scholarly journals The crystal structure of diphenyalmine hydrochloride antimony trichloride co-crystallizate, C12H12Cl4NSb – Localization of hydrogen atoms

2021 ◽  
Vol 236 (2) ◽  
pp. 439-441
Author(s):  
Arthur Averdunk ◽  
Eric C. Hosten ◽  
Richard Betz
Keyword(s):  
Crystal Structure ◽  
Antimony Trichloride ◽  
Hydrogen Atoms

Abstract C12H12Cl4NSb, monoclinic, P21/n (no. 14), a = 5.6693(2) Å, b = 20.2385(7) Å, c = 14.3908(5) Å, β = 100.3830(10)°, V = 1624.14(10) Å3, Z = 4, R gt (F) = 0.0192, wR ref (F 2) = 0.0430, T = 200 K.

Crystal structure of pomalidomide Form I, C13H11N3O4

2021 ◽  
pp. 1-6
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Double Layers ◽  
Carbonyl Groups ◽  
Hydrogen Atoms ◽  
Powder Diffraction File ◽  
Functional Theory ◽  
Amine Hydrogen

The crystal structure of pomalidomide Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Pomalidomide Form I crystallizes in the space group P-1 (#2) with a = 7.04742(9), b = 7.89103(27), c = 11.3106(6) Å, α = 73.2499(13), β = 80.9198(9), γ = 88.5969(6)°, V = 594.618(8) Å3, and Z = 2. The crystal structure is characterized by the parallel stacking of planes parallel to the bc-plane. Hydrogen bonds link the molecules into double layers also parallel to the bc-plane. Each of the amine hydrogen atoms acts as a donor to a carbonyl group in an N–H⋯O hydrogen bond, but only two of the four carbonyl groups act as acceptors in such hydrogen bonds. Other carbonyl groups participate in C–H⋯O hydrogen bonds. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

scholarly journals Crystal structure analysis of LiN(DxH1-x)4SO4by neutron diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C1703-C1703
Author(s):  
Shin Ae Kim ◽  
Chang-Hee Lee
Keyword(s):  
Crystal Structure ◽  
Neutron Diffraction ◽  
Diffraction Method ◽  
Crystal Structure Analysis ◽  
Ferroelectric Materials ◽  
Lattice Parameters ◽  
Least Square ◽  
Intensity Data ◽  
Hydrogen Atoms ◽  
Neutron Intensity

The crystal structure of Li(ND4)SO4 was analysed by neutron diffraction method. The crystal is a partially deuterated Li(NH4)SO4 and one of the ferroelectric materials with hydrogen atoms. The crystal is orthorhombic at room temperature with lattice parameters of a=5.2773(5) Å, b=9.124(2) Å, c=8.772(1) Å and Z=4. Neutron intensity data were collected on the Four-Circle Diffractometer (FCD) at HANARO in Korea Atomic Energy Research Institute. The structure was refined by full-matrix least-square to final R value of 0.049 for 745 observed reflections by neutron diffraction. All atomic positions of four hydrogen atoms at NH4 and the occupation factors of D and H were refined. From these results we obtained the average chemical structure of this sample, LiND3.05H0.95SO4. Five years later, neutron intensity data were collected and analysed once more with same crystal. The crystal is orthorhombic but with different lattice parameters, or hexagonal. We will report and discuss these results in this presentation.

Crystal structure of atropine sulfate monohydrate, (C17H24NO3)2(SO4)·(H2O)

2019 ◽  
Vol 34 (4) ◽  
pp. 389-395 ◽  
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Water Molecule ◽  
Powder Diffraction ◽  
Density Functional ◽  
Atropine Sulfate ◽  
Strong Hydrogen Bond ◽  
Hydroxyl Groups ◽  
Hydrogen Atoms ◽  
Sulfate Anion

The crystal structure of atropine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atropine sulfate monohydrate crystallizes in space group P21/n (#14) with a = 19.2948(5), b = 6.9749(2), c = 26.9036(5) Å, β = 94.215(2)°, V = 3610.86(9) Å3, and Z = 4. Each of the two independent protonated nitrogen atoms participates in a strong hydrogen bond to the sulfate anion. Each of the two independent hydroxyl groups acts as a donor in a hydrogen bond to the sulfate anion, but only one of the water molecule hydrogen atoms acts as a hydrogen bond donor to the sulfate anion. The hydrogen bonds are all discrete but link the cations, anion, and water molecule along [101]. Although atropine and hyoscyamine (atropine is racemic hyoscyamine) crystal structures share some features, such as hydrogen bonding and phenyl–phenyl packing, the powder patterns show that the structures are very different. The powder pattern for atropine sulfate monohydrate has been submitted to ICDD for inclusion in the Powder Diffraction File™.

