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

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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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

Australian Journal of Chemistry ◽

10.1071/ch17270 ◽

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)°.

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Reactions between Co(II), 1,2-bis(diphenylphosphino)ethane, and NaBH3CN in the presence and absence of CO. The crystal structure of bis(cyanotrihydroborato)tetrakis(N,N-dimethylformamide)cobalt(II)

Canadian Journal of Chemistry ◽

10.1139/v88-285 ◽

1988 ◽

Vol 66 (7) ◽

pp. 1770-1775 ◽

Cited By ~ 7

Author(s):

David J. Elliot ◽

Sanna Haukilahti ◽

David G. Holah ◽

Alan N. Hughes ◽

Stanislaw Maciaszek ◽

...

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Unit Cell ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Triclinic Space Group ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

R Factor

Reactions between Co(II), Diphos, and NaBH3CN lead to Co(BH3CN)2(Diphos)2, 1, or [Co(BH3CN)(Diphos)2]X, 2 (X = ClO4 or BPh4), and, in certain solvents, 2 reacts to produce [Co(CN)(Diphos)2](ClO4). Compound 1 can be reversibly converted to Co(BH3CN)2(DMF)4, 4, via Co(BH3CN)2(Diphos)(DMF). In addition, 1 reacts with CO to form the Co(I) and Co(III) compounds [Co(Diphos)2](CO)]X and [Co(Diphos)2(CN)2]X (X = BH3CN or BPh4). Single crystal X-ray diffraction studies of 4 show that the compound crystallizes in the triclinic space group [Formula: see text], with unit cell parameters a = 7.572(6), b = 9.695(6), c = 9.395(6) Å, α = 81.06(4), β = 68.46(5), γ = 68.19(5)°, V = 595.5 Å3, Z = 1, and dcalcd = 1.202 g cm−3. The structure converged to a conventional R factor of 0.040 for 2841 observations and showed an octahedral arrangement of four O atoms from DMF molecules and two trans N-bound BH3CN groups around the Co(II) center.

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Crystallization and preliminary X-ray analysis of 3-deoxy-D-arabino-heptulosonate-7-phosphate synthase (tyrosine inhibitable) from Saccharomyces cerevisiae

Acta Crystallographica Section D Biological Crystallography ◽

10.1107/s0907444999007830 ◽

1999 ◽

Vol 55 (9) ◽

pp. 1586-1588 ◽

Cited By ~ 3

Author(s):

Thomas R. Schneider ◽

Markus Hartmann ◽

Gerhard H. Braus

Keyword(s):

Saccharomyces Cerevisiae ◽

Aromatic Amino Acids ◽

Diffusion Method ◽

Hanging Drop ◽

Unit Cell Parameters ◽

Data Set ◽

Triclinic Space Group ◽

X Ray ◽

Cell Parameters ◽

Phosphate Synthase

3-Deoxy-D-arabino-heptulosonate-7-phosphate synthase (E.C. 4.1.2.15) catalyzes the first step in the biosynthesis of aromatic amino acids: the condensation of phophoenolpyruvate and erythrose 4-phosphate to 3-deoxy-D-arabino-heptulosonate-7-phosphate. Diffraction-quality crystals of the tyrosine-inhibitable form of the enzyme from Saccharomyces cerevisiae have been obtained by the hanging-drop vapour-diffusion method in the presence of polyethylene glycol. The crystals belong to the triclinic space group P1, with unit-cell parameters a = 81.5, b = 94.0, c = 104.6 Å, α = 65.5, β = 85.2, γ = 75.0°, and can be flash-cooled using glycerol as a cryoprotectant. A data set to 2.3 Å has been collected at 120 K.

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Synthesis, spectroscopic characterization, and structural studies of new Cu(I) and Cu(II) complexes containing organophosphorus ligands, and crystal structures of (Ph3P)2Cu[S2PMe2], (Ph3P)2Cu[(OPPh2)2N], Cu[(OPPh2)2N]2, and Cu[(OPPh2)(SPPh2)N]2

Canadian Journal of Chemistry ◽

10.1139/v01-048 ◽

2001 ◽

Vol 79 (5-6) ◽

pp. 983-991 ◽

Cited By ~ 26

Author(s):

Anca Silvestru ◽

Adina Rotar ◽

John E Drake ◽

Michael B Hursthouse ◽

Mark E Light ◽

...

Keyword(s):

