An X-ray crystallographic, Raman, and infrared spectral study of crystalline potassium uranyl carbonate, K4UO2(CO3)3

1980 ◽  
Vol 58 (16) ◽  
pp. 1651-1658 ◽  
Author(s):  
Anthony Anderson ◽  
Chung Chieh ◽  
Donald E. Irish ◽  
James P. K. Tong
Keyword(s):  
Infrared Spectra ◽  
Equatorial Plane ◽  
Spectral Study ◽  
The Other ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Uranyl Carbonate ◽  
Infrared Spectral

X-ray diffraction studies have revealed that K4UO2(CO3)3 is isostructural with (NH4)4UO2(CO3)3; the crystal is monoclinic with a = 10.247(3), b = 9.202(2), c = 12.226(3) Å, β = 95.11(2)°, Z = 4, and space group C2/c. Three carbonate anions are arranged in bidentate fashion in the equatorial plane of UO22+; one of these occupies a C2 site and the other two occupy C1 sites. All carbonates are significantly distorted from D3h symmetry. The binding of carbonates to uranyl is strong and thus the lattice can be considered to be composed of [UO2(CO3)3]4− anions and K+ cations. The Raman and infrared spectra exhibit fewer lines than predicted for such a crystal. Tentative assignments are suggested for the more prominent bands of the constituent polyatomic species.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Bildung eines Kupfer-Nitratokomplexes aus einem Azidokomplex und Ozon. Die Kristallstruktur von (PPh4)2[CuCl(NO3)3] · CH2Cl2/ Formation of a Copper Nitrato Complex from an Azido Complex. Crystal Structure of (PPh4)2[CuCl(NO3)3] · CH2Cl2

1992 ◽  
Vol 47 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred D. Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
The Other ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Complex Crystal Structure ◽  
Monodentate Ligands ◽  
Complex Crystal

(PPh4)2[CuCl(NO3)3] · CH2Cl2 is formed when ozone reacts with (PPh4)2[Cu2(N3)6] in dichloromethane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1113(1), b = 1156(1), c = 1965(2) pm , α = 101.02(1), β = 93.74(1), γ = 104.05(2)° at 130 K, space group P1̄, Z = 2, R = 0.057 for 3951 observed reflexions. The structure contains CH2Cl2 molecules and PPh4+ and [CuCl(NO3)3]2- ions, with copper having coordination number 5. One nitrate ligand acts as a bidentate chelating unit, and the other two as monodentate ligands.

Preparation, infrared spectra, and crystal structure of two modifications of the (thymidinato-N3)methylmercury(II) complex

1985 ◽  
Vol 63 (12) ◽  
pp. 3456-3463 ◽  
Author(s):  
France Guay ◽  
André L. Beauchamp
Keyword(s):  
Infrared Spectra ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Hydroxyl Groups ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Preparation Conditions

Reaction of CH3HgOH with thymidine (HT) yielded the neutral CH3HgT complex crystallizing as a hydrated or an anhydrous material, depending on preparation conditions. Both forms were examined by X-ray diffraction. The anhydrous variety is monoclinic, space group P21, a = 4.798(6), b = 14.270(8), c = 10.390(4) Å, β = 102.74(9)°, and Z = 2 molecules per cell. The structure was refined on 1552 nonzero MoKα reflections to a conventional R factor of 0.034. The hydrated form belongs to the orthorhombic space group P212121, a = 10.484(3), b = 14.633(3), c = 18.538(5), Z = 8. The structure was refined on 1816 nonzero MoKα reflections to R = 0.036. In both forms, the CH3Hg+ ion is linearly bonded to the deprotonated N(3) site of thymidine. The water molecules and hydroxyl groups in the ribose unit participate in a hydrogen bonding network, in which the carbonyl groups are involved as acceptors. The infrared spectra of the two forms differ significantly only by the absorptions due to the water molecules. By comparing with the spectrum of thymidine, diagnostic regions for complexation with deprotonated thymidine have been proposed

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

The structure and conformation of cis-2-phenylcyclobutanecarboxylic acid and cis-3-(p-fluorophenyl)cyclobutanecarboxylic acid

1983 ◽  
Vol 61 (7) ◽  
pp. 1422-1427 ◽  
Author(s):  
George M. Reisner ◽  
James D. Korp ◽  
Ivan Bernal ◽  
Richard Fuchs
Keyword(s):  
Unit Cell ◽  
The Other ◽  
Dihedral Angles ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cyclobutanecarboxylic Acid ◽  
Cyclobutane Ring

