Triorganophosphinegold(I) Carbonimidothioates

1993 ◽  
Vol 46 (4) ◽  
pp. 561 ◽  
Author(s):  
VJ Hall ◽  
G Siasios ◽  
ERT Tiekink
Keyword(s):  
Spectroscopic Data ◽  
Gold Atom ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Thiolate Ligand ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The title compounds, R3PAuSC(= NPh )OR′, R = Et, Ph or Cy and R′ = Me, Et, Pr, Pri or Cy, have been prepared and characterized by spectroscopic methods ( i.r., 1H and 13C n.m.r. and f.a.b . m.s .) and, in the case of the R = Ph and R′ = Me compound, by single-crystal X-ray diffraction methods. The spectroscopic data are consistent with the R3PAu moiety being coordinated by the sulfur atom of the thiolate ligand. This has been confirmed by an X-ray study on Ph3PAuSC(= NPh )OMe which shows the gold atom to be linearly coordinated by the phosphorus and sulfur atoms; Au-P(1) 2.258(1), Au-S(1) 2.301(1) Ǻ and P-Au-S 177.7(1)°. Crystals of Ph3PAuSC(= NPh ) OMe are triclinic, space group pī, with unit cell dimensions: a 10.825(1), b 12.553(2), c 8.914(2) Ǻ, α 97.86(2), β 93.79(1), γ 88.60(1)°, V 1197.1 Ǻ3, Z 2. The structure was refined by a full-matrix least-squares procedure to R 0.028 for 4409 reflections with I ≥ 2.5σ(I).

Phosphinegold(I) Complexes Containing the Purine-6-thiolate Anion, and Their Antiarthritic Activity

1994 ◽  
Vol 47 (4) ◽  
pp. 577 ◽  
Author(s):  
PD Cookson ◽  
ERT Tiekink ◽  
MW Whitehouse
Keyword(s):  
Spectroscopic Data ◽  
Gold Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Thiolate Ligand ◽  
Cell Dimensions ◽  
Ethanol Solvate ◽  
Thiolate Anion ◽  
Unit Cell Dimensions

A series of complexes of the general formulae R3PAu(6-mp), R3P = Et3P, Ph3P, Cy3P, PhMe2P, (o-tol)3P, (m-tol)3P or (p-tol)3P, (AuCl)Ph2P(CH2)nPPh2(Au(6-mp)), n = 2 or 3, and Ph2P(CH2)nPPh2(Au(6-mp))2, n = 1, 2 or 3 and 6-mp is the anion derived from 6-mercaptopurine (purine-6-thiol), have been prepared and characterized by spectroscopic methods (i.r., 1H, 13C, 31P n.m.r. and f.a.b. m.s.) and, in the case of the Ph3PAu(6-mp) complex, by single-crystal X-ray diffraction methods. The spectroscopic data show that the 6-mp ligand coordinates as a thiolate ligand and that the gold atoms exist in linear P-Au-S (or P-Au-Cl) geometries. This has been confirmed by an X-ray study on Ph3PAu(6-mp), isolated as an ethanol solvate; the study shows the gold atom to be linearly coordinated by the phosphorus and sulfur atoms: Au-P(1) 2.237(2), Au-S(6) 2.287(1) Ǻ and P-Au-S 173.71(6)°. Crystals of Ph3PAu(6-mp).EtOH are triclinic, space group Pī, with unit cell dimensions a 11.066(3), b 13.552(3), c 8.705(2) Ǻ, α 91.51(2), β 113.06(2), γ 89.69(2)°, V 1200.8(5) Ǻ3, Z 2. The structure was refined by a full-matrix least-squares procedure to R 0.034 for 3978 reflections with I ≥ 3.0σ(I). Preliminary results of testing for antiarthritic activity among the new complexes in rats are also reported showing that some of them are more potent/less toxic than current gold(I) thiolates used clinically.

Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XL. X-Ray Crystal Structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru, Os)

1995 ◽  
Vol 48 (11) ◽  
pp. 1887 ◽  
Author(s):  
MI Bruce ◽  
PJ Low ◽  
BW Skelton ◽  
ERT Tiekink ◽  
A Werth ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Chloro Complexes ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru and Os) have been determined. A revised synthesis of the bromo osmium complex is given. The coordination geometry about the metal atom is based on a distorted octahedron with one face being occupied by the cyclopentadienyl group [average Ru -C(Cp) 2.214(3), Os-C(Cp) 2.177(3)Ǻ] and the other by the bromide [ Ru -Br 2.5683(8), Os-Br 2.5438(9)Ǻ] and the two phosphorus atoms [ Ru -P 2.323(2), 2.329(1); Os-P 2.290(2), 2.297(2)Ǻ]. Structural parameters are compared with those of the corresponding chloro complexes and differ only minimally. Crystals of MBr (PPh3)2(η-C5H5).CH2Cl2 are triclinic, space group Pī , with unit cell dimensions ( Ru [Os]): a 14.374(5) [14.276(4)], b 14.057(4) [13.959(3)], c 10.012(5) [9.903(3)]Ǻ, α 99.43(3) [99.79(2)], β 105.60(3) [105.74(2)], γ 100.42(3) [100.39(2)]°, V 1868(1) [1817.7(9)] Ǻ3, Z 2. The structures were refined by a full-matrix least-squares procedure to R 0.050 [0.036] for 7365 [5108] reflections with I ≥ 3σ(I).

Cluster Chemistry. XLVII. X-Ray Crystal Structure of OsPt2(μ-CO)3(CO)2(PPh3)3

1986 ◽  
Vol 39 (12) ◽  
pp. 2145 ◽  
Author(s):  
MI Bruce ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
Metal Metal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Triphenylphosphine Ligand

The crystal structure of OsPt2(μ-CO)3(CO)2(PPh3)3 has been determined by single-crystal X-ray diffraction techniques. Crystals are triclinic, space group Pī with unit cell dimensions a 13.593(4), b 15.839(4), c 12.633(8) Ǻ, α 102.97(3), β 108.18(2), γ 84.86(3)° with Z2. The structure was refined by a full-matrix least-squares procedure on 5896 reflections [I ≥ 2.5σ(I)] to final R 0.028 and Rw 0.034. A triphenylphosphine ligand binds each of the metal atoms disposed at the corners of a triangle. Each metal-metal bond is spanned by a bridging carbonyl group. The coordination about the osmium atom is completed by two terminal carbonyl groups.

The Preparation, Spectroscopic Characterization and X-Ray Structure of the Salt [Pt(η1 -C6H9)(Cy2PCH2CH2PCy2)(PPh3)]HCO3·3H2O Containing the Discrete, Uncoordinated, Hydrogen-Bonded Dimeric Bicarbonate Dianion [(HCO3)(H2O)3]22-

1999 ◽  
Vol 52 (10) ◽  
pp. 949 ◽  
Author(s):  
Martin A. Bennett ◽  
Glen B. Robertson ◽  
Pramesh N. Kapoor
Keyword(s):  
Low Temperature ◽  
Spectroscopic Characterization ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
R Value ◽  
Unit Cell Dimensions ◽  
Hydrogen Bonded

Reaction of the cyclohexyne–platinum(0) complex [Pt(η2-C6H8)(Cy2PCH2CH2PCy2)]* with water and CO2 in the presence of triphenylphosphine gives the bicarbonate salt of the (η1-cyclohexenyl)platinum(II) cation, [Pt(η1-C6H9)(Cy2PCH2CH2 PCy2)(PPh3)] [HCO3] · 3H2O, which has been characterized by n.m.r. spectroscopy and single-crystal X-ray diffraction at low temperature. Crystals are triclinic, space group P1– with unit cell dimensions a 20.315(2), b 12.782(1), c 10.694(1) Å, α 66.61(1), β 104.73(1), γ 102.11(1)˚, and Z 2. The structure was refined to a final R value of 0.036 with use of 7553 reflections [I > 3σ(I)]. The cation has the expected, somewhat distorted planar coordination geometry; the anion consists of discrete, hydrogen-bonded dimers [(HCO3)(H2O)3]22-.

