The title two-dimensional coordination polymer, {[Ag(C6H8N2)2]PF6}n, has been formed by the self-assembly of 4-aminomethylpyridine (amp) ligands with silver(I) hexafluorophosphate in a 2:1 ratio. The polymer consists of dimeric silver–amp rectangles that are linked together to make a larger hexametallic rectangle.
Supporting information
CCDC reference: 283962
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.002 Å
- R factor = 0.021
- wR factor = 0.051
- Data-to-parameter ratio = 18.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P1
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.
Phyllo-poly[[silver(I)-di-µ
2-4-aminomethylpyridine-
κ2N:
N']
hexafluorophosphate]
top
Crystal data top
[Ag(C6H8N2)2]PF6 | F(000) = 928 |
Mr = 469.13 | Dx = 1.781 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6955 reflections |
a = 11.2159 (12) Å | θ = 2.3–28.2° |
b = 11.7722 (12) Å | µ = 1.30 mm−1 |
c = 13.2758 (13) Å | T = 110 K |
β = 93.454 (4)° | Block, colorless |
V = 1749.7 (3) Å3 | 0.18 × 0.13 × 0.11 mm |
Z = 4 | |
Data collection top
Bruker–Nonius X8 APEX diffractometer | 4333 independent reflections |
Radiation source: fine-focus sealed tube | 3950 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 28.3°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→12 |
Tmin = 0.844, Tmax = 0.867 | k = −15→14 |
23273 measured reflections | l = −17→17 |
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)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0235P)2 + 1.0267P] where P = (Fo2 + 2Fc2)/3 |
4333 reflections | (Δ/σ)max = 0.001 |
229 parameters | Δρmax = 0.65 e Å−3 |
0 restraints | Δρmin = −0.44 e Å−3 |
Special details top
Experimental. 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 > 2sigma(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. |
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 | 0.325590 (10) | 0.947725 (10) | 0.188911 (8) | 0.02554 (5) | |
N1 | 0.35986 (12) | 0.91617 (12) | 0.02107 (10) | 0.0236 (3) | |
N2 | 0.52797 (13) | 1.00178 (13) | −0.31077 (10) | 0.0256 (3) | |
N3 | 0.20622 (12) | 0.79975 (11) | 0.24512 (9) | 0.0226 (3) | |
H3A | 0.5632 (19) | 0.9920 (18) | −0.3657 (16) | 0.034* | |
H3B | 0.477 (2) | 1.0542 (17) | −0.3197 (16) | 0.034* | |
N4 | −0.17845 (13) | 0.59671 (13) | 0.31536 (11) | 0.0270 (3) | |
H4A | −0.1894 (19) | 0.6531 (19) | 0.3543 (17) | 0.041* | |
