scholarly journals Multivariant Crystallization of Tetraplatin Precursors from Solutions Containing 1,2-C6H10(NH3)2 2+ and [PtCl6]2– Ions

2017 ◽  
Vol 2017 ◽  
pp. 1-12
Author(s):  
R. F. Mulagaleev ◽  
D. Y. Leshok ◽  
A. K. Starkov ◽  
A. N. Matsulev ◽  
S. D. Kirik
Keyword(s):  
Crystal Structures ◽  
Crystallization Rate ◽  
Minor Variation ◽  
Crystal Lattices ◽  
X Ray ◽  
Synthesis Conditions ◽  
H Nmr ◽  
Phase Diversity ◽  
Solvent Molecules ◽  
Solvent Acidity

Seven new phases containing hexachloroplatinate [PtCl6]2− and trans-1,2-dl-diammoniumcyclohexane 1,2-C6H10NH322+ ions were obtained by crystallization from solutions with minor variation of synthesis conditions. The compounds can be applied as precursors for the synthesis of effective anticancer drug tetraplatin ([PtC6H10(NH2)2Cl4]). The phase diversity was achieved by alterations including solvent acidity, crystallization rate, temperature, type of solvent, and the reagents ratio. The compounds were characterized by chemical and thermal analysis, IR, and 1H NMR spectroscopy. Crystal structures of the five compounds were determined by X-ray powder diffraction technique. The phases have ionic structures involving H2O, HCl molecules, or Cl− ions as supplementary species in the lattices. It helps to arrange some frames additionally interconnected by hydrogen bonds between ions and solvent molecules. It was suggested that crystal lattices adapted associated particles presented in solutions. It results in observed variety of the crystal structures. Besides the basic interest the obtained results are important for tetraplatin synthesis control.

Synthesis, Characterisation and Structural Studies of [Zn(phen)3][Fe(CN)5(NO)]·2H2O·0.25MeOH and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)]·0.5H2O

2003 ◽  
Vol 58 (9) ◽  
pp. 916-921 ◽  
Author(s):  
Amitabha Datta ◽  
Samiran Mitra ◽  
Georgina Rosair
Keyword(s):  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Structural Studies ◽  
Crystal Lattices ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Solvent Molecules

Two new bimetallic complexes [Zn(phen)3][Fe(CN)5(NO)] · 2 H2O · 0.25 MeOH, (1) and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)] · 0.5 H2O, (2), have been isolated (where phen = 1,10-phenanthroline and bipy = bipyridyl) and characterised by X-ray crystallography [as the 2 H2O · 0.25 CH3OH solvate for (1) and hemihydrate for (2)] infrared spectroscopy and thermogravimetric analysis. Substitution of phenanthroline for bipyridyl resulted in a cyano-bridged bimetallic species rather than two discrete mononuclear metal complexes. The bond angles of Fe-N-O were shown to be practically linear for both 1 [179.2(7)°] and 2 [178.3(3)°], and the Zn atoms have distorted octahedral geometry. The solvent molecules in both crystal lattices take part in forming hydrogen-bonded networks.

scholarly journals Crystal structures of 5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane cobalt(III) mono-phenylacetylide and bis-phenylacetylide

2018 ◽  
Vol 74 (4) ◽  
pp. 522-529 ◽  
Author(s):  
Benjamin M. Oxley ◽  
Brandon Mash ◽  
Matthias Zeller ◽  
Susannah Banziger ◽  
Tong Ren
Keyword(s):  
Crystal Structures ◽  
Symmetry Operator ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Weak Base ◽  
Monoclinic Symmetry ◽  
X Ray ◽  
Independent Molecules ◽  
Solvent Molecules ◽  
Occupancy Rates

