Bromide hydrogen oxalate salts with the diprotonated 1,4-diazabicyclo[2.2.2]octane counterion

2020 ◽  
Vol 75 (9-10) ◽  
pp. 815-820
Author(s):  
Mamadou Ndiaye ◽  
Mouhamadou Birame Diop ◽  
Abdoulaye Samb ◽  
Libasse Diop ◽  
Allen G. Oliver ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Hydrogen Bonding Networks

AbstractTwo new salts composed of the diprotonated 1,4-diazabicyclo[2.2.2]octane (DABCO) molecule as the cations and bromide and hydrogen oxalate as the anions have been isolated and structurally characterized by X-ray diffraction analysis. The salt [DABCOH2]{[HC2O4][Br]} (1) crystallizes in the orthorhombic system, space group P212121 with a = 9.0809(7), b = 9.5156(7), c = 12.3558(9) Å, V = 1067.67(14) Å3 and Z = 4. The salt [DABCOH2]2{[HC2O4][Br]3}·H2O (2) crystallizes in the orthorhombic system, space group Pnma with a = 26.6554(17), b = 7.3711(4), c = 10.7421(7) Å, V = 2110.6(2) Å3 and Z = 4. The compounds were prepared from ethanolic solutions of [DABCOH2][HC2O4]2 (L1) and ZnBr2 in molar ratios of 2:1 and 1:1, respectively. The salts 1 and 2 exhibit extended hydrogen bonding networks leading to supramolecular topologies.

scholarly journals The New Complexes of Tris(2-Methoxy-5-Bromophenyl)Stibine with Silver Nitrate

2021 ◽  
Vol 13 (1) ◽  
pp. 21-30
Author(s):  
O.K. Sharutina ◽  
Keyword(s):  
Diffraction Analysis ◽  
Silver Nitrate ◽  
Silver Atom ◽  
Nitrate Solution ◽  
Silver Nitrate Solution ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystallographic Characteristics ◽  
Group A

By mixing solutions of tris(2-methoxy-5-bromophenyl)antimony and silver nitrate in a methanol : acetonitrile mixture (1:1 vol.), nitrato-O,O'-(acetonitrile)[tris(2-methoxy-5-bromophenyl)antimony]silver complex with the general formula [(C6H3ОMe-2-Br-5)3SbAg(μ2-NO3)(Ме3CN)]2•2[(C6H3ОMe-2-Br-5)3SbAgNO3(Ме3CN)] (1) has been obtained. An addition of silver nitrate solution in the methanol : acetonitrile mixture to the tris(2-methoxy-5-bromophenyl)antimony dioxane solution has led to the formation of a small amount of dark crystals of the ionic complex [(2-MeО-5-Br-C6H3)3SbAg(H2O)Sb(C6H3Br-5-OMe-2)3]+[(2-MeО-5-Br-C6H3)3SbAg(m-NO3)3 AgSb(C6H3Br-5-OMe-2)3]-×3C4H8O2 (2). Complexes 1 and 2 have been characterized by IR spectroscopy, and their structures have been determined by X-ray diffraction analysis. The IR spectra of complexes 1 and 2 contain the bands characterizing the Sb-O, Sb-C, С≡N-, and NO3-group band vibrations. X-ray diffraction analysis of the complexes has been carried out on an automatic four-circle D8 Quest Bruker diffractometer (МоКα radiation, λ = 0.71073 Å, graphite monochromator) at 293 K. Crystallographic characteristics of 1: triclinic, P-1 space group, a = 9.32(3), b = 17.50(7), c = 17.97(5) Å, a = 97.56(14), β = 92.90(19), g = 99.45(19) grad., V = 2859(16) Å3, Z = 2, rcalc = 2.069 g/cm3, 2: monoclinic, С2/с space group, a = 17.417(14), b = 21.041(15), c = 32.01(2) Å, a = 90, β = 97.79(3), g = 90 grad., V = 11624(15) Å3, Z = 4, rcalc = 2.006 g/cm3. In the monomeric and dimeric molecules of crystal 1, nitrate ligands are chelating and bridging, respectively. In the cation of complex 2, the silver atom is bonded to two antimony ligands, the third coordination site is occupied by a water molecule. In the dimeric anion there are one antimony ligand and three bridging nitrate groups surrounding each silver atom.

