Copper(II) and Cobalt(III) Complexes of a Mixed Secondary and Tertiary Nitrogen Donor Tetraaza Macrocycle. Crystal Structure of Aqua(7-methyl-7-nitro-1,5,9,13-tetraaza-bicyclo[11.2.2]heptadecane)copper(II) Perchlorate Hydrate

1989 ◽  
Vol 42 (11) ◽  
pp. 1859 ◽  
Author(s):  
LM Engelhardt ◽  
GA Lawrance ◽  
TM Manning ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Copper Ion ◽  
Chloride Ion ◽  
Macrocyclic Complex ◽  
High Yield ◽  
Tetraaza Macrocycle ◽  
Orthorhombic Space Group ◽  
Nitrogen Donor ◽  
Perchlorate Salt ◽  
Tertiary Nitrogen

Reaction of (bis(3-aminopropyl) piperazine )copper(11) ion with nitroethane and formaldehyde in basic methanol results in the ready formation of (7-methyl-7-nitro-1,5,9,13- tetraazabicyclo [11.2.2] heptadecane )copper(11) ion in high yield. The perchlorate salt of the macrocyclic complex crystallizes in the orthorhombic space group Pbca, a 19.144(8), b 17.499(5), c 14.635(5) �, Z=8, with the copper ion in a square-pyramidal environment of four nitrogen donors and a water molecule. The Cu-secondary N and Cu-tertiary N distances are 2.044(8), 2.056(8) and 2.053(8), 2.072(8) � respectively, with the Cu-O distance 2.259(8)�. Reduction of the complex with Zn/ HCl yields the 7-methyl-1,5,9,13-tetraazabicyclo [l1.2.2]heptadecane-7-amine analogue, characterized as copper(II) and cobalt(III) complexes. The cobalt(III) complex contains the latter macrocycle as a quinquedentate ligand with the pendant primary amine coordinated trans to a chloride ion, identified as the only isomer by chromatography, and characterized by electronic and n.m.r. spectroscopy. Consequences of 'reinforcement' of the macrocycle by the extra ethane bridge are discussed.

Synthesis of a Cis-N2s2 Donor Macrocycle by Metal-Directed Condensation of Formaldehyde, Nitroethane and a Diaminodithiaalkane - Crystal-Structure of the (6-Methyl-6-Nitro-1,11-Dithia-4,8-Diazacyclotetradecane)-Copper(II) Perchlorate Product

1988 ◽  
Vol 41 (5) ◽  
pp. 773 ◽  
Author(s):  
P Comba ◽  
GA Lawrance ◽  
M Rossignoli ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Structural Properties ◽  
Copper Ion ◽  
Macrocyclic Complex ◽  
High Yield ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Complex Ion ◽  
Perchlorate Salt

Reaction of (3,7-dithianonane-1,9-diamine)copper(II) ion with nitroethane and formaldehyde in basic methanol gives the macrocyclic complex ion (6-methyl-6-nitro-1,II-dithia-4,8- diazacyclotetradecane )copper(II) in high yield. The complex as the perchlorate salt crystallizes in the monoclinic space group P21/n, a 15.008(5), b 8.606(3), c 17.967(4)Ǻ, β 113.79(2)�. The copper ion lies in a square plane of two nitrogen (average Cu-N 2.02 Ǻ) and two thioether (average Cu-S 2.295 Ǻ) donors, with perchlorate oxygens (Cu-O 2.46 and 2.70 Ǻ) in axial sites. Physical and structural properties of the CuIII complexes of the 14-membered cis-N2S2 macrocycle and the known analogous 14-membered N4-donor macrocycle 6-methyl-6-nitro-1,4,8,11- tetraazacyclotetradecane are compared.

The direct electrochemical synthesis of thiolato complexes of cobalt and nickel, and the crystal structure of bis(phenylthiolato)bis(1,10-phenanthroline)cobalt(III) perchlorate

1988 ◽  
Vol 66 (9) ◽  
pp. 2151-2156 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Jaime Romero Lopez-Grado ◽  
Dennis G. Tuck
Keyword(s):  
Crystal Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Crystallographic Analysis ◽  
High Yield ◽  
X Ray ◽  
Metal Anode ◽  
Aerial Oxidation ◽  
Perchlorate Salt ◽  
Cobalt And Nickel

Cobalt(II) and nickel(II) thiolates, M(SR)2, can be prepared in high yield by the electrochemical oxidation of a metal anode in an acetonitrile or acetone solution of RSH (R = C6H5, o-CH3C6H4, 2-C10H7, 2,3,4,5-C6F4H; not all combinations). When 2,2-bipyridine or 1,10-phenanthroline (=L) is added to the electrolyte phase, the products are the adducts M(SR)2L2. In the case of Co(SC6H5)2(phen)2, aerial oxidation leads to the formation of the cobalt(III) cation [Co(SC6H5)2(phen)2]+, isolated as the perchlorate salt. X-ray crystallographic analysis showed that this cation has a cis-CoS2(N2)2 kernel.

