supplementary materials
catena-Poly[[silver(I)-[![[mu]](/logos/entities/mu_rmgif.gif)
-4-(2-pyridyl)pyrimidine-2-sulfonato]] monohydrate]
In the title compound, {[Ag(C9H6N3O3S)]·H2O}n, the AgI atom is coordinated by three N atoms and two sulfonate O atoms from two different 4-(2-pyridyl)pyrimidine-2-sulfonate ligands. The ligand bridges two AgI atoms, forming a polymeric zigzag chain propagating parallel to [001]. The uncoordinated water molecule is involved in hydrogen bonds with sulfonate O atoms.
A colorless solution of AgNO3 (0.017 g, 0.1 mmol) in CH3CN (5 ml) was
carefully layered onto a solution of 4-(2-pyridyl)pyrimidine-2-sulfonic
acid (0.026 g, 1 mmol) in H2O (5 ml). Diffusion between the two phases over
a period of 5 d produced light-yellow crystals (yield: 0.026 g, 72% based on
silver nitrate).
H atoms bounded to C atoms were positioned geometrically and allowed to ride on
their parent atoms, with C—H =0.93 Å and with Uiso(H) =
1.2Ueq(C). The positions of the water H atoms were found from a
difference Fourier map and refined as riding with O—H = 0.85 Å and
Uiso(H) = 1.2Ueq(O).
Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
catena-Poly[[silver(I)-[µ-4-(2-pyridyl)pyrimidine-2-sulfonato]]
monohydrate]
top
Crystal data top
| [Ag(C9H6N3O3S)]·H2O | F(000) = 712 |
| Mr = 362.12 | Dx = 2.147 Mg m−3 |
| Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2ybc | Cell parameters from 2533 reflections |
| a = 6.9020 (3) Å | θ = 2.3–27.5° |
| b = 13.6228 (6) Å | µ = 1.99 mm−1 |
| c = 12.1337 (5) Å | T = 298 K |
| β = 99.975 (2)° | Block, colorless |
| V = 1123.62 (8) Å3 | 0.18 × 0.15 × 0.12 mm |
| Z = 4 | |
Data collection top
Bruker APEXII CCD
diffractometer | 2533 independent reflections |
| Radiation source: fine-focus sealed tube | 2160 reflections with I > 2σ(I) |
| graphite | Rint = 0.015 |
| φ and ω scans | θmax = 27.5°, θmin = 2.3° |
Absorption correction: multi-scan
(SADABS; Bruker, 2001) | h = −8→8 |
| Tmin = 0.706, Tmax = 0.788 | k = −17→15 |
| 6630 measured reflections | l = −15→13 |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.071 | H-atom parameters constrained |
| S = 1.02 | w = 1/[σ2(Fo2) + (0.0401P)2 + 0.5886P]
where P = (Fo2 + 2Fc2)/3 |
| 2533 reflections | (Δ/σ)max < 0.001 |
| 163 parameters | Δρmax = 0.51 e Å−3 |
| 0 restraints | Δρmin = −0.53 e Å−3 |
Crystal data top
| [Ag(C9H6N3O3S)]·H2O | V = 1123.62 (8) Å3 |
| Mr = 362.12 | Z = 4 |
| Monoclinic, P21/c | Mo Kα radiation |
| a = 6.9020 (3) Å | µ = 1.99 mm−1 |
