The crystal structure of cis-chlorobis(triethylphosphine)phthalazineplatinum(II) tetrafluoroborate, [PtC](PEt3)2(phth)]BF4

1978 ◽  
Vol 56 (6) ◽  
pp. 878-883 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon
Keyword(s):  
Crystal Structure ◽  
Elevated Temperatures ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
Dissociative Mechanism ◽  
Interatomic Distances ◽  
Heterocyclic Ligand ◽  
Square Planar ◽  
Cell Dimensions

The crystal structure of cis-chlorobis(triethylphosphine)phthalazineplatinum(II) tetrafluoroborate has been determinee by single crystal X-ray diffraction and refined to an R-value of 0.076 for 1935 reflections. The cell dimensions are a = 1315.7(2), b = 2462.7(4), c = 899.6(3) pm, β = 104.99(2)°. The space group is P21/c with 4 molecules per unit cell, ρo = 1.593, ρc = 1.613 g cm−3. The structure is a square planar 4-coordinate platinum(II) complex with an angle of 80.0° between the plane of the phthalazine molecule and that of the coordination. Interatomic distances to platinum are Pt—Cl, 235.4(9); Pt—P(1), 225.2(8); Pt—P(2), 226.9(8); Pt—N(1), 208(3); and Pt—N(2), 297(3) pm, the phthalazine ligand being monodentate. The structure is compared to previous results and discussed in relation to variable temperature nmr studies of solutions, which show that the heterocyclic ligand exchanges its point of attachment to and fro between N(1) and N(2) by a dissociative mechanism at elevated temperatures.

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.

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 Crystal Structure of cis-Chlorobis(triethylphosphine)-1,10-phenanthrolineplatinum(II) fluoroborate, (PtCl(PEt3)2(phen))BF4, a Complex Containing Monodentate 1,10-Phenanthroline

1974 ◽  
Vol 52 (8) ◽  
pp. 1367-1376 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon ◽  
Masood A. Khan
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
Interatomic Distances ◽  
Square Planar ◽  
Cell Dimensions ◽  
Tetragonal Pyramidal ◽  
R Value ◽  
First Time

The crystal structure of cis-chlorobis(triethylphosphine)-1,10-phenanthrolineplatinum(II) fluoroborate has been determined and refined to an R-value of 0.051. The space group is P21/c and the cell dimensions are a = 0.9215(2), b = 1.1991(3), c = 2.6832(6) nm, β = 99.38(3)°, with 4 molecules per unit cell. The interatomic distances to Pt are: Pt—N(1), 213.7(19); Pt—N(2), 284.3(20); Pt—P(1), 223.9(7); Pt—P(2), 224.1(6); Pt—Cl, 236.1(6) pm.The coordination number and geometry is discussed in terms of 5-coordinate tetragonal pyramidal and 4-coordinate square planar models, the latter being regarded as the more acceptable.Monodentate o-phenanthroline is thus observed for the first time in the solid state. The structure of the complex in solution is discussed with the aid of conductance and nuclear magnetic resonance results which suggest the possibility of a novel fluxional system.

Reactions of "cyclen-" and "cyclam-phosphorane" with [Pt2Cl4(PEt3)2]. Monodentate and bidentate complexes and the crystal and molecular structure of [PtCl(PEt3)(cyclamPH)]Cl•CH2Cl2

1989 ◽  
Vol 67 (1) ◽  
pp. 48-53 ◽  
Author(s):  
David Eric Berry ◽  
Jane Browning ◽  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Alan Pidcock
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Simple Formula ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Square Planar ◽  
Coordination Plane

Reaction of "cyclamphosphorane" (cyclamPH) with [Pt2Cl4(PEt3)2] yields [PtCl(PEt3)(cyclamPH)]Cl. The complex crystallizes as a dichloromethane solvate in the monoclinic space group P21/n, with a = 13.877(3), b = 23.231(7), c = 8.295(2)Å, β = 91.86(4)°, and an X-ray diffraction study shows square planar platinum coordination in which the labile proton of cyclamPH has transferred from phosphorus to nitrogen and the ligand is attached via simple [Formula: see text] chelation. The phosphorus is trans to chlorine in the platinum coordination plane.The corresponding product, trans-[PtCl2(PEt3)(cyclenPH2)]Cl, derived from reaction of "cyclenphosphorane" (cyclenPH) with [Pt2Cl4(PEt3)2], is shown by NMR studies to have a quite different structure in which the ligand is protonated at two nitrogen sites but not at phosphorus. The phosphorus is pentacoordinate with four attachments to nitrogen atoms and one to platinum. The two chlorine atoms are mutually trans in the platinum coordination plane. Keywords: crystal structure, cyclenphosphorane reaction, cyclamphosphorane reaction, X-ray diffraction.

