Tetrazido-Nitrido-Molybdat(VI); Darstellung, IR-Spektrum und Kristallstruktur von AsPh4[MoN(N3)4] / Tetrazido-nitrido-molybdate(VI); Preparation, IR Spectrum and Crystal Structure of AsPh4[MoN(N3)4]

1980 ◽  
Vol 35 (9) ◽  
pp. 1070-1074 ◽  
Author(s):  
Kurt Dehnicke ◽  
Josef Schmitte ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectrum ◽  
Sodium Sulfate ◽  
Triple Bond ◽  
Steric Effects ◽  
X Ray Diffraction ◽  
Silver Azide ◽  
Triclinic Space Group ◽  
X Ray ◽  
Covalently Bonded

The complex AsPh4[MoN(N3)4] is prepared by the reaction of AsPh4[MoNCl4] with silver azide in dichloromethane suspension in the presence of dry sodium sulfate. The IR spectrum indicates an Mo≡N group and four covalently bonded N3 groups for the [MoN(N3)4]⊖ anion. AsPh4[MoN(N3)4] crystallizes in the triclinic space group P1̄ with two formula units in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0,038; 4049 independent reflexions). The structure consists of AsPh4⊕ cations and [MoN(N3)4]⊖ anions. The short MoN bond length of the nitrido ligand (163 pm) corresponds to an Mo ≡ N triple bond. The steric effects of the lone pairs of the α-N atoms of the azido groups with tho MoN ligand cause a propellerlike twisted conformation of the four azido groups.

Darstellung, Kristallstruktur und Infrarotspektrum von [MoNCl3 · POCl3]4/Preparation, Crystal Structure and Infrared Spectrum of [MoNCl3 · POCl3]4

1978 ◽  
Vol 33 (11) ◽  
pp. 1347-1351 ◽  
Author(s):  
Joachim Strähle ◽  
Ulrich Weiher ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Infrared Spectrum ◽  
Ir Spectrum ◽  
Triple Bond ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral

Abstract [MoNCl3 · POCl3]4 is prepared both by the reaction of MoNCl3 with POCl3 as well as by the reaction of MoCl5 with NCl3 in the presence of POCl3. [MoNCl3 · POCl3]4 crystallizes in the monoclinic space group P21/c with 2 tetrameric molecules in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0.033, 1821 observed reflections). The structure consists of planar and almost square Mo4N4-eight-membered rings with alternating Mo-N bond lengths. The distorted octahedral environment of the molybdenum atoms is completed by three terminal Cl-ligands and by the oxygen atom of a POCl3 molecule, which is coordinated trans to the Mo ≡ N triple bond. The IR spectrum is discussed with respect to the vibrational spectra of the isoelectronic niobium complex [NbOCl3 · POCl3]4.

AsPh4[W(O)Cl3(HN3S2)]; Synthese, IR-Spektrum und Kristallstruktur / AsPh4[W(O)Cl3(HN3S2)]; Synthesis, IR Spectrum and Crystal Structure

1986 ◽  
Vol 41 (1) ◽  
pp. 48-52 ◽  
Author(s):  
Elke Conradi ◽  
Heribert Wadle ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectrum ◽  
Crystal Packing ◽  
Partial Hydrolysis ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Distorted Octahedral ◽  
Oxo Ligand ◽  
Hydrolysis Of

Violet crystals of AsPh4[W(O)Cl3(HN3S2)] were obtained by partial hydrolysis of AsPh4[WCl4(N3S2)] in a saturated solution in CH2Cl2/CCl4. Its IR spectrum is reported. The crystal structure was determined by X-ray diffraction (2284 independent observed reflexions, R = 0.041). Crystal data: triclinic, space group P1̄, Z = 2, a = 812.2, b = 1268.4, c = 1343.9 pm, α = 88.58, β = 82.04 and γ = 88.26°. The compound consists of AsPh4⊕ cations and [W(O)Cl3(HN3S2)⊖ anions in which the tungsten atoms have a distorted octahedral coordination with one oxo-ligand (171 pm), three chlorine atoms and two nitrogen atoms of the planar (HN3S7)2⊖ ligand. The WN bond lengths are 183 and 226 pm; the longer WN bond is due to the hydrogen atom attached to its N atom and to the trans influence of the oxo group. The crystal packing corresponds to one of the types frequently found among tetraphenylphosphonium compounds with cations stacked to parallel columns.