The structure of cis-2-phenylcyclobutanecarboxylic acid (1) and cis-3-(p-fluorophenyl)cyclobutanecarboxylic acid (2) have been determined by X-ray diffraction methods. Crystals of 1 are monoclinic, space group C2/c with a = 15.420(8), b = 11.687(6), c = 11.226(5) Å, β = 112.45(4)°, and eight molecules in the unit cell. Crystals of 2 are monoclinic, space group P21/n, a = 8.038(5), b = 5.405(4), c = 22.69(1) Å, and β = 97.30(4)°, with four molecules in the unit cell. In both compounds the cyclobutane ring is puckered, with dihedral angles of 27° and 31°. The bond joining the substituted ring atoms in 1 is significantly longer (1.581(2) Å) than the other three (average 1.535(2) Å), due to crowding of substituents. In 2 both the carboxyl and phenyl substituents are close to the bisecting geometry, whereas in 1 both substituents deviate from this conformation, the carboxyl more than the phenyl.

Complexes of 1,2,4-Triazoles, Part XVII The Crystal Structure of Tris-μ-(4-ethyl-1,2,4-triazole-N1,N2)- (4-ethyl-1,2,4-triazole-N1)-aquo-bis [bis(thiocyanato-N)- nickel(II)]hydrate, Ni2(C4N3H7)4(H2O)(NCS)4 ·H2O(x ≃ 2.5)

1981 ◽  
Vol 36 (7) ◽  
pp. 809-813 ◽  
Author(s):  
Ger Vos ◽  
Anthonie J. de Kok ◽  
Gerrit C. Verschoor
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
The Other ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Coordinated Water

Abstract The crystal structure of Ni2(C4N3H7)4(H2O)(NCS)4 · 2.5 H2O has been determined by X-ray diffraction techniques. The compound crystallizes in the monoclinic space group P21/n with a = 15.121(4), b= 13.237(2), c= 18.069(3), β = 94.71(2)° and Z = 4; R = 0.040 (Rm = 0.051). The compound consists of dimeric units in which two Ni ions are bridged by three ethyltriazole (Ettrz) groups. For one Ni, two N donating NCS- groups and an Ettrz coordinating by only one N atom complete the NiNe octahedron. The other Ni atom, which is also octahedrally coordinated, has a coordinated water molecule instead of a monodentate Ettrz.

N,O- and S,O-bonded Hg(II) complexes with S-substituted amino acids: synthesis and crystal structures of bis(S-methyl-L-cysteinato)mercury(II) and bis(D,L-ethioninato)-mercury(II) diperchlorate

1981 ◽  
Vol 59 (1) ◽  
pp. 144-150 ◽  
Author(s):  
Langford Book ◽  
Arthur J. Carty ◽  
Chung Chieh
Keyword(s):  
Amino Acids ◽  
Equatorial Plane ◽  
Low Ph ◽  
Monoclinic Space Group ◽  
Amino Group ◽  
Distorted Tetrahedron ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Complexes Hg[CH3SCH2CH(NH2)COO]2 and Hg[CH3CH2SCH2CH2CH(NH3COO]2(ClO4)2 obtained from reactions of yellow HgO with S-methyl-L-cysteine and ethionine respectively have been characterized by X-ray diffraction methods. The former is monoclinic, space group P21, with a = 13.790(4), b = 4.994(1), c = 9.898(2) Å, and β = 106.20(2)°. The R and Rw factors were 0.063 and 0.075 respectively for 980 independent reflections. The S-methyl-L-cysteine complex is N,O bonded with two Hg—N bond lengths of 2.16(3) and 2.13(3) Å and [Formula: see text]. There are eight [Formula: see text] distances within the range of 2.54–3.75 Å. The three shortest of these are distributed in an equatorial plane with respect to the N—Hg—N moiety. The Hg—O bond length of 2.54(2) Å is associated with the chelate ligand.The ethionine complex is triclinic, space group [Formula: see text] with a = 11.376(7), b = 12.009(8), c = 9.495(6) Å, α = 94.74(6), β = 108.01(5), and γ = 71.78(5)°. The R and Rw values for all 3526 reflections were 0.083 and 0.10 respectively but R became 0.058 for only observed reflections (I > 3 σ(I)). The Hg2+ is bonded to two sulfur, Hg—S = 2.436(5) and 2.537(4) Å, and two oxygen, Hg—O = 2.28(1) and 2.259(9) Å, atoms in a distorted tetrahedron. The Hg2+–carboxylate interactions are stronger in the S-bonded than the N-bonded complex probably indicating a preference for Hg–amine coordination. At low pH when the amino group is protonated, Hg–thioether coordination becomes important for S-substituted amino acids.

