scholarly journals Synthesis, spectroscopic studies and X-ray structure determination of two mononuclear copper complexes derived from the Schiff base ligand N,N-dimethyl-N'-((5-methyl-1H-imidazol-4-yl)methylene)ethane-1,2-diamine

2019 ◽  
Vol 10 (3) ◽  
pp. 201-208
Author(s):  
Pokpa Haba ◽  
Adama Sy ◽  
Farba Bouyagui Tamboura ◽  
Mamour Sarr ◽  
Ibrahima Elhadji Thiam ◽  
...  
Keyword(s):  
Schiff Base ◽  
Crystal Lattice ◽  
Structure Determination ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Reactions of the Schiff base N,N-dimethyl-N'-((5-methyl-1H-imidazol-4-yl)methylene) ethane-1,2-diamine (HL), synthesised in situ, with chloride or thiocyanate copper (II) salt; afforded two new mononuclear complexes, [Cu(HL)Cl2]·H2O (1) and [Cu(HL)(SCN)2] (2). These compounds have been studied and characterized by elemental analysis, IR and UV-Vis spectroscopies, electrochemistry, molar conductivity and room temperature magnetic measurements. Single crystal X-ray structure determination of the complexes revealed the presence of neutral moieties in the asymmetric unit. The mononuclear (1) crystallises in the monoclinic space group P21/c with the following unit cell parameters a = 7.4355(3) Å, b = 7.2952(3) Å, c = 26.2729(11) Å, β = 93.461(4)°, V = 1422.52(10) Å3, Z = 4, R1 = 0.033 and wR2 = 0.082 and the mononuclear complex (2) crystallises in the monoclinic space group C2/c with the following unit cell parameters a = 26.2578(7) Å, b = 7.4334(2) Å, c = 16.6237(5) Å, β = 99.089(3)°, V = 3203.95(16) Å3, Z = 8, R1 = 0.037 and wR2 = 0.104. In both complexes the ligand acts in tridentate fashion and the coordination environment of the copper atom can be described as distorted square pyramidal. The crystal lattice of the complex 1 is stabilized by electrostatic forces of attraction and O–H···Cl, C–H···O, N–H···Cl, and C–H···Cl, hydrogen bonding interactions while the crystal lattice of the complex 2 is stabilized by N–H···S and C–H···N.

scholarly journals The crystal structure of alstonite, BaCa(CO3)2: an extraordinary example of ‘hidden’ complex twinning in large single crystals

2020 ◽  
Vol 84 (5) ◽  
pp. 699-704
Author(s):  
Luca Bindi ◽  
Andrew C. Roberts ◽  
Cristian Biagioni
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Determinations

AbstractAlstonite, BaCa(CO3)2, is a mineral described almost two centuries ago. It is widespread in Nature and forms magnificent cm-sized crystals. Notwithstanding, its crystal structure was still unknown. Here, we report the crystal-structure determination of the mineral and discuss it in relationship to other polymorphs of BaCa(CO3)2. Alstonite is trigonal, space group P31m, with unit-cell parameters a = 17.4360(6), c = 6.1295(2) Å, V = 1613.80(9) Å3 and Z = 12. The crystal structure was solved and refined to R1 = 0.0727 on the basis of 4515 reflections with Fo > 4σ(Fo) and 195 refined parameters. Alstonite is formed by the alternation, along c, of Ba-dominant and Ca-dominant layers, separated by CO3 groups parallel to {0001}. The main take-home message is to show that not all structure determinations of minerals/compounds can be solved routinely. Some crystals, even large ones displaying excellent diffraction quality, can be twinned in complex ways, thus making their study a crystallographic challenge.

scholarly journals Crystallization and preliminary X-ray diffraction studies of guanidinoacetate methyltransferase from rat liver

1999 ◽  
Vol 55 (11) ◽  
pp. 1928-1929 ◽  
Author(s):  
Junichi Komoto ◽  
Yafei Huang ◽  
Yongbo Hu ◽  
Yoshimi Takata ◽  
Kiyoshi Konishi ◽  
...  
Keyword(s):  
Rat Liver ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Guanidinoacetate methyltransferase is the enzyme which catalyzes the last step of creatine biosynthesis. The enzyme is found ubiquitously and in abundance in the livers of all vertebrates. Recombinant rat-liver guanidinoacetate methyltransferase has been crystallized with guanidinoacetate and S-adenosylhomocysteine. The crystals belong to the monoclinic space group P21, with unit-cell parameters a = 54.8, b = 162.5, c = 56.1 Å, β = 96.8 (1)° at 93 K, and typically diffract beyond 2.8 Å.