scholarly journals Recombinant expression, purification, crystallization and preliminary X-ray diffraction analysis ofHaemophilus influenzaeBamD and BamCD complex

2015 ◽  
Vol 71 (2) ◽  
pp. 234-238
Author(s):  
Jintang Lei ◽  
Xun Cai ◽  
Xiaodan Ma ◽  
Li Zhang ◽  
Yuwen Li ◽  
...  
Keyword(s):  
Diffraction Analysis ◽  
Recombinant Expression ◽  
Outer Membrane Proteins ◽  
Gel Filtration ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The Bam machinery, which is highly conserved from bacteria to humans, is well recognized as the apparatus responsible for the insertion and folding of most outer membrane proteins in Gram-negative bacteria. InEscherichia coli, the Bam machinery consists of five components (i.e.BamA, BamB, BamC, BamD and BamE). In comparison, there are only four partners inHaemophilus influenzae: a BamB homologue is not found in its genome. In this study, the recombinant expression, purification, crystallization and preliminary X-ray diffraction analysis ofH. influenzaeBamD and BamCD complex are reported. The genes encoding BamC and BamD were cloned into a pET vector and expressed inE. coli. Affinity, ion-exchange and gel-filtration chromatography were used to obtain high-purity protein for further crystallographic characterization. Using the hanging-drop vapour-diffusion technique, BamD and BamCD protein crystals of suitable size were obtained using protein concentrations of 70 and 50 mg ml−1, respectively. Preliminary X-ray diffraction analysis showed that the BamD crystals diffracted to 4.0 Å resolution and belonged to space groupP212121, with unit-cell parametersa= 54.5,b= 130.5,c= 154.7 Å. The BamCD crystals diffracted to 3.8 Å resolution and belonged to space groupI212121, with unit-cell parametersa= 101.6,b= 114.1,c= 234.9 Å.

Metallaborane Reaction Chemistry. Part 3. Reaction of Carbon Monoxide with [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] and the Isolation and Characterisation of Two arachno-6-Monoiridadecaboranes [6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] and sym-[6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11]

1997 ◽  
Vol 62 (8) ◽  
pp. 1239-1253 ◽  
Author(s):  
Jonathan Bould ◽  
Paul Brint ◽  
John D. Kennedy ◽  
Mark Thornton-Pett ◽  
Lawrence Barton ◽  
...  
Keyword(s):  
Carbon Monoxide ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Reaction System ◽  
Structural Type ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

[6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] (1) results from the reaction of [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] (2) with carbon monoxide in refluxing benzene. It is characterised by NMR spectroscopy and by single-crystal X-ray diffraction analysis. Crystals were triclinic, space group P1, with a = 10.688(2), b = 13.114(3), c = 22.356(5) Å, α = 78.33(2), β = 89.482(10), γ = 70.884(12)°, and Z = 2. The compound is of the little-examined arachno ten-vertex metallaborane structural type. A second compound of this type, [6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11] (3), isolated from a reaction system involving [Ir(CO)Cl(PPh3)2], PMe2Ph and the [nido-B9H12]- anion, has also been characterised crystallographically. Crystals were triclinic, space group P1, with a = 10.389(1), b = 10.511(1), c = 19.699(3) Å, α = 75.03(1), β = 85.53(1), γ = 74.88(1)°, and Z = 2.