The crystal structure of a dinuclear platinum(II) complex with a bent dihydroxy bridge, di-(μ-hydroxy)tetrakis(triethylphosphine)diplatinum(II).tetrafluoroborate

1978 ◽  
Vol 56 (13) ◽  
pp. 1773-1778 ◽  
Author(s):  
G. W. Bushnell
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atoms ◽  
Interatomic Distances ◽  
Partial Structures ◽  
Square Planar ◽  
Dinuclear Platinum ◽  
Cell Dimensions ◽  
Open Side ◽  
The Mean ◽  
Platinum Species

The crystal structure of di-(μ-hydroxo)tetrakis(triethylphosphine)diplatinum(II)fluoroborate has been determined and refined to an R value of 0.032. The space group is P21/c and the cell dimensions are a = 1.604(1), b = 1.847(1), c = 1.336(1) nm, β = 101.6 °, with 4 molecules per unit cell. The dimeric cation consists of two square planar Pt(II) centres bridged by a pair of hydroxo ligands. The angle between the mean plane normals is 36.4°. One of the BF4− groups, situated close to the dihydroxo bridge on the more open side, and having lower thermal parameters than the second fluoroborate anion, is hydrogen bonded to the oxygen atoms. The hydrogen atoms were not located. The interatomic distances (pm) are Pt—P = 223.5 (mean), Pt—O = 213.3 (mean), Pt(1)—Pt(2) = 312.1(1), O(1)—O(2) = 272(2), O(1)—F(1) = 288(2), O(2)—F(2) = 282(3). The mean bond angles (deg) are O—Pt—O = 79.4, P—Pt—P = 97.7, P—Pt—O = 91.5, and Pt—O—Pt = 94. One of the triethylphosphine groups is disordered or in thermal motion and was refined by constrained least squares using two superimposed partial structures. The results are discussed in relation to other known hydroxo bridged platinum species relevant to the field of platinum containing, cancer chemotherapeutic drugs.

Synthesis, structural and magnetic properties of macrocyclic aza-amido binuclear copper(II) complexes

1989 ◽  
Vol 67 (4) ◽  
pp. 662-670 ◽  
Author(s):  
Sanat K. Mandal ◽  
Laurence K. Thompson ◽  
Michael J. Newlands ◽  
Amal K. Biswas ◽  
Bibhutosh Adhikary ◽  
...  
Keyword(s):  
Variable Temperature ◽  
Complex Iii ◽  
Azomethine Nitrogen ◽  
X Ray Diffraction ◽  
Binuclear Copper ◽  
Magnetic Studies ◽  
Monoclinic System ◽  
Space Group ◽  
Pyramidal Geometry ◽  
Square Planar

Binuclear, antiferromagnetically coupled, macrocyclic copper(II) complexes, [Cu2(C28H32N4O4)]•H2O (II) and [Cu2(C36H32N4O4)]•CH3CN•H2O (III), involving asymmetric ligands with two deprotonated amide, two azomethine nitrogen, and two phenoxide donors at the binuclear centre, have been synthesized and characterized by single-crystal X-ray diffraction and variable temperature magnetic studies. Complex II crystallizes in the monoclinic system, space group P21/n, with a = 16.4854(9) Å, b = 7.6005(13) Å, c = 21.1617(11) Å, β = 104.090(5)°, Z = 4, Rf = 0.068 for 2062 significant reflections. The two copper(II) centres have square planar N2O2 donor sets with two phenoxide oxygen atoms bridging the copper centres with a copper–copper separation of 2.898(2) Å. A long copper–oxygen (amide) contact (2.808(10) Å) forms a weak dimer association. Complex III crystallizes in the triclinic system, space group [Formula: see text], with a = 8.7771(9) Å, b = 12.3983(16) Å, c = 15.7299(16) Å, α = 85.003(11)°, β = 84.574(8)°, γ = 76.838(10)°, Z = 2, Rf = 0.041 for 2966 significant reflections. The two copper(II) centres have distorted square-pyramidal geometry involving an N2O2 in plane donor set and two phenoxide oxygen bridges with a copper–copper separation of 3.018(1) Å. The fifth coordination site at each copper centre involves an amide oxygen from a neighbouring molecule (Cu(1)—O 2.371(4), Cu(2)—O 2.413(3) Å) in a staggered intermolecular array. Very strong antiferromagnetic exchange is observed in both cases (−2J = 689 ± 7 cm−1 (II), −2J = 816 ± 8 cm−1 (III)). Keywords: macrocycles, binuclear copper(II) complexes.

