Crystal structure of methyl,2-mercaptopyrimidinatomercury(II)

1978 ◽  
Vol 56 (4) ◽  
pp. 560-563 ◽  
Author(s):  
Chung Chieh
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Nmr Spectra ◽  
Heavy Atom ◽  
Pyrimidine Ring ◽  
Optically Active ◽  
Hydrogen Atoms ◽  
H Nmr ◽  
R Factor ◽  
Heavy Atom Method

Methyl,2-mercaptopyrimidinatomercury(II) was synthesized from methylmercuric hydroxide and 2-mercaptopyrimidine in aqueous solution. The crystal is orthorhombic with a = 4.063(2), b = 9.901(4), c = 18.808(15) Å, Dm = 2.88(1), Z = 4, Dc = 2.867 g cm−3, space group P212121. The structure was solved by the heavy atom method using 605 diffractometer measured reflections. The final R factor was 0.069. The key bond lengths and angles are: Hg—S, 2.39(2) Å, Hg—CH3, 2.13(6) Å, [Formula: see text] 174°. The CH3HgS— group bends out of the plane of the pyrimidine ring and the Hg atom interacts rather strongly with one of the ring nitrogens with an Hg—N distance of 2.83 Å. However, the Hg … N interaction is very labile in solution, since the two hydrogen atoms in the meta positions are equivalent from the 1H nmr spectra in both CDCl3 and DMSO solutions. The solution of the compound is not optically active.

The crystal and molecular structure of thiamine iodide hydroiodide

1976 ◽  
Vol 54 (19) ◽  
pp. 3001-3006 ◽  
Author(s):  
William Edward Lee ◽  
Mary Frances Richardson
Keyword(s):  
Heavy Atom ◽  
Pyrimidine Ring ◽  
Side Chain ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Iodide Ions ◽  
Cell Parameters ◽  
Weak Hydrogen Bonds ◽  
Ring Nitrogen ◽  
Heavy Atom Method

The X-ray crystal structure of thiamine iodide hydroiodide, C12H18N4OSI2, has been determined. The unit cell parameters are: a = 13.835(7), b = 7.442(4), c = 20.243(9) Å, β = 120.52(7)°, monoclinic space group P21/c, Z = 4. A total of 1445 reflections having F2 > 2σ(F2), 2θ < 40° were collected on a Picker 4-circle diffractometer with MoKα radiation by the 2θ scan technique. The structure was solved by the heavy-atom method. The iodide and sulphur atoms were refined anisotropically; only positional parameters were refined for the hydrogen atoms. Successive full-matrix least-squares refinements yielded an unweighted R-factor of 0.054. The pyrimidine ring is protonated on the ring nitrogen opposite the amino group. The relative disposition of the pyrimidine and thiazolium rings is similar to that observed in most other thiamine structures. The β-hydroxyethyl side chain of the thiazolium ring is folded in such a way that there is a short S … O contact, 2.97 Å in length. The iodide ions are involved in a number of weak hydrogen bonds.

Crystal Structure of Adeninium Trichloromercurate(II),

1975 ◽  
Vol 53 (15) ◽  
pp. 2345-2350 ◽  
Author(s):  
Monique Authier-Martin ◽  
André L. Beauchamp
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chloride Ions ◽  
Water Molecules ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Heavy Atom Method

The title compound belongs to space group P21/c with a = 23.99(1), b = 4.245(2), c = 25.98(1) Å, β = 117.58(7)°, and Z = 8. The structure was solved by the heavy-atom method and refined by block-diagonal least squares on 2589 independent observed reflections. All non-hydrogen atoms were refined anisotropically and some of the hydrogen atoms were located but their parameters were not refined. The final values of R and Rw were 0.042 and 0.047, respectively.The two nonequivalent mercury atoms have very similar environments. Two short Hg—Cl bonds (2.34–2.38 Å) at ∼ 165° define a quasi-molecular HgCl2 unit. Overall octahedral coordination is completed with two chloride ions at 2.76–2.84 Å and two chlorine atoms at 3.19–3.26 Å on neighboring HgCl2 quasi-molecules. HgCl6 octahedra share edges to form twofold ribbons in the b direction. This pattern of octahedra is identical with the onereported for β-NH4HgCl3. The cations are pairs of N(1)-protonated adenine molecules linked by two N(10)—H(10)… N(7) hydrogen bonds and stacked in the b direction. Water molecules act as acceptors in moderately strong hydrogen bonds with acidic protons H(1) and H(9) of adeninium ions. Other generally weaker hydrogen bonds exist between the various parts of the structure.

