Table 1. Crystal Data and Structure Refinement for Compounds 1 to 3.
| compound | 1 | 2 | 2a | 3 | 3a |
|---|---|---|---|---|---|
| empirical formula | C38H57Ag8N24O26.5S4 | C36H55Ag8N24O27.5S4 | C36H59Ag8N24O29.5S4 | C36H50Ag8N23O22S4 | C36H45Ag8N23O19.5S4 |
| formula weight | 2265.27 | 2255.24 | 2291.27 | 2148.19 | 2103.15 |
| temperature/K | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) |
| wavelength/Å | 0.71073 | 0.71073 | 0.71073 | 0.71073 | 0.71073 |
| crystal system | triclinic | triclinic | triclinic | orthorhombic | orthorhombic |
| space group |
P
|
P
|
P
|
Pna21 | Pna21 |
| unit cell dimensions | |||||
| a/Å | 14.528(4) | 14.4297(5) | 14.5438(4) | 30.9867(12) | 30.9915(12) |
| b/Å | 14.826(4) | 14.8045(5) | 14.9365(4) | 15.0720(5) | 15.0756(5) |
| c/Å | 16.510(4) | 16.5989(6 | 16.6151(4) | 13.5982(5) | 13.6003(5) |
| α/° | 78.840(4) | 78.355(2) | 78.8090(10) | 90 | 90 |
| β/° | 87.479(4) | 87.561(2) | 88.3910(10) | 90 | 90 |
| γ/° | 77.325(4) | 75.984(2) | 75.023(2) | 90 | 90 |
| volume/Å–3 | 3403.9(16) | 3369.5(2) | 3419.52(16) | 6350.8(4) | 6354.3(4) |
| Z | 2 | 2 | 2 | 4 | 4 |
| calc. density/Mg/m3 | 2.210 | 2.223 | 2.225 | 2.247 | 2.198 |
| absorp. coefc./mm–1 | 2.469 | 2.494 | 2.462 | 2.634 | 2.627 |
| F(000) | 2210 | 2198 | 2238 | 4172 | 4072 |
| crystal size | 0.20 × 0.08 × 0.05 | 0.16 × 0.11 × 0.04 | 0.08 × 0.08 × 0.06 | 0.16 × 0.05 × 0.05 | 0.16 × 0.05 × 0.05 |
| θ range/° | 1.719–25.681 | 1.455–27.877 | 1.713–25.682 | 1.885–30.533 | 1.885–30.516 |
| limiting indices/h,k,l | –17/17,–17/18,0/20 | –18/18,–18/19,0/21 | –17/17,–17/18,0/20 | 0/44,0/21,–19/19 | –44/43,–21/21,–19/19 |
| refl. collect/unique | 38502/12898 | 86514/16007 | 78787/12884 | 130098/19259 | 128576/19312 |
| Rint | 0.0379 | 0.0492 | 0.0542 | 0.0533 | 0.0674 |
| absorp. correct. | multiscan | multiscan | multiscan | multiscan | multiscan |
| max. /min transm. | 1.000/0.639 | 1.000/0.845 | 1.000/0.713 | 1.000/0.735 | 1.000/0.873 |
| data/rest/parameters | 12898/30/875 | 16007/24/901 | 12884//96/909 | 19259/73/819 | 19312/19/823 |
| goodness-of-fit on F2 | 1.046 | 1.027 | 0.991 | 1.037 | 1.057 |
| final R indices | R1 = 0.0468, wR2 = 0.1046 | R1 = 0.0354, wR2 = 0.0844 | R1 = 0.0624, wR2 = 0.1385 | R1= 0.0688, wR2 = 0.1572 | R1 = 0.0702, wR2 = 0.1610 |
| R indices (all data) | R1 = 0.0837, wR2 = 0.1146 | R1 = 0.0497, wR2 = 0.0916 | R1 = 0.1217, wR2 = 0.1575 | R1 = 0.0864, wR2 = 0.1651 | R1 = 0.0895, wR2 = 0.1719 |
| largest dif. peak/hole | 2.296/–1.227 | 2.517/–1.327 | 1.943/–1.208 | 3.814/–1.840 | 3.612/–1.885 |
| CCDC number | 2321205 | 2321206 | 2321207 | 2321208 | 2321204 |