Structure of mono-acid even-numbered β-triacylglycerols

1999 ◽  
Vol 55 (1) ◽  
pp. 114-122 ◽  
Author(s):  
Arjen van Langevelde ◽  
Kees van Malssen ◽  
Frank Hollander ◽  
René Peschar ◽  
Henk Schenk
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Chain Length ◽  
Tuning Fork ◽  
The Other ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Overlap Model

The crystal structure of the β polymorph of tripalmitin (1,2,3-trihexadecanoylglycerol, β-PPP) has been determined by single-crystal X-ray diffraction. The molecules crystallize in space group P1¯ in an asymmetric tuning-fork conformation. This structure and the already-known crystal structures of β-tricaprin (β-CCC) and β-trilaurin (β-LLL) could be matched in an overlap model. Apart from a difference in chain length, the three structures are almost identical. The overlap model can be used to predict the crystal structure of the other members of the C n C n C n -type (n = even) TAG series reasonably accurately. This is demonstrated by predicting the crystal structure for β-trimyristin (β-MMM) and successively comparing the experimental and calculated X-ray powder diagrams.

Interaction of the methylmercury cation with glycine and alanine: a vibrational and X-ray diffraction study

1986 ◽  
Vol 64 (9) ◽  
pp. 1876-1884 ◽  
Author(s):  
Marie-Claude Corbeil ◽  
André L. Beauchamp ◽  
Serge Alex ◽  
Rodrigue Savoie
Keyword(s):  
Aqueous Solutions ◽  
Diffraction Study ◽  
Raman Spectra ◽  
Infrared Spectra ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Carboxylate Oxygen

The complexes (CH3Hg)Gly, (CH3Hg)(L-Ala), and (CH3Hg)(DL-Ala) were prepared by reacting CH3HgOH with glycine (HGly) and alanine (HAla). Crystals of (CH3Hg)(DL-Ala) are monoclinic, space group P21/c, a = 9.460(2), b = 8.794(2), c = 8.723(2) Å, β = 97.49(2)°, Z = 4. The structure was refined on 935 MoKα reflections to R = 0.042. The complex results from displacement of an alanine NH3+ proton by the CH3Hg+ ion, which is linearly bonded to the —NH2 group. An intramolecular Hg … O contact of 2.63 Å is also formed with a carboxylate oxygen. The Raman and infrared spectra of solid (CH3Hg)Gly and (CH3Hg)(L-Ala) are compared with those of the ligands. Raman spectra of aqueous solutions at different pH indicate that the NH2-bonded structure is retained in solution, although no complexation via the carboxylate occurs.

Complexes of 15-crown-5 and cyclohexano-15-crown-5 with lithium, sodium, and potassium phenoxide having macrocycle: salt ratios of 1:1 and 1:2. The crystal structures of two polymorphs of 15-crown-5•2LiOPh

1988 ◽  
Vol 66 (10) ◽  
pp. 2515-2523 ◽  
Author(s):  
Michael P. Murchie ◽  
John W. Bovenkamp ◽  
André Rodrigue ◽  
Kimberley A. Watson ◽  
Suzanne Fortier
Keyword(s):  
Crystal Structures ◽  
Direct Methods ◽  
The Other ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Diffraction Structure ◽  
Structure Determinations ◽  
Sodium And Potassium

The syntheses, in ethereal solvents, of the complexes of 15-crown-5 and cyclohexano-15-crown-5 with lithium, sodium, and potassium phenoxide are described. The two macrocycles form complexes with lithium and sodium phenoxide with host:guest ratios of 1:2. Potassium phenoxide, however, was complexed by the two macrocycles to give products with macrocycle:salt ratios of 1:1. Crystals of 15-crown-5•2LiOPh were obtained for X-ray diffraction structure determinations. In fact, the crystal structures of two co-crystallizing polymorphs of this complex (1a and 1b) have been determined. Polymorph 1a crystallizes in space group [Formula: see text] with a = 11.386(4), b = 11.901(4), c = 10.654(4) Å, α = 106.53(3), β = 112.60(3), γ = 106.52(3)°, and Z = 2. Polymorph 1b crystallizes in space group P21/n with a = 15.355(4), b = 11.642(2), c = 13.595(6) Å, β = 104.56(3)°, and Z = 4. Both structures were solved by direct methods, and refined by full-matrix least-squares calculations to residuals, R, of 0.053 and 0.055 for polymorphs 1a and 1b, respectively. The structures of the two polymorphs differ only in the orientation of the phenoxides. The structures show a dimer, (15-crown-5•2LiOPh)2, which consists of an aggregate of four lithium phenoxide molecules complexed by two 15-crown-5 macrocycles. The two lithiums of each monomeric unit of this dimer have different crystallographic and chemical environments. One lithium is coordinated to all five oxygens of the macrocycle and to one of the phenoxide oxygens while the other lithium is coordinated to only one oxygen of the macrocycle and to three phenoxide oxygens.

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