The Crystal Structures of Chlorodimethyl( dimethylamino)silane and Dimethyl-bis-(dimethylamino)silane

2003 ◽  
Vol 58 (7) ◽  
pp. 708-710 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Krunoslav Vojinović
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Low Temperatures ◽  
Structural Parameters ◽  
X Ray Diffraction ◽  
X Ray

Single crystals of chlorodimethyl(dimethylamino)silane, Me2NSiMe2Cl, and dimethyl-bis-(dimethylamino)silane, (Me2N)2SiMe2, have been grown in situ from the melt at low temperatures and their structures determined by X-ray diffraction. Important structural parameters (Å / °): Me2NSiMe2Cl (C2/m) Si-N 1.686(2), Si-C 1.851(1), Si- Cl 2.109(1), N-Si-Cl 111.7(1), C-Si-Cl 105.1(1), C-N-C 112.8(2), Si-N-C 123.4(1); (Me2N)2SiMe2 (P21/c) Si-N(1) 1.725(1), Si-C(1) 1.868(1), N(1)-Si-N(2) 105.7(1), C(3)- N(1)-C(4) 111.6(1), Si-N(1)-C(3) 122.4(1), Si-N(1)-C(4) 120.0(1).

Synthesis and Structures of Simple (Silylmethyl)(methyl)ethers

2003 ◽  
Vol 58 (8) ◽  
pp. 759-763 ◽  
Author(s):  
Norbert W. Mitzel
Keyword(s):  
Crystal Structures ◽  
Structural Parameters ◽  
Structural Basis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Donor Acceptor

The compound Cl3SiCH2OCH3 was prepared by reacting ClCH2OCH3 with the Cl3SiH/NEt3 reagent. H3SiCH2OCH3 and F3SiCH2OCH3 were synthesized from Cl3SiCH2OCH3 by reduction with LiAlH4 and by fluorination with SbF3, respectively. The crystal structures of the low-melting compounds H3SiCH2OCH3 and F3SiCH2OCH3 were determined by X-ray diffraction of in situ grown crystals. Both compounds do not show any observable β -donor-acceptor interactions, but behave structurally like usual dialkylethers or silanes, as is obvious from the structural parameters in H3SiCH2OCH3 (<SiCO 108.4(3)-109.4(3)°, <COC 111.0(4)-111.6(4)°) and in F3SiCH2OCH3 (<SiCO 107.1(1), <COC 111.2(2)°). Earlier postulates of Si· · ·O interactions in compounds with SiCO units could thus not be confirmed on a structural basis.

In situ characterization of strain-induced crystallization of natural rubber by synchrotron radiation wide-angle X-ray diffraction: construction of a crystal network at low temperatures

Soft Matter ◽  
2019 ◽  
Vol 15 (4) ◽  
pp. 734-743 ◽  
Author(s):  
Pinzhang Chen ◽  
Jingyun Zhao ◽  
Yuanfei Lin ◽  
Jiarui Chang ◽  
Lingpu Meng ◽  
...  
Keyword(s):  
Low Temperatures ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
X Ray ◽  
Crystal Network ◽  
Strain Induced Crystallization ◽  
Induced Crystallization

The structural evolution of NR during stretching at −40 °C and in the strain–temperature space.

scholarly journals The Stability of Icosahedral Cd-Yb

2003 ◽  
Vol 805 ◽  
Author(s):  
Günter Krauss ◽  
Sofia Deloudi ◽  
Andrea Steiner ◽  
Walter Steurer ◽  
Amy R. Ross ◽  
...  
Keyword(s):  
Low Temperature ◽  
Ambient Temperature ◽  
Mechanical Stress ◽  
Single Crystals ◽  
High Temperatures ◽  
Low Temperatures ◽  
Ambient Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Stability

ABSTRACTThe stability of single-crystalline icosahedral Cd-Yb was investigated using X-ray diffraction methods in the temperature range 20 K ≤ T ≤ 900 K at ambient pressure and from ambient temperature to 873 K at about 9 GPa. Single-crystals remain stable at low temperatures and in the investigated HP-HT-regime. At high temperatures and ambient pressure, the quasicrystal decomposes. The application of mechanical stress at low temperatures yields to the same decomposition, the formation of Cd. A reaction of icosahedral Cd-Yb with traces of oxygen or water causing the decomposition seems reasonable, but a low-temperature instability of this binary quasi-crystal cannot be ruled out totally.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.