Spectroscopic Characterization ◽

Molecular Structures ◽

Orthorhombic Space Group ◽

Phosphorus Ligands ◽

Triclinic Space Group ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

X Ray Crystallography ◽

Multinuclear Nmr Spectroscopy

The Cu(I) complexes, (Ph3P)2CuL (L = [S2PMe2]-, [OSPR2]- (R = Me, Ph), [(XPR2)(YPR'2)N]- (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph; O, S, OEt, Ph; S, S, Me, Me)) and Cu(II) complexes, CuL2 (L = [(XPR2)(YPR'2)N]- (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph)), have been prepared. The Cu(I) derivatives were characterized by multinuclear NMR spectroscopy and in two cases by X-ray crystallography. (Ph3P)2Cu[S2PMe2] (1) crystallizes in the orthorhombic space group P212121 (No. 19) with cell parameters a = 9.782(2), b = 17.808(4), c = 20.216(4) Å, V = 3521(6) Å3 and Z = 4, and (Ph3P)2Cu[(OPPh2)2N] (4) in the triclinic space group P[Formula: see text] (No. 2) with cell parameters a = 9.8079(2), b = 12.9141(3), c = 22.5666(5) Å, α = 75.714(2), β = 79.465(2), γ = 68.2770(8)°, V = 2559.9(1) Å3 and Z = 2. In both cases the phosphorus ligands are bidentate, thus resulting in monomeric molecules that contain tetrahedral CuP2S2 and CuP2O2 cores. The molecular structures of two of the Cu(II) derivatives were also determined. Cu[(OPPh2)2N]2 (8) and Cu[(OPPh2)(SPPh2)N]2 (9) crystallize in the triclinic space group P[Formula: see text] (No. 2) with cell parameters a = 8.887(2), b = 10.739(2), c = 12.477(3) Å, α = 77.61(3), β = 76.15(5), γ = 79.46(3)°, V = 1118.3(4) Å3 and Z = 1 for 8, and a = 9.626(2), b = 14.151(3), c = 24.752(5) Å, α = 88.23(3), β = 79.93(3), γ = 89.77(3)°, V = 3181(1) Å3 and Z = 3 for 9. The molecule of Cu[(OPPh2)2N]2 (8) has a planar CuO4 core, while in Cu[(OPPh2)(SPPh2)N]2 (9) both planar and tetrahedral copper cores are observed in a ratio of 1:2.Key words: structure, copper, thiophosphinates, oxo- and thio-imidodiphosphinates

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

Natural Product Communications ◽

10.1177/1934578x1701200704 ◽

2017 ◽

Vol 12 (7) ◽

pp. 1934578X1701200 ◽

Cited By ~ 1

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.

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Armstrongite from the Strange Lake Alkalic Complex, on the Quebec – Labrador Boundary, Canada

Powder Diffraction ◽

10.1017/s0885715600012148 ◽

1987 ◽

Vol 2 (1) ◽

pp. 2-4 ◽

Cited By ~ 12

Author(s):

John L. Jambor ◽

Andrew C. Roberts ◽

Joel D. Grice

Keyword(s):

Electron Microprobe ◽

Unit Cell ◽

Powder Pattern ◽

Theoretical Formula ◽

Monoclinic Space Group ◽

Unit Cell Parameters ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

No Absorption

AbstractTabular untwinned crystals of colorless transparent armstrongite from the Strange Lake Alkalic Complex, on the Quebec – Labrador boundary, Canada are monoclinic, space group choices I2/m, I2, Im (diffraction aspect I*/*), with refined unit-cell parameters a = 13.599 (9), b = 14.114(9), c = 7.833 (4) Å, β = 103.41 (5)°, V = 1462.4 (±3.0) Å3. a:b:c = 0.9635:1:0.5550, Z = 4 and D(x) = 2.696 g/cm3. A fully indexed X-ray powder pattern is presented. Averaged electron-microprobe analyses suggest a theoretical formula of CaZrSi6O15 · 3 H2O. The Strange Lake armstrongite is biaxial negative, α = 1.567 (1), β = 1.576 (1), γ = 1.577 (1), 2V (meas.) = 39 (1)°, 2V (calc.) = 37°, Z∥b, X Λc = +4°, with no absorption and weak dispersion r < v.

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

Beilstein Journal of Organic Chemistry ◽

10.3762/bjoc.15.134 ◽

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.

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Amphiphilic aluminium(III) and gallium(III) corroles

Journal of Porphyrins and Phthalocyanines ◽

10.1142/s1088424607000242 ◽

2007 ◽

Vol 11 (03) ◽

pp. 189-197 ◽

Cited By ~ 14

Author(s):

Karn Sorasaenee ◽

Pouyan Taqavi ◽

Lawrence M. Henling ◽

Harry B. Gray ◽

Elena Tkachenko ◽

...

Keyword(s):

Crystal Structure ◽

Electronic Absorption ◽

Spectroscopic Properties ◽

Fluorescence Band ◽

Unit Cell Parameters ◽

Triclinic Space Group ◽

X Ray ◽

Cell Parameters ◽

Polar Head ◽

Head Groups

The preparation and spectroscopic properties of a series of metallocorroles with polar head groups CHO and CH = C ( CN )( COOH ) are reported, as well as the X-ray crystal structure of 5,10,15-tris(pentafluorophenyl)corrolatoaluminium(III)bispyridine (triclinic space group (P-1) with unit cell parameters: a = 9.426(1) Å; b = 13.202(1) Å; c = 19.936(1) Å; α = 74.19(1)°; β = 78.47(1)°; γ = 75.75(1)°; V = 2289.57(8) Å3). Amphiphilic aluminium(III) and gallium(III) corroles exhibit electronic absorption (Soret peaks between 410 and 448 nm; Q-bands between 584 and 638 nm) and fluorescence (band maxima between 634 and 706 nm) at lower energies than their hydrophobic analogs.

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

Acta Crystallographica Section D Biological Crystallography ◽

10.1107/s0907444998010464 ◽

1999 ◽

Vol 55 (2) ◽

pp. 379-385 ◽

Cited By ~ 13

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.

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

Materials ◽

10.3390/ma14227094 ◽

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.

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