Preparation and 31P NMR characterization of N-bonded complexes of platinum(II) with a phosphadithiatriazine: X-ray structure of trans-PtCl2(Pet3)(η1-N-Ph2PS2N3)

1992 ◽  
Vol 70 (10) ◽  
pp. 2602-2606 ◽  
Author(s):  
Tristram Chivers ◽  
Robert W. Hilts ◽  
Ian H. Krouse ◽  
A. Wallace Cordes ◽  
Randal Hallford ◽  
...  
Keyword(s):  
Nitrogen Atom ◽  
Free Ligand ◽  
Heterocyclic Ring ◽  
Structural Features ◽  
The Other ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Absorption Bands ◽  
X Ray ◽  
Nmr Characterization

The reaction of Ph2PS2N3 with [Pt2(μ-Cl)2(PEt3)4][BF4]2 or [PtCl2(PEt3)]2, in dichloromethane at 23° C produces the 1:1 adducts cis-[PtCl(PEt3)2(Ph2PS2N3)][BF4], 3, and trans-[PtCl2(PEt3)(Ph2PS3N2)], 4, respectively, in good yields. The 31P NMR data for 3 and 4 indicate that (i) the platinum is attached to a nitrogen atom adjacent to phosphorus in both these adducts, (ii) the PEt3 ligands in 3 are in mutually cis positions, and (iii) the PEt3 ligand in 4 is trans to the heterocyclic nitrogen. These structural features were confirmed by an X-ray analysis of 4. Crystals of 4 are monoclinic, space group P21/c, with a = 14.920(3) Å, b = 8.966(5) Å, c = 19.103(5) Å, β = 109.32(2)°, V = 2411.6(16) Å3, and Z = 4. The least-squares refinement with anisotropic thermal parameters for all non-hydrogen atoms converged at R = 0.050 and Rw = 0.053. The Pt—N bond length is 2.122(15) Å and the coordinated nitrogen atom is lifted ca. 0.63(2) Å out of the plane containing the other heterocyclic ring atoms. The attachment of a platinum(II) centre to the PN3S2 ring perturbs the S—N bond lengths significantly. The S—N distance involving the coordinated nitrogen is 1.672(16) Å, while the other S—N distances are 1.631(19), 1.555(19), and 1.562(19) Å, indicative of a localized sulfur diimide (-N=S=N-) structure. The UV–visible spectra of 3 and 4 in CH2Cl2 exhibit absorption bands at 514 and 528 nm, respectively, but dissociation of these adducts to give the free ligand Ph2PS2N3 occurs readily in dilute solution.

The structural features of a tetrahedral 1,3-monothiolate complex: The crystal and molecular structure of Bis(ethyl 3-mercaptobut-2-enoato)zinc(II)

1977 ◽  
Vol 30 (5) ◽  
pp. 993 ◽  
Author(s):  
BF Hoskins ◽  
CD Pannan
Keyword(s):  
Molecular Structure ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Lone Pair ◽  
Structural Features ◽  
The Other ◽  
Zinc Atom ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Mean Values

The crystal and molecular structure of bis(ethy 3-mercaptobut-2- enoato)zinc(II) has been determined by single-crystal X-ray diffraction techniques. Solved by conventional Patterson and Fourier methods the structure was refined by a least-squares method employing anisotropic thermal parameters to all non-hydrogen atoms to R and Rw values of 0.040 and 0.046 respectively. The complex crystallizes in the monoclinic space group P21/c with four molecules in a unit cell of dimensions a 11.107(1), b 18.239(2) and c 8.438(1) Ǻ and β 107.7(1)�. The intensities of 2274 independent and statistically significant [I ≥ 3σ(I)] reflections with θ values ≤ 70� were measured by counter methods using nickel- filtered Cu Kα radiation. The crystals comprise discrete monomeric molecules with the zinc atom bonded to two sulphur atoms and two oxygen atoms giving a coordination arrangement which is substantially distorted from an ideal tetrahedron. The mean values for the Zn-S and Zn-O bond distances are 2.247(1) and 2.007(3) Ǻ respectively and the average S-Zn-O intraligand bond angle is 99.25(8)�. The geometries of the ligands differ in two ways. Firstly, the two ethyl groups adopt differing conformations and secondly, while one ligand moiety is essentially planar with the zinc atom displaced about 0.1 Ǻ from that plane, the displaced atom in the other ligand is the carbon bonded to the sulphur atom and not the metal which is, in this instance, coplanar with the other members of the ring. Bond distances in each chelate ring indicate aromatic character with a lone pair of electrons on the ethoxy-oxygen participating in the delocalization.

