Synthese von Wolframkomplexen des Typs [LW(CO)3X]+ (X = H, F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [LW(CO)3Br]BF4 und [LW(CO)3H]2[WOCl5]·H2O / Synthesis of Tungsten Complexes of the Type [LW(CO)3X]+ (X=H, F, Br; L=1,4,7-triazacyclononane). The Crystal Structures of [LW(CO)3Br]
Synthese von Wolframkomplexen des Typs [LW(CO)3X]+ (X = H, F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [LW(CO)3Br]BF4 und [LW(CO)3H]2[WOCl5]·H2O / Synthesis of Tungsten Complexes of the Type [LW(CO)3X]+ (X=H, F, Br; L=1,4,7-triazacyclononane). The Crystal Structures of [LW(CO)3Br]
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合成 Wolframkomplexen des Typs [LW(CO)3X]+ (X = H, F, Br; L = 1,4,7-三氮杂环壬烷) 3H]2[WOCl5]·H2O / 类型钨配合物的合成 [ LW(CO)3X]+（X=H、F、Br；L=1,4,7-三氮杂环壬烷）[LW(CO)3Br]的晶体结构。
DOI：
10.1515/znb-1987-1105
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发表时间：
1987
期刊：
影响因子：
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通讯作者：
H. Haupt
中科院分区：
文献类型：
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作者：
P. Schreiber;K. Wieghardt;U. Flörke;H. Haupt
LW（CO）_3（L = 1，4，7-三氮杂环壬烷）与Br_2在CHCl_3中反应生成橙子[LW（CO）_3 Br]（Br_3），将其转化为BF_4盐。[LW（CO）_3Br] BF_4晶体属三斜晶系，空间群为P_1Br（a = 8.273（3），B = 8.628（2），c = 13.034（3）°，α = 80.10（2），β = 72.69（2），γ = 61.14（2）°，Z = 2），由具有七配位W原子的阳离子[LW（CO）3Br]+和BF 4-阴离子组成。LW（CO）_3与20%HF水溶液在空气存在下和加入NaPF_6得到相应的盐[LW（CO）_3F]（PF_6）。在37%盐酸水溶液中进行类似反应，得到绿色晶体[LW（CO）3 H]2[WOCl 5]·H2O，属单斜晶系P21/c（a = 12.234（4），B = 18.853（7），c = 14.609（5）nm，β = 105.65（3）°，Z = 4）。[LW（CO）_3H]~+阳离子中的W原子为七配位，而六配位的[WOCl_5]_2 ~-阴离子中的W原子没有无序。W = O键距较短（1.72（1）），平均赤道W-Cl键距为2.390，而W = O基团的反式W-Cl键距为2.562（5）。
The reaction of LW(CO)3 (L = 1,4,7-triazacyclononane) with Br2 in CHCl3 yields orange [LW(CO)3Br](Br3) which was converted to its BF4- salt. [LW(CO)3Br]BF4 crystallizes in the triclinic space group P1̅ (a = 8.273(3), b = 8.628(2), c = 13.034(3) Å , α = 80.10(2), β = 72.69(2), γ = 61.14(2)°, Z = 2); it consists of cations [LW(CO)3Br]+ , with seven-coordinate W atoms, and BF4- anions. The corresponding salt [LW(CO)3F](PF6) was obtained from LW(CO)3 with 20% aqueous HF in the presence of air and addition of NaPF6. The analogous reaction with 37% aqueous HCl affords green crystals of [LW(CO)3H]2[WOCl5]·H2O which crystallize in the monoclinic space group P21/c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Å, β = 105.65(3)°, Z = 4). The W atoms in the [LW(CO)3H]+ cations are seven-coordinate; the six-coordinate [WOCl5]2- anions are not disordered. The W = O distance is short (1.72(1) Å ), the mean equatorial W-Cl distance is 2.390 Å whereas the W-Cl bond distance trans to the W = O group is 2.562(5) Å.