Studies on tellurium-carbon bonded compounds. II. The crystal structure of [Heptane-3,5-dionato(2 - )]tellurium(II) ('1,1′-Dimethylacetylacetone tellurium(II)')

1977 ◽  
Vol 30 (3) ◽  
pp. 487 ◽  
Author(s):  
JC Dewan ◽  
J Silver
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chair Conformation ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
Heavy Atom Method

The structure of the title compound has been determined by the heavy- atom method from 973 reflections, measured with a diffractometer, and refined by full-matrix least-squares methods to R 0.030. Crystals are monoclinic, space group P21, a = 8.69(1), b = 4.86(1), c = 10.14(2) Ǻ, β = 98.7(1)�, Z = 2. In the discrete molecules of the complex a tellurium(II) atom is bonded to one bivalent heptane-3,5-dione ligand through the α-carbon atoms [Te-C 2.184(6), 2.206(7) Ǻ; C-Te-C 89.7(3)�], forming a heterocyclic ring of chair conformation with the methyl substituents both in equatorial positions. The molecules are arranged in a zig-zag polymeric manner about the 21 axes at x = 0 and z = 0. All hydrogen atoms have been located.

Metal binding to N(9), N(7), and N(3) of adenine. Crystal structure of μ-(adeninato-N3,N7,N9)tris(methylmercury(II)) perchlorate

1980 ◽  
Vol 58 (14) ◽  
pp. 1439-1443 ◽  
Author(s):  
Joseph Hubert ◽  
André L. Beauchamp
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Metal Binding ◽  
Heavy Atom ◽  
Individual Species ◽  
Cell Parameters ◽  
R Factor ◽  
Dimeric Unit ◽  
Adenine Ring ◽  
Heavy Atom Method

The title compound belongs to space group [Formula: see text] with the following cell parameters: a = 6.304, b = 11.925, c = 25.946 Å, α = 85.76, β = 89.78, γ = 83.57°, and Z = 4. The structure was solved by the heavy-atom method and refined on 2570 nonzero reflections to an R factor of 0.044. In the two crystallographically independent [Adeninato(CH3Hg)3]2+ ions, methylmercury groups are linearly bonded to N(3), N(7), and N(9) of a deprotonated adenine ring, forming Hg—N bonds of normal lengths (ave. 2.08 Å) for two-coordinated mercury. One half of the complex cations are associated in a dimeric unit by a pair of strong [Formula: see text] hydrogen bonds, while the others are packed as individual species in the crystal. The structure is stabilized by a number of contacts between mercury and perchlorate oxygens.

The synthesis, crystal and molecular structure of 1,1,3,3-tetramethylimidazolidinium diiodide methylene dichloride solvate, (C7H18N2)I2•CH2Cl2

1984 ◽  
Vol 62 (9) ◽  
pp. 1662-1665 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Title Compound ◽  
Nmr Spectra ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Space Group ◽  
Simple Preparation ◽  
Methylene Dichloride ◽  
Heavy Atom Method

A simple preparation of the title compound, its crystal structure, and nmr spectra are reported. The compound crystallizes in the space group P21/n, with a = 8.109(2) Å, b = 16.183(4) Å, c = 11.968(4) Å, β = 93.45(2)°, V = 1567.7(7) Å−3, ρ = 1.987 g cm−3, Z = 4 (MoKα, λ = 0.71069 Å). The structure was solved by the heavy atom method and refined to the final R = 0.0415 for 1261 "observed" reflections. The structure consists of five-membered cyclic C7H18N22+ cations, iodide anions, and methylene dichloride molecules which are held loosely in the lattice.

Synthesis of chloro(2-methylimidazole) ruthenium(III) complexes and their aqueous solution chemistry, and the crystal structure of [2-MeImH]2[RuCl52-MeIm]

2001 ◽  
Vol 79 (10) ◽  
pp. 1477-1482 ◽  
Author(s):  
Craig Anderson
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Solution Chemistry ◽  
Proton Nmr Spectroscopy ◽  
Line Broadening ◽  
Reaction Conditions ◽  
H Nmr ◽  
Paramagnetic Complexes

2-Methylimidazole (2-MeIm) reacts with RuCl3 in aqueous acidic ethanolic medium to give (2-MeImH)2[RuCl5(2-MeIm)] (1) and (2-MeImH)[RuCl4(2-MeIm)2] (2) (2-MeImH = protonated 2-methylimidazole), the ratio depending on reaction conditions used. Molecule 1 crystallizes in the space group Pnma: a = 14.046(2), b = 17.294(2), and c = 8.2778(12) Å. The 1H NMR spectra of these ruthenium(III) complexes have been measured and show peaks with large isotropic shifts and large line broadening characteristic of such paramagnetic complexes. The aquation of complexes 1 and 2 were followed by proton NMR spectroscopy. 1,2-Dimethyl imidazole (1,2-diMeIm) reacts with RuCl3 in methanolic solution to give [RuCl3(1,2-diMeIm)(H2O)S] (S=H2O (3a) or CH3OH (3b)). The aquation reactions of complexes 3a and 3b were followed by 1H NMR.Key words: ruthenium, paramagnetic, antitumour, NMR.