Preparation and nuclear magnetic resonance characterization of N-bonded complexes of platinum(II) with phosphorus-nitrogen rings containing three-coordinate chalcogens: X-ray structure of [PtCl2(PEt3)]2(Ph4P2N4Se2Et2)

1993 ◽  
Vol 71 (11) ◽  
pp. 1821-1827 ◽  
Author(s):  
Tristram Chivers ◽  
Daniel D. Doxsee ◽  
Robert W. Hilts ◽  
Masood Parvez
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Nitrogen Atom ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
X Ray ◽  
X Ray Crystallography

The reaction of 1,5-Ph4P2N4S2Ph2 with [PtCl2CPEt3)]2 in chloroform at 60 °C produces the 1:1 adduct trans-PtCl2(PEt3)(Ph4P2N4S2Ph2) in which the platinum is attached to a nitrogen atom on the basis of 31P nmr spectroscopy. By contrast, the corresponding reactions of 1,5-Ph4P2N4Se2R2 (R = Me, Et, Ph) produce the 2:1 adducts [PtCl2(PEt3)]2(Ph4P2N4Se2R2) (7a, R = Me; 7b, R = Et; 7c, R = Ph) which have been characterized by 1H, 31P and 77Se nmr spectroscopy and, in the case of 7b, by X-ray crystallography. Crystals of 7b are monoclinic, space group C2/c, with a = 27.803(7) Å, b = 12.378(7) Å, c = 15.752(8) Å, β = 115.49(2)°, V = 4893(3) Å3, and Z = 4. The least-squares refinement with anisotropic thermal parameters for all non-hydrogen atoms converged at R = 0.037 and Rw = 0.022. The platinum centres in 7b are attached to distal nitrogen atoms of the disordered P2N4Se2 ring. The reaction of the six-membered ring Ph4P2N3SPh with [PtCl2(PEt3)]2 in dichloromethane at 23 °C occurs in a regiospecific manner to give the 1:1 adduct PtCl2(PEt3)(Ph4P2N3SPh) in which, on the basis of 31P nmr spectroscopy, the platinum is coordinated to a nitrogen atom between phosphorus and sulfur.

Preparation and X-ray crystal structures of the arsenic pentafluoride adducts of benzo-2,1,3-thiadiazole and benzo-1,2,3-thiadiazole

1986 ◽  
Vol 64 (5) ◽  
pp. 849-853 ◽  
Author(s):  
Allen Apblett ◽  
Tristram Chivers ◽  
John F. Richardson
Keyword(s):  
Nitrogen Atom ◽  
Crystal Structures ◽  
Benzene Ring ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

The reaction of arsenic pentafluoride with benzo-2,1,3-thiadiazole, 1, or benzo-1,2,3-thiadiazole, 2, in liquid SO2 gave 1:1 adducts that were characterized spectroscopically (infrared and 13C nmr) and by X-ray crystallography. Crystal data: for 1•AsF5, monoclinic, space group P21/n, a = 6.932(1), b = 9.113(1), c = 15.136(2) Å, β = 98.035(7)°, V = 946.8(2) Å3, Z = 4; for 2•AsF5, monoclinic, space group P21/a, a = 7.573(2), b = 13.101(2), c = 9.514(3) Å, β = 90.95(2)°, V = 943.9(4) Å3, Z = 4. The coordination of AsF5 to one of the nitrogen atoms in 1 introduces asymmetry in the heterocyclic ring, with the longer bond lengths being associated with the coordinated nitrogen atom, d(S—N) = 1.633(5) and 1.577(6) Å, d(C—N) = 1.364(7) and 1.339(8) Å. The quinonoid character of the benzene ring is still apparent in the adduct. In 2•AsF5, the AsF5 molecule is coordinated to the nitrogen atom that is bonded to carbon.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