H4B | −0.186 (2) | 0.6213 (19) | 0.2568 (18) | 0.041* | |
P1 | 0.76423 (4) | 0.61349 (3) | 0.98117 (3) | 0.02251 (8) | |
F1 | 0.80689 (12) | 0.58093 (10) | 1.09465 (8) | 0.0467 (3) | |
F2 | 0.73258 (12) | 0.48271 (9) | 0.95928 (9) | 0.0472 (3) | |
F3 | 0.63127 (11) | 0.63246 (13) | 1.01491 (10) | 0.0591 (4) | |
F4 | 0.71793 (10) | 0.64614 (9) | 0.86741 (7) | 0.0374 (2) | |
F5 | 0.79576 (14) | 0.74397 (9) | 1.00225 (8) | 0.0527 (3) | |
F6 | 0.89449 (11) | 0.59366 (12) | 0.94598 (11) | 0.0542 (3) | |
C1 | 0.31165 (14) | 0.98434 (14) | −0.05217 (12) | 0.0255 (3) | |
H1 | 0.2540 | 1.0389 | −0.0347 | 0.031* | |
C2 | 0.34203 (14) | 0.97866 (14) | −0.15173 (12) | 0.0249 (3) | |
H2 | 0.3051 | 1.0279 | −0.2009 | 0.030* | |
C3 | 0.42717 (13) | 0.90006 (13) | −0.17898 (11) | 0.0210 (3) | |
C4 | 0.47605 (15) | 0.82922 (13) | −0.10382 (12) | 0.0260 (3) | |
H4 | 0.5337 | 0.7738 | −0.1193 | 0.031* | |
C5 | 0.44040 (15) | 0.83972 (14) | −0.00629 (12) | 0.0267 (3) | |
H5 | 0.4748 | 0.7902 | 0.0439 | 0.032* | |
C6 | 0.46796 (15) | 0.89406 (14) | −0.28526 (11) | 0.0265 (3) | |
H6A | 0.5240 | 0.8298 | −0.2910 | 0.032* | |
H6B | 0.3983 | 0.8810 | −0.3333 | 0.032* | |
C7 | 0.16049 (14) | 0.72139 (14) | 0.18014 (12) | 0.0257 (3) | |
H7 | 0.1862 | 0.7215 | 0.1132 | 0.031* | |
C8 | 0.07777 (15) | 0.64028 (14) | 0.20551 (13) | 0.0289 (3) | |
H8 | 0.0487 | 0.5861 | 0.1570 | 0.035* | |
C9 | 0.03794 (14) | 0.63912 (14) | 0.30258 (13) | 0.0267 (3) | |
C10 | 0.08518 (14) | 0.71997 (14) | 0.37056 (12) | 0.0265 (3) | |
H10 | 0.0607 | 0.7218 | 0.4378 | 0.032* | |
C11 | 0.16816 (14) | 0.79770 (13) | 0.33932 (12) | 0.0245 (3) | |
H11 | 0.1996 | 0.8521 | 0.3866 | 0.029* | |
C12 | −0.05550 (17) | 0.55443 (15) | 0.33177 (16) | 0.0363 (4) | |
H12A | −0.0470 | 0.4841 | 0.2920 | 0.044* | |
H12B | −0.0407 | 0.5347 | 0.4039 | 0.044* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.02130 (7) | 0.03094 (8) | 0.02476 (7) | −0.00096 (5) | 0.00456 (4) | 0.00095 (4) |
N1 | 0.0230 (7) | 0.0257 (6) | 0.0222 (6) | −0.0017 (5) | 0.0021 (5) | 0.0001 (5) |
N2 | 0.0238 (7) | 0.0327 (8) | 0.0205 (6) | 0.0028 (6) | 0.0042 (5) | 0.0025 (5) |
N3 | 0.0211 (6) | 0.0220 (6) | 0.0246 (6) | 0.0012 (5) | 0.0010 (5) | 0.0002 (5) |
N4 | 0.0245 (7) | 0.0277 (7) | 0.0291 (7) | −0.0038 (6) | 0.0042 (5) | −0.0062 (6) |
P1 | 0.0259 (2) | 0.02062 (19) | 0.02091 (17) | 0.00260 (15) | 0.00047 (14) | 0.00117 (14) |
