Zirconium Reagents for Organometallic Synthesis. Crystal Structures of ZrCl4 ·2Et2O and (Et2N)ZrCl3·Et2O

1999 ◽  
Vol 54 (12) ◽  
pp. 1563-1567 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Konstantin A. Rufanov
Keyword(s):  
Crystal Structures ◽  
Diethyl Ether ◽  
Elemental Analysis ◽  
Octahedral Geometry ◽  
Quantitative Yield ◽  
Coordination Polyhedra ◽  
Organometallic Synthesis ◽  
X Ray ◽  
Acidic Compounds ◽  
C Nmr

Reaction of 3 equivalents of ZrCl4 · 2Et2O (1) with 1 equivalent of (Et2N4Zr in diethyl ether readily affords crystalline (Et2N)ZrCl3 · 2Et2O (2) in almost quantitative yield. The product was characterised by elemental analysis and by 1H. 13 C NMR, and MS techniques. The reactivity of this reagent towards C-H acidic compounds has been studied using cyclopentadiene as a C-H acid. The crystal structures of both 1 and 2 have been determined by X-ray diffractometry. The coordination polyhedra reveal a nearly perfect octahedral geometry with a trans Et2O ligation for 1 and a cis one for 2.

Bis(1-phenyl-1-propyne) complexes of tungsten(II): crystal structures of [WI2(CO)(NCR)(η2-MeC2Ph)2] (R = Me, Et, or Ph)

2001 ◽  
Vol 79 (3) ◽  
pp. 263-271
Author(s):  
Paul K Baker ◽  
Michael GB Drew ◽  
Deborah S Evans
Keyword(s):  
Carbon Monoxide ◽  
Solid State ◽  
Crystal Structures ◽  
Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Alkyne Complexes ◽  
First Time

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.

Crystal structures of tricalcium citrates

2018 ◽  
Vol 33 (2) ◽  
pp. 98-107 ◽  
Author(s):  
James A. Kaduk
Keyword(s):  
Crystal Structures ◽  
Density Functional ◽  
Three Dimensional ◽  
Water Molecules ◽  
Calcium Citrate ◽  
Powder Diffraction Data ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Calcium Supplements ◽  
Dimensional Network

The crystal structures of calcium citrate hexahydrate, calcium citrate tetrahydrate, and anhydrous calcium citrate have been solved using laboratory and synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Both the hexahydrate and tetrahydrate structures are characterized by layers of edge-sharing Ca coordination polyhedra, including triply chelated Ca. An additional isolated Ca is coordinated by water molecules, and two uncoordinated water molecules occur in the hexahydrate structure. The previously reported polymorph of the tetrahydrate contains the same layers, but only two H2O coordinated to the isolated Ca and two uncoordinated water molecules. Anhydrous calcium citrate has a three-dimensional network structure of Ca coordination polyhedra. The new polymorph of calcium citrate tetrahydrate is the major crystalline phase in several commercial calcium supplements.

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

Über die Reaktion von C(NMe2)4 mit zweikernigen Übergangsmetallcarbonylen; Kristallstrukturen von [C(NMe2)3][Mn(CO)5] und [C(NMe2)3][Co(CO)4] / On the Reaction of C(NMe2)4 with Binuclear Transition Metal Carbonyls: Crystal Structures of [C(NMe2)3][Mn(CO)5] and [C(NMe2)3][Co(CO)4]

1991 ◽  
Vol 46 (3) ◽  
pp. 297-302 ◽  
Author(s):  
Wolfgang Petz ◽  
Frank Weller
Keyword(s):  
Transition Metal ◽  
Crystal Structures ◽  
Structure Determination ◽  
Metal Carbonyls ◽  
Space Group ◽  
X Ray ◽  
Transition Metal Carbonyls ◽  
C Nmr