Molecular and crystal structure of a copper(II) complex of sildenafil

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Akhmatkhodja N. Yunuskhodjayev ◽  
Shokhista F. Iskandarova ◽  
Vahobjon Kh. Sabirov
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Piperazine Ring ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Abstract The crystal structure of a copper(II) complex of protonated sildenafil, CuCl3C22H31N6O4S⋅2H2O was studied by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with the unit cell parameters a = 15.4292(2), b = 9.06735(12), c = 21.1752(2) Å, V = 2945.48(7) Å3, Z = 4. The Cu atom is coordinated by the sildenafil ligand via the N2 atom of the pyrazolopyrimidine ring and by three chloride anions. Sildenafil is protonated at the methylated N6 atom of the piperazine ring and it is cation ligand with a 1+ charge.

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).

X-ray powder diffraction data for five lanthanoid chromates [Ln2(CrO4)3(H2O)5]·2H2O (Ln=La,Pr,Nd,Sm,Eu)

1994 ◽  
Vol 9 (2) ◽  
pp. 98-104
Author(s):  
Jaakko Leppä-aho ◽  
Jussi Valkonen
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Diffraction Patterns

X-ray powder diffraction data are reported for a series of isomorphous compounds of [Ln2(CrO4)3(H2O)5]·2H2O, where Ln=La, Pr, Nd, Sm, or Eu. The compounds crystallize in monoclinic space group P21/c (No: 14) with Z=4. Refined unit cell parameters and indexed powder diffraction patterns are given.

Die Röntgenstrukturanalyse der Pyrrolide (CH3)2Al - C4H3NCH3 und (CH3)2Ga - N(CCH3)4 / The X-Ray Structure Determination of the Pyrrolides (CH3)2Al - C4H3NCH3 and (CH3)2Ga - N(CCH3)4

1994 ◽  
Vol 49 (3) ◽  
pp. 430-433 ◽  
Author(s):  
Hans-Dieter Hausen ◽  
Jochen Tödtmann ◽  
Johann Weidlein
Keyword(s):  
Structure Determination ◽  
Unit Cell ◽  
Lattice Parameters ◽  
Metal Ring ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

AbstractN-M ethyl-2-dimethylaluminium pyrrolide, (CH3)2Al -C4H3NCH3, crystallizes in the triclinic space group P1̄ with the lattice constants a = 700.5(1), b = 725.9(1), c = 886.8(1) pm, α = 67.69(1)°, β = 70.99(1)°, γ = 88.48(1)°, and Z = 2. This compound is isotypic with the gallium homologue [1], the shortest metal-ring contact between the two molecules of one unit cell decreases to 228.6 pm. N-dimethylgallium tetramethylpyrrolide has been synthesized from Li-N (CCH3)4 and (CH3)2GaCl. This “π-associate” crystallizes in the monoclinic space group P21/c with the lattice parameters a = 989.9(2), b = 1305.4(3), c = 878.3(2) pm, β - 112.73(1)° and 4 units per cell. Again two centrosymmetrically orientated molecules form a dimer by short (224.0 pm) intermolecular “Ga - πC ” contacts but the structure differs significant from the structure of the indium homologue [1].