Dative behavior of N-heterocyclic carbenes (NHCs) with selenium in Se-NHC compounds

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Munazzah Yaqoob ◽  
Mahvish Abbasi ◽  
Hira Anwar ◽  
Javed Iqbal ◽  
Mohammad Asad ◽  
...  
Keyword(s):  
Nitrogen Atom ◽  
Carbon Atom ◽  
Lone Pair ◽  
Heterocyclic Ring ◽  
Heterocyclic Carbenes ◽  
The Other ◽  
Donor Ligands ◽  
Important Research ◽  
Dative Bond ◽  
Back Bonding

Abstract N-heterocyclic carbenes (NHCs) are an eminent class of carbenes having a heterocyclic ring in which a divalent carbon atom is attached directly to a nitrogen atom. In the NHCs, the donation of lone pair is another important research in the dative bonding and not only in NHCs the dative bond plays a functionalized role in the other classes of complex formation like ylidones L → E ← L and carbones L → C ← L. M–NHC bond is L-M sigma-dative bond and NHCs are considered as strong sigma-donor ligands. The clear picture of the M–NHC bond can be better understood by M–NHC pi-interaction. M-L pi interaction is comprised of two steps. One is L → M sigma-donation and M → L π* back bonding. This dative donor nature of NHC and also its behavior in organoselenium is studied through DFT in which it’s optimized structure, bond lengths, molecular vibrations are calculated.

scholarly journals SOLVENT-FREE SYNTHESIS AND CRYSTAL STRUCTURE OF rac-2-THIOHYDANTOIN-VALINE

2019 ◽  
Vol 16 (31) ◽  
pp. 347-352
Author(s):  
G. E. DELGADO ◽  
Asiloé J. MORA ◽  
T. GONZÁLEZ ◽  
I. SANTOS ◽  
P. RIVAS ◽  
...  
Keyword(s):  
Heterocyclic Ring ◽  
Solvent Free ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network ◽  
Nmr Techniques ◽  
Solvent Free Synthesis

Thiohydantoins have been used in the manufacture of medicines and in industrial processes. Depending on the nature and type of substitution on the heterocyclic ring, these compounds may display pharmaceutical and biological activity with a variety of applications as antiepileptic, antitumoral, antiinflammatory, and principally for the treatment of prostate cancer. In this study, a new thiohydantoin was synthetized from the valine amino acid and structurally characterized. The title compound, C6H10N2O2S, with systematic name rac-5-isopropyl-2-tioxoimidazolidin-4-one, has been synthetized by a solvent-free synthesis. The heterocyclic compound was characterized by spectroscopic infrared (FTIR) and nuclear magnetic resonance (NMR) techniques, powder and single-crystal X-ray diffraction analysis (XRD). This material crystallizes in the monoclinic space group P21/c. In the supramolecular structure, the molecules are joined by N- --H···O and N---H···S hydrogen bonds, forming centrosymmetric R2 2(8) dimers and C2 2(9) chains that run along the [001] direction in an infinite one-dimensional network.

Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-NM-benzoylphosphoryltriamide and Dimorpholido-N-benzoylphosphorylamide

2000 ◽  
Vol 55 (6) ◽  
pp. 495-498 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Viktor V. Skopenkoa ◽  
Oleg V. Shishkinb
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Sodium Salts ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

