Palominos Franco, Muñoz Carolina, Oyarzun Poldie, Saldías Marianela, Vega Andrés
Universidad Andrés Bello, Departamento de Ciencias Químicas, Facultad de Ciencias Exactas, Quillota 980, Viña del Mar, Chile.
Laboratorio de Análisis de Sólidos, Facultad de Ciencias Exactas, Salvador Sanfuentes 2357, Santiago, Chile.
Acta Crystallogr E Crystallogr Commun. 2019 Jun 21;75(Pt 7):1005-1010. doi: 10.1107/S2056989019008089. eCollection 2019 Jul 1.
The coordination of the ligands with respect to the central atom in the complex bromido-tricarbon-yl[diphen-yl(pyridin-2-yl)phosphane-κ ,]rhenium(I) chloro-form disolvate, [ReBr(CHNP)(CO)]·2CHCl or [κ-,-{(CH)(CHN)P}Re(CO)Br]·2CHCl, (·2CHCl), is best described as a distorted octa-hedron with three carbonyls in a facial conformation, a bromide atom, and a biting ,-di-phenyl-pyridyl-phosphine ligand. Hirshfeld surface analysis shows that C-Cl⋯H inter-actions contribute 26%, the distance of these inter-actions are between 2.895 and 3.213 Å. The reaction between and piperidine (CHN) at 313 K in di-chloro-methane leads to the partial decoord-ination of the pyridyl-phosphine ligand, whose pyridyl group is replaced by a piperidine mol-ecule, and the complex bromido-tricarbon-yldiphen-yl(pyridin-2-yl)phosphane-κrhenium(I), [ReBr(CHN)(CHNP)(CO)] or [-{(CH)(CHN)P}(CHN)Re(CO)Br] (). The mol-ecule has an intra-molecular N-H⋯N hydrogen bond between the non-coordinated pyridyl nitro-gen atom and the amine hydrogen atom from piperidine with ⋯ = 2.992 (9) Å. Thermogravimetry shows that ·2CHCl losses 28% of its mass in a narrow range between 318 and 333 K, which is completely consistent with two solvating chloro-form mol-ecules very weakly bonded to . The remaining is stable at least to 573 K. In contrast, seems to lose solvent and piperidine (12% of mass) between 427 and 463 K, while the additional 33% loss from this last temperature to 573 K corresponds to the release of 2-pyridyl-phosphine. The contribution to the scattering from highly disordered solvent mol-ecules in was removed with the SQUEEZE routine [Spek (2015 ▸). Acta Cryst. C71, 9-18] in . The stated crystal data for , μ . do not take this solvent into account.
在配合物溴代 - 三羰基[二苯基（吡啶 - 2 - 基）膦 - κ，]铼（I）氯仿溶剂化物[ReBr(CHNP)(CO)]·2CHCl 或 [κ -,-{(CH)(CHN)P}Re(CO)Br]·2CHCl（·2CHCl）中，配体相对于中心原子的配位情况最好描述为一个扭曲的八面体，其中三个羰基呈面式构象，一个溴原子，以及一个螯合的， - 二苯基 - 吡啶基 - 膦配体。 Hirshfeld表面分析表明，C - Cl⋯H相互作用占26%，这些相互作用的距离在2.895至3.213 Å之间。 在313 K下，于二氯甲烷中，与哌啶（CHN）的反应导致吡啶基 - 膦配体的部分去配位，其吡啶基团被一个哌啶分子取代，生成配合物溴代 - 三羰基[二苯基（吡啶 - 2 - 基）膦 - κ](哌啶 - κ)铼（I），[ReBr(CHN)(CHNP)(CO)] 或 [-{(CH)(CHN)P}(CHN)Re(CO)Br]（）。 该分子在未配位的吡啶氮原子与哌啶的胺氢原子之间存在分子内N - H⋯N氢键，⋯ = 2.992 (9) Å。 热重分析表明，·2CHCl在318至333 K的狭窄温度范围内损失其质量的28%，这与两个与 非常弱结合的溶剂化氯仿分子完全一致。 剩余的 在至少573 K时是稳定的。 相比之下， 在427至463 K之间似乎失去了溶剂和哌啶（质量的12%），而从最后这个温度到573 K额外损失的33%对应于2 - 吡啶基 - 膦的释放。 在 中，使用SQUEEZE程序[Spek (2015 ▸). Acta Cryst. C71, 9 - 18]去除了 中高度无序的溶剂分子对散射的贡献。 所给出的 的晶体数据，μ. 未考虑这种溶剂。