The Crystal Structures at 10 K of the Trigonal Salts KMIII(NH3)6(ClO4)2Cl2, MIII = Os and Cr, and the Possibility of Phase Transitions

1999 ◽  
Vol 52 (3) ◽  
pp. 219 ◽  
Author(s):  
Philip A. Reynolds ◽  
Brian N. Figgis ◽  
Alexander N. Sobolev
Keyword(s):  
Differential Scanning Calorimetry ◽  
Transition Temperature ◽  
Crystal Structures ◽  
Low Temperatures ◽  
Simple Structure ◽  
Alkali Metal Cations ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Threefold Axis ◽  
X Ray

The crystal structures of KOs(NH3)3(ClO4)2Cl2 and KCr(NH3)6(ClO4)2Cl2 were determined at 10 K by X-ray diffraction, and for the osmium salt also at 293 K. At 293 K the osmium salt is trigonal, space group R 3m, with the same simple structure as others of this class of double salt. At 10 K, in agreement with previous radius ratio predictions, both crystals are best described as remaining R 3m. All previously studied members, with larger alkali metal cations, are twinned R 3 at low temperatures, with small, symmetry-breaking rotations of the hexaamminemetal(III) and perchlorate ions about the threefold axis. Differential scanning calorimetry on CsRu(NH3)6(ClO4)2Cl2 suggests that the R 3m to R 3 change is very extended in temperature with only a small discontinuity at the transition temperature.

Recrystallization of AA1050 Studied by 3DXRD

2006 ◽  
Vol 519-521 ◽  
pp. 1569-1578
Author(s):  
Dorte Juul Jensen
Keyword(s):  
Single Crystals ◽  
High Energy ◽  
Nucleation And Growth ◽  
X Rays ◽  
X Ray Diffraction ◽  
Orientation Relationships ◽  
X Ray ◽  
3 Dimensional ◽  
Kinetics Of

By 3 dimensional X-ray diffraction (3DXRD) using high energy X-rays from synchrotron sources it is possible to study in-situ the nucleation and growth during recrystallization. In this paper it is described and discussed how 3DXRD can supplement EBSP measurements of nucleation and growth. Three types of studies are considered: i) orientation relationships between nuclei and parent deformed matrix, ii) recrystallization kinetics of individual bulk grains and iii) filming of growing grains in deformed single crystals.

Orthoborate Halides with the Formula (M+II)5(BO3)3X: Syntheses, Crystal Structures and Raman Spectra of Eu5(BO3)3Cl and Ba5(BO3)3X (X = Cl, Br)

2011 ◽  
Vol 66 (4) ◽  
pp. 359-365 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Raman Spectra ◽  
Direct Synthesis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Incremental Volume

Single crystals of Eu5(BO3)3Cl were obtained by serendipity by reacting Eu2O3 and Mg with B2O3 at 1300 K in the presence of an NaCl melt for 13 h in silica-jacketed Nb ampoules. Ba5(BO3)3X (X = Cl, Br) crystals were formed by direct synthesis from appropriate amounts of Ba(OH)2, H3BO3 and the respective barium halide (hydrate) in alumina crucibles kept in the open atmosphere at 1300 K for 13 h. The crystal structures of the title compounds were determined with single-crystal X-ray diffraction. All compounds crystallize isotypically to Sr5(BO3)3Cl in the orthorhombic space group C2221 (no. 20, Z = 4) with the lattice parameters a = 1000.34(7), b = 1419.00(9), c = 739.48(5) pm for Eu5(BO3)3Cl, a = 1045.49(5), b = 1487.89(8), c = 787.01(4) pm for Ba5(BO3)3Cl, and a = 1048.76(7), b = 1481.13(9) and c = 801.22(5) pm for Ba5(BO3)3Br. The Raman spectra of all compounds were acquired and are presented and compared to literature data. The incremental volume of the orthoborate (BO3)3− anion has been determined and is compared to the Biltz volume

Direct observation of monoclinic ferroelectric phase and domain switching process in (K0.25Na0.75)NbO3 single crystals

CrystEngComm ◽  
2015 ◽  
Vol 17 (14) ◽  
pp. 2872-2877 ◽  
Author(s):  
Hao Deng ◽  
Haiwu Zhang ◽  
Xiangyong Zhao ◽  
Chao Chen ◽  
Xi'an Wang ◽  
...  
Keyword(s):  
Light Microscopy ◽  
Single Crystals ◽  
Direct Observation ◽  
Ferroelectric Phase ◽  
Domain Switching ◽  
Polarized Light ◽  
Switching Process ◽  
X Ray Diffraction ◽  
X Ray

The domain-switching process of monoclinic K0.25Na0.75NbO3 single crystals were studied by in situ polarized light microscopy and X-ray diffraction.

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