scholarly journals Structures 4-n-propyl Piperazines as Non-Imidazole Histamine H3 Antagonists

Materials ◽  
2021 ◽  
Vol 14 (22) ◽  
pp. 7094
Author(s):  
Andrzej Olczak ◽  
Jarosław Sukiennik ◽  
Beata Olszewska ◽  
Monika Stefaniak ◽  
Krzysztof Walczyński ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Low Temperature ◽  
Unit Cell Parameters ◽  
Receptor Antagonists ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
H3 Receptor ◽  
Drug Similarity ◽  
Histamine H3

Seven new low-temperature structures of 4-n-propylpiperazine derivatives, potential H3 receptor antagonists, have been determined by X-ray crystallography, with the following symmetry and unit cell parameters: 2-(4-propyl-piperazin-1-yl)oxazolo[4,5-c]pyridine (compound 1), P-1, 5.9496 Å, 12.4570 Å, 12.8656 Å, 112.445°, 95.687°, 103.040°; 2-(4-propyl-piperazin-1-yl)thia-zolo[4,5-c]pyridine (compound 2), I2/a, 22.2087 Å, 7.5519 Å, 19.9225 Å, β = 92.368°; 2-(4-propyl-piperazin-1-yl)oxazolo[5,4-c]pyridine (compound 3), C2/c, 51.1351 Å, 9.36026 Å, 7.19352 Å, β = 93.882°; 2-(4-propyl-piperazin-1-yl)thiazolo[5,4-c]pyridine (compound 4), Pbcn, 19.2189 Å, 20.6172 Å, 7.4439 Å; 2-(4-propylpiperazin-1-yl)[1,3]oxazolo[4,5-b]pyridine, hydrate (structure 5), Pbca, 7.4967 Å, 12.2531 Å, 36.9527 Å; 2-(4-propylpiperazin-1-yl)[1,3]oxazolo[4,5-b]pyridine, first polymorph (structure 6), P-1, 7.2634 Å, 11.1261 Å, 18.5460 Å, 80.561°, 80.848°, 76.840°; 2-(4-propylpiperazin-1-yl)[1,3]oxazolo[4,5-b]pyridine, second polymorph (structure 7), P21, 8.10852 Å, 7.06025 Å, 12.41650 Å, β = 92.2991°. All the compounds crystallized out as hydrobromides. Oxazole structures show a much greater tendency to form twin crystals than thiazole structures. All the investigated structures display N—H···Br hydrogen bonding. (ADME) analysis, including the assessment of absorption, distribution, metabolism, and excretion, determined the physicochemical properties, pharmacokinetics, drug similarity, and bioavailability radar, and confirmed the usefulness of the compounds in question for pharmaceutical utility. This work is a continuation of the research searching for a new lead of non-imidazole histamine H3 receptor antagonists.

Silicate-germanate K2Y[(Si3Ge)O10(OH)] with unusual complex corrugated layer and its correlation to ring silicate gerenite and chain silicate chkalovite

2020 ◽  
Vol 235 (4-5) ◽  
pp. 167-172
Author(s):  
Anastasiia P. Topnikova ◽  
Elena L. Belokoneva ◽  
Olga V. Dimitrova ◽  
Anatoly S. Volkov ◽  
Leokadiya V. Zorina
Keyword(s):  
Low Temperature ◽  
Cross Section ◽  
Complex Anion ◽  
Diffraction Experiment ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Chain Silicate ◽  
Novel Complex

