 | −4.4 (3) |
C2—C3—C4—C5 | −2.0 (3) | C9—C10—C12—N4 | 174.9 (2) |
C2—C3—C4—C6 | 179.45 (18) |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x+1, −y+2, −z+1; (iii) −x, −y+2, −z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···F6iv | 0.95 | 2.50 | 3.182 (3) | 128 |
C1—H1···N5i | 0.95 | 2.56 | 3.336 (3) | 138 |
C2—H2···F2v | 0.95 | 2.48 | 3.174 (3) | 130 |
C5—H5···F1 | 0.95 | 2.46 | 3.291 (3) | 146 |
C5—H5···F6 | 0.95 | 2.53 | 3.318 (3) | 140 |
C9—H9···F3vi | 0.95 | 2.51 | 3.160 (3) | 126 |
C11—H11···N5i | 0.95 | 2.51 | 3.311 (3) | 142 |
Symmetry codes: (i) −x, −y+2, −z; (iv) −x+1, −y+2, −z; (v) x, y+1, z; (vi) −x, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Ag(C12H10N4)]PF6·C2H3N |
Mr | 504.13 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 98 |
a, b, c (Å) | 7.917 (3), 10.416 (3), 11.357 (5) |
α, β, γ (°) | 75.58 (5), 70.66 (3), 81.11 (4) |
V (Å3) | 853.2 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.35 |
Crystal size (mm) | 0.30 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Rigaku AFC12κ/SATURN724 |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.406, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9571, 3508, 3404 |
Rint | 0.019 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.061, 1.12 |
No. of reflections | 3508 |
No. of parameters | 244 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.58, −0.42 |
Computer programs: CrystalClear (Rigaku/MSC, 2005), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006).
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···F6i | 0.95 | 2.50 | 3.182 (3) | 128 |
C1—H1···N5ii | 0.95 | 2.56 | 3.336 (3) | 138 |
C2—H2···F2iii | 0.95 | 2.48 | 3.174 (3) | 130 |
C5—H5···F1 | 0.95 | 2.46 | 3.291 (3) | 146 |
C5—H5···F6 | 0.95 | 2.53 | 3.318 (3) | 140 |
C9—H9···F3iv | 0.95 | 2.51 | 3.160 (3) | 126 |
C11—H11···N5ii | 0.95 | 2.51 | 3.311 (3) | 142 |
Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x, −y+2, −z; (iii) x, y+1, z; (iv) −x, −y+1, −z. |
The structure of the title compound (I) was investigated as part of an on-going study of the structural chemistry of silver salts of the isomeric n-pyridinealdazine, n = 2, 3 and 4, molecules (Broker & Tiekink, 2007a-c).
Compound (I) features an Ag cation in a general position, two half 3-pyridinealdazine molecules, each disposed about a centre of inversion, an hexafluorophosphate anion and an acetonitrile solvent molecule, each in general positions (Fig. 1 & Table 1). The 3-pyridinealdazine molecule is bidentate bridging leading to a zigzag chain with a linear N2 coordination geometry for Ag.
The chains thus formed are linked via weakly bridging acetonitrile molecules with Ag···N5 and N5···Agi of 2.800 (3) and 2.826 (2) Å, respectively, as well as Ag···Agi interactions of 3.2590 (15) Å for (i): -x, 2 - y, -z. The topology of the resulting layer in the ac plane resembles a brick wall (Fig. 2).
The layers stack along the b axis and are interspersed by layers of PF6 anions. Various C—H···N and F interactions consolidate the structure (Fig. 3 & Table 2).
The zigzag topology found for the [Ag(C12H10N4)]n chain in (I) has precedents in the perchlorate, tetrafluoroborate salts (each as acetonitrile solvates) (Kennedy et al., 2005), and the methansulfonate salt (Broker & Tiekink, 2007c).