Platinum(II) Template Synthesis of a Pendant-Arm Macrocycle

1998 ◽  
Vol 51 (9) ◽  
pp. 871 ◽  
Author(s):  
Hong Xiao ◽  
Geoffrey A. Lawrance ◽  
Trevor W. Hambley
Keyword(s):  
Crystal Structure ◽  
Template Synthesis ◽  
Crystal Structure Analysis ◽  
Macrocyclic Complex ◽  
Triclinic Space Group ◽  
X Ray ◽  
Pendant Arm ◽  
Major Isomer ◽  
Square Planar ◽  
R Value

Platinum(II)-directed condensation of ethane-1,2-diamine with nitroethane and formaldehyde yields the colourless macrocyclic complex (trans-6,13-dimethyl-6,13-dinitro-1,4,8,11-tetraazacyclotetradecane)plat- inum(II), [Pt(1)]2+, in good yield. This parallels chemistry reported earlier around other triad members nickel(II) and palladium(II). The pendant nitro groups in the major isomer are disposed on opposite sides of the macrocycle in a trans geometry, as confirmed by the X-ray crystal structure analysis of [Pt(1)] (ClO4)2, which crystallizes in the triclinic space group P-1, a 8·041(4), b 8·482(4), c 9·443(3) Å, α 69·44(3), β 67·66(4), γ 71·73(4)°,Z1, and was refined to an R value of 0·027 on 1920 F. The platinum ion lies in a square planar environment of four nitrogen donors, with typical Pt–N distances; comparisons between the platinum(II) and palladium(II) complexes of (1) and its analogue (2), with diammonio groups in place of dinitro groups, are discussed

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Synthesis, Crystal Structure and Magnetic Properties of a (μ-Hydroxo)(μ-Pyrazolato) Dicopper(II) Complex

2000 ◽  
Vol 55 (9) ◽  
pp. 796-802 ◽  
Author(s):  
H. Kara ◽  
Y. Elerman ◽  
K. Prout
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Variable Temperature ◽  
Powdered Sample ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Present Complex ◽  
Square Planar ◽  
Super Exchange Interaction

Preparation and magnetic properties of a 3,5-dimethylpyrazolate bridged binuclear copper(II) complex [Cu2(L)(3 ,5 -pyz)] (L = 1,3-Bis(2-Hydroxy-5-Chlorosalicylideneamino)propan- 2-ol) is reported. The crystal structure determined by X-ray diffraction methods. (C22H20N4O3CI2CU2), triclinic, space group P1̄, a = 9.622(3), b = 10.921(2), c = 11.420(3) Å, α = 100.73(2), β = 94.04(2), Υ = 108.08(2)°, V = 1110.2(5) Å3, Z = 2. Two copper(II) ions in a square-planar coordination are bridged via alkoxide oxygen and 3,5-dimethyl pyrozolate nitrogen atoms to form a dinuclear unit. The metal coordination sphere is four-coordinate, planar with an N2O2 donor set. The dihedral angle between the two coordination planes is 166.83°. There are significant intermolecular interactions between neighbouring binuclear entities. The shortest intermolecular Cu (1) ... Cu(1)i distance is 3.383(1) Å and the Cu(1) - O ( 1)i distance is 2.666(3) Å (i = 1 -x, -y, 1 - z). The variable-temperature magnetic susceptibility measurement for a powdered sample of the complex was carried out in the temperature range 5 - 350 K and analysed to obtain values of the parameter J in the exchange Hamiltonian ℋ = -2JScu Scu; 2J = -164 cm-1. The magnetic moment at 300 K is about 2.42 μB, and 0.22 μB at 5 K. The weak antiferromagnetism of the present complex is reasonably explained in terms of the orbital countercomplementary effect based on Hoffmann's theory for super-exchange interaction

The Dichloroplatinum(II) Complex of 5,5,7-Trimethyl-1,4-diazacycloheptane: Preparation, Crystal Structure and Binding to Nucleotides and DNA

