scholarly journals Synthesis and X-ray Crystal Structures of Novel Spiro 1,3-benzoxazine Dimers

2002 ◽  
Vol 2002 (10) ◽  
pp. 473-474 ◽  
Author(s):  
H.Z. Alkhathlan ◽  
M.A. Al-Saad ◽  
H.M. Al-Hazimi ◽  
K.A. Al-Farhan ◽  
A.A. Mousa
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Mass Spectra ◽  
X Ray ◽  
New Compounds

Novel spiro 1,3-benzoxazine dimers are obtained when hydrazones of 2-hydroxyacetophenone are treated with triphosgene. An X-ray crystal structure, and the NMR and mass spectra of these new compounds, are reported and discussed.

Reactivity of 4-Nitrosoanilines Towards Dimeric Halogenido-bridged Complexes of Iridium(III) and Rhodium(III) of the Type [(η5- C5Me5)MX2]2

2012 ◽  
Vol 67 (6) ◽  
pp. 532-542
Author(s):  
Stefan Wirth ◽  
Ingo-Peter Lorenz
Keyword(s):  
Crystal Structures ◽  
Mass Spectra ◽  
Spectroscopic Characterization ◽  
Melting Points ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Vis Spectroscopy ◽  
New Compounds ◽  
Octahedral Configuration

The synthesis, spectroscopic characterization and crystal structures of new C-nitrosoaryl complexes of iridium(III) and rhodium(III) are reported. The reactions of the μ2-halogenido-bridged dimers [(η5-C5Me5)IrX2]2 [X = Cl (1a), Br (1b), I (1c)] and [(η5-C5Me5)RhCl2]2 (2a) with N,N-dimethyl- (3) and N,N-diethyl-4-nitrosoaniline (4) yield the mononuclear complexes [(η5- C5Me5)MX2(3)] [M = Ir, X = Cl (5a), Br (5b), I (5c);M= Rh, X = Cl (7a)] and [(η5-C5Me5)MX2(4)] [M = Ir, X = Cl (6a), Br (6b), I (6c); M = Rh, X = Cl (8a)]. All new compounds were characterized by their melting points, NMR, IR and mass spectra as well as in selected cases by UV/Vis spectroscopy. The X-ray structure analyses revealed a slightly distorted pseudo-octahedral configuration (“three-legged pianostool”) and σ-N coordination of the C-nitroso ligand.

scholarly journals Monofluorophosphates—New Examples and a Survey of the PO3F2− Anion

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 45-73
Author(s):  
Matthias Weil
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Inorganic Compounds ◽  
X Ray Diffraction ◽  
X Ray ◽  
Type D ◽  
Index 2 ◽  
New Compounds ◽  
Relationship Of ◽  
Tetrahedral Anion

During a systematic study of monofluorophosphates, i.e., compounds comprising the tetrahedral anion PO3F2−, twelve, for the most part new, compounds were obtained from aqueous solutions. Crystal structure refinements based on single crystal X-ray diffraction data revealed the previously unknown crystal structures of CdPO3F(H2O)2, Cr2(PO3F)3(H2O)18.8, Pb2(PO3F)Cl2(H2O), (NH4)2M(PO3F)2(H2O)2 (M = Mg, Mn, Co), NH4Cr(PO3F)2(H2O)6, NH4Cu2(H3O2)(PO3F)2, (NH4)2Zn(PO3F)2(H2O)0.2, and (NH4)2Zn3(PO3F)4(H2O), as well as redeterminations of ZnPO3F(H2O)2.5 and (NH4)2Ni(PO3F)2(H2O)6. From the previously unknown crystal structures, CdPO3F(H2O)2 (space group P-1), Cr2(PO3F)3(H2O)18.8 (P-1), Pb2(PO3F)Cl2(H2O) (Pnma), NH4Cr(PO3F)2(H2O)6 (R-3m), (NH4)2Zn(PO3F)2(H2O)0.2 (C2/c), and (NH4)2Zn3(PO3F)4(H2O) (I-43d) each crystallizes in an unique crystal structure, whereas compounds (NH4)2M(PO3F)2(H2O)2 (M = Mg, Co) crystallize in the (NH4)2Cu(PO3F)2(H2O)2 type of structure (C2/m) and (NH4)2Mn(PO3F)2(H2O)2 in a subgroup thereof (P21/n, with a klassengleiche relationship of index 2), and NH4Cu2(H3O2)(PO3F)2 (C2/m) crystallizes isotypically with natrochalcite-type KCu2(H3O2)(SO4)2. A survey on the PO3F2− anion, including database entries of all inorganic compounds comprising this group, revealed mean bond lengths of P–O = 1.506(13) Å, P–F = 1.578(20) Å, and angles of O–P–O = 113.7(1.7)° and O–P–F = 104.8(1.7)°, using a dataset of 88 independent PO3F2− anions or entities. For those crystal structures of monofluorophosphates where hydrogen bonding is present, in the vast majority of cases, hydrogen bonds of the type D–H···F–P (D = O, N) are not developed.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate / Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates

1982 ◽  
Vol 37 (11) ◽  
pp. 1393-1401 ◽  
Author(s):  
Beatrix Milewski-Mahrla ◽  
Hubert Schmidbaur
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Molar Ratio ◽  
Ionic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Donor Acceptor ◽  
New Compounds

Reactions of pentamethylantimony (CH3)5Sb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramothylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed.The crystal structures of the hydrogen-dibenzoato (1), hydrogen-ortho-plithalato (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter­actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH3)4Sb-tetrahedron in 1 is distorted by two benzoate oxygon atoms (at 304(2) and 340(2) pin). The cation in 2 is largely undistorted and the anion has a hydrogenphthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate.

scholarly journals Crystal structures of two novel iron isocyanides from the reaction of 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate(−1)

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
William W. Brennessel ◽  
John E. Ellis
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Tridentate Ligand ◽  
Reductive Cyclization ◽  
X Ray Diffraction ◽  
X Ray

The reaction of the [K(18-crown-6)(thf)2]1+ (thf is tetrahydrofuran) salt of bis(anthracene)ferrate(−1), or [Fe(C14H10)2]−, with 2,6-dimethylphenyl isocyanide (CNXyl) in thf resulted in the formation of two new iron isocyanide complexes, namely, [(1,2,3,4-η)-anthracene]tris(2,6-dimethylphenyl isocyanide)iron, [Fe(C14H10)(C9H9N)3] or [Fe(1,2,3,4-η-C14H10)(CNXyl)3], and {5,6-bis(2,6-dimethylanilino)-3-(2,6-dimethylphenyl)-1,2,7-tris[(2,6-dimethylphenyl)imino]-3-azoniahept-3-ene-1,4,7-triido}tris(2,6-dimethylphenyl isocyanide)iron tetrahydrofuran disolvate, [Fe(C54H56N6)(C9H9N)3]·2C4H8O or [Fe(C54H56N6)(CNXyl)3]·2C4H8O, which were characterized by single-crystal X-ray diffraction. The former is likely an intermediate along the path to the known homoleptic [Fe(CNXyl)5], while the latter contains a tridentate ligand that is formed from the `coupling' of six CNXyl ligands. A third crystal structure from this reaction, (7-methylindol-1-ido-κN)(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6 O)potassium, [K(C9H8N)(C12H24O6)] or [K(C9H8N)(18-crown-6)], contains a 7-methylindol-1-ide anion, in which one CNXyl ligand has shed a proton during its reductive cyclization.

scholarly journals E. S. Fedorov Promoting the Russian-German Scientific Interrelationship

Minerals ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 181 ◽  
Author(s):  
Peter Paufler ◽  
Stanislav K. Filatov
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structure Analysis ◽  
Crystalline State ◽  
Crystal Structure Analysis ◽  
Present Knowledge ◽  
Personal Contact ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Impact

At the dawn of crystal structure analysis, the close personal contact between researchers in Russia and Germany, well documented in the “Zeitschrift für Krystallographie und Mineralogie”, contributed significantly to the evolution of our present knowledge of the crystalline state. The impact of the Russian crystallographer E. S. Fedorov upon German scientists such as A. Schoenflies and P. Groth and the effect of these contacts for Fedorov are highlighted hundred years after the death of the latter. A creative exchange of ideas paved the way for the analysis of crystal structures with the aid of X-ray diffraction.

scholarly journals New Compounds RE(Zn,Al)8 and Yb4Zn20.3Al12.7 and their Crystal Structures

2006 ◽  
Vol 61 (7) ◽  
pp. 779-784 ◽  
Author(s):  
Ol’ga Stel’makhovych ◽  
Yurij Kuz’ma
Keyword(s):  
Intermetallic Compound ◽  
Crystal Structures ◽  
Structure Type ◽  
Type Structure ◽  
Space Group ◽  
X Ray ◽  
Structure Space ◽  
New Compounds ◽  
First Time ◽  
The Relationship