| b = 13.6228 (6) Å | T = 298 K |
| c = 12.1337 (5) Å | 0.18 × 0.15 × 0.12 mm |
| β = 99.975 (2)° | |
Data collection top
Bruker APEXII CCD
diffractometer | 2533 independent reflections |
Absorption correction: multi-scan
(SADABS; Bruker, 2001) | 2160 reflections with I > 2σ(I) |
| Tmin = 0.706, Tmax = 0.788 | Rint = 0.015 |
| 6630 measured reflections | θmax = 27.5° |
Refinement top
| R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
| wR(F2) = 0.071 | Δρmax = 0.51 e Å−3 |
| S = 1.02 | Δρmin = −0.53 e Å−3 |
| 2533 reflections | Absolute structure: ? |
| 163 parameters | Flack parameter: ? |
| 0 restraints | Rogers parameter: ? |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top| | x | y | z | Uiso*/Ueq | |
| Ag1 | 0.81252 (4) | 0.174975 (15) | 0.078449 (17) | 0.04992 (10) | |
| N2 | 0.7873 (3) | 0.14417 (14) | −0.11767 (17) | 0.0335 (4) | |
| N3 | 0.7593 (3) | 0.00808 (15) | 0.04023 (18) | 0.0389 (4) | |
| C3 | 0.7075 (4) | 0.03190 (19) | −0.2672 (2) | 0.0420 (6) | |
| H3A | 0.6753 | −0.0311 | −0.2936 | 0.050* | |
| C4 | 0.7418 (3) | 0.05178 (16) | −0.1536 (2) | 0.0333 (5) | |
| C6 | 0.6871 (4) | −0.1210 (2) | −0.0934 (3) | 0.0480 (6) | |
| H6A | 0.6683 | −0.1416 | −0.1675 | 0.058* | |
| C9 | 0.7459 (4) | −0.0571 (2) | 0.1213 (3) | 0.0477 (6) | |
| H9A | 0.7662 | −0.0355 | 0.1950 | 0.057* | |
| C8 | 0.7034 (4) | −0.1546 (2) | 0.1002 (3) | 0.0527 (7) | |
| H8A | 0.6952 | −0.1977 | 0.1586 | 0.063* | |
| C7 | 0.6733 (4) | −0.1873 (2) | −0.0083 (3) | 0.0544 (8) | |
| H7A | 0.6440 | −0.2529 | −0.0246 | 0.065* | |
| C5 | 0.7293 (3) | −0.02331 (18) | −0.0662 (2) | 0.0359 (5) | |
| S1 | 0.85817 (10) | 0.33521 (4) | −0.14563 (5) | 0.04032 (15) | |
| N1 | 0.7693 (3) | 0.19927 (16) | −0.30431 (18) | 0.0410 (5) | |
| C1 | 0.7996 (3) | 0.21175 (17) | −0.1937 (2) | 0.0338 (5) | |
| O2 | 0.6717 (4) | 0.38366 (17) | −0.1628 (2) | 0.0786 (8) | |
| C2 | 0.7221 (4) | 0.1074 (2) | −0.3396 (2) | 0.0463 (6) | |
| H2B | 0.6986 | 0.0947 | −0.4160 | 0.056* | |
| O1 | 0.9932 (4) | 0.36957 (18) | −0.21511 (19) | 0.0694 (7) | |
| O3 | 0.9460 (3) | 0.32665 (13) | −0.02960 (17) | 0.0521 (5) | |
| O4 | 1.2896 (6) | 0.4143 (3) | 0.0834 (5) | 0.189 (3) | |
| H2 | 1.1797 | 0.3920 | 0.0504 | 0.226* | |
| H1 | 1.3116 | 0.4722 | 0.1086 | 0.226* | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Ag1 | 0.07851 (18) | 0.03703 (13) | 0.03468 (13) | 0.00054 (9) | 0.01113 (10) | −0.00254 (7) |