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

Crystal Structure and Vibrational Behaviour of Aqua Di(saccharinato)di(nicotinamide)copper(II)

2002 ◽  
Vol 57 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Beatriz S. Parajón-Costaa ◽  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Eduardo E Castellano
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of [Cu(sac)2(nic)2(H2O)] (sac = saccharinate anion; nic = nicotinamide) has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c with Z = 4 and the Cu(II) ion presents a CuN4O square pyramidal coordination. Some comparisons with related structures are made and the most important features of its IR spectrum were also discussed.

scholarly journals Fogoite-(Y), Na3Ca2Y2Ti(Si2O7)2OF3, a Group I TS-block mineral from the Lagoa do Fogo, the Fogo volcano, São Miguel Island, the Azores: Description and crystal structure

2017 ◽  
Vol 81 (2) ◽  
pp. 369-381 ◽  
Author(s):  
F. Cámara ◽  
E. Sokolova ◽  
Y. A. Abdu ◽  
F. C. Hawthorne ◽  
T. Charrier ◽  
...  
Keyword(s):  
Crystal Structure ◽  
New Mineral ◽  
X Ray Diffraction ◽  
Titanium Silicate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Group I ◽  
Mohs Hardness ◽  
Fogo Volcano ◽  
The Ideal

AbstractFogoite-(Y), Na3Ca2Y2Ti(Si2O7)2OF3, is a new mineral from the Lagoa do Fogo, São Miguel Island, the Azores. It occurs in cavities as highly elongated (on [001]) prisms, up to 2000 μm long and 50 μm× 50 μm in cross-section, associated with sanidine, astrophyllite, fluornatropyrochlore, ferrokentbrooksite, quartz and ferro-katophorite. Crystals are generally transparent and colourless, with vitreous lustre, occasionally creamy white. Fogoite-(Y) has a white streak, splintery fracture and very good {100} cleavage. Mohs hardness is ∼5. Dcalc. = 3.523 g/cm3. It is biaxial (+) with refractive indices (λ = 590 nm) α = 1.686(2), β = 1.690(2), γ = 1.702(5); 2Vmeas. = 57(1)° and 2Vcalc. = 60°. It is nonpleochroic. Fogoite-(Y) is triclinic, space group P1, a = 9.575(6), b = 5.685(4), c = 7.279(5) Å, α = 89.985(6), β = 100.933(4), γ = 101.300(5)°, V = 381.2 (7) Å3. The six strongest reflections in the powder X-ray diffraction data [d (Å), I, (hkl)] are: 2.954, 100, (1̄1̄2, 3̄10); 3.069, 42, (300, 01̄2); 2.486, 24, (310, 21̄2); 3.960, 23, (1̄1̄1, 2̄10); 2.626, 21, (2̄20); 1.820, 20, (1̄04). Electron microprobe analysis gave the following empirical formula calculated on 18 (O + F) (Na2.74Mn0.15)∑2.89Ca2[Y1.21(La0.01Ce0.03Nd0.03Sm0.02Gd0.08Dy0.08Er0.05Yb0.04Lu0.01)∑0.35Mn0.16Zr0.11Na0.09Fe0.072+Ca0.01]∑2(Ti0.76Nb0.23Ta0.01)∑1(Si4.03O14)O1.12F2.88, Z = 1. The crystal structure was refined on a twinnedcrystal to R1 = 2.81% on the basis of 2157 unique reflections (Fo > 4σFo) and is a framework of TS (Titanium Silicate) blocks, which consist of HOH sheets (H – heteropolyhedral, O – octahedral) parallel to (100). In the O sheet, the the [6]MO(1) site is occupied mainly by Ti, <MO(1)–ϕ> = 1.980 Å, and the [6]MO(2) and [6]MO(3) sites are occupied by Na and Na plus minor Mn, <MO(2)–ϕ>= 2.490 Å and <MO(3)–ϕ> = 2.378 Å. In the H sheet, the two [4]Si sites are occupied by Si, with <Si–O> = 1.623 Å; the [6]MH site is occupied by Y and rare-earth elements (Y > REE), with minor Mn, Zr, Na, Fe2+ and Ca, <MH–ϕ> = 2.271 Å and the [6]AP site is occupied by Ca, <AP–ϕ> = 2.416 Å. The MH and AP octahedra and Si2O7 groups constitute the H sheet. The ideal compositions of the O and two H sheets are Na3Ti(OF)F2 and Y2Ca2(Si2O7)2 apfu. Fogoite-(Y) is isostructural with götzenite and hainite. The mineral is named after the type locality, the Fogo volcano in the Azores.