F1 | 0.0702 (9) | 0.0390 (6) | 0.0289 (5) | −0.0009 (6) | −0.0150 (5) | 0.0081 (5) |
F2 | 0.0611 (8) | 0.0257 (5) | 0.0527 (7) | −0.0081 (5) | −0.0137 (6) | 0.0007 (5) |
F3 | 0.0461 (7) | 0.0754 (9) | 0.0589 (8) | 0.0292 (7) | 0.0292 (6) | 0.0337 (7) |
F4 | 0.0463 (6) | 0.0421 (6) | 0.0232 (4) | −0.0044 (5) | −0.0038 (4) | 0.0062 (4) |
F5 | 0.1011 (11) | 0.0221 (5) | 0.0342 (6) | −0.0060 (6) | −0.0032 (6) | −0.0020 (4) |
F6 | 0.0305 (6) | 0.0615 (8) | 0.0715 (9) | 0.0072 (6) | 0.0118 (6) | 0.0021 (7) |
C1 | 0.0223 (8) | 0.0272 (8) | 0.0272 (7) | 0.0038 (6) | 0.0029 (6) | 0.0004 (6) |
C2 | 0.0233 (8) | 0.0270 (8) | 0.0242 (7) | 0.0021 (6) | −0.0012 (6) | 0.0031 (6) |
C3 | 0.0200 (7) | 0.0221 (7) | 0.0208 (6) | −0.0044 (6) | 0.0006 (5) | −0.0025 (5) |
C4 | 0.0278 (8) | 0.0232 (8) | 0.0270 (7) | 0.0054 (6) | 0.0022 (6) | −0.0015 (6) |
C5 | 0.0299 (8) | 0.0255 (8) | 0.0244 (7) | 0.0034 (7) | −0.0004 (6) | 0.0041 (6) |
C6 | 0.0285 (8) | 0.0314 (8) | 0.0197 (7) | −0.0017 (7) | 0.0014 (6) | −0.0038 (6) |
C7 | 0.0230 (8) | 0.0306 (8) | 0.0232 (7) | 0.0050 (6) | −0.0004 (6) | −0.0053 (6) |
C8 | 0.0247 (8) | 0.0261 (8) | 0.0350 (8) | 0.0010 (6) | −0.0056 (6) | −0.0099 (6) |
C9 | 0.0186 (7) | 0.0220 (7) | 0.0390 (8) | 0.0010 (6) | −0.0025 (6) | 0.0007 (6) |
C10 | 0.0265 (8) | 0.0271 (8) | 0.0262 (7) | −0.0009 (7) | 0.0035 (6) | 0.0000 (6) |
C11 | 0.0269 (8) | 0.0220 (7) | 0.0244 (7) | −0.0015 (6) | 0.0008 (6) | −0.0045 (6) |
C12 | 0.0264 (9) | 0.0286 (9) | 0.0532 (11) | −0.0067 (7) | −0.0035 (8) | 0.0066 (8) |
Geometric parameters (Å, º) top
Ag1—N1 | 2.3139 (13) | C1—C2 | 1.386 (2) |
Ag1—N2i | 2.3126 (14) | C1—H1 | 0.9500 |
Ag1—N3 | 2.3461 (13) | C2—C3 | 1.393 (2) |
Ag1—N4ii | 2.4066 (14) | C2—H2 | 0.9500 |
N1—C5 | 1.341 (2) | C3—C4 | 1.388 (2) |
N1—C1 | 1.349 (2) | C3—C6 | 1.511 (2) |
N2—C6 | 1.484 (2) | C4—C5 | 1.383 (2) |
N2—Ag1i | 2.3126 (14) | C4—H4 | 0.9500 |
N2—H3A | 0.86 (2) | C5—H5 | 0.9500 |
N2—H3B | 0.85 (2) | C6—H6A | 0.9900 |
N3—C7 | 1.343 (2) | C6—H6B | 0.9900 |
N3—C11 | 1.346 (2) | C7—C8 | 1.387 (2) |
N4—C12 | 1.470 (2) | C7—H7 | 0.9500 |
N4—Ag1iii | 2.4066 (14) | C8—C9 | 1.389 (2) |
N4—H4A | 0.86 (2) | C8—H8 | 0.9500 |
N4—H4B | 0.83 (2) | C9—C10 | 1.394 (2) |
P1—F6 | 1.5778 (13) | C9—C12 | 1.514 (2) |
P1—F5 | 1.5972 (12) | C10—C11 | 1.386 (2) |
P1—F3 | 1.5984 (12) | C10—H10 | 0.9500 |
P1—F1 | 1.5996 (11) | C11—H11 | 0.9500 |
P1—F2 | 1.6025 (12) | C12—H12A | 0.9900 |
