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.

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.

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.

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 and molelcular structure of benzil bisthiosemicarbazonatocopper(II) and the antitumour mechanism of related compounds

1979 ◽  
Vol 57 (6) ◽  
pp. 603-607 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Annie Y. M. Tsang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atoms ◽  
Copper Coordination ◽  
Cell Dimensions ◽  
Phenyl Rings ◽  
The Mean ◽  
R Value ◽  
Related Compounds ◽  
Double Hydrogen ◽  
Coordination Plane

The crystal structure of benzil bisthiosemicarbazonatocopper(II) has been solved and refined to an R-value of 0.082. The dark red triclinic crystal has cell dimensions a = 960.8(4), b = 1090.7(6), c = 895.8(4) pm, α = 106.23°(4), β = 92.36°(7), γ = 99.50°(7), and belongs to space group [Formula: see text] with two molecules per cell. The measured and calculated densities are 1.571 and 1.568 g cm−3, respectively, using C16H14CuN6S2 (mol. wt. 417.99). The copper coordination is significantly non-planar. The five non-hydrogen atoms of each original thiosemicarbazide molecule lie close to planes set at a dihedral angle of 8.9°. The fold is away from the origin and the neighbouring molecule. Bond lengths to copper are: Cu—S(1) = 223.7(3), Cu—S(2) = 223.4(3), Cu—N(13) = 197.1(6), Cu—N(23) = 197.0(7) pm. The bond angles at the Cu atom are S(1)—Cu—S(2) = 108.62°(9), N(13)—Cu—N(23) = 81.1°(3), N(13)—Cu—S(1) = 85.1°(2), and N(23)—Cu—S(2) = 85.0°(2). The first and second phenyl rings are at 100.3° and 93.0° to the mean Cu coordination plane, which is at a perpendicular distance of 330 pm from a similar plane in the inverse molecule. Intermolecular double hydrogen bonding occurs at each side of the complex between the uncoordinated nitrogen atoms, thus linking the molecules into parallel ribbons.

scholarly journals Crystal structure oftrans-dichlorido(4-nitroaniline-κN1)(piperidine-κN)platinum(II)

2015 ◽  
Vol 71 (6) ◽  
pp. 644-646 ◽  
Author(s):  
Chi Nguyen Thi Thanh ◽  
Truong Hoang Van ◽  
Thong Pham Van ◽  
Ngan Nguyen Bich ◽  
Luc Van Meervelt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Title Complex ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
Hydrogen Bond Interactions ◽  
Square Planar ◽  
Benzene Rings ◽  
The Mean ◽  
Structure Inversion

In the title complex, [PtCl2(C5H11N)(C6H6N2O2)], the PtIImetal atom displays a slightly distortedtrans-PtN2Cl2square-planar coordination geometry. The dihedral angle between the mean plane of the benzene and piperidine rings is 89.03 (3)°. In the crystal structure, inversion dimers are formedviaN—H...Cl hydrogen-bond interactions, resulting in chains parallel to the [001] direction. The benzene rings within the chains show π–π stacking interactions [centroid-to-centroid distances of 3.801 (3) Å] and neighbouring chains interactviaN—H...O hydrogen bonds.

An X-Ray Structure Determination of the Twinned Crystals of Dinitrato-2,2′-dipyridylsilver(II)

1972 ◽  
Vol 50 (3) ◽  
pp. 315-323 ◽  
Author(s):  
G. W. Bushnell ◽  
M. A. Khan
Keyword(s):  
Silver Atom ◽  
Unit Cell ◽  
Planar Geometry ◽  
X Ray ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
The Mean ◽  
Unit Cell Dimensions

The crystal structure of dinitrato-2,2′-dipyridylsilver(II) has been solved and refined to an R-value of 0.070. Four circle diffractometer measurements were obtained from the twinned triclinic crystals. The unit cell dimensions at 22 °C are: a = 697.5 ± 0.2 pm, b = 999.4 ± 0.2 pm, c = 1032.2 ± 0.2 pm, α = 113.46 ± 0.02°, β = 100.71 ± 0.02°, γ = 95.28 ± 0.02°. The space group is [Formula: see text] (No. 2) with two molecules per unit cell. The density is 2.06 ± 0.04 g cm−3 (measured), 2.02 g cm−3 (calculated). The four shortest bond lengths to silver are: Ag—O(1), 214.8 ± 1.5 pm; Ag—O(4), 213.6 ± 1.5 pm; Ag—N(1), 212.4 ± 1.6 pm; Ag—N(2), 220.7 ± 1.6 pm. These four bonds are distorted from square planar geometry with the silver atom lying 19.90 ± 0.17 pm out of the mean plane of the other four atoms. There are also long bonds to the nitrato groups of neighboring molecules: Ag—O(1′), 275.3 ± 1.3 pm; Ag—O(2″), 276.3 ± 1.6 pm. Inclusion of these bonds gives a distorted octahedral silver coordination. Though predominantly unidentate, there is a slight tendency toward bidentate bonding in both nitrato ligands: Ag—O(2), 305.8 ± 1.4 pm; Ag—O(5), 295.0 ± 1.7 pm. O(2) and O(5) approach the convex side of the distorted square planar coordination. The deviation from planarity of the closely bonded square, and angular distortions in the above mentioned octahedral coordination can be rationalized by considering the silver as eight coordinate. The bonds to silver may be grouped 4:2:2 by length or 4:3:1 by angular disposition.

