Hybrid adamantane-type cluster compounds with group 14 elements in the Q position and group 16 atoms in the E positiona.
| Compound | Reagents/conditions | Method |
|---|---|---|
| [(MeSi)4S6] (565) | MeSiCl3, H2S/200 °C, 12 h | F304,305 |
| [(EtSi)4S6] (566) | EtSiCl3, H2S/150 °C, 3 h | F304 |
| [(ThexSi)4S6] (567) | 1. Li2S, ThexSiCl3/THF, 0 °C to RT, 14 days | D306,307 |
| 2. Decaline, 195 °C, 24 h | ||
| [(PhSi)4S6] (568) | PhSiCl3, Na2S/THF, 0 °C to RT, 24 h | D310 |
| [(RSi)4S6] (569–570, R = 1-Np, Sty) | Na2S, 1-NpSiCl3/THF, 0 °C, 18 h | D309 |
| [(MeSi)4Se6] (571) | MeSiCl3, H2Se/400 °C, 1 h | F304 |
| [(EtSi)4Se6] (572) | EtSiCl3, H2Se, Al/150 °C, 3 h | F304 |
| [(ThexSi)4Se6] (573) | 1. Li2S, ThexSiCl3/THF, 0 °C to RT, 5 days | D306,307 |
| 2. Decaline, 150 °C, 3 h | ||
| [(PhSi)4Se6] (574) | Na2Se, PhSiCl3/THF, 0 °C, 18 h | D308 |
| [(MeGe)4S6] (575) | MeGeBr3, H2S, NEt3/C6H6, 80 °C, 1 h | D311,312 |
| [(EtGe)4S6] (576) | EtGeCl3, (SiH3)2S, Al2Cl6/CS2, 75 °C, 7 days | D313 |
| [(CF3Ge)4S6] (577) | CF3GeCl3, (SiH3)2S, Al2Cl6/CS2, 80 °C, 10 days | D313 |
| [(ThexGe)4S6] (578) | 1. Li2S, ThexGeCl3/THF, 0 °C to RT, 24 h | D306,307 |
| 2. Decaline, 195 °C, 24 h | ||
| [{HOOC(CH2)2Ge}4S6] (579) | HOOC(CH2)2GeCl3, Na2S/Me2CO, H2O, 3 h | D323 |
| [{Me(O)CCH2CMe2Ge}4S6] (580) | MeOCCH2CMe2GeCl3, Na2S/Me2CO, H2O, 4 h | D323 |
| [{NC(CH2)2Ge}4S6] (581) | NC(CH2)2GeCl3, Na2S/Me2CO, H2O, 5 h | D314 |
| [(PhGe)4S6] (582) | PhGeCl3, Na2S/Me2CO, H2O, 1 h | D310 |
| [(CF3Ge)4Se6] (583) | CF3GeCl3, (SiH3)2Se, Al2Cl6/n-hexane, 110 °C, 4 days | D313 |
| [(ThexGe)4Se6] (584) | 1. Li2Se, ThexGeCl3/THF, 0 °C to RT, 24 h | D306,307 |
| 2.C6H6, 80 °C, 24 h | ||
| [{NC(CH2)2Ge}4Se6] (585) | NC(CH2)2GeCl3, Na2Se/THF, 30 h | D314 |
| [(MeSn)4S6] (586) | MeSnI3, H2S, HCl/H2O or MeSnCl3, Na2S/Me2CO, H2O, 3 h | G/D303,304,315,316 |
| [(PhSn)4S6] (587) | PhSnCl3, Na2S/Me2CO, H2O, 4 h | D304 |
| [(nBuSn)4S6] (588) | n BuSnCl3, Na2S/Me2CO, H2O, 3 h | D304,316,317 |
| [(nPrSn)4S6] (589) | (nPrSn)2O3, Na2S, HCl/H2O, 3 h | D316 |
| [(mesSn)4S6] (590) | mesSnCl3, Na2S/H2O, Me2CO, 0 °C, 12 h | D319 |
| [(1-NpSn)4S6] (591) | 1-NpSnCl3, Na2S/H2O, Me2CO, 0 °C, 18 h | D319 |
| [(4-MeC6H4Sn)4S6] (592) | 4-MeC6H4SnCl3, Na2S/H2O, Me2CO, 0 °C, 4 h | D319 |
| [(4-MeOC6H4Sn)4S6] (593) | 4-MeOC6H4SnCl3, Na2S/H2O, Me2CO, 0 °C, 2 h | D319 |
| [(4-FC6H4Sn)4S6] (594) | 4-FC6H4SnCl3, Na2S/H2O, Me2CO, 0 °C, 14 h | D319 |
| [(3-FC6H4Sn)4S6] (595) | 3-FC6H4SnCl3, (SiMe3)2S/10 °C, 1 h | D319 |
| [(C6F5Sn)4S6] (596) | C6F5SnCl3, (SiMe3)2S/C6H6, 10 °C, 15 min | D319 |
| [{(Me3Si)3CSn}4S6] (597) | [(Me3Si)3CSnBr3], Na2S/NH3, 24 h | D317 |
| [(StySn)4S6] (598) | PhSnCl3, Na2S/THF, 0 °C to RT, 24 h | D320 |
| [(CySn)4S6] (599) | CySnCl3, (SiMe3)2S/toluene, 24 h | D321 |