P1—F4 | 1.6136 (10) | C12—H12B | 0.9900 |
| | | |
N1—Ag1—N2i | 124.25 (5) | C2—C1—H1 | 118.4 |
N1—Ag1—N3 | 108.55 (5) | C1—C2—C3 | 119.44 (14) |
N1—Ag1—N4ii | 104.35 (5) | C1—C2—H2 | 120.3 |
N2i—Ag1—N3 | 111.30 (5) | C3—C2—H2 | 120.3 |
N2i—Ag1—N4ii | 106.64 (5) | C4—C3—C2 | 117.36 (13) |
N3—Ag1—N4ii | 98.33 (5) | C4—C3—C6 | 120.98 (14) |
C5—N1—C1 | 116.85 (13) | C2—C3—C6 | 121.63 (14) |
C5—N1—Ag1 | 121.49 (10) | C5—C4—C3 | 119.70 (15) |
C1—N1—Ag1 | 121.07 (10) | C5—C4—H4 | 120.2 |
C6—N2—Ag1i | 111.88 (9) | C3—C4—H4 | 120.2 |
C6—N2—H3A | 108.5 (15) | N1—C5—C4 | 123.43 (14) |
Ag1i—N2—H3A | 106.5 (14) | N1—C5—H5 | 118.3 |
C6—N2—H3B | 110.1 (14) | C4—C5—H5 | 118.3 |
Ag1i—N2—H3B | 110.9 (14) | N2—C6—C3 | 109.88 (13) |
H3A—N2—H3B | 109 (2) | N2—C6—H6A | 109.7 |
C7—N3—C11 | 117.01 (14) | C3—C6—H6A | 109.7 |
C7—N3—Ag1 | 120.58 (10) | N2—C6—H6B | 109.7 |
C11—N3—Ag1 | 121.87 (10) | C3—C6—H6B | 109.7 |
C12—N4—Ag1iii | 113.11 (11) | H6A—C6—H6B | 108.2 |
C12—N4—H4A | 109.9 (15) | N3—C7—C8 | 123.50 (15) |
Ag1iii—N4—H4A | 117.2 (15) | N3—C7—H7 | 118.3 |
C12—N4—H4B | 107.5 (16) | C8—C7—H7 | 118.3 |
Ag1iii—N4—H4B | 101.5 (16) | C7—C8—C9 | 119.29 (14) |
H4A—N4—H4B | 107 (2) | C7—C8—H8 | 120.4 |
F6—P1—F5 | 89.71 (8) | C9—C8—H8 | 120.4 |
F6—P1—F3 | 178.92 (8) | C8—C9—C10 | 117.57 (15) |
F5—P1—F3 | 90.97 (8) | C8—C9—C12 | 120.68 (16) |
F6—P1—F1 | 90.78 (8) | C10—C9—C12 | 121.73 (16) |
F5—P1—F1 | 90.85 (6) | C11—C10—C9 | 119.53 (15) |
F3—P1—F1 | 90.04 (7) | C11—C10—H10 | 120.2 |
F6—P1—F2 | 90.18 (8) | C9—C10—H10 | 120.2 |
F5—P1—F2 | 179.65 (7) | N3—C11—C10 | 123.10 (14) |
F3—P1—F2 | 89.13 (8) | N3—C11—H11 | 118.5 |
F1—P1—F2 | 89.49 (6) | C10—C11—H11 | 118.5 |
F6—P1—F4 | 90.55 (7) | N4—C12—C9 | 113.38 (14) |
F5—P1—F4 | 89.44 (6) | N4—C12—H12A | 108.9 |
F3—P1—F4 | 88.62 (6) | C9—C12—H12A | 108.9 |
F1—P1—F4 | 178.64 (7) | N4—C12—H12B | 108.9 |
F2—P1—F4 | 90.22 (6) | C9—C12—H12B | 108.9 |
N1—C1—C2 | 123.21 (15) | H12A—C12—H12B | 107.7 |
N1—C1—H1 | 118.4 | | |
Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x, y+1/2, −z+1/2; (iii) −x, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H3A···F3iv | 0.86 (2) | 2.32 (2) | 3.0852 (19) | 148.5 (19) |
N4—H4B···F1v | 0.83 (2) | 2.20 (2) | 2.9308 (19) | 147 (2) |
N4—H4A···F5vi | 0.86 (2) | 2.32 (2) | 3.1374 (19) | 159.5 (19) |
Symmetry codes: (iv) x, −y+3/2, z−3/2; (v) x−1, y, z−1; (vi) x−1, −y+3/2, z−1/2. |