Crystallization and preliminary X-ray diffraction studies of human catalase

1999 ◽  
Vol 55 (9) ◽  
pp. 1614-1615 ◽  
Author(s):  
R. A. P. Nagem ◽  
E. A. L. Martins ◽  
V. M. Gonçalves ◽  
R. Aparício ◽  
I. Polikarpov
Keyword(s):  
Search Model ◽  
Molecular Replacement ◽  
X Ray Diffraction ◽  
Beef Liver ◽  
X Ray ◽  
Diffusion Technique ◽  
Cell Dimensions ◽  
Synchrotron Radiation Diffraction ◽  
Replacement Solution ◽  
Unit Cell Dimensions

The enzyme catalase (H2O2–H2O2 oxidoreductase; E.C. 11.1.6) was purified from haemolysate of human placenta and crystallized using the vapour-diffusion technique. Synchrotron-radiation diffraction data have been collected to 1.76 Å resolution. The enzyme crystallized in the space group P212121, with unit-cell dimensions a = 83.6, b = 139.4, c = 227.5 Å. A molecular-replacement solution of the structure has been obtained using beef liver catalase (PDB code 4blc) as a search model.

The high-pressure cadmium borate Cd6B22O39·H2O

2015 ◽  
Vol 70 (3) ◽  
pp. 183-190 ◽  
Author(s):  
Gerhard Sohr ◽  
Nina Ciaghi ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Structural Characteristics ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Cell Dimensions ◽  
Temperature Experiment ◽  
Unit Cell Dimensions ◽  
Ir And Raman

AbstractSingle crystals of the hydrous cadmium borate Cd6B22O39·H2O were obtained through a high-pressure/high-temperature experiment at 4.7 GPa and 1000 °C using a Walker-type multianvil apparatus. CdO and partially hydrolyzed B2O3 were used as starting materials. A single crystal X-ray diffraction study has revealed that the structure of Cd6B22O39·H2O is similar to that of the type M6B22O39·H2O (M=Fe, Co). Layers of corner-sharing BO4 groups are interconnected by BO3 groups to form channels containing the metal cations, which are six- and eight-fold coordinated by oxygen atoms. The compound crystallizes in the space group Pnma (no. 62) [R1=0.0379, wR2=0.0552 (all data)] with the unit cell dimensions a=1837.79(5), b=777.92(2), c=819.08(3) pm, and V=1171.00(6) Å3. The IR and Raman spectra reflect the structural characteristics of Cd6B22O39·H2O.

X–Ray Powder Diffraction Data for Synthetic Varieties of Tetrahedrite

1991 ◽  
Vol 6 (1) ◽  
pp. 43-47 ◽  
Author(s):  
Neil E. Johnson
Keyword(s):  
Powder Diffraction ◽  
Experimental Unit ◽  
Regression Equations ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Validation Test ◽  
Cell Dimensions ◽  
Synthetic Varieties ◽  
Unit Cell Dimensions

AbstractA series of five synthetic tetrahedrite-group minerals has been prepared and examined using powder X-ray diffraction in order to update current powder data and provide a validation test of cell dimension prediction equations. The tetrahedrites (nominally (Cu10X2)Sb4S13 with X = Zn, Cd, Mn, Hg and Fe) have the following properties: zincian tetrahedrite, a = 10.3833 (1) Å, Dx = 4.974 (1) g/cm3, F30 = 264 (0.004, 31), M20 = 279; cadmian tetrahedrite, a = 10.5066 (1) Å, Dx = 5.073 (1) g/cm3, F30 = 208 (0.004, 37), M20 = 249; manganoan tetrahedrite, a = 10.4384 (1) Å, Dx = 4.822 (1) g/cm3, F30 = 274 (0.003, 33), M20 = 302; mercurian tetrahedrite, a = 10.5071 (1) Å, Dx = 5.570 (1) g/cm3, F30 = 150 (0.006, 35), M20 = 156; ferroan tetrahedrite, a = 10.3630 (1) Å, Dx = 5.002 (1) g/cm3, F30 = 253 (0.004, 33), M20 = 281. The experimental unit cell dimensions obtained in this study are in excellent agreement with calculated values produced using regression equations developed previously.