| [(BnSn)4S6] (600) | BnSnCl3, (SiMe3)2S/toluene, 5 min | D321 |
| [{EtO2C(C6H4)CH2CH2Sn}4S6] (601) | EtO2C(C6H4)CH2CH2SnCl3, (SiMe3)2S/toluene, 2 h | D321 |
| [(CpSn)4S6] (602) | 1. SnCl4, NaCp/toluene, 0 °C, 5 h | D321 |
| 2. (SiMe3)2S/toluene, 1 h | ||
| [(MeSn)4Se6] (603) | MeSnBr3, NaHSe, Na[BH4]/H2O, 1 h | D318 |
| [(nBuSn)4Se6] (604) | Na2Se, nBuSnCl3/NH3, −33 °C, 5 h | D317 |
| [{(Me3Si)3CSn}4Se6] (605) | [(Me3Si)3CSnBr3], Na2Se/NH3, 24 h | D317 |
| [(iPrSn)4Se6] (606) | iPrSnCl3, Na2S/H2O, Me2CO, 0 °C, 18 h | D322 |
| [(PhSn)4Se6] (607) | PhSnCl3, (SiMe3)2Se/toluene, 5 min | D321 |
| [(BnSn)4Se6] (608) | BnSnCl3, (SiMe3)2Se/toluene, 5 min | D321 |
| [EtO2C(C6H4)CH2CH2Sn)4Se6] (609) | EtO2C(C6H4)CH2CH2SnCl3, (SiMe3)2Se/toluene, 16 h | D321 |
| [(CpSn)4Se6] (610) | 1. SnCl4, NaCp/toluene, 0 °C, 5 h | D321 |
| 2. (SiMe3)2S/toluene, 5 min | ||
| [(CySn)4Se6] (611) | CySnCl3, (SiMe3)2Se/toluene, 1 h | D321 |
| [{Me(PhNHN)CCH2CMe2Ge}4S6] (612) | [(MeOCCH2CMe2Ge)4S6], H2NNHPh/CH2Cl2, 3 h | Q323 |
| [(N(SiMe3)DippSi)4Te6] (613) | [Si4{N(SiMe3)Dipp}4], (nBu)3PTe/toluene, 110 °C, 2 h | J324 |
| [{N(2,6-iPr2C6H3)(SiMe3)Sn}4E6] (614–615, E = S, Se) | N(2,6-iPr2C6H3)(SiMe3)SnCl, E/THF, 18 h | C325 |
| [({Cp(CO)2Fe}Sn)4Se6] (616) | [{Cp(CO)2Fe}2SnCl2], (SiMe3)2Se/THF | D326 |
| [({Cp(CO)3Mo}Sn)4Te6] (617) | [{Cp(CO)3Mo}SnCl3], (SiMe3)2Te/THF, −78 to −18 °C, 19 days | D327 |
| [({Cp(CO)Fe}2Sn)4S6] (618) | [{Cp(CO)2Fe}SnCl3], (Bu3Sn)2S/toluene, 12 h | D328 |
| [(FcSn)4S6] (619) | FcSnCl3, Na2S/THF, 0 °C, 31 h | D329 |
| [(FcSn)4Se6] (620) | FcSnCl3, K2Se/THF, 48 h | D330 |
| [{(PhSn)3SnS6}{(MCp)3S4}] (621–622, M = Mo, W) | [(PhSn)4S6] (587), [M(CO)3CpCl], (Me3Si)2S/THF, 15 h | R331 |
| [Au(dppe)2][{Me(H2NN)CCH2CMe2Sn}4S6Cl] (623) | 1. [{Me(O)CCH2CMe2Sn}3S4]Cl, AuCl, dppe, (Me3Si)2S,/CH2Cl2, 17 h | R332 |
| 2. PhNHNH2/CH2Cl2, 45 min | ||
| [(μ4-O)Pb4(OSiPh3)6] (624) | Ph3SiOH, [Pbcp2]/Et2O, 35 °C, 30, min | D333,334 |
| [(tBuSi)4O6] (625) | t BuSiCl3, H2O/Et2O, 24 h | I335 |
| [(iPrSi)4O6] (626) | iPrSiCl3, H2O/Et2O, −80 °C to RT, 2 days | I335 |
| [{(Me3Si)3CSn}4O6] (627) | [(Me3Si)3CSnBr3], Na2O/NH3, THF, −78 °C, 6 h | D317 |
| [({Cp*(CO)2Ru}2Ge)4O6] (628) | 1. [Cp*RuCO(GeCl2)]2, K/THF, 48 h | I336 |
| 2. O2 | ||
| [{(CO)5WGe}4O2(OH)4] (629) | 1. 2-Methoxybenzyl alcohol, Ge[N(SiMe3)2]2/Et2O, 30 min | I337 |
| 2. [W(CO)5(thf)]/THF, 12 h | ||
| 3. H2O in pentane | ||
| [(Sn(DMEGqu)Br)4O4(OH)2]Br2 (630) | SnBr4, 3,5-ditert-butyl-o-benzoquinone, DMEGqu/THF, H2O | I338 |
a
Thex = 1,1,2-trimethylpropyl, Np = naphthyl, Sty = para-styryl, Cy = cyclohexyl, Cp = cyclopentadienyl, Dipp = 2,6-diisopropylphenyl, DMEGqu = N-(1,3-dimethylimidazolidin2-ylidene)quinoline-8-amine.