Halfsandwich complexes containing the tetrathiotungstate chelate ligand. Crystal and molecular structure of Cp*Rh(PMe3)[(mu-S)(2) WS2] (Cp* = eta(5-) pentamethylcyclopentadienyl)

Herberhold M; Jin GX; Rheingold AL

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Halfsandwich complexes containing the tetrathiotungstate chelate ligand. Crystal and molecular structure of CpRh(PMe3)[(mu-S)(2) WS2] (Cp = eta(5-) pentamethylcyclopentadienyl)

机译：含有四硫钨酸盐螯合物的半三明治复合物。 Cp * Rh（PMe3）[（mu-S）（2）WS2]（Cp * = eta（5-）五甲基环戊二烯基）的晶体和分子结构

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The reactions of Cp*M(PMe3)Cl-2 (M = Rh (1a), Ir (1b)) with (NEt4)(2)[WS4] led to the heterodimetallic -sulfido-bridged complexes Cp*M(PMe3)[(mu-S)(2)WS2] (M Rh (2a), Ir (2b)), whereas the dimers [Cp*MCl(mu-Cl)](2) (M = Rh (4a), Ir (4b)) reacted with (NEt4)(2)[WS4) to give the known trinuclear compounds [Cp*M(Cl)](2)(mu-WS4) (M = Rh (5a), Ir (5b)). Hydrolysis of the terminal W=S bonds converts 2a,b into Cp*M(PMe3)[(mu-S)(2)WO2] (M = Rh (3a), Ir (3b)). Salts of a heterodimetallic anion, A[CpMo(1)(NO)(WS4)] (6) (A(+) = NEt4+, NPh4+) were obtained by reactions of [CpMo(NO)I-2](2) with tetrathiotungstates, A(2)[WS4]. The complexes were characterized by IR and NMR (H-1, C-13, P-31) spectroscopy, and the X-ray crystallographic structure of Cp*Rh(PMe3)[(mu-S)(2)WS2] (2a) has been determined. The bond lengths and angles in the coordinations spheres of Rh and W in 2a (Rh...W 288.5(1) pm) are compared with related complexes containing terminal [WS42-] chelate ligands.

机译：Cp * M（PMe3）Cl-2（M = Rh（1a），Ir（1b））与（NEt4）（2）[WS4]的反应生成杂双金属-硫桥键联的络合物Cp * M（PMe3） [（mu-S）（2）WS2]（M Rh（2a），Ir（2b）），而二聚体[Cp * MCl（mu-Cl）]（2）（M = Rh（4a），Ir（ 4b））与（NEt4）（2）[WS4）反应，得到已知的三核化合物[Cp * M（Cl）]（2）（mu-WS4）（M = Rh（5a），Ir（5b））。末端W = S键的水解将2a，b转换为Cp * M（PMe3）[（mu-S）（2）WO2]（M = Rh（3a），Ir（3b））。杂二金属阴离子A [CpMo（1）（NO）（WS4）]（6）（A（+）= NEt4 +，NPh4 +）的盐是通过[CpMo（NO）I-2]（2）与四硫钨酸盐，A（2）[WS4]。配合物的特征在于IR和NMR（H-1，C-13，P-31）光谱，以及Cp * Rh（PMe3）[（mu-S）（2）WS2]（2a）的X射线晶体结构）已确定。将Rh和W在2a（Rh ... W 288.5（1）pm）的配位域中的键长和键角与含有末端[WS42-]螯合物的相关配合物进行了比较。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2005年第1期|共6页
作者
Herberhold M; Jin GX; Rheingold AL;
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正文语种 eng
中图分类化学;
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tetrathiotungstate ligands; sulfido bridges; rhodium; iridium; molybdenum; crystal structure; M = MO; IRIDIUM COMPLEXES; TRANSITION-METALS; S COMPLEXES; CHEMISTRY; DINUCLEAR; DERIVATIVES; SULFUR; THIOTUNGSTATES; MOLYBDENUM;

机译：四硫钨酸盐配体;硫桥键;铑;铱;钼;晶体结构;M = MO;铱络合物;过渡金属;S络合物;化学性质;粒径;衍生物;硫;硫代钨酸盐;钼;

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1. Halfsandwich complexes containing the tetrathiotungstate chelate ligand. Crystal and molecular structure of Cp*Rh(PMe3)[(mu-S)(2) WS2] (Cp* = eta(5-) pentamethylcyclopentadienyl) [J] . Herberhold M, Jin GX, Rheingold AL Zeitschrift fur Anorganische und Allgemeine Chemie . 2005,第1期