AbstractA new silicate-germanate K2Y[(Si3Ge)O10(OH)] was synthesized hydrothermally in a system Y2O3:GeO2:SiO2 = 1:1:2 (T = 280 °C; P = 90–100 atm.); K2CO3 was added to the solution as a mineralizer. Single-crystal X-ray diffraction experiment was carried out at low temperature (150 K). The unit cell parameters are a = 10.4975(4), b = 6.9567(2), c = 15.4001(6) Å, β = 104.894(4)°; V = 1086.86(7) Å3; space group is P 21/c. A novel complex anion is presented by corrugated (Si,Ge) tetrahedral layers connected by couples of YO6 octahedra into the mixed microporous framework with the channels along b and a axes, the maximal size of cross-section is ~5.6 Å. This structure has similarity with the two minerals: ring silicate gerenite (Ca,Na)2(Y,REE)3Si6O18 · 2H2O and chain silicate chkalovite Na2BeSi2O6. Six-member rings with 1̅ symmetry as in gerenite are distinguished in the new layer. They are mutually perpendicular to each other and connected by additional tetrahedra. Straight crossing chains in chkalovite change to zigzag four-link chains in the new silicate-germanate layer.

Crystal structure of potassium tetraperoxomolybdate (VI) K2[Mo(O2)4]

2005 ◽  
Vol 20 (3) ◽  
pp. 203-206 ◽  
Author(s):  
M. Grzywa ◽  
M. Różycka ◽  
W. Łasocha
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Rietveld Method ◽  
Structure Refinement ◽  
Crystal Structure Refinement ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters

Potassium tetraperoxomolybdate (VI) K2[Mo(O2)4] was prepared, and its X-ray powder diffraction pattern was recorded at low temperature (258 K). The unit cell parameters were refined to a=10.7891(2) Å, α=64.925(3)°, space group R−3c (167), Z=6. The compound is isostructural with potassium tetraperoxotungstate (VI) K2[W(O2)4] (Stomberg, 1988). The sample of K2[Mo(O2)4] was characterized by analytical investigations, and the results of crystal structure refinement by Rietveld method are presented; final RP and RWP are 9.79% and 12.37%, respectively.

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

The Crystal Structures of the Diastereoisomers (+)589-(Λ-δ-δ)-cis-Bis(ethylenediamine)dinitrocobalt(III)Hydrogen-D-tartrate Monohydrate and (-)589-(Λ-λ-λ)-cis-Bis(ethylenediamine)dinitrocobalt(III) Hydrogen-D-tartrate Dihydrate

1988 ◽  
Vol 41 (9) ◽  
pp. 1305 ◽  
Author(s):  
JM Frederiksen ◽  
E Horn ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Layer Structure ◽  
Three Dimensional ◽  
Water Molecules ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Tartrate Anion

The crystal structures of the diastereoisomers formed between the hydrogen-D-tartrate anion and the cations (+)-(Λ-[Co(en)2(NO2)2]+ (1) and (-)-(Δ)-[Co(en)2(NO2)2]+ (2) have been determined by three-dimensional X-ray analysis. The crystal structures are comprised of octahedrally coordinated cobalt atoms, hydrogentartrate anions and water molecules interconnected by a complex hydrogen bonding network. In (1), columns of complex parallel to a 21 screw axis along a, are linked via hydrogen bonding contacts to a total of six chains of 'head-to-tail' hydrogentartrate strands. In contrast, in (2) the chains of hydrogentartrate anions associate with each other to form well defined 'walls' which sandwich hydrogen-bonded columns of complex cations such that the structure may be thought of as a layer structure of hydrogentartrate anions and complex cations. Crystals of both compounds are orthorhombic, space group P212121 with Z = 4, unit cell parameters for (1): a 7.670(1), b 12.160(1), c 18.028(1)Ǻ, V 1681.4 Ǻ3 and for (2): a 7.735(2), b 8.505(5), c 26.846(9) Ǻ, V 1766 1 Ǻ3. The structures were each refined by a full-matrix least-squares procedure to final R 0.026, Rw 0.027 for 1764 reflections with I ≥ 2.5σ(I) for (1) and R 0.065, Rw 0.073 for 1322 reflections for (2).

scholarly journals Structural Reassignment of Koetjapic Acid following X-ray Crystallography and NMR Spectroscopy