Synthesis and Spectroscopic Characterization of Mixed Diamidophosphoric Acid Esters: X-Ray Crystal Structure of [(CH3)2N]-[p-H3C-C6H4-O]P(O)X (X = NHC(CH3)3 and p-H3C-C6H4-NH)

2009 ◽  
Vol 64 (5) ◽  
pp. 565-569 ◽  
Author(s):  
Saied Ghadimi ◽  
Mehrdad Pourayoubi ◽  
Ali Asghar Ebrahimi Valmoozi
Keyword(s):  
Spectroscopic Characterization ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
R Value ◽  
Acid Esters

Mixed diamidophosphoric acid esters [(CH3)2N][p-H3C-C6H4-O]P(O)X, where X = NH(CH3) (1), NHCH(CH3)2 (2), NHC(CH3)3 (3) and p-H3C-C6H4-NH (4) were synthesized and characterized by 31P, 31P{1H}, 13C, 1H NMR, and IR spectroscopy and mass spectrometry, and single crystal X-ray diffraction analysis for the compounds 3 and 4. Compound 3 crystallizes in the monoclinic, space group P21/c with unit cell parameters a = 9.006(3), b = 16.286(5), c = 10.319(3) A° , β = 99.633(6)◦, V = 1492.2(8) °A3, Z = 4. The final R value is 0.0622 for 2074 reflections [I ≥ 2σ (I)]. Compound 4 crystallizes in the orthorhombic, space group Pna21 with unit cell parameters a = 7.0459(14), b = 20.934(4), c = 10.436(2) ° A, V = 1539.3(5) °A3, Z = 4. The final R value is 0.0530 for 3025 reflections [I ≥ 2σ (I)].

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

1987 ◽  
Vol 2 (1) ◽  
pp. 2-4 ◽  
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.

scholarly journals Purification, crystallization and preliminary X-ray characterization ofBacillus cereusarylamineN-acetyltransferase 3 [(BACCR)NAT3]

2012 ◽  
Vol 68 (2) ◽  
pp. 196-198 ◽  
Author(s):  
Xavier Kubiak ◽  
Benjamin Pluvinage ◽  
Inès Li de la Sierra-Gallay ◽  
Patrick Weber ◽  
Ahmed Haouz ◽  
...  
Keyword(s):  
Bacillus Cereus ◽  
Catalytic Triad ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Metabolizing Enzymes ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

ArylamineN-acetyltransferases (NATs) are xenobiotic metabolizing enzymes (XMEs) that catalyze the acetylation of arylamines. All functional NATs described to date possess a strictly conserved Cys-His-Asp catalytic triad. Here, the purification, crystallization and preliminary X-ray characterization ofBacillus cereusarylamineN-acetyltransferase 3 [(BACCR)NAT3], a putative NAT isoenzyme that possesses a unique catalytic triad containing a glutamate residue, is reported. The crystal diffracted to 2.42 Å resolution and belonged to the monoclinic space groupC121, with unit-cell parametersa= 90.44,b= 44.52,c = 132.98 Å, β = 103.8°.

scholarly journals Chemical Preparation, Crystal Structure Reinvestigation and Vibrational Study of CoNa3P3O10.12H2O and X-ray Characterization of the New Anhydrous Triphosphate CoNa3P3O10

2021 ◽  
Vol 12 (2) ◽  
pp. 2586-2602
Keyword(s):  
Ion Exchange Resin ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Compound A ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The triphosphate dodecahydrate of cobalt and sodium CoNa3P3O10.12H2O was prepared by the ion exchange resin process. Its structure was studied by X-ray diffraction and determined in the monoclinic space group P121/c1with the unit-cell parameters a = 14.6650(5) Å, b=9.1916(3) Å, c = 15.0239(5) Å, =90.2210(10) °, Z = 4 and V = 2025.13(12) Å3. The thermal dehydration of this compound was performed, leading to an anhydrous new form, CoNa3P3O10, which was characterized by X-ray diffraction. The obtained CoNa3P3O10 crystallized in monoclinic space group P21/n with the unit-cell parameters a=15,3774 Å, b=7,6988 A°, c=14,2832A°, β=92,9115°.The characteristic IR wavenumbers of the P3O105− ions observed in the vibrational spectra were calculated using isotopic substitutions, which confirms the existence of these groups in the studied compound. A comparison between the IR and Raman wavenumbers of CoNa3P3O10.12H2O, CoNa3P3O10 and Na5P3O10.12H2O was performed. A kinetic study was also made for CoNa3P3O10·12H2O.

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