Reported in this contribution are the synthesis and crystal structures of new mono- and bis-phenylacetylides based on CoIII(DMC) (DMC is 5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane). Chlorido(5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane)(phenylethynyl)cobalt(III) chloride–acetonitrile–methanol (1/1/1), [Co(C8H5)Cl(C12H28N4)]Cl·CH3CN·CH3OH, 1, and (5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane)bis(phenylethynyl)cobalt(III) trifluoromethanesulfonate–dichloromethane (2/1), [Co(C8H5)2(C12H28N4)]2(CF3SO3)2·CH2Cl2, 2, were prepared under weak-base conditions in satisfactory yields. Single-crystal X-ray diffraction studies revealed that both 1 and 2 adopt a pseudo-octahedral symmetry in which the Cl—Co—C angles of 1 and C—Co—C of 2 range from 177.7 (2) to 178.0 (2)° and from 177.67 (9) to 179.67 (9)°, respectively. In both structures, the CoIII metal center is coordinated in the equatorial plane by four N atoms, in which the N—Co—N angles range from 85.6 (3) to 94.4 (3)°. The structure of 1 features two crystallographically independent molecules in its triclinic cell (Z′ = 2), which are related to each other by pseudo-monoclinic symmetry. The crystal investigated was twinned by a symmetry operator of the approximate double-volume C-centered cell (180° rotation around [201] of the actual triclinic cell), with a refined twin ratio of 0.798 (3) to 0.202 (3). Both methanol solvent molecules in 1 are disordered, the major occupancy rates refined to 0.643 (16) and 0.357 (16). Compound 2 also contains two molecules in the asymmetric unit, together with two trifluoromethanesulfonate anions [of which one is disordered; occupancy values of 0.503 (16) and 0.497 (16)] and a disordered dichloromethane [occupancy values of 0.545 (12) and 0.455 (12)].

Pd(II) and Pt(II) Complexes of 1,2-Bis(pyridin-2-yl)ethane-N,N'

1994 ◽  
Vol 49 (6) ◽  
pp. 844-848 ◽  
Author(s):  
A. McFarlane ◽  
J. R. Lusty ◽  
J. J. Fiol ◽  
A. Terrón ◽  
E. Molins ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Spectroscopic Data ◽  
Low Energy ◽  
X Ray ◽  
H Nmr ◽  
Direct Bond ◽  
Structures And Properties ◽  
C Nmr

X-ray crystal structures and properties of the two Pd(II) and Pt(II) complexes [bpeH2][PdCl4] and [Pt(bpe)Cl2], [bpe = 1,2-bis(pyridin-2-yl)ethane] are described and correlated with the IR and 1H NMR/13C NMR spectroscopic data. In the case of the Pt(II) complex, the 1,2-bis(pyridin-2-yl)ethane is bound to the metal by the heterocycle nitrogen atoms but no direct bond is found in the case of the Pd(II) complex. The ligand exhibits low energy geometries in both compounds: the cis-conformation in the Pt(II) complex, and the transconformation in the Pd(II) complex

A new method of syntheses of 18-membered macrocyclic diphenyltin(IV) compounds and crystal structures of {Ph2Sn[S(C6H3NO)O]}3·Y (Y = 2H2O or 4C6H6) and {Ph3Sn[S(C6H3NO)O]SnPh3(EtOH)}·[EtOH]

2004 ◽  
Vol 82 (5) ◽  
pp. 608-615 ◽  
Author(s):  
Chunlin Ma ◽  
Qin Jiang ◽  
Rufen Zhang
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
New Method ◽  
Macrocyclic Compounds ◽  
X Ray ◽  
Stacking Interaction ◽  
Π Stacking ◽  
Triphenyltin Chloride ◽  
Π Stacking Interaction ◽  
Solvent Molecules

Two diphenyltin(IV) compounds: {Ph2Sn[S(C6H3NO)O]}3·Y (Y = 2H2O, 1; 4C6H6, 2) have been unexpectedly obtained by the reactions of triphenyltin chloride with 2-mercaptonicotinic acid in the presence of Et3N. However, by the reaction of the same reactants in the presence of EtONa, only a new triphenyltin(IV) compound ({Ph3Sn[S(C6H3NO)O]SnPh3(EtOH)}·[EtOH], 3) was obtained. The X-ray analyses reveal that compounds 1 and 2 are trinuclear, 18-membered macrocyclic compounds while 3 is a dinuclear compound. Specially, π-π stacking interaction was recognized in crystals of compound 1, which makes it a dimer. Co-crystallization was found in the crystals of all the three compounds 1, 2, and 3, the co-crystallized solvent molecules are water, benzene, and ethanol molecules, respectively. A possible dephenylation mechanism of 1 and 2 was illustrated in detail.Key words: triphenyltin, 2-mercaptonicotinic acid, dephenylation, macrocyclic, π-π stacking interaction, co-crystallization, crystal structure.