Synthese und Röntgenstrukturanalyse von [Fe(η6-C6H4{1,3-(CH3)2})(η5 -C5(C6H5)5]+ [FeCl4]- / Synthesis and X-Ray Structure Analysis of [Fe(η6-C6H4{1 ,3 -(CH3)2})(η5-C5(C6H5)5]+ [FeCl4]-

1997 ◽  
Vol 52 (5) ◽  
pp. 573-576 ◽  
Author(s):  
Herbert Schumann ◽  
Alexander Lentz ◽  
Roman Weimann
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Structure Analysis ◽  
Mass Spectra ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Abstract Fe[C5(C6H5)5](CO)2Br (1) reacts with m-xylene at 80°C followed by hydrolysis with diluted HCl in the presence of air, to give [Fe(η6-C6H4{1,3-(CH3)2})(775-C5(C6H5)5)]+[FeCl4]- (3). The 1H, 13CNMR and mass spectra as well as the single crystal X-ray diffraction analysis confirm the proposed sandwich cation structure. 3 crystallizes in the space group P 21/n with a = 984,0(1), b = 2201,0(7), c = 1684,9(2) pm, β = 91,94(1)° and V = 3647(1) x 10-30m3. The final refinement resulted in R = 0,054 for 2982 observed reflections with F0 ≥4σ (F0)

THE CRYSTAL STRUCTURE OF K2TeBr6

1964 ◽  
Vol 42 (12) ◽  
pp. 2758-2767 ◽  
Author(s):  
I. D. Brown
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Least Squares ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cubic Form ◽  
Efficient Packing

Crystals of K2TeBr6 are monoclinic, space group [Formula: see text] with a = 7.521, b = 7.574, and c = 10.730 Å; β = 89° 40′. Atomic positions have been found by three dimensional X-ray diffraction analysis (least squares R = 0.12). The crystals possess a K2PtCl6 structure which is distorted to allow a more efficient packing of the comparatively large anions than is possible with the undistorted cubic form. The stereochemistry of the octahedral TeBr6− ion (Te—Br = 2.71 Å) is discussed.

scholarly journals Crystallization and preliminary X-ray diffraction analysis of the BRPF1 bromodomain in complex with its H2AK5ac and H4K12ac histone-peptide ligands

2014 ◽  
Vol 70 (10) ◽  
pp. 1389-1393 ◽  
Author(s):  
Mulu Y. Lubula ◽  
Amanda Poplawaski ◽  
Karen C. Glass
Keyword(s):  
Diffraction Analysis ◽  
National Laboratory ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Direct Role ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The bromodomain-PHD finger protein 1 (BRPF1) is an essential subunit of the monocytic leukemia zinc (MOZ) histone acetyltransferase (HAT) complex and is required for complex formation and enzymatic activation. BRPF1 contains a structurally conserved bromodomain, which recognizes specific acetyllysine residues on histone proteins. The MOZ HAT plays a direct role in hematopoiesis, and deregulation of its activity is linked to the development of acute myeloid leukemia. However, the molecular mechanism of histone-ligand recognition by the BRPF1 bromodomain is currently unknown. The 117-amino-acid BRPF1 bromodomain was overexpressed inEscherichia coliand purified to homogeneity. Crystallization experiments of the BRPF1 bromodomain in complex with its H4K12ac and H2AK5ac histone ligands yielded crystals that were suitable for high-resolution X-ray diffraction analysis. The BRPF1 bromodomain–H4K12ac crystals belonged to the tetragonal space groupP43212, with unit-cell parametersa= 75.1,b= 75.1,c= 86.3 Å, and diffracted to a resolution of 1.94 Å. The BRPF1 bromodomain–H2AK5ac crystals grew in the monoclinic space groupP21, with unit-cell parametersa= 60.9,b= 55.6,c= 82.1 Å, β = 93.6°, and diffracted to a resolution of 1.80 Å. Complete data sets were collected from both crystal forms using synchrotron radiation on beamline X29 at Brookhaven National Laboratory (BNL).

scholarly journals Crystallization and preliminary X-ray diffraction analysis of Lin1840, a putative β-glucosidase fromListeria innocua

2014 ◽  
Vol 70 (10) ◽  
pp. 1398-1401 ◽  
Author(s):  
Masahiro Nakajima ◽  
Ryuta Yoshida ◽  
Akimasa Miyanaga ◽  
Hayao Taguchi
Keyword(s):  
Diffraction Analysis ◽  
Gene Cluster ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Gene Encoding ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Lin1840 is a putative β-glucosidase that is predicted to be involved in 1,2-β-glucan metabolism since thelin1839gene encoding a 1,2-β-oligoglucan phosphorylase and thelin1840gene are located in the same gene cluster. Here, Lin1840 was crystallized. The crystals of Lin1840 diffracted to beyond 1.8 Å resolution. The crystal belonged to space groupI121, with unit-cell parametersa= 89.75,b= 95.10,c= 215.00 Å, α = 90.00, β = 96.34, γ = 90.00°.