Structural and IR-spectroscopic characterization of magnesium acesulfamate

2016 ◽  
Vol 71 (1) ◽  
pp. 51-55 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Elemental Analysis ◽  
Spectroscopic Characterization ◽  
Magnesium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic

AbstractMagnesium acesulfamate, Mg(C4H4NO4S)2·6H2O, was prepared by the reaction of acesulfamic acid and magnesium carbonate in aqueous solution, and characterized by elemental analysis. Its crystal structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the triclinic space group P1̅ with one molecule per unit cell. The FTIR spectrum of the compound was also recorded and is briefly discussed. Some comparisons with other simple acesulfamate and saccharinate salts are also made.

Bildung von Arsensäure aus [As2Cl8]2Ionen und Ozon. Die Kristallstruktur von PPh4Cl · H3AsO4 / Formation of Arsenic Acid from [As2Cl8]2- Ions and Ozone. Crystal Structure of PPh4Cl · H3AsO4

1992 ◽  
Vol 47 (12) ◽  
pp. 1677-1680 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred-Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
X Ray Diffraction ◽  
Arsenic Acid ◽  
Subsequent Reaction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Reaction of ozone with (PPh4)2[As2Cl8] in CH2C12 at low temperatures yields a red compound, possibly an ozonide. Upon evaporation of the solvent at –78 °C the ozone is released again. At -40 °C or above a subsequent reaction yields PPh4[AsCl6], PPh4Cl · H3AsO4, and other products. The crystal structure of PPh4Cl · H3AsO3 was determined by X-ray diffraction (4253 observed reflexions, R = 0.031). It is triclinic, space group P1̅, and consists of H3AsO4 molecules joined to dimer units via H bridges and associated via O–H · · · Cl- bridges to strands. The packing of the PPh4+ ions is discussed. Products of the reaction of (PPh4)2[Sb2Cl8] with ozone in CH2C12 are PPh4[SbCl6] and (PPh4)2[SbOCl4]2 · 2 CH2Cl2.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der 10B-und 11B-Isotopomeren von [B2(NCS)6]2- sowie Kristallstruktur von (Ph3P=N=PPh3)2[B2(NCS)6] / Preparation, Vibrational Spectra and Normal Coordinate Analysis of the 10B and 11B Isotopomers of [B2(NCS)6]2- and Crystal Structure of (Ph3P=N=PPh3)2[B2(NCS)6]

1996 ◽  
Vol 51 (4) ◽  
pp. 551-556 ◽  
Author(s):  
W. Preetz ◽  
B. Steuer
Keyword(s):  
Crystal Structure ◽  
Normal Coordinate Analysis ◽  
Force Constants ◽  
Potential Energy Distribution ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Fractionated Crystallization ◽  
Good Agreement

Abstract By reaction of [B6H6]2- with a solution of (SCN)2 in dichloromethane in the presence of solid KOH the hexaisothiocyanatodiborate anion [B2(NCS)6]2- is formed and can be isolated by fractionated crystallization. The crystal structure of (PNP)2[B2(NCS)6] has been determined by single crystal X-ray diffraction analysis; triclinic space group P1̄ with a=12,282(5), b=12,416(5), c=14,155(5)Å, a=68,36(5), β=70,59(5), γ=80,93(5)°.The [B2(NCS)6]2- anion reveals a staggered conformation with nearly local D3d symmetry and a B-B bond length of 1,73(2) Å. Using the crystallographic data a normal coordinate analysis has been performed. With a set of 12 force constants (e.g. fd(BB)=3,62, fd(BN)=4,21 mdyn/Å) a good agreement between observed and calculated frequencies for the 10B and 11B isotopomers has been achieved. The potential energy distribution on the force constants reveals strong vibrational couplings within the B2N6 framework.

Sign in / Sign up

Export Citation Format

Share Document