Powder X-Ray Diffraction Data for Ca2Bi2O5and C4Bi6O13

1992 ◽  
Vol 7 (2) ◽  
pp. 109-111 ◽  
Author(s):  
C.J. Rawn ◽  
R.S. Roth ◽  
H.F. McMurdie
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Neutron Powder Diffraction ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Powder Samples ◽  
Orthorhombic Cell ◽  
Unit Cell Dimensions

AbstractSingle crystals and powder samples of Ca2Bi5O5and Ca4Bi6O13have been synthesized and studied using single crystal X-ray diffraction as well as X-ray and neutron powder diffraction. Unit cell dimensions were calculated using a least squares analysis that refined to a δ2θof no more than 0.03°. A triclinic cell was found with space group , a = 10.1222(7), b = 10.1466(6), c = 10.4833(7) Å. α= 116.912(5), β= 107.135(6) and γ= 92.939(6)°, Z = 6 for the Ca2Bi2O5compound. An orthorhombic cell was found with space group C2mm, a = 17.3795(5), b = 5.9419(2) and c = 7.2306(2) Å, Z = 2 for the Ca4Bi6O13compound.

scholarly journals X-ray Crystallographic Study of Ranaconitine

2011 ◽  
Vol 6 (11) ◽  
pp. 1934578X1100601
Author(s):  
Yang Li ◽  
Jun-Hui Zhou ◽  
Gui-Jun Han ◽  
Min-Juan Wang ◽  
Wen-Ji Sun ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Diffraction Analysis ◽  
Critical Role ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
Crystallographic Study ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structure of natural diterpenoid alkaloid ranaconitine isolated from Aconitum sinomontanum Nakai has been determined by single crystal X-ray diffraction analysis. The crystal presents a monoclinic system, space group C2 with Z = 4, unit cell dimensions a = 30.972(19) Å, b = 7.688(5) Å, and c = 19.632(12) Å. Moreover, the intermolecular O–H···O hydrogen bonds and weak π-π interactions play a critical role in expanding the dimensionality.

Synthesis, Crystal Structure and Magnetic Properties of a Copper(II) p-Formylbenzoate Complex

2012 ◽  
Vol 67 (11) ◽  
pp. 1185-1190 ◽  
Author(s):  
Jin-Li Qi ◽  
Wei Xu ◽  
Yue-Qing Zheng
Keyword(s):  
Room Temperature ◽  
Magnetic Measurements ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Ferromagnetic Interactions ◽  
Aqueous Conditions ◽  
Discrete Complex

A new Cu(II) complex was prepared at room temperature from the reaction of p-formylbenzoic acid, phenanthroline, CuCl2⋅2H2O, and NaOH under ethanolic aqueous conditions. The complex has been characterized by X-ray diffraction, IR spectroscopy, TG-DTA analyses, and magnetic measurements. Single-crystal X-ray diffraction analysis indicated that the complex crystallizes in the triclinic space group P1̄ with the cell dimensions a=7.875(2), b=10.724(2), c=15.317(3) Å , α =102.65(3), β =93.71(3), γ =107:64(3)°. The Cu atoms are in the environment of distorted CuN2O3 tetragonal pyramids. These discrete complex molecules are packed through intermolecular π...π-stacking interactions and C-H...O hydrogen bonds forming a supramolecular structure. The title complex obeys the Curie-Weiss law with a Curie constant C=0:53 cm3 K mol-1 and a Weiss constant θ = -0:27 K. The shape of the xmT curve is characteristic of weak ferromagnetic interactions between the Cu(II) centers from 300 to 7 K, while there are weak antiferromagnetic interactions below 7 K.

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