scholarly journals A history of experimental phasing in macromolecular crystallography

2016 ◽  
Vol 72 (3) ◽  
pp. 293-295 ◽  
Author(s):  
Neil Isaacs
Keyword(s):  
Crystal Structures ◽  
Electron Density ◽  
Diffraction Data ◽  
Fourier Transforms ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
Crystal Lattices ◽  
X Ray ◽  
Experimental Phasing ◽  
History Of

It was just over a century ago that W. L. Bragg published a paper describing the first crystal structures to be determined using X-ray diffraction data. These structures were obtained from considerations of X-ray diffraction (Bragg equation), crystallography (crystal lattices and symmetry) and the scattering power of different atoms. Although W. H. Bragg proposed soon afterwards, in 1915, that the periodic electron density in crystals could be analysed using Fourier transforms, it took some decades before experimental phasing methods were developed. Many scientists contributed to this development and this paper presents the author's own perspective on this history. There will be other perspectives, so what follows isahistory, rather thanthehistory, of experimental phasing.

Assigning structures to diastereomeric aliphatic α,α'-dibromo ketones

2002 ◽  
Vol 80 (4) ◽  
pp. 413-417 ◽  
Author(s):  
Masood Parvez ◽  
SM Humayan Kabir ◽  
Ted S Sorensen ◽  
Fang Sun ◽  
Brian Watson
Keyword(s):  
Liquid Chromatography ◽  
Key Words ◽  
Crystal Structures ◽  
Chemical Shifts ◽  
Gas Liquid Chromatography ◽  
X Ray ◽  
Nmr Chemical Shifts ◽  
H Nmr ◽  
Dibromo Ketones

X-ray crystal structures are reported for two symmetrical aliphatic α,α'-dibromo ketones: a meso diastereomer of 3,5-dibromo–2,2,6,6-tetramethylheptan-4-one, and a rac isomer of 4,6-dibromo–2,2,3,3,7,7,8,8-octamethylnonan-5-one. Using these secure assignments and a previously confirmed structure for the diastereomers of 2,4-dibromopentan-3-one, we show in this study that gas-liquid chromatography (GLC) retention times (meso > rac) can be used to confidently assign the diastereomers for a range of symmetrical and unsymmetrical aliphatic α,α'-dibromo ketones. 1H NMR chemical shifts for the >CHBr hydrogen(s) can also be corroboratively used for assignment purposes (δracH > δmesoH).Key words: α,α'-dibromo ketones, X-ray crystal structures, GLC retention times, isomer assignment

Synthesis and characterization of [MII(bqb)] (M = Co, Ni, Cu), [N(n-Bu)4][CoIII(bqb)(CN)2], and [N(n-Bu)4][CoIII(bqb)(N3)2] containing deprotonated N,N'-bis(2-quinolinecarboxamide)-1,2-benzene (bqb) – X-ray crystal structures of [NiII(bqb)] and [N(n-Bu)4][CoIII(bqb)(N3)2]

2006 ◽  
Vol 84 (7) ◽  
pp. 971-978 ◽  
Author(s):  
Soria Meghdadi ◽  
Mehdi Amirnasr ◽  
Vratislav Langer ◽  
Alison Zamanpoor
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Elemental Analyses

Cobalt(II), nickel(II), copper(II), and two cobalt(III) complexes of a new dianionic ligand, bqb, [H2bqb = N,N'-bis(2-quinolinecarboxamide)-1,2-benzene] have been synthesized and characterized by elemental analyses, IR, and 1H NMR spectroscopy. The crystal and molecular structures of the [Ni(bqb)] (2) and [N(n-Bu)4][CoIII(bqb)(N3)2] (5) complexes were determined by X-ray crystallography. Complex 2 crystallizes in the monoclinic space group C2/c with a distorted square-planar structure including two short Ni–N (1.848 Å) and two long Ni–N (1.958 Å) bonds. The structure consists of sheets formed in the plane parallel to the b axis and diagonal to vectors a and c by intermolecular hydrogen bonds. Complex 5 crystallizes in the monoclinic space group C2 with a distorted octahedral structure. The [N(n-Bu)4]+ ion is disordered at the C3A and C4A atoms of one Bu. The IR and 1H NMR spectra of the complexes are also discussed.Key words: N4-dianionic amido ligand (bqb), (bqb) complexes of Co(II), Ni(II), Cu(II), and Co(III), azide, cyanide, X-ray crystal structures.