1998 ◽  
Vol 51 (11) ◽  
pp. 977 ◽  
Author(s):  
Chih-Lynne Teo ◽  
Ronald R. Fenton ◽  
Peter Turner ◽  
Trevor W. Hambley
Keyword(s):  
Crystal Structure ◽  
Dna Binding ◽  
Molecular Mechanics ◽  
X Ray Diffraction ◽  
Binding Studies ◽  
Triclinic Space Group ◽  
X Ray ◽  
Dna Binding Studies ◽  
Total Dna ◽  
R Value

The preparation of [Pt(tmdz)Cl2] (tmdz = 5,5,7-trimethyl-1,4-diazacycloheptane) is described. The crystal structure has been determined by X-ray diffraction methods and refined to an R value of 0·048 (764F). The crystals are triclinic, space group P -1, a 8·023(2), b 10·874(4), c 14·207(3) Å, α 95·34(3), β 94·96(2), γ 94·97(3)°. N.m.r. studies and molecular mechanics methods show that only one diastereomer of the complex—that observed in the crystal structure—is energetically accessible. In total DNA binding studies, [Pt(tmdz)Cl2] binds less effectively and at a lower rate than cisplatin. The complex reacts with dG and d(GpG) to form a variety of isomeric products, as indicated by h.p.l.c. analysis.

Preparation and Crystal Structure of a Mixed Metal Assembly [Ni(phen)3][Cu(H-1pap)]2(NO3) · 8 H2O Featuring Octahedral Cationic and Square-planar Anionic Modules

2000 ◽  
Vol 55 (10) ◽  
pp. 966-970 ◽  
Author(s):  
Igor O. Fritsky ◽  
Jolanta Świątek-Kozlowska ◽  
Anatoliy A. Kapshuk ◽  
Henryk Kozłowski ◽  
Tatiana Yu. Sliva ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Water Molecules ◽  
Aromatic Rings ◽  
Triclinic Space Group ◽  
X Ray ◽  
Mixed Metal ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Different Types ◽  
Nitrate Anions

AbstractThe new mixed metal assembly [Ni(phen)3][Cu(H-1pap)]2(NO3 ) · 8 H2O (2) (H2pap = CH3- C(=NO H)-C(O )-NH-(CH2)3-NH-C(O )-C(=NOH)-CH3) was obtained by co-crystallisation of [Li(H2O)4][Cu(H-1pap)] · 2 H2O (1) and tris(1,10-phenanthroline)nickel(II) nitrate and studied by means of X-ray crystallography (triclinic, space group P1, a = 13.471(3), b = 13.641(3), c = 15.401(3) Å, α = 108.21(3), β = 97.73(3), γ = 107.74(3)°, V = 2476.6(9) Å , Z = 2 ,R1 = 0.0677 for 4672 unique reflections with I > 2σ(I)). The assembly indicates a network structure and consists of isolated cationic and anionic modules (octahedral [Ni(phen)3]2+ and square-planar [Cu(H-1pap)]-), non-coordinated nitrate anions and solvating water molecules. The elements of the crystal structure are linked by interactions of different types: by an extended system of H bonds, stacking interactions between aromatic rings, long apical Cu-N contacts and specific π-π interaction between a deprotonated oxime group of the complex anion and a phenanthroline ligand

Transition Metal Complexes of Derivatized Chiral Dihydro-1,2,4-triazin-6-ones. Part III [1]. X-Ray Crystal Structure Analysis of N,N’-Bis[(1-phenyl-5-isopropyl-4,5-dihydro-6-oxo-1,2,4-triazin-3-yl)ethylidene]- propane-1,3-diamine Nickel(II)