Die Kristallstruktur des Tetraphenylphosphonium-Monoiodohexahydroc/ oso-Hexaborats [P(C6H5)4][B6H6I] / The Crystal Structure of Tetraphenylphosphonium Monoiodohexahydro-closo-hexaborate [P(C6H5)4][B6H6I]

1994 ◽  
Vol 49 (12) ◽  
pp. 1809-1812 ◽  
Author(s):  
W. Preetz ◽  
D. Sonnak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structure of [P(C6H5)4][B6H6I] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.5137(9), b = 12.623(2), c = 13.6363(13) Å, α = 87.787(13)°, β = 83.836(13)°, γ = 88.156(10)°. The additional H atom could be refined with B-H distances of 1.13 to 1.31 A above one of the facettes of the B6 octahedron opposite to the I substituent.

A Chain-like Polyoxotungstate Constructed from [CeW10O36]9–, [Na5(H2O)17Cl]4+, and [Na2(H2O)8]2+ Units: (NH4)3[Na5(H2O)17Cl]{[Na(H2O)4]2[CeW10O36]}· 6 H2O

2007 ◽  
Vol 62 (12) ◽  
pp. 1471-1475 ◽  
Author(s):  
Ling Yuan ◽  
Chao Qin ◽  
Xinlong Wang ◽  
Enbo Wang
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Supramolecular Network ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Linear Chains ◽  
A Chain

An unusual cerium-containing decaoxotungstate complex, (NH4)3[Na5(H2O)17Cl]{[Na(H2O)4]2- [CeW10O36]} · 6H2O (1) has been synthesized and characterized by IR, TG, and single crystal X-ray diffraction studies (yellow crystals, orthorhombic, space group Imm2, a = 11.473(2), b = 15.225(3), c = 17.646(7) Å, V = 3082.3(15) °A3, Z = 2, R = 0.046). In this compound, sandwichtype [CeW10O36]9− clusters are linked by binuclear [Na2(H2O)8]2+ units by sharing oxygen atoms into linear chains, which are further extended into a 2D supramolecular network via pentanuclear [Na5(H2O)17Cl]4+ units by strong hydrogen bonding interactions.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-(n-Bu4N)2[ReBr4(NCS)2 ], cis-(n-Bu4N)2[ReBr4(NCSe)2] und cis-(n-Bu4N)2[ReBr4(NCS)(NCSe)] / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of cis-(n-Bu4N)2[ReBr4(NCS)2], cis-(n-Bu4N)2[ReBr4(NCSe)2,] and cis -(n -Bu4N)2[ReBr4(NCS)(NCSe)]

2000 ◽  
Vol 55 (2) ◽  
pp. 178-184 ◽  
Author(s):  
L. Homolya ◽  
W. Preetz
Keyword(s):  
Low Temperature ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Vibrational Spectra ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReBr4(NCS)2] (1) (triclinic, space group P1̄, a = 11.475(6), b = 20.096(16), c = 22.144(11) Å, α = 110.56(6), β = 92.97(5), γ = 99.77(7)°, Z = 4), cis-(n-Bu4N)2[ReBr4(NCS)2] (2) (triclinic, space group P1̄, a = 11.527(3), b = 20.237(7), c = 22.07(2) Å, α = 110.05(4), β = 93.86(6), γ = 99.49(4)°, Z = 4) and cis-{n- Bu4N)2[ReBr4(NCS)(NCSe)] (3) (triclinic, space group P1̄, a = 11.488(2), b = 20.164(6), c = 22.158(5) Å, α = 110.44(2), β = 93.34(2), γ = 99.626(18)°. Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on these molecular parameters the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(ReN) = 1.70 (1), 1.70 (2) and 1.72 (3), fd(ReBr) = 1.36 (1), 1.30 (2) and 1.36 mdyn/Å (3).

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