Iridium(I) complexes containing bidentate pyrazolylgallate ligands. X-ray crystal structures of [Me2Gapz2]Ir(COD), [Ir(μ-pz)(CO)2]2, and [Ir(μ-3,5-Me2pz)(CO)2]2

1985 ◽  
Vol 63 (3) ◽  
pp. 692-702 ◽  
Author(s):  
Sophia Nussbaum ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structures ◽  
Variable Temperature ◽  
Hydrogenation Reaction ◽  
Synthesis And Characterization ◽  
Nmr Studies ◽  
X Ray ◽  
H Nmr ◽  
Measurable Activity

The synthesis and characterization of a number of Ir(I) complexes incorporating bidentate, chelating, pyrazolylgallate ligands are described. Non-rigidity for some of the complexes in solution has been demonstrated by variable temperature 1H nmr studies. Crystal structures of three complexes, [Me2Gapz2]Ir(COD), [Ir(μ-pz)(CO)2]2, and [Ir(μ-3,5-Me2pz)(CO)2]2 are reported and confirm the expected boat conformations for the six-membered M—(N—N)2—Ir rings (where M = Ir or Ga) in the compounds. One of the complexes studied has exhibited measurable activity as a catalyst in the hydrogenation reaction of cyclohexene.

X-Ray structures and binding properties of molecular clips based on diethoxycarbonyl glycoluril

2007 ◽  
Vol 85 (9) ◽  
pp. 586-591 ◽  
Author(s):  
Bao H Zhou ◽  
Li P Cao ◽  
Guo D Yin ◽  
M Gao ◽  
An X Wu
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Good Evidence ◽  
Binding Properties ◽  
X Ray ◽  
H Nmr ◽  
Binding Behavior ◽  
High Affinity ◽  
Molecular Clips

The crystal structures of two molecular clips derived from diethoxycarbonyl glycoluril were reported. Their unique binding behavior towards hydroquinone, which is different from Nolte's clips (high affinity for resorcinol), has been characterized through 1H NMR and IR. Job-plot analyses provide good evidence of a 1:1 stoichiometry for the complexes.Key words: crystal structure, molecular clips, binding properties

scholarly journals Synthesis and crystal structures of multifunctional tosylates as basis for star-shaped poly(2-ethyl-2-oxazoline)s

2010 ◽  
Vol 6 ◽  
pp. 773-783 ◽  
Author(s):  
Richard Hoogenboom ◽  
Martin W M Fijten ◽  
Guido Kickelbick ◽  
Ulrich S Schubert
Keyword(s):  
Crystal Structures ◽  
Ring Opening ◽  
Functional Materials ◽  
Diode Array ◽  
X Ray ◽  
H Nmr ◽  
Tosyl Chloride ◽  
Array Detectors ◽  
Polymer Architectures ◽  
Cationic Ring Opening Polymerization

The synthesis of well-defined polymer architectures is of major importance for the development of complex functional materials. In this contribution, we discuss the synthesis of a range of multifunctional star-shaped tosylates as potential initiators for the living cationic ring-opening polymerization (CROP) of 2-oxazolines resulting in star-shaped polymers. The synthesis of the tosylates was performed by esterification of the corresponding alcohols with tosyl chloride. Recrystallization of these tosylate compounds afforded single crystals, and the X-ray crystal structures of di-, tetra- and hexa-tosylates are reported. The use of tetra- and hexa-tosylates, based on (di)pentaerythritol as initiators for the CROP of 2-ethyl-2-oxazoline, resulted in very slow initiation and ill-defined polymers, which is most likely caused by steric hindrance in these initiators. As a consequence, a porphyrin-cored tetra-tosylate initiator was prepared, which yielded a well-defined star-shaped poly(2-ethyl-2-oxazoline) by CROP as demonstrated by SEC with RI, UV and diode-array detectors, as well as by 1H NMR spectroscopy.

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