2000 ◽  
Vol 55 (11) ◽  
pp. 1074-1078 ◽  
Author(s):  
Ahmad S. Abushamleh ◽  
Mustafa M. El-Abadelahb ◽  
Wolfgang Voelter
Keyword(s):  
Crystal Structure ◽  
Transition Metal ◽  
Transition Metal Complexes ◽  
Structure Determination ◽  
Nickel Complex ◽  
Crystal Structure Analysis ◽  
High Yield ◽  
X Ray ◽  
Square Planar ◽  
Template Reaction

Template reaction of L-3-acetyl-1-phenyl-5-isopropyl-4,5-dihydro-1,2,4-triazin-6-one (lb) with 1,3-diaminopropane and nickel acetate gave the corresponding chiral complex 4 in high yield. X-ray structure determination showed that the nickel complex is square planar, and the ligand N,N’-bis[(l-phenyl-5-isopropyl-4,5-dihydro-6-oxo-1,2,4-triazin-3-yl)ethylid-ene]- propane-1,3-diamine is of tetra-aza type where the imine nitrogens and the ring HN(4) nitrogens are the coordinating sites. MS-FAB and NMR spectral data are in agreement with the X-ray structure.

The crystal structure of cis-chlorobis(triethylphosphine)-1,8-naphthyridineplatinum(II) tetrafluoroborate, [PtCl(PEt3)2(naph)]BF4, a complex containing a monodentate 1,8-naphthyridine ligand

1978 ◽  
Vol 56 (4) ◽  
pp. 450-455 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon ◽  
Masood A. Khan
Keyword(s):  
Crystal Structure ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
Interatomic Distances ◽  
X Ray ◽  
Heterocyclic Ligand ◽  
Square Planar ◽  
Cell Dimensions ◽  
R Value

The crystal structure of cis-chlorobis(triethylphosphine)-1,8-naphthyridineplatinum(II) tetrafluoroborate has been determined by single crystal X-ray diffraction and refined to an R-value of 0.063. The cell dimensions are a = 1.4246, b = 1.2676, c = 1.6530 nm, β = 115.66°. The space group is P21/c with 4 molecules per unit cell, and the measured density is 1.665 g cm−3. The structure is essentially a 4-coordinate square planar platinum(II) complex containing monodentate 1,8-naphthyridine. Interatomic distances to platinum are: Pt—Cl, 236.6(4); Pt—P(1), 225.4(4); Pt—P(2), 225.2(4); Pt—N(1), 208.3(11); and Pt—N(2), 304.5(14) pm. The structure is discussed in relation to variable temperature nmr studies of solutions, which indicate fluxional behaviour of the heterocyclic ligand.

Davidlloydite, ideally Zn3(AsO4)2(H2O)4, a new arsenate mineral from the Tsumeb mine, Otjikoto (Oshikoto) region, Namibia: description and crystal structure

2012 ◽  
Vol 76 (1) ◽  
pp. 45-57 ◽  
Author(s):  
F.C. Hawthorne ◽  
M. A. Cooper ◽  
Y. A. Abdu ◽  
N. A. Ball ◽  
M. E. Back ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Optical Properties ◽  
Direct Methods ◽  
Crystal Structure Analysis ◽  
Width Ratio ◽  
Calculated Density ◽  
Triclinic Space Group ◽  
X Ray ◽  
Fine Grained ◽  
Mohs Hardness