The crystal structures of several new compounds have been determined using X-ray analysis. The intermetallic compound HoZn5Al3 (a = 8.586(3), c = 16.538(5) Å , RF = 0.0413, RW = 0.0521) has its own structure type (space group I4/mmm), which has been found for the first time. The following compounds are isostructural with the previous one: YZn5.52Al2.48 (a = 8.6183(1), c = 16.5048(3) Å , RI = 0.078, RP = 0.116), DyZn4.96Al3.04 (a = 8.5887(1), c = 16.5002(3) Å , RI = 0.077, RP = 0.114), ErZn5.37Al2.63 (a = 8.5525(2), c =16.3997(5) Å , RI = 0.081, RP = 0.111), TmZn5.64Al2.36 (a = 8.70429(8), c = 16.3943(4) Å , RI = 0.088, RP = 0.095), LuZn5.58Al2.42 (a = 8.5616(1), c= 16.3052(3) Å , RI =0.081, RP =0.101). The intermetallic compound Yb4Zn20.3Al12.7 (a = 8.6183(1), c = 16.5048(3) Å , RI = 0.085, RP = 0.112) adopts the Yb8Cu17Al49 - type structure (space group I4/mmm). The relationship between the HoZn5Al3-type and the Yb8Cu17Al49-type structures is discussed.

scholarly journals The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

1996 ◽  
Vol 74 (9) ◽  
pp. 1671-1681 ◽  
Author(s):  
Jack Passmore ◽  
Paul D. Boyle ◽  
Gabriele Schatte ◽  
Todd Way ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Ft Raman Spectroscopy ◽  
New Phase ◽  
Ft Raman

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

Crystal structure of Nd3Au4 and Nd17Au36

1994 ◽  
Vol 209 (8) ◽  
Author(s):  
M. L. Fornasini ◽  
A. Saccone
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray ◽  
Two Phases

AbstractThe crystal structures of two phases in the neodymium-gold system were determined by single crystal X-ray diffractometer methods,

Organoamido- and Aryloxo-lanthanoids. XII. The Coordination Chemistry of Bis(2-phenylindol-1-yl)ytterbium(II), and the X-Ray Crystal Structures of Yb(pin)2(diglyme)(thf) and [Yb(pin)2(dme)]2 (pin = 2-Phenylindol-1-yl, diglyme = Bis(2-methoxyethyl) Ether, thf Equals Tetrahydrofuran, dme = 1,2-Dimethoxyethane)

1995 ◽  
Vol 48 (12) ◽  
pp. 1933 ◽  
Author(s):  
CT Abrahams ◽  
GB Deacon ◽  
CM Forsyth ◽  
WC Patalinghug ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
Coordination Polyhedron ◽  
Basal Plane ◽  
Monoclinic Space Group ◽  
Coordinate Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrogen Donor

With the facile displacement being utilized of thf from Yb(pin)2(thf)4 (pin = 2-phenylindol-1-yl, thf = tetrahydrofuran) in toluene solution, the complexes Yb(pin)2(dme)2 (dme = 1,2- dimethoxyethane), Yb(pin)2 (tmen)(tmen = N,N,N′,N′-tetramethylethane-1,2-diamine) and Yb(pin)2(diglyme)(thf) (diglyme = bis(2-methoxyethyl) ether) have been prepared from the respective ligands and Yb(pin)2(thf)4. Yb(pin)2 (diglyme) (thf) [monoclinic, space group P 21 /c, a 15.35(1), b 16.179(5), c 14.45(2) Ǻ, β 107.51(8)°, Z 4, R 0.044 for 2956 (I > 3σ(I)) 'observed' reflections] has a monomeric six-coordinate structure with transoid nitrogen donor atoms, N-Yb-N 143.6(4)° and an irregular coordination polyhedron described as either a distorted trigonal prism or a monocapped square pyramid. Attempted crystallization of Yb(pin)2 (thf) by partial desolvation of Yb(pin)2(thf)4 in hot toluene, containing a trace of dme, gave a mixture of red Yb(pin)2(thf) and orange [Yb(pin)2(dme)]2. The latter was independently synthesized by partial desolvation of Yb(pin)2(dme)2 in toluene. An X-ray crystal structure showed [Yb(pin)2(dme)]2 [monoclinic, space group P 21/c, a 11 .614(2), b 15.945(7), c 15.327(4) Ǻ, β 110.19(2)°, Z 2 dimers, R 0.070 for 2314 (I ≥ 3σ(I)) 'observed' reflections] to be a dimer with two bridging pin ligands, coordinated through nitrogen only. There is an approximately square pyramidal five-coordinate ytterbium environment with an apical dme oxygen, and with two bridging nitrogens, a terminal nitrogen, and a dme oxygen in the basal plane.

Sign in / Sign up

Export Citation Format

Share Document