scholarly journals Crystal structure of bis[2-(1H-benzimidazol-2-yl)aniline]silver(I) nitrate

2015 ◽  
Vol 71 (9) ◽  
pp. 1058-1060 ◽  
Author(s):  
Yongtae Kim ◽  
Sung Kwon Kang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Rotation Axis ◽  
Ring System ◽  
Planar Geometry ◽  
Nitrate Anion ◽  
Inversion Center ◽  
Benzimidazole Ring ◽  
Square Planar ◽  
The Mean

In the cation of the title salt, [Ag(C13H11N3)2]NO3, the AgIatom lies on a crystallographic inversion center and is coordinated by four N atoms from two bidentate 2-(1H-benzimidazol-2-yl)aniline ligands in a distorted square-planar geometry. The Ag—N(aniline) bond [2.729 (2) Å] is significantly longer than the Ag—N(imidazole) bond [2.165 (1) Å]. In the ligand, the aniline ring is twisted by 37.87 (6)° from the mean plane of the benzimidazole ring system. The nitrate anion lies on a crystallographic twofold rotation axis which passes through the N atom and one of the O atoms. In the crystal, N—H...O hydrogen bonds link the components, forming a layer parallel to thebcplane.

The crystal structure of deuterated benzene

1987 ◽  
Vol 414 (1846) ◽  
pp. 47-57 ◽  
Keyword(s):  
Crystal Structure ◽  
Neutron Diffraction ◽  
Molecular Orbital Calculations ◽  
Bond Lengths ◽  
M 10 ◽  
Cell Dimensions ◽  
Experimental Errors ◽  
The Mean ◽  
Unit Cell Dimensions ◽  
Deuterated Benzene

The crystal structure of deuterated benzene has been refined by single-crystal neutron diffraction analysis at 15 and 123 K. The unit-cell dimensions were also measured at 52.6 and 80 K, and the thermalexpansion coefficients at all four temperatures were calculated. The molecules have C 3v symmetry with a small chair-distortion from D 6h , which is possibly significant for the carbon atoms and significant for the deuterium atoms. The mean observed bond lengths at 15 K [123 K] are C-C = 1.3972(5) Å [1.3940(9) Å] (1 Å = 10 -10 m = 10 -1 nm); C-D = 1.0864(7) Å [1.0838(10) Å]. When corrected for molecular libration, the corresponding rest values are 1.3980 Å [1.3985 Å]; 1.088 Å [1.088 Å]. Ab initio molecular orbital calculations at the MP-2/6-31G* level gave energy-optimized bond lengths of 1.395 and 1.087 Å for the isolated molecule at rest, in agreement with the corrected values from the crystal structure within the experimental errors.

An X-Ray Study of the Synthetic Intermediate 9-Cyano-1,10-Dimethyl-6-Ethylenedioxy-1-Octalin

1975 ◽  
Vol 53 (2) ◽  
pp. 192-194 ◽  
Author(s):  
Harry Lynton ◽  
Pik-Yuen Siew
Keyword(s):  
Crystal Structure ◽  
Total Synthesis ◽  
Direct Methods ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Ring Junction ◽  
Cell Dimensions ◽  
R Value ◽  
Synthetic Intermediate

The crystal structure of the synthetic intermediate, 9-cyano-1,10-dimethyl-6-ethy]enedioxy-1-octalin, C15H21O2N, was solved by direct methods. The compound crystallizes in the space group p21/c with cell dimensions a = 12.282(4), b = 7.144(3), c = 15.619(5) Å, β = 104.04(1)°. Refinement was carried out isotropically for hydrogen and anisotropically for non-hydrogen atoms using full matrix least squares to an R-value of 0.043 for 1669 observed reflections.This compound, which has a cis configuration at the octalin ring junction, is a precursor to a moiety of the alkaloid thelepogine. The cis conformation is essential for total synthesis of thelopogine by this route.

Crystallographic studies on neuroleptics of the benzocycloheptapyridoisoquinoline series. The crystal structure of butaclamol hydrobromide and the absolute configuration and crystal structure of dexclamol hydrobromide

1976 ◽  
Vol 54 (17) ◽  
pp. 2715-2722 ◽  
Author(s):  
P. H. Bird ◽  
F. T. Bruderlein ◽  
L. G. Humber
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atom ◽  
Membered Ring ◽  
Axial Position ◽  
Aromatic Rings ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Cell Dimensions ◽  
R Value ◽  
Hydroxy Groups

The compound butaclamol hydrobromide crystallizes in space group P21/c with cell dimensions; a = 14.38(3), b = 13.31(3), c = 12.07(3) Å, β = 101.64(8)°. The structure was solved by Patterson methods and non-hydrogen atoms have been refined isotropically using a full-matrix least-squares to an R value of 0.17 for 779 observed reflections.The compound dexclamol hydrobromide crystallizes in space group P212121 with a = 8.412(2), b = 24.392(7), c = 10.465(2) Å. Refinement of non-hydrogen atoms using isotropic thermal parameters and rigid aromatic rings converted at R = 0.090 using 1249 observed reflections, for the preferred enantiomorph, and R = 0.099 for the other enantiomorph.Both compounds have their hydroxy groups in the axial position, and both adopt conformations of the seven membered ring such that the C13b hydrogen atom experiences a flagpolebowsprit interaction with a hydrogen atom of C9.

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