| N2 | 0.0349 (10) | 0.0297 (9) | 0.0368 (11) | −0.0010 (8) | 0.0082 (8) | −0.0028 (8) |
| N3 | 0.0411 (11) | 0.0335 (10) | 0.0430 (11) | 0.0032 (9) | 0.0096 (9) | 0.0039 (9) |
| C3 | 0.0486 (14) | 0.0329 (12) | 0.0455 (14) | −0.0056 (11) | 0.0107 (11) | −0.0092 (10) |
| C4 | 0.0272 (11) | 0.0300 (11) | 0.0432 (13) | 0.0012 (8) | 0.0076 (9) | −0.0016 (9) |
| C6 | 0.0498 (15) | 0.0319 (13) | 0.0616 (18) | −0.0013 (11) | 0.0077 (13) | −0.0046 (11) |
| C9 | 0.0497 (15) | 0.0428 (14) | 0.0526 (16) | 0.0047 (12) | 0.0144 (12) | 0.0088 (12) |
| C8 | 0.0436 (15) | 0.0419 (14) | 0.074 (2) | 0.0054 (11) | 0.0144 (14) | 0.0200 (14) |
| C7 | 0.0494 (16) | 0.0296 (13) | 0.083 (2) | 0.0000 (11) | 0.0094 (15) | 0.0069 (13) |
| C5 | 0.0283 (11) | 0.0305 (11) | 0.0496 (14) | 0.0021 (9) | 0.0091 (10) | 0.0000 (10) |
| S1 | 0.0537 (4) | 0.0295 (3) | 0.0366 (3) | −0.0036 (3) | 0.0045 (3) | −0.0018 (2) |
| N1 | 0.0530 (13) | 0.0370 (10) | 0.0342 (11) | −0.0035 (9) | 0.0110 (9) | −0.0035 (8) |
| C1 | 0.0352 (11) | 0.0318 (11) | 0.0354 (12) | −0.0005 (9) | 0.0089 (9) | −0.0030 (9) |
| O2 | 0.0733 (15) | 0.0478 (13) | 0.105 (2) | 0.0202 (11) | −0.0121 (14) | −0.0218 (13) |
| C2 | 0.0590 (16) | 0.0432 (14) | 0.0368 (13) | −0.0060 (12) | 0.0087 (11) | −0.0094 (11) |
| O1 | 0.0992 (17) | 0.0608 (14) | 0.0516 (12) | −0.0412 (13) | 0.0224 (12) | −0.0040 (10) |
| O3 | 0.0732 (13) | 0.0410 (11) | 0.0394 (11) | −0.0113 (9) | 0.0021 (9) | −0.0044 (8) |
| O4 | 0.113 (3) | 0.114 (3) | 0.304 (7) | 0.030 (2) | −0.063 (4) | −0.126 (4) |
Geometric parameters (Å, °) top
| Ag1—N1i | 2.279 (2) | C9—C8 | 1.374 (4) |
| Ag1—N2 | 2.393 (2) | C9—H9A | 0.9300 |
| Ag1—N3 | 2.337 (2) | C8—C7 | 1.370 (5) |
| Ag1—O1i | 2.668 (2) | C8—H8A | 0.9300 |
| Ag1—O3 | 2.693 (2) | C7—H7A | 0.9300 |
| N2—C1 | 1.317 (3) | S1—O2 | 1.429 (2) |
| N2—C4 | 1.351 (3) | S1—O3 | 1.438 (2) |
| N3—C9 | 1.340 (3) | S1—O1 | 1.439 (2) |
| N3—C5 | 1.342 (3) | S1—C1 | 1.803 (2) |
| C3—C2 | 1.368 (4) | N1—C1 | 1.333 (3) |
| C3—C4 | 1.384 (3) | N1—C2 | 1.344 (3) |
| C3—H3A | 0.9300 | N1—Ag1ii | 2.279 (2) |
| C4—C5 | 1.487 (3) | C2—H2B | 0.9300 |
| C6—C7 | 1.388 (4) | O4—H2 | 0.8500 |
| C6—C5 | 1.389 (4) | O4—H1 | 0.8500 |
| C6—H6A | 0.9300 | | |
| | | |
| N1i—Ag1—N3 | 145.30 (7) | C8—C9—H9A | 118.5 |
| N1i—Ag1—N2 | 139.26 (7) | C7—C8—C9 | 119.0 (3) |
| N3—Ag1—N2 | 69.52 (7) | C7—C8—H8A | 120.5 |
| O1i—Ag1—N2 | 146.68 (7) | C9—C8—H8A | 120.5 |
| O1i—Ag1—N3 | 89.82 (7) | C8—C7—C6 | 119.0 (3) |
| O1i—Ag1—N1i | 71.05 (8) | C8—C7—H7A | 120.5 |