Spezielle Alkylammoniumhexachlorometallate, II [1] Synthese und Kristallstruktur von Bis(1,2-diammoniopropan)hexachlororhodat(III)-chlorid, [H3N-CH(CH3)-CH2-NH3]2[RhCl6]Cl/ Alkylammonium Hexachlorometallates, II [1] Synthesis, and Crystal Structure of Bis(1,2-diammoniopropane) Hexachlororhodate(III) Chloride, (H3N-CH(CH3)-CH2-NH3]-[RhCl6]Cl

1996 ◽  
Vol 51 (10) ◽  
pp. 1459-1463 ◽  
Author(s):  
Walter Frank ◽  
Guido J. Reiß
Keyword(s):  
Crystal Structure ◽  
Hydrochloric Acid ◽  
Hydrogen Bonds ◽  
Acid Solution ◽  
Crystal Lattice ◽  
Ternary Compound ◽  
Chloride Ion ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Packing Scheme

Bis(1,2-diammoniopropane) hexachlororhodate(III) chloride, [H3N-CH(CH3)-CH2-NH3]2 [RhCl6]Cl (1) has been obtained by the reaction of rhodium(III) chloride with rac-1,2- diammoniopropane dihydrochloride in hydrochloric acid solution. The quasi-ternary compound, which crystallizes in the orthorhombic space group Pbca (a - 11.0007(13) Å, b = 22.181(2) A, c = 14.638(2) A, V = 3571.7(7) Å3, \ T = -120 °C, Z - 8) contains two crystallographically independent 1,2-diammoniopropane ions beside one hexachlororhodate and one chloride ion. One of the cations shows a R/S-S/R-disorder of enantiomeric pairs in the centrosymmetric crystal lattice. The packing scheme is determined by a complex framework of hydrogen bonds.

Synthesis, Characterization and Enhanced Cleavage of Diphosphate and Triphosphate Bound to Tetraaminecobalt(III) Centers. Crystal Structure of [N,N-Bis(2-aminoethyl)ethane-1,2-diamine](diphosphato)cobalt(III) Perchlorate Monohydrate

1989 ◽  
Vol 42 (7) ◽  
pp. 1045 ◽  
Author(s):  
LM Engelhardt ◽  
EA Keegan ◽  
GA Lawrance ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Adenosine Triphosphate ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Nitrogen Donor ◽  
Oxygen Donors ◽  
Hydrolysis Of ◽  
Tertiary Nitrogen

The complexes [Co( tren )(P2O7H2)] (ClO4).H2O, [Co( tren )(P3010H3)] (ClO4) (tren = N,N-bis(2- aminoethyl )ethane-1,2-diamine) and [Co( cyclen )(P2O7H2)](ClO4)(cyclen = 1,4,7,10-tetraazacy-clododecane ) have been prepared and characterized. The complex [Co( tren )(P207H2)](C104).H20 crystallized in the monoclinic space group P21/n,a 10.655(3), b 14.675(5), c 11.260(4) � , β 98.49(3) for a single-crystal structure determination R was 0.041 for 4043 'observed' reflections. Despite the presence of a primary and a tertiary nitrogen donor in the plane of the cobalt and the phosphate oxygen donors, bond distances to Co-N(primary) and Co-N(tertiary) at 1.926(3) and 1.924(3) � respectively are equivalent, as are the Co-O distances of 1.940(2) and 1 .943(3) to the N(primary) and N(tertiary) respectively. Axial Co-N(primary) bonds (av. 1.952 A) are elongated compared with the in-plane N(primary), and the axial N-Co-N angle is distorted (171.6�). The hydrolysis of the diphosphate and triphosphate complexes at pH 7.3 in the presence of an assisting complex, [Co( tn )2(OH2)(OH)]2+ ( tn = propane-1,3-diamine) or [Co( tren )(OH2)(0H)]2+, was followed by 31P n.m.r. spectroscopy, and rate enhancements of up to about 104 compared with free polyphosphate were observed, with the diphosphato complexes being least sensitive to cleavage by added complex. Intermediates in which the polyphosphate bridges two metal centres are apparently involved; the inability of [Pd(en)(0H2)2]2+(en= 1,2-ethanediamine) to enhance cleavage is consistent with this, since this ion does not form complexes with polyphosphates. [Co( tren )(ATP)](ATP=adenosine triphosphate ) was also prepared but not isolated; assisted hydrolysis with [Co( tren )(OH2)(OH)]2+ is about 104 faster than unassisted hydrolysis of free ATP under similar conditions.