The reactions of C(NMe2)4 (1) with Mn2(CO)10 or Co2(CO)8 in THF yield[C(NMe2)3][Co(CO)4] (3) and [C(NMe2)3][Mn(CO)5] (4), respectively. The compounds Co(CO)4NMe2 (5) and Mn(CO)5NMe2 (6) could not be found. With CH2Cl2 4 is quantitatively converted into [C(NMe2)3][Mn(CO)4Cl2] (7) as shown by IR and 13C NMR investigations. 3 and 4 were characterized by an X-ray structure determination. 3: Space group Pnma, Z = 4, a = 7.435(2), b = 10.79(2), c = 20.299(5)Å. 4: Space group C2/c, Z = 4, a = 11.378(2), b = 10.165(1), c = 14.533(1) Å; β = 103.37(1)°. The compounds form independent ions with no bonding interactions between cation and anion; the central CN3 unit of the [C(NMe2)3]+ cation in 3 and 4 is disordered.

scholarly journals Synthesis and Single Crystal X-Ray Structure of Bis[4-oxo-3- (2-ethoxycarbonylphenyl)-3,4-dihydroquinazolin-2-yl]disulfide

2009 ◽  
Vol 64 (9) ◽  
pp. 1065-1069 ◽  
Author(s):  
Mehdi Rimaz ◽  
Jabbar Khalafy ◽  
Khadijeh Tavana ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Structure Determination ◽  
Room Temperature ◽  
Sodium Ethoxide ◽  
Reaction Conditions ◽  
X Ray ◽  
Ethyl Nitroacetate ◽  
C Nmr

Diethyl 2,2´-thiocarbonyl-bis(azanediyl)dibenzoate was synthesized from the reaction of ethyl anthranilate with thiophosgene. Its treatment with sodium ethoxide in ethanol at room temperature gave ethyl 2-(4-oxo-2-thioxo-1,2-dihydroquinazolin-3(4H)-yl) benzoate, whereas in the presence of ethyl nitroacetate and under the same reaction conditions, the corresponding bis(quinazolin)disulfide was formed. Its structure was confirmed by IR, 1H and 13C NMR spectroscopy elemental analysis and single crystal X-ray structure determination.

3-Hexyne Complexes of M olybdenum(II) and Tungsten(II) Containing 2, 2 '-Bipyridine. X-Ray Crystal Structure of [MoI2(CO)(bipy)(η2-EtC2Et)]

2000 ◽  
Vol 55 (11) ◽  
pp. 1095-1098
Author(s):  
Mutlaq Al-Jahdali ◽  
Paul K. Baker ◽  
Michael B. Hursthouse ◽  
Simon J. Coles
Keyword(s):  
Crystal Structure ◽  
Carbon Monoxide ◽  
Room Temperature ◽  
Octahedral Geometry ◽  
Cationic Complex ◽  
Molybdenum Complex ◽  
Neutral Complex ◽  
Nmr Studies ◽  
X Ray ◽  
C Nmr

Reaction of [MI2(CO)(NCMe)(η2-EtC2Et)2] (M = Mo,W) with one equivalent of 2,2' -bipyridine (bipy) in CH2C12 at room temperature gives either the neutral complex, [MoI2(CO)(bipy)- (η2-EtC2Et)] (1) or the cationic complex, [WI(CO)(bipy)(η2-EtC2Et)2]I (2). The neutral molybdenum complex 1, has been crystallographically characterised, and has a pseudo-octahedral geometry with the iodo-ligand trans to the 3-hexyne, and with the bipy, carbon monoxide and other iodo-ligand occupying the equatorial face. 13C NMR studies show the 3-hexyne is donating four electrons to the molybdenum in 1.

