고체 및 용액 상 반응을 통한 새로운 크롬 클러스터 황화물의 합성
Preparations of New Chromium Sulfides through Solid and Solution State Synthetic Routes
- 주제(키워드) 재료화학
- 발행기관 아주대학교
- 지도교수 윤호섭
- 발행년도 2017
- 학위수여년월 2017. 2
- 학위명 석사
- 학과 및 전공 일반대학원 에너지시스템학과
- 실제URI http://www.dcollection.net/handler/ajou/000000024939
- 본문언어 영어
- 저작권 아주대학교 논문은 저작권에 의해 보호받습니다.
초록/요약
A quaternary thiophosphate, Cs2CrPS6 has been synthesized with alkali metal halide flux and the structure of the compound has been determined by single crystal X-ray diffraction methods. A black block-shaped crystal of Cs2CrPS6 is crystallized in the space group P21/n of the monoclinic system and the unit cell parameters of the compound are a = 9.0707(3), b = 9.0139(4), c = 14.5484(5) Å, β = 102.6418(4)˚ and V = 1160.68(8) Å3. The compound includes the anionic binuclear [Cr2(PS4)2S4]4- clusters which are isolated from each other by Cs+ cations. The clusters are composed of two edge-sharing Cr-centered octahedra and pair of P-centered tetrahedra. The cluster anions, [Cr2(PS4)2S4]4- are stabilized through the electrostatic interactions with the cations, Cs+. In order to isolate the anionic species, Cs2CrPS6 has been dissolved in the polar solvents such as DMF at elevated temperatures. Counter cations such as PPh4+ have been added to the DMF-Cs2CrPS6 solution in order to stabilize the inorganic cluster anions. After recrystallization, dark blue needle-shaped crystals have been obtained at room temperature. The structure of the crystals have been determined by X-ray diffraction technique and it showed that these compounds are Cr(C3H6NS2)3 and Cr(C3H6NS2)3(DMF). In both crystals, Cr atoms are octahedrally coordinated by three dimethyldithiocarbamate anions, [C3H6NS2]-. Cr(C3H6NS2)3 is crystallized in the space group Pbca of the orthorhombic system and the unit cell parameters of the compound are a = 10.1874(7), b = 17.5629(14), c = 20.4466(18) Å and V = 3658.3(5) Å3. The crystal is made up of the neutral molecule, Cr(C3H6NS2)3. And only van der Waals interactions exist among them. Cr(C3H6NS2)3(DMF) is crystallized in the space group PĪ of the triclinic system and the unit cell parameters of the compound are a = 9.5271(10), b = 9.6622(10), c = 13.1238(12) Å, α = 103.2879(10), β = 93.9714(10), γ = 94.5344(29)˚ and V = 1160.68(8) Å3. In this compound, Cr(C3H6NS2)3 clusters are separated by neutral DMF molecules.
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CONTENTS
ABSTRACT
INTRODUCTION ------------------------------------------------------------------------- 1
CHAPTER Ι. Solid state synthesis of 0-dimentional thiophosphate, Cs2CrPS6 ---------------------------------------------------------------------------------------3
1. Experiment ------------------------------------------------------------------------- 4
Synthesis
X-ray Crystallography
Solublization
2. Result and discussion ---------------------------------------------------------7
3. Figures --------------------------------------------------------------------------------------8
4. Tables --------------------------------------------------------------------------9
CHAPTER ΙΙ. Solubilization and crystallization of Cs2CrPS6 in DMF solution ------------------------------------------------------------18
1. Experiment ---------------------------------------------------------------- 19
Solubilization and recrystallization
X-ray Crystallography
2. Result and discussion ------------------------------------------------------ 22
3. Figures ---------------------------------------------------------------------- 24
4. Tables ------------------------------------------------------------------------ 26