N,N′-Tetramethyl-N"-benzoylphosphoryltriamide (I) and dimorpholido-N-benzoylphosphorylamide (II), and their sodium salts Nal, Nall were synthesized and characterized by means of IR and 1H, 31P NMR spectroscopy. The structures of I, II were determined by X-ray diffraction: I monoclinic, space group P2i/c with a = 10.162(3), b= 11.469(4), c = 12.286(4) Å , β = 94.04°, V = 1428.4(8) A 3, Z = 4, p(calcd) = 1.187 g/cm3; II monoclinic, space group C2/c with a = 15.503(4), b = 10.991(3), c = 22.000(6) Å, β = 106.39°, V = 3596.3(17) Å3, Z = 8, p(calcd.) = 1.253 g/cm3. The refinement of the structures converged at R = 0.0425 for I, and R = 0.068 for II. In both structures the molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis

1998 ◽  
Vol 53 (12) ◽  
pp. 1528-1530 ◽  
Author(s):  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Data Collection ◽  
Single Crystals ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Mecn Solution

Abstract Benzo-18 -crown-6 -Acetonitrile (1/2), Crystal Structure Single crystals of the title complex resulted fortuitously during an attempt to co-crystallise MeN(SO2Me)2 with benzo-18-crown-6 from an MeCN solution at -30 °C. The crystal structure has been determined via data collection at -100 °C (monoclinic, space group P21/n, Z = 4). The nitrile molecules are located with their me­ thyl groups above and below the plane of the 18-membered crown ring, the Me hydrogen atoms being rotationally disordered about the MeCN axes; C(methyl)···O(crown) distances range from 309.4(3) to 384.9(3) pm.

One-dimensional ribbons of solvated Ag sulfonates

1999 ◽  
Vol 77 (3) ◽  
pp. 313-318 ◽  
Author(s):  
George KH Shimizu ◽  
Gary D Enright ◽  
Gabriela S Rego ◽  
John A Ripmeester
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
The Other ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Single crystal X-ray structure determinations of two solvated silver sulfonates have been obtained and these compounds have been shown to adopt infinite one-dimensional motifs. {AgOTs(MeCN)}[Formula: see text] (OTs = p-toluenesulfonate) crystallizes in the monoclinic space group, P21, a = 8.4278(5) Å, b = 5.7413(3) Å, c = 12.1057(7) Å, β = 109.24(1)°. {Ag(NDSA)(MeCN)2(H3O)(H2O)2}[Formula: see text] (NDSA = 1,5-naphthalenedisulfonate) crystallizes in the triclinic space group, P[Formula: see text], a = 8.3407(4) Å, b = 10.4374(5) Å, c = 12.3399(6) Å, α = 101.941(8)°, β = 109.24(1)°, γ = 102.190(8)°. Despite one compound containing a monosulfonate and the other a disulfonate, both complexes form infinite one-dimensional arrays.Key words: silver, sulfonates, coordination polymer.

Untersuchungen an Stickstoff-Brom-Verbindungen, IV / Studies on Nitrogen-Bromine Compounds, IV

1977 ◽  
Vol 32 (12) ◽  
pp. 1416-1420 ◽  
Author(s):  
Omar Jabay ◽  
Hans Pritzkow ◽  
Jochen Jander
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Analysis ◽  
Electron Acceptors ◽  
Molecular Structures ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Solid Nitrogen ◽  
Intermolecular Contacts

The crystal and molecular structures of N-bromobenzamide (NBB), N-bromosuccinimide (NBS), and N,N-dibromobenzenesulfonamide (NBBS) were determined by X-ray structure analysis. The nitrogen atoms in NBB and NBS have a trigonal planar coordination (sp2) and the N—Br distances lie in the same range (1.82 A, 1.84 A). The N—Br distance in NBBS, where the nitrogen atom is sp3-hybridized, is somewhat longer (1.88 A). In these structures the molecules are connected by O···H—N (NBB), O···Br—N (NBS) or N···Br—N (NBBS) intermolecular bonds forming endless chains; positivated hydrogen atoms or, in case that they are absent, positivated bromine atoms act as electron acceptors with oxygen or sp3- hybridized nitrogen atoms. These results suggest, that in solid nitrogen tribromide, the crystal structure of which cannot be determined, the nitrogen atoms will be sp3-hybridized and intermolecular contacts via N—Br···N will occur.

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