New Cu(II), Co(II), and Ni(II) complexes with thieno[2,3-b]pyridine and 2-methylthieno[2,3-b]pyridine as ligands: Synthesis and crystal structures

2009 ◽  
Vol 63 (3) ◽  
Author(s):  
Ján Halgaš ◽  
Viera Kolenová ◽  
Zuzana Števíková ◽  
Lucia Perašínová ◽  
Jozef Kožíšek
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Elemental Analysis ◽  
Zinc Chloride ◽  
Coordination Compounds ◽  
Biological Activities ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir

AbstractAlthough thienopyridines attract attention because of their biological activities, they have not been used as ligands in coordination compounds. Thieno[2,3-b]pyridine was prepared by known procedures; by reduction of 2-nitrothiophene, and reaction of the resulting 2-thienyl ammonium salt with malondialdehyde tetramethylacetal in the presence of zinc chloride. The same procedure was used for the preparation of a new derivative, 2-methylthieno[2,3-b]pyridine, starting from 2-methyl-5-nitrothiophene. The thienopyridines were used in the synthesis of coordination compounds. Chlorides, isothiocyanates, acetates, and chloroacetates of copper(II), nickel(II), or cobalt(II) were used as starting salts. The prepared complexes were characterized by elemental analysis and FT IR. Structures of the four complexes were determined by single-crystal X-ray diffraction analysis.

1-Allylgermatrane. Synthesis, Structure and Reaction with Diazomethane

1997 ◽  
Vol 52 (1) ◽  
pp. 30-34 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Sergey S. Karlov ◽  
Elena S. Alekseyeva ◽  
Leonid A. Aslanov ◽  
Evgeni V. Avtomonov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Structure Study ◽  
Quantitative Yield ◽  
High Yield ◽  
Crystalline Solid ◽  
Conformational Disorder ◽  
X Ray ◽  
C Nmr

Reaction of allyltribromogermane (2), readily available from dibromo(1,4-dioxane)germanium(II) (1) and allylbromide, with tris(2-tributylstannoxyethyl)-amine (4) gives 1-allylgermatrane (3) in almost quantitative yield. 3 crystallizes from n-pentane as a colourless crystalline solid which was characterized by 1H and 13C NMR spectroscopy and by an X-ray crystal structure study. The “atrane” skeleton shows a strong conformational disorder; the Ge-N distance of 2.208(3) Å suggests the presence of a coordinative Ge-N bond. Treatment of 1-allylgermatrane (3) with CH2N2 in the presence of catalytic amounts of Pd(OAc)2 affords 1-cyclopropylmethylgermatrane (5) in high yield

scholarly journals Crystal structures of two magnesium citrates from powder diffraction data

2020 ◽  
Vol 76 (10) ◽  
pp. 1611-1616
Author(s):  
James A. Kaduk
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Density Functional ◽  
Powder Diffraction Data ◽  
Magnesium Citrate ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cation Coordination ◽  
Citrate Anion

The crystal structures of magnesium hydrogen citrate dihydrate, Mg(HC6H5O7)(H2O)2, (I), and bis(dihydrogen citrato)magnesium, Mg(H2C6H5O7)2, (II), have been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. In (I), the citrate anion occurs in the trans, trans-conformation, and triply chelates to the Mg cation. In (II), the citrate anion is trans, gauche, and doubly chelates to the Mg cation. In both compounds the Mg cation coordination polyhedron is an octahedron. In (I), the MgO6 coordination polyhedra are isolated, while in (II), they share edges to form chains. Strong O—H...O hydrogen bonds are prominent in the two structures, as well as in the previously reported magnesium citrate decahydrate.

Retention of (4,4) Connectivity in the Absence of π…π Interactions in a Cadmium tris-Dicyanamide Compound

2006 ◽  
Vol 59 (2) ◽  
pp. 115 ◽  
Author(s):  
Moumita Biswas ◽  
Stuart R. Batten ◽  
Paul Jensen ◽  
Samiran Mitra
Keyword(s):  
Thermogravimetric Analysis ◽  
Ir Spectroscopy ◽  
Powder Diffraction ◽  
Elemental Analysis ◽  
Octahedral Geometry ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography ◽  
Extended Sheets

An anionic cadmium tris-dicyanamide compound (Et4N)[Cd(N(CN)2)3]·3/4H2O 1 has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, X-ray powder diffraction, and X-ray crystallography. The anions form extended sheets with retention of (4,4) connectivity in the absence of π···π interactions within the cation layers, and with octahedral geometry about individual CdII ions.

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