AbstractDavidlloydite, ideally Zn3(AsO4)2(H2O)4, is a new supergene mineral from the Tsumeb mine, Otjikoto (Oshikoto) region, Namibia. It occurs as elongated prisms (∼10:1 length-to-width ratio) that are flattened on {010}, and up to 100 × 20 × 10 μm in size. The crystals occur as aggregates (up to 500 μm across) of subparallel to slightly diverging prisms lying partly on and partly embedded in fine-grained calcioandyrobertsite. Crystals are prismatic along [001] and flattened on {010}, and show the forms {010} dominant and {100} subsidiary. Davidlloydite is colourless with a white streak and a vitreous lustre; it does not fluoresce under ultraviolet light. The cleavage is distinct on {010}, and no parting or twinning was observed. The Mohs hardness is 3 – 4. Davidlloydite is brittle with an irregular to hackly fracture. The calculated density is 3.661 g cm–3. Optical properties were measured with a Bloss spindle stage for the wavelength 590 nm using a gel filter. The indices of refraction are α = 1.671, β = 1.687, γ = 1.695, all ±0.002; the calculated birefringence is 0.024; 2Vobs = 65.4(6)°, 2Vcalc = 70°; the dispersion is r < v, weak; pleochroism was not observed. Davidlloydite is triclinic, space group P1, with a = 5.9756(4), b = 7.6002(5), c = 5.4471(4) Å, α = 84.2892(9), β = 90.4920(9), γ = 87.9958(9)°, V = 245.99(5) Å3, Z = 1 and a:b:c = 0.7861:1:0.7167. The seven strongest lines in the X-ray powder diffraction pattern [listed as d (Å), I, (hkl)] are as follows: 4.620, 100, (011, 10); 7.526, 71, (010); 2.974, 49, (200, 01); 3.253, 40, (021, 120); 2.701, 39, (10, 002, 1); 5.409, 37, (001); 2.810, 37, (210). Chemical analysis by electron microprobe gave As2O5 43.03, ZnO 37.95, CuO 5.65, H2O(calc) 13.27, sum 99.90 wt.%. The H2O content and the valence state of As were determined by crystal structure analysis. On the basis of 12 anions with H2O = 4 a.p.f.u., the empirical formula is (Zn2.53Cu0.39)Σ2.92As2.03O8(H2O)4.The crystal structure of davidlloydite was solved by direct methods and refined to an R1 index of 1.51% based on 1422 unique observed reflections collected on a three-circle rotating-anode (MoKα radiation) diffractometer equipped with multilayer optics and an APEX-II detector. In the structure of davidlloydite, sheets of corner-sharing (As5+O4) and (ZnO4) tetrahedra are linked by ZnO2(H2O)4 octahedra. The structure is related to that of parahopeite.

Crystal Structure of Cs2 [Pt(CN)4] · H2O

1977 ◽  
Vol 32 (2) ◽  
pp. 127-130 ◽  
Author(s):  
H. H. Otto ◽  
Heinz Schulz ◽  
K. H. Thiemann ◽  
H. Yersin ◽  
G. Gliemann
Keyword(s):  
Crystal Structure ◽  
Optical Emission ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
R Value ◽  
The Given ◽  
Emission Studies ◽  
Atomic Coordinates

The crystal structure of Cs2[Pt(CN)4] · H2O has been determined from X-ray diffraction data and refined to a conventional R value of 0.068 from 2210 reflections. The compound is hexagonal, α = 9.687(2) and c = 19.336(6) A, space group C62-P 61, Z = 6. The given atomic coordinates represent the absolute configuration. The nearly square planar Pt(CN)42- groups form a helix with respect to the c axis. The distance between neighbouring Pt atoms in the helix is 3.543(1) A. The normal of the Pt(CN)42- group is tilted about 15 deg to the c axis leading to a considerable overlap of metal orbitals which is suggested from optical emission studies. The protons of the water molecules form hydrogen bonds to nitrogen atoms of different helices. Both Cs atoms have similar sevenfold coordination.