Die Kristallstruktur von N,N,N'-tris(trimethylsilyl)benzamidin sowie die Synthese und Kristallstruktur von DichIorantimon-N,N'-bis(trimethylsilyl)benzamidinat

1988 ◽  
Vol 43 (9) ◽  
pp. 1119-1124 ◽  
Author(s):  
Christina Ergezinger ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Steric Effect ◽  
Lone Pair ◽  
Antimony Atom ◽  
Antimony Trichloride ◽  
Chlorine Atoms ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Structure Determinations ◽  
Distorted Trigonal Bipyramidal

Abstract N,N,N'-Tris(trimethylsilyl)benzamidine, [C6H5-C(NSiMe3)N(SiMe3)2], reacts with antimony trichloride in CH2Cl2 solution to form monomeric dichloroantimony-N,N'-bis(trimethylsilyl)- benzamidine, [SbCl2(NSiMe3)2C-C6H5]. Both benzamidine derivatives have been character­ized by crystal structure determinations. [C6H5-C(NSiMe3)N(SiMe3)2]: space group P21/c, Z = 4, 2278 observed independent refle­xions, R = 0,038. Lattice dimensions (19 °C): a = 1521,0(1); b = 656.7(1); c = 2163,0(1) β = 94,21(1)°. The compound forms monomeric molecules with CN distances of 126,6 pm, and 141,0 pm, respectively, corresponding to C=N̄-SiMe3 and C-N(SiMe3)2 moieties. [SbCl2(NSiMe3)2C-C6H5]: space group P21/c, Z = 4, 2707 observed independent reflexions, R = 0,027. Lattice dimensions (19 °C): a = 1212,7(1); b = 962,1(1); c = 1728,9(1) pm; β = 98,02(1)°. The compound forms monomeric molecules in which the antimony atom is surrounded by two chlorine atoms, and by the N atoms of the benzamidine chelate, forming a distorted trigonal bipyramidal arrangement, which is a consequence of the steric effect of the lone pair on the Sb atom.

Studies Directed Towards the Total Synthesis of Anticapsin. X-Ray Crystal-Structure of (1RS,2SR,4RS,5RS,6SR)-5-Hydroxy-2-phthalimido-1-trimethylsilyloxy-bicyclo[2.2.2]octane-2,6-carbolactone

1990 ◽  
Vol 43 (11) ◽  
pp. 1827 ◽  
Author(s):  
MJ Crossley ◽  
TW Hambley ◽  
AW Stamford
Keyword(s):  
Crystal Structure ◽  
Amino Acid ◽  
Total Synthesis ◽  
Synthetic Approach ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
X Ray Crystallography ◽  
Relative Stereochemistry ◽  
Atomic Parameters

The relative stereochemistry of methyl 2-phthalimido-1- trimethylsilyloxybicyclo[2.2.2]oct-5-ene-2-carboxylate (9) and its 5,6-epoxide (10), intermediates in a synthetic approach to the amino acid antibiotic anticapsin, were established by the TiCl4-mediated cyclization of (10) to the carbolactone (12); the structure of which was proved by single-crystal X-ray crystallography. Full-matrix least- squares refinement of all atomic parameters with individual isotropic thermal parameters for the hydrogen atoms by using 1446 reflections converged at R 0.036. Crystals of (12) are monoclinic, P21/c, a 12.342(3), b 12.239(2), c 13.405(3) Ǻ, β 99.34(2)°, Z 4.

Die Kristallstruktur des 1:1-Komplexes von Antimontrichlorid und 2.2′-Bipyridin / The Crystal Structure of the 1:1 Complex of Antimony Trichloride and 2,2′-Bipyridine

1980 ◽  
Vol 35 (12) ◽  
pp. 1548-1551 ◽  
Author(s):  
Annegret Lipka ◽  
Hartmut Wunderlich
Keyword(s):  
Crystal Structure ◽  
Complex Compound ◽  
Antimony Trichloride ◽  
Unit Cell ◽  
Space Group ◽  
Distorted Octahedral

The crystal structure of the complex compound of SbCl3 with a chelating bipyridyl group was determined. Sb(C10H8N2)Cl3 crystallizes in the space group P21/c with a = 818.9(4), b = 695.8(7), c = 2331.3(12) pm, β = 103.59(4)° and Z = 4 molecules per unit cell. The SbCl3 fragment is T-shaped with <Sb-Cl> at 254.7 pm. Taking into account also the N atoms of the chelating 2,2′-bipyridyl group (<Sb-N> = 228.1 pm) and an intermolecular Sb···Cl contact at 334.0 pm the Sb coordination is distorted octahedral.