机译：含有四硫钨酸盐螯合物的半三明治复合物。 Cp * Rh（PMe3）[（mu-S）（2）WS2]（Cp * = eta（5-）五甲基环戊二烯基）的晶体和分子结构
2. Synthesis and reactivity of rhodium(III) pentamethylcyclopentadienyl complexes of N - B - PTA(BH3): X-ray crystal structures of [Cp*RhCl2{N - B - PTA(BH3)}] and [Cp*Rh{N-B-PTA(BH3)}(eta(2)- CH2 = CHPh)] [J] . Bolano S, Albinati A, Bravo J, Journal of Organometallic Chemistry . 2008,第14期

机译：N-B-PTA（BH3）的铑（III）五甲基环戊二烯基铑配合物的合成和反应性：[Cp * RhCl2 {N-B-PTA（BH3）}]和[Cp * Rh {NB-PTA （BH3）}（eta（2）-CH2 = CHPh）]
3. New monocyclopentadienyl complexes of group 4 and 5 metals with chelating nitrogen ligands. Crystal and molecular structures of [Zr(eta(3)-C3H5)(eta(4)-Ph2N2C2Me2-2,3)Cp ''] and [TaCl2{,eta(4)-C6H4C(NSiMe3-1,2)(2)}Cp ''] [Cp '' = C5H3(SiMe3)(2)-1,3] [J] . Pindado GJ., Bochmann M., Thornton-Pett M. Journal of the Chemical Society, Dalton Transactions. Inorganic Chemistry . 1998,第3期

机译：具有螯合氮配体的4和5族金属的新单环戊二烯基配合物。 [Zr（eta（3）-C3H5）（eta（4）-Ph2N2C2Me2-2,3）Cp''和[TaCl2 {，eta（4）-C6H4C（NSiMe3-1,2）（ 2）} Cp''] [Cp” = C5H3（SiMe3）（2）-1,3]
4. Dehydrogenation of dimethylamine-borane catalyzed by halfsandwich Ir and Rh complexes: Mechanism and the role of Cp* non-innocence [C] . Shrinwantu Pal, Shuhei Kusumoto, Kyoko Nozaki 日本化学会春季年会講演予稿集 . 2018

机译：半肢体和rh复合物催化催化的二甲胺 - 硼烷的脱氢：CP *非innocence的机制和作用
5. The preparation, structures and spectroscopic properties of binuclear rhodium complexes and [platinum(phosphorus hydrogen oxygen)]/viologen systems: Time-resolved photocrystallography and the study of photoinduced intermolecular electron transfer. [D] . Gerlits, Oksana O. 2005

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6. Synthesis Structures and Reactivity of Single andDouble Cyclometalated Complexes Formed by Reactions of Cp*MCl22 (M = Ir and Rh) with Dinaphthyl Phosphines [O] . Shaowei Zhang, Xiaodan Chu, Tongyu Li, 2018

机译：单和二甲苯的合成结构和反应性Cp * MCl2 2（M = Ir和Rh）与二萘并膦反应形成的双环金属配合物
7. Synthesis and crystal structure of lanthanide sandwich complexes with mixed cyclooctatetraenyl and chelating ether side chain-cyclopentadienyl ligands : crystal structures of (η(5)-MeOCH(2)CH(2)Cp)Nd(η(8)-C(8)H(8))(THF) and (η(5)-C(4)H(7)OCH(2)C(5)H(4))La(η(8)-C(8)H(8))(THF) [O] . Liu Q, Shen X, Huang J, 2000

机译：具有混合的环辛酸酯基和螯合的醚侧链-环戊二烯基配体的镧系元素三明治配合物的合成和晶体结构：（η（5）-MeOCH（2）CH（2）Cp）Nd（η（8）-C（8）的晶体结构H（8））（THF）和（η（5）-C（4）H（7）OCH（2）C（5）H（4））La（η（8）-C（8）H（8 ））（四氢呋喃）
8. Synthesis and Characterization of Tungsten-Cobalt, -Rhodium and -Platinum Compounds and the X-Ray Crystal Structures of RhW(mu-CC6H4Me-4)(CO)2(PMe3)(eta5-C5H5)(eta5-C9H7) and PtW mu-C(C6H4Me-4)C(O) (CO)(PMe3)(eta4-C8H12)(eta5-C5H5 [R] . Jeffery, J. C., Sambale, C., Schmidt, M. F., 1982

机译：钨钴，铑和铂化合物的合成和表征以及RhW（μ-CC6H4me-4）（CO）2（pme3）（eta5-C5H5）（eta5-C9H7）和ptW的X射线晶体结构-C（C6H4me-4）C（O）（CO）（pme3）（eta4-C8H12）（eta5-C5H5）

Halfsandwich complexes containing the tetrathiotungstate chelate ligand. Crystal and molecular structure of Cp*Rh(PMe3)[(mu-S)(2) WS2] (Cp* = eta(5-) pentamethylcyclopentadienyl)

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Halfsandwich complexes containing the tetrathiotungstate chelate ligand. Crystal and molecular structure of CpRh(PMe3)[(mu-S)(2) WS2] (Cp = eta(5-) pentamethylcyclopentadienyl)