Organoamidometallics. V. Syntheses of [N,N-diethyl-N'-polyfluorophenyl-ethane-1,2-diaminato(1-)]platinum(II) Complexes by Decarboxylation Reactions, and the X-Ray Crystal Structure of trans-[Pt(NC6F5CH2CH2Net2)I(Py)]

1991 ◽  
Vol 44 (12) ◽  
pp. 1669 ◽  
Author(s):  
GB Deacon ◽  
BM Gatehouse ◽  
J Ireland
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Spectroscopic Data ◽  
Coupling Constants ◽  
Methyl Groups ◽  
Triclinic Space Group ◽  
Double Bond Character ◽  
X Ray ◽  
Square Planar ◽  
Bond Character

From reactions between PtX2( deen ) (X=I, Br or Cl ; deen = N,N-diethylethane-1,2-diamine), thallous pentafluorobenzoate or 2,3,5,6-tetrafluorobenzoate, and the appropriate polyfluorobenzene in pyridine (py) or 4-methylpyridine ( mepy ), the organoamidoplatinum (II) complexes [Pt(NRCH2CH2Net2)X(L)](R = p-HC6F4 or C6F5, X = 1, Br or Cl , L = py; R = p-HC6F4, X = I, L = mepy ; R = p-MeC6F4 or p-IC6F4, X = I, L = py; R = 2,3,5-F3C6H2, X = Br, L = py) have been prepared. The X-ray crystal structure of [Pt(NC6F5CH2CH2Net2)I(py)](triclinic, space group Pī (No. 2), a 9.308(1), b 9.615(2), C 11.143(2)Ǻ, α 88.70(2),β 88.58(1), γ 89.60(2)°, R 0.0518, Rw 0.0704 for 3237 observed reflections) shows the complex to have square planar stereo-chemistry with py trans to NEt2 and NC6F5 trans to iodine. The stereochemistry of the amido nitrogen approaches triangular (sum of angles 353°) and the N-C6F5 bond has partial double-bond character. Surprisingly, the ethyl substituents have a configuration in which the methyl groups are orientated back towards platinum. Other [Pt(NRCH2CH2Net2)X(L)] complexes are considered to have similar stereochemistry on the basis of comparison of spectroscopic data, particularly 3JPt,H(py) and 3JPt,H(CH2) coupling constants.

Isolation, X-Ray Crystal Structure and 59Co Nuclear Magnetic Resonance Spectral Investigation of the Partially Nitrated Cobalt(III) Acetylacetonato Complex [Co(acac)2(NO2acac)]

1992 ◽  
Vol 45 (5) ◽  
pp. 797 ◽  
Author(s):  
TG Appleton ◽  
LR Gahan ◽  
PJ Oliver
Keyword(s):  
Crystal Structure ◽  
Chelate Ring ◽  
Cobalt Atom ◽  
Relaxation Rates ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
X Ray ◽  
Oxygen Oxygen ◽  
R Value ◽  
Discrete Complex

The complex [Co( acac )2(NO2acac)] has been isolated after fractional crystallization from a reaction mixture of [Co( acac )3] and nitrating agent. The complex crystallizes in the triclinic space group P1, with c 14.557(2) � , α 78.98(1), β 83.71(2), γ75.32(1)° and Z 2. The structure refined to a final R value of 0.074 for 2287 'observed' [I > 3 σ(I)] reflections. The structure consists of discrete complex molecules with the cobalt atom surrounded by six oxygen atoms at the corners of a distorted octahedron. The NO2 group is twisted at 50.7� to the chelate ring on which it is situated and has little influence on the geometry, with intrachelate and interchelate oxygen-oxygen separations essentially the same as those found in [Co( acac )3]. The 59Co n.m.r. spectra of the [Co( acac )2(NO2acac)] complex, as well as [Co( acac )3], [Co(NO2acac)3] and [Co( acac )(NO2acac)2], have been recorded, this resonance being particularly sensitive to substitution on they γcarbon atom of the acetylacetonato chelate ring. The 59CO relaxation rates for the [Co( acac )2(NO2acac)] and [Co( acac )(NO2acac)2] complexes are faster than that displayed by the symmetric [Co(NO2acac)3] complex, (1948 � 20, 2765 � 30 and 1696 � 20 s-1, respectively). The results obtained for the relaxation rates for these complexes are compared with those obtained for similar halide-substituted complexes [Co( acac )3-n( Xacac )n] � (X = Cl , Br, I; n = 0-3).

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