The Crystal and Molecular Structure of sym-fac-(1,4,7-Triazaheptane)-(S)-aspartatocobalt(III) Diperchlorate Dihydrate

1994 ◽  
Vol 59 (5) ◽  
pp. 1052-1058 ◽  
Author(s):  
Jan Ondráček ◽  
Jana Ondráčková ◽  
Jaroslav Maixner ◽  
František Jursík
Keyword(s):  
Molecular Structure ◽  
Aspartic Acid ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Membered Ring ◽  
Boat Conformation ◽  
Hydrogen Atoms ◽  
Orthorhombic System ◽  
Anisotropic Temperature ◽  
Heavy Atom Method

The crystal and molecular structure of s-fac-[Co((S)-Asp)(dien)]ClO4 . HClO4 .2 H2O (dien = 1,4,7-triazaheptane) was solved by the heavy atom method. The position parameters of the non-hydrogen atoms and their anisotropic temperature parameters were refined based on 1 726 observed reflections with a final value of R = 0.073. The substance crystallizes in the orthorhombic system in the space group P212121, Z = 4, a = 8.506(1), b = 17.171(2), c = 13.277(1) Å. The structure involves hydrogen bonds between the O2, O4 and HN2 atoms of aspartic acid and the two molecules of water. The five-membered dien chelate rings take the asymmetric envelope conformations. The five-membered ring of (S)-aspartic acid possesses the symmetric envelope conformation whereas the six-membered ring exhibits the skew boat conformation.

Structure cristalline et moléculaire du cis-dithiocyanatobis(phénanthroline-1,10)mercure(II), Hg(SCN)2(C12H8N2)2

1974 ◽  
Vol 52 (16) ◽  
pp. 2923-2927 ◽  
Author(s):  
André L. Beauchamp ◽  
Bernard Saperas ◽  
Roland Rivest
Keyword(s):  
Heavy Atom ◽  
Octahedral Geometry ◽  
Van Der Waals Interactions ◽  
Distorted Octahedral Geometry ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
R Factor ◽  
Distorted Octahedral ◽  
Phenanthroline Ligands ◽  
Heavy Atom Method

The compound cis-Hg(SCN)2(Phen)2 belongs to the triclinic space group [Formula: see text] with a = 13.252(5), b = 11.077(4), c = 8.443(3) Å, α = 105.20(3), β = 83.25 (3), γ = 90.92(3)°, and Z = 2. The structure was solved by the heavy atom method and refined on 1718 independent reflections to an R factor of 0.069. The crystal contains discrete molecules, in which mercury is coordinated to four nitrogen atoms from two phenanthroline molecules and to two sulfur atoms from thiocyanate groups. These donor atoms define a distorted octahedral geometry around mercury. The Hg—N bond lengths are in the range 2.42(2)–2.52(2) Å, whereas the Hg—S bonds are equal to 2.622(8) and 2.582(8) Å. The molecules are packed in layers parallel to the (110) planes and the layers are held together by normal van der Waals interactions. Within the layers, the packing of the complex is characterized by parallel stacking of phenanthroline ligands at distances of ∼3.4 Å. The terminal nitrogen atoms of the thiocyanate groups are uncoordinated.

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.

The crystal structure of diamminesilver dinitroargentate, [Ag(NH3)2]Ag(NO2)2*

1977 ◽  
Vol 146 (4-6) ◽  
Author(s):  
H. M. Maurer ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Heavy Atom ◽  
Anisotropic Temperature ◽  
Light Atoms ◽  
Difference Fourier ◽  
Temperature Factors ◽  
Heavy Atom Method ◽  
Silver Atoms ◽  
Block Diagonal

AbstractThe crystal structure of diamminesilver dinitroargentate, [Ag(NHThe point positions of the silver atoms were obtained by the heavy-atom method whereas those of the light atoms were found by difference Fourier syntheses. Coordinates and anisotropic temperature factors were refined by block-diagonal least-squares methods with the result

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