2017 ◽  
Vol 12 (7) ◽  
pp. 1934578X1701200 ◽  
Author(s):  
Saifullah Abubakar ◽  
Vikneswaran Murugaiyah ◽  
Chin-Hoe Teh ◽  
Kit-Lam Chan
Keyword(s):  
Spectroscopic Data ◽  
Strong Support ◽  
Chair Conformation ◽  
Unit Cell Parameters ◽  
Orthorhombic Crystal ◽  
Dioic Acid ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
First Time

The crystal structure and absolute configuration of koetjapic acid were unambiguously reassigned by X-ray crystallography with strong support from NMR spectroscopic data. The acid contained 9 quaternary carbon atoms existing as an orthorhombic crystal with a space group of P21 21 21 and unit cell parameters of a = 7.6641(2), b = 14.6844(4) and c = 23.9316(6). Ring A adopted a chair conformation, ring B has an envelope conformation, whilst ring C assumed a half-chair and D displayed a chair conformation. The absolute configurations at C1 ( R), C5 ( R), C7 ( S), C10 ( S), C13 ( R), C14 ( R), C17 ( S) and C18 ( S) were assigned for the first time. The X-ray crystal of koetjapic acid was therefore reassigned as 3,4-seco-olean-4(23),12-diene-3,30-dioic acid. A plausible biogenetic synthetic pathway for compound 1 is also proposed.

scholarly journals Formation of an unexpected 3,3-diphenyl-3H-indazole through a facile intramolecular [2 + 3] cycloaddition of the diazo intermediate

2019 ◽  
Vol 15 ◽  
pp. 1347-1354
Author(s):  
Andrew T King ◽  
Hugh G Hiscocks ◽  
Lidia Matesic ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
...  
Keyword(s):  
Single Crystal ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
One Pot ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
The One ◽  
Close Contacts

The one-pot reaction of 2,6-bis(diphenylmethyl)-4-methoxyaniline with tert-butylnitrite, BTEAC and DABSO in the presence of CuCl2 provided an unexpected 3H-indazole product 8. The structure of the compound was determined by HRMS, IR, NMR and further confirmed by single crystal X-ray crystallography. The compound crystallises in the triclinic P-1 space group, with unit cell parameters a = 9.2107 (4), b = 10.0413 (5), c = 14.4363 (6) Å, α = 78.183 (2), β = 87.625 (2), γ = 71.975 (2)°. The formation of 8 proceeded through a facile intramolecular [2 + 3] cycloaddition of the diazo intermediate 9. The molecules of 8 are organised by edge–face Ar–H···π, face–face π···π, and bifurcated OCH2–H···N interactions. In addition to these, there are Ar–H···H–Ar close contacts, (edge–edge and surrounding inversion centres) arranged as infinite tapes along the a direction.

scholarly journals Structures of ruthenium-modified Pseudomonas aeruginosa azurin and [Ru(2,2′-bipyridine)2(imidazole)2]SO4·10H2O

1999 ◽  
Vol 55 (2) ◽  
pp. 379-385 ◽  
Author(s):  
Salem Faham ◽  
Michael W. Day ◽  
William B. Connick ◽  
Brian R. Crane ◽  
Angel J. Di Bilio ◽  
...  
Keyword(s):  
Monoclinic Space Group ◽  
Native Protein ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Peg 4000 ◽  
Dark Green ◽  
Atomic Coordinates

The crystal structure of Ru(2,2′-bipyridine)2(imidazole)(His83)azurin (RuAz) has been determined to 2.3 Å resolution by X-ray crystallography. The spectroscopic and thermodynamic properties of both the native protein and [Ru(2,2′-bipyridine)2(imidazole)2]2+ are maintained in the modified protein. Dark-green RuAz crystals grown from PEG 4000, LiNO3, CuCl2 and Tris buffer are monoclinic, belong to the space group C2 and have cell parameters a = 100.6, b = 35.4, c = 74.7 Å and β =  106.5°. In addition, [Ru(2,2′-bipyridine)2(imidazole)2]SO4·10H2O was synthesized, crystallized and structurally characterized by X-ray crystallography. Red–brown crystals of this complex are monoclinic, space group P21/n, unit-cell parameters a = 13.230 (2), b = 18.197 (4), c = 16.126 (4) Å, β = 108.65 (2)°. Stereochemical parameters for the refinement of Ru(2,2′-bipyridine)2(imidazole)(His83) were taken from the atomic coordinates of [Ru(2,2′-bipyridine)2(imidazole)2]2+. The structure of RuAz confirms that His83 is the only site of chemical modification and that the native azurin structure is not perturbed significantly by the ruthenium label.