| O3—Ag1—N1i | 79.63 (7) | C6—C7—H7A | 120.5 |
| O3—Ag1—N2 | 67.83 (7) | N3—C5—C6 | 121.6 (2) |
| O3—Ag1—N3 | 134.83 (6) | N3—C5—C4 | 116.7 (2) |
| C1—N2—C4 | 117.7 (2) | C6—C5—C4 | 121.7 (2) |
| C1—N2—Ag1 | 124.89 (16) | O2—S1—O3 | 113.36 (16) |
| C4—N2—Ag1 | 117.21 (15) | O2—S1—O1 | 115.00 (18) |
| C9—N3—C5 | 118.4 (2) | O3—S1—O1 | 113.20 (14) |
| C9—N3—Ag1 | 121.87 (19) | O2—S1—C1 | 103.76 (13) |
| C5—N3—Ag1 | 119.59 (16) | O3—S1—C1 | 105.92 (11) |
| C2—C3—C4 | 118.3 (2) | O1—S1—C1 | 104.21 (12) |
| C2—C3—H3A | 120.9 | C1—N1—C2 | 115.2 (2) |
| C4—C3—H3A | 120.9 | C1—N1—Ag1ii | 121.18 (17) |
| N2—C4—C3 | 119.6 (2) | C2—N1—Ag1ii | 123.49 (17) |
| N2—C4—C5 | 116.7 (2) | N2—C1—N1 | 126.8 (2) |
| C3—C4—C5 | 123.7 (2) | N2—C1—S1 | 117.60 (18) |
| C7—C6—C5 | 119.0 (3) | N1—C1—S1 | 115.62 (18) |
| C7—C6—H6A | 120.5 | N1—C2—C3 | 122.4 (2) |
| C5—C6—H6A | 120.5 | N1—C2—H2B | 118.8 |
| N3—C9—C8 | 122.9 (3) | C3—C2—H2B | 118.8 |
| N3—C9—H9A | 118.5 | H2—O4—H1 | 126.2 |
| Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H2···O3 | 0.85 | 1.95 | 2.793 (4) | 173 |
| O4—H1···O2iii | 0.85 | 2.07 | 2.913 (4) | 173 |
| Symmetry codes: (iii) −x+2, −y+1, −z. |
Table 1
Selected geometric parameters (Å) top| Ag1—N1i | 2.279 (2) | Ag1—O1i | 2.668 (2) |
| Ag1—N2 | 2.393 (2) | Ag1—O3 | 2.693 (2) |
| Ag1—N3 | 2.337 (2) | | |
| Symmetry codes: (i) x, −y+1/2, z+1/2. |
Table 2
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H2···O3 | 0.85 | 1.95 | 2.793 (4) | 173 |
| O4—H1···O2ii | 0.85 | 2.07 | 2.913 (4) | 173 |
| Symmetry codes: (ii) −x+2, −y+1, −z. |
The author acknowledges financial support from the Young Teachers' Starting Fund
of Southeast University.
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Zhu, H.-B., Dong, H.-Z., Huang, W. & Gou, S.-H. (2007). J. Mol. Struct. 831, 55–60.
![[Figure 1]](./hy2295fig1thm.gif)
In our previous work, we have reported several divalent transition metal coordination compounds with 4-(2-pyridyl)pyrimidine-2-sulfonate (L) ligand (Zhu et al., 2007). Herein, we present a new silver(I) coordination polymer with L.
The title compound has a polymeric zigzag chain structure, where the AgI atom is penta-coordinated by three N atoms and two sulfonate O atoms from two L ligands (Fig. 1). The Ag—N bond lengths vary between 2.279 (2) and 2.393 (2) Å, and the Ag—O distances are in the range of 2.668 (2) and 2.693 (2)Å (Table 1). The uncoordinated water molecule is involved in hydrogen bonds with sulfonate O atoms (Table 2).