scholarly journals Investigation of Solvatomorphism and Its Photophysical Implications for Archetypal Trinuclear Au3(1-Methylimidazolate)3

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4404
Author(s):  
Shengyang Guan ◽  
David C. Mayer ◽  
Christian Jandl ◽  
Sebastian J. Weishäupl ◽  
Angela Casini ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Density Functional ◽  
Bulk Material ◽  
Variable Temperature ◽  
Active Phase ◽  
Solvent Free ◽  
X Ray Diffraction ◽  
X Ray ◽  
Aurophilic Interactions

A new solvatomorph of [Au3(1-Methylimidazolate)3] (Au3(MeIm)3)—the simplest congener of imidazolate-based Au(I) cyclic trinuclear complexes (CTCs)—has been identified and structurally characterized. Single-crystal X-ray diffraction revealed a dichloromethane solvate exhibiting remarkably short intermolecular Au⋯Au distances (3.2190(7) Å). This goes along with a dimer formation in the solid state, which is not observed in a previously reported solvent-free crystal structure. Hirshfeld analysis, in combination with density functional theory (DFT) calculations, indicates that the dimerization is generally driven by attractive aurophilic interactions, which are commonly associated with the luminescence properties of CTCs. Since Au3(MeIm)3 has previously been reported to be emissive in the solid-state, we conducted a thorough photophysical study combined with phase analysis by means of powder X-ray diffraction (PXRD), to correctly attribute the photophysically active phase of the bulk material. Interestingly, all investigated powder samples accessed via different preparation methods can be assigned to the pristine solvent-free crystal structure, showing no aurophilic interactions. Finally, the observed strong thermochromism of the solid-state material was investigated by means of variable-temperature PXRD, ruling out a significant phase transition being responsible for the drastic change of the emission properties (hypsochromic shift from 710 nm to 510 nm) when lowering the temperature down to 77 K.

The molecular and crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2

1979 ◽  
Vol 57 (1) ◽  
pp. 57-61 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Least Squares ◽  
Platinum Atom ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
Square Planar ◽  
Coordination Plane

The crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 12.486(6), b = 13.444(7), c = 14.678(11) Å, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.050 and a weighted Rw = 0.045.The coordination around the platinum atom is square planar. Guanosine is bonded to platinum through N(7). The purine planar ring makes an angle of 62.7° with the platinum coordination plane. The structure is stabilized by hydrogen bonding.

scholarly journals Ba5(IO6)2: crystal structure evolution from room temperature to 80 K

2021 ◽  
Vol 77 (6) ◽  
pp. 634-637
Author(s):  
David Wenhua Bi ◽  
Priya Ranjan Baral ◽  
Arnaud Magrez
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Structural Transition ◽  
Rietveld Method ◽  
Structural Parameters ◽  
Structure Evolution ◽  
X Ray Diffraction ◽  
Lattice Contraction ◽  
Interatomic Distances ◽  
Crystallographic Axes

The crystal structure of Ba5(IO6)2, pentabarium bis(orthoperiodate), has been re-investigated at room temperature based on single-crystal X-ray diffraction data. In comparison with a previous crystal structure determination by the Rietveld method, an improved precision of the structural parameters was achieved. Additionally, low-temperature measurements allowed the crystal structure evolution to be studied down to 80 K. No evidence of structural transition was found even at the lowest temperature. Upon cooling, the lattice contraction is more pronounced along the b axis. This contraction is found to be inhomogeneous along different crystallographic axes. The interatomic distances between different Ba atoms reduce drastically with lowering temperature, resulting in a closer packing around the IO6 octahedra, which remain largely unaffected.

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

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