Synthesis and crystal structure analyses of tri-substituted guanidine-based copper(II) complexes

2021 ◽  
Vol 76 (3-4) ◽  
pp. 193-199
Author(s):  
Muhammad Said ◽  
Sadia Rehman ◽  
Muhammad Ikram ◽  
Hizbullah Khan ◽  
Carola Schulzke
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Molecular Structures ◽  
Hydroxyl Groups ◽  
Synthesis And Crystal Structure ◽  
Pyramidal Geometry ◽  
Tautomeric Forms ◽  
Square Planar ◽  
Nitrogen Donor ◽  
Square Pyramidal Geometry

Abstract Three guanidine-derived tri-substituted ligands viz. N-pivaloyl-N′,N″-bis-(2-methoxyphenyl)guanidine (L1), N-pivaloyl-N′-(2-methoxyphenyl)-N″-phenylguanidine (L2) and N-pivaloyl-N′-(2-methoxyphenyl)-N″-(2-tolyl)guanidine (L3) were reacted with Cu(II) acetate to produce the corresponding complexes. The significance of the substituent on N″ for the resulting molecular structures and their packing in the solid state has been studied with respect to the structural specifics of the corresponding Cu(II) complexes. The key characteristic of the guanidine-based metal complexation with Cu(II) is the formation of an essentially square planar core with an N2O2 donor set. As an exception, in the complex of L1, the substituent’s methoxy moiety also interacts with the Cu(II) center to generate a square-pyramidal geometry. The hydroxyl groups of the imidic acid tautomeric forms of L1–L3, in addition to N″, are also bonded to Cu(II) in all three complexes rather than the nitrogen donor of the guanidine motif.

Crystal structure of the anticancer drug carmustine determined by X-ray powder diffraction

2021 ◽  
pp. 1-3
Author(s):  
Carina Schlesinger ◽  
Edith Alig ◽  
Martin U. Schmidt
Keyword(s):  
Crystal Structure ◽  
Anticancer Drug ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Powder Diffraction Data ◽  
Orthorhombic Space Group ◽  
Commercial Sample ◽  
One Dimensional ◽  
X Ray ◽  
Hydrogen Bond Pattern

The structure of the anticancer drug carmustine (1,3-bis(2-chloroethyl)-1-nitrosourea, C5H9Cl2N3O2) was successfully determined from laboratory X-ray powder diffraction data recorded at 278 K and at 153 K. Carmustine crystallizes in the orthorhombic space group P212121 with Z = 4. The lattice parameters are a = 19.6935(2) Å, b = 9.8338(14) Å, c = 4.63542(6) Å, V = 897.71(2) ų at 153 K, and a = 19.8522(2) Å, b = 9.8843(15) Å, c = 4.69793(6) Å, V = 921.85(2) ų at 278 K. The Rietveld fits are very good, with low R-values and smooth difference curves of calculated and experimental powder data. The molecules form a one-dimensional hydrogen bond pattern. At room temperature, the investigated commercial sample of carmustine was amorphous.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

Komplexe des 1-Thia-4,7-diazacyclononans (L) mit Blei(II), Indium(III), Thallium(I) und (III) Kristallstruktur von [LPb][PbBr4] / Complexes of 1-Thia-4,7-diazacyclononane (L) with Lead(II), Indium(III), Thallium(I) and (III) Crystal Structure of [LPb][PbBr4]

1988 ◽  
Vol 43 (5) ◽  
pp. 567-570 ◽  
Author(s):  
Peter Hoffmann ◽  
Franz-Josef Hermes ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Lone Pair ◽  
Tridentate Ligand ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group

Abstract The reaction of 1-thia-4,7-diazacyclononane (C6H14N2S = L) with salts containing Tl(I) and (III), In(III) and Pb(II) ions yields 1:1 complexes, which can be crystallized as halide or Perchlorate salts. The structure of [LPb][PbBr4] (5) has been determined: Crystal data: orthorhombic, space group P212121, a = 853.2(6), b = 1000.1(4), c = 1860(1) pm, Z = 4. Pb2+ in the [LPb]2+ cation is seven-coordinated by the tridentate ligand and a square of four Br- ions. The Pb-S distance, 286.0(5) pm, is rather short, the lone pair stereochemically activ. The PbBr4- ions are polymeric with octahedrally coordinated lead(II) atoms.

Crystalline magnesium chloride–electron donor complexes: new support materials for Ziegler–Natta catalysts

2017 ◽  
Vol 46 (13) ◽  
pp. 4452-4460 ◽  
Author(s):  
V. H. Nissinen ◽  
I. O. Koshevoy ◽  
T. T. Pakkanen
Keyword(s):  
Crystal Structure ◽  
Structure Formation ◽  
Magnesium Chloride ◽  
Donor Ligands ◽  
Nitrogen Donor Ligands ◽  
Support Materials ◽  
Polymerization Catalyst ◽  
Nitrogen Donor ◽  
Crystal Structure Formation ◽  
Ziegler Natta Catalysts

Chelating oxygen and nitrogen donor ligands (1,2-dimethoxyethane, 1,3-dimethoxypropane, and N,N′-diethylethylenediamine) are found to dictate the crystal structure formation of MgCl2, the important support component of a polymerization catalyst.

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