A refinement of the dickite structure and some remarks on polymorphism in kaolin minerals

1961 ◽  
Vol 32 (252) ◽  
pp. 683-704 ◽  
Author(s):  
Robert E. Newnham
Keyword(s):  
Crystal Structure ◽  
Absorption Spectra ◽  
Infrared Absorption ◽  
Structural Features ◽  
Mirror Image ◽  
Hydrogen Atoms ◽  
Octahedral Layer ◽  
Layer Structures ◽  
Infrared Absorption Spectra ◽  
Interlayer Bonding

SummaryThe crystal structure of the clay mineral dickite (Al2Si2H4O9) has been refined to a greater accuracy than that reported in an earlier analysis. Improved lattiçe parameters are: a 5·15±0·001, b 8·940±0·001, c 14·424 ± 0·002Å., β 96° 44′± 1′. The dickite structure shows several significant distortions from the geometry of the idealized kaolin layer, including deformation and rotation of the silica tetra-hedra. The most striking features of the octahedral layer are the extremely short shared edges of 2·37 Å. Although the analysis was not sufficiently accurate to position the hydrogen atoms with certainty, a model consistent with the infrared absorption spectra is proposed. The stacking sequences of kaolin-layer minerals have been considered with reference to the structural features observed in dickite. There are thirty-six ways of superposing two kaolin layers commensurate with the OH-O bonds found in kaolinite, dickite, and nacrite. The twelve sequences showing the least amount of cation-cation superposition between consecutive kaolin layers can be used to construct two one-layer cells, kaolinite and its mirror image, and twelve two-layer cells, including dickite and nacrite. The distortions of the kaolin layer introduce secondary variations in the interlayer bonding that suggest that dickite and nacrite are the most stable of the kaolin layer structures, since they possess the shortest oxygen-hydroxyl contacts.

scholarly journals Redetermination of the crystal structure of tetrakis(tricarbonyl-μ3-methane thiolato-rhenium(I) – Localization of hydrogen atoms, C16H12O12Re4S4

2015 ◽  
Vol 230 (2) ◽  
pp. 93-94
Author(s):  
Xandri Schoultz ◽  
Thomas I. A. Gerber ◽  
Eric C. Hosten ◽  
Richard Betz
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atoms

Abstract C16H12O12Re4S4, trigonal, P3121 (no. 152), a = 10.0250(4) Å, c = 25.809(1) Å, V = 2246.4 Å3, Z = 3, Rgt(F) = 0.0192, wRref(F2) = 0.0320, T = 200 K.

Alkalimetallformiate, V Die Kristallstruktur von Natriumformiat-Dihydrat, NaHCO2·2H2O [1] Alkali Metal Formates, V The Crystal Structure of Sodium Formate Dihydrate, NaHCO2·2H2O [1]

1994 ◽  
Vol 49 (9) ◽  
pp. 1179-1182 ◽  
Author(s):  
Kerstin Müller ◽  
Klaus-Jürgen Range ◽  
Anton M. Heyns
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Sodium Formate ◽  
Sodium Ions ◽  
Hydrogen Atoms ◽  
Orthorhombic Space Group ◽  
Bonding System ◽  
Water Oxygen ◽  
Metal Formates ◽  
Oxygen Atoms

Single crystals of sodium formate dihydrate, NaHCO2·2H2O, have been prepared from aqueous solutions of sodium formate, NaHCO2, via the trihydrate, NaHCO2-3H2O. They are orthorhombic, space group Cmca, with a = 7.070(4), b = 14.534(2), c = 8.706(2) Å and Z = 8. The structure, including the hydrogen atoms, was refined to R = 0.054, Rw = 0.065 for 479 unique reflections with I > 3 σ (I). It comprises buckled layers formed by NaO6 octahedra which are edge- and corner-sharing. The octahedral coordination of the sodium ions is achieved by two oxygen atoms from two different end-on bonded formate ions and four water oxygen atoms. The O···H distances show clearly that strong hydrogen bonds are not involved in the bonding system

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