scholarly journals Synthesis and spectroscopic properties of geminal-bis(tertbutylamino) phosphazenes obtained by the reaction of spiro and ansa phenoxyphosphazenes with the tert-butylamine and the crystal structure of 2,2-[2,2’-metheylenebis(4-chlorophenoxy)]-4,4-bis(tert-butylamino)-6,6-dichlorocyclo- 2λ5,4λ5,6λ5-triphosphazatriene

2011 ◽  
Vol 76 (6) ◽  
pp. 831-840
Author(s):  
Diğdem Erdener ◽  
Mustafa Yildiz ◽  
Hüseyin Ünver ◽  
Ocak İskeleli ◽  
Nuri Durlu
Keyword(s):  
Crystal Structure ◽  
31P Nmr ◽  
Spectroscopic Properties ◽  
Monoclinic Space Group ◽  
Spectroscopic Techniques ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Tert Butylamine

The condensation reactions of partly substituted spiro and ansa phenoxycyclotriphosphazenes, N3P3[2,2'-methylenebis(4-chlorophenoxide)]Cl4 (1 and 2) with tert-butylamine produce disubstituted geminal-bis(tert-butylamino)phenoxyphosphazene derivatives (3 and 4). The structures of these compounds were characterized by elemental analysis, and IR, 1H-, 13C-, 31P-NMR and mass spectroscopic techniques. Compound 3 was also examined by X-ray crystallography and found to be crystallized in the monoclinic space group P21/n with the unit cell parameters: a = 10.842(4), b = 9.375(5), c = 29.104(11) ?, ? = 99.25(3)?, V = 2920(2) ?3, Dx = 1.404 g cm-3.

The X-Ray Crystallography of Tavorite from the Tip Top Pegmatite, Custer, South Dakota

1988 ◽  
Vol 3 (2) ◽  
pp. 93-95 ◽  
Author(s):  
Andrew C. Roberts ◽  
Pete J. Dunn ◽  
Joel D. Grice ◽  
Dale E. Newbury ◽  
Willard L. Roberts
Keyword(s):  
Optical Absorption ◽  
South Dakota ◽  
Theoretical Formula ◽  
Unit Cell Parameters ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Spectroscopic Analyses ◽  
Secondary Ion

AbstractBright apple green millimeter-sized crystals of tavorite from the Tip Top pegmatite, near Custer, South Dakota are triclinic, space group , with refined unit-cell parameters a = 5.340(2), b = 7.283(2), c = 5.110(2)Å, α = 109.29(2)°, β = 97.86(3)°, γ = 106.32(3)°, V = 174.1(3)Å3, a:b:c = 0.7332:1:0.7016, Z = 2, D(m) (suspension in methylene iodide) = 3.32(1) and D(x) = 3.33 g/cm3 (for the theoretical formula). A fully indexed X-ray powder pattern is presented. Semiquantitative electron microprobe and secondary ion mass spectroscopic analyses indicate a formula near end-member LiFe + 3(PO4)(OH). The Tip Top tavorite is biaxial positive, α = 1.795(5), β = 1.81(1), γ = 1.86(1), 2V(meas.) = 50(2)°, 2V(calc.) = 59°, XΛa ≃ 15°, YΛb ≃ 0°, and ZΛc ≃ 38°. There is no evidence for optical absorption, pleochroism or dispersion.

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