On the Reaction of Hexachlorocyclotriphosphazene with Heptamethyldisilazane. Crystal Structure of P3N3Cl5{N(CH3)[Si(CH3)3]}

2007 ◽  
Vol 72 (10) ◽  
pp. 1407-1419 ◽  
Author(s):  
Radka Voznicová ◽  
Milan Alberti ◽  
Jan Taraba ◽  
Dalibor Dastych ◽  
Pavel Kubáček ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Experimental Data ◽  
Dft Calculations ◽  
Crystal Structures ◽  
Elemental Analysis ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular And Crystal Structures

The reaction of P3N3Cl6 (1) with heptamethyldisilazane in the molar ratio 1:1 leads to the formation of 2,4,4,6,6-pentachloro-N-methyl-N-(trimethylsilyl)cyclotriphosphazen-2-amine, P3N3Cl5{N(CH3)[Si(CH3)3]} (2). Compound 2 was characterized by elemental analysis and spectroscopically. Molecular and crystal structures of 2 were determined by X-ray diffraction. 2 is monoclinic, space group P21/n. Experimental data were compared with results of DFT calculations.

scholarly journals Tl2C2O4·H2C2O4: a new crystalline form of thallium(I) oxalate

2015 ◽  
Vol 70 (4) ◽  
pp. 249-252 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Ana C. González-Baró ◽  
Enrique J. Baran
Keyword(s):  
Crystal Structure ◽  
Oxalic Acid ◽  
Crystalline Form ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Acid Molecule ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxalate Anion ◽  
Ft Raman

AbstractThe title compound was prepared by reaction, in aqueous solution, of Tl2CO3 and H2C2O4·2H2O in a molar ratio of 1:2. Its crystal structure was solved by X-ray diffraction methods. It crystallizes in the monoclinic space group P21/a with Z = 2 molecules per unit cell. The oxalic acid molecule and the oxalate anion are planar, residing on crystallographic inversion centers, and linked to each other by strong O–H···O hydrogen bonds giving rise to a polymeric structure. The Tl(I) ion is in a distorted polyhedral coordination with nine neighboring O atoms, five of oxalate anions and four others of oxalic acid molecules. The FTIR and FT-Raman spectra of the compound were also recorded and are briefly discussed.

New Insights into Hexacoordinated Silicon Complexes with 8- Oxyquinolinato Ligands: 1,3-Shift of Si-Bound Hydrocarbyl Substituents and the Influence of Si-Bound Halides on the 8-Oxyquinolinate Coordination Features

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1402-1418 ◽  
Author(s):  
Erik Wächtler ◽  
Alexander Kämpfe ◽  
Katrin Krupinski ◽  
Daniela Gerlach ◽  
Edwin Kroke ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
Quantum Chemical ◽  
Poor Response ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Torsion Angles ◽  
X Ray ◽  
Cp Mas Nmr

Abstract The transsilylation reaction between allyltrichlorosilane and 8-trimethylsiloxyquinoline in the molar ratio 1 : 3 yields the hexacoordinated silicon tris-chelate (oxinate)2Si(adho) (“oxinate” = 8- oxyquinolinate, “adho” = di-anion of 2-allyl-1,2-dihydro-8-oxyquinoline) comprising an SiO3N3 skeleton. The identity of this complex was established by single-crystal X-ray diffraction analysis and 29Si CP=MAS NMR spectroscopy of its chloroform solvate. Benzyltrichlorosilane and dibenzyldichlorosilane, comprising benzyl (Bn) as an “aromatically stabilized allyl moiety” did not undergo such rearrangement. Instead, the complexes (oxinate)2SiBnCl and (oxinate)2SiBn2 were obtained even upon using three molar equivalents of 8-trimethylsiloxyquinoline. We determined the crystal structure of a non-disordered bis-chelate (oxinate)2SiBnCl with Sibound hydrocarbyl and halogen substituents (the previously published (oxinate)2SiMeCl was disordered with alternative Me=Cl site occupancies). (Oxinate)2SiBnCl exhibits surprisingly poor response of the N-Si bonds to the different trans-disposed Si-X (X=Bn, Cl) bonds. For comparison and deeper insights into the coordination chemistry of oxinato silicon complexes with halide substituents, we determined the crystal structures of (oxinate)2SiPhCl·CHCl3, (oxinate)2SiCl2, (oxinate)2SiF2·1.5(CHCl3), and (8-oxyquinaldinate)2SiF2. Furthermore, the crystal structures of BnSiCl3 and Bn2SiCl2 (and its dibromo analog) are reported. The influence of the Si-C-C-C torsion angles of the benzyl group on the 29Si NMR shift of benzylsilanes (which is noticeably upfield with respect to analogous methyl silanes) was analyzed by quantum-chemical calculations.

Element–Element-Bindungen, IV. Molekül-und Kristallstruktur des Tetramethyldiphosphans und -diarsans /Element–Element Bonds, IV. Molecular and Crystal Structure of Tetramethyldiphosphane and -diarsane

1988 ◽  
Vol 43 (8) ◽  
pp. 952-958 ◽  
Author(s):  
Otto Mündt ◽  
Heinz Riffel ◽  
Gerd Becker ◽  
Arndt Simon
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Molecular And Crystal Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Linear Chains ◽  
Extended Interaction ◽  
Molecular And Crystal Structures

Abstract The molecular and crystal structures of the isotypic compounds tetramethyldiphosphane 1 and -diarsane 2 have been determined by single crystal X-ray diffraction (monoclinic; C2/m; Z = 2; 1/2: -155/-144 °C\a = 540.6(2)/555.8(2); b = 1131.0(6)/l 136.7(6); c -602.5(2)/612.8(2) pm;β = 97.31(3)/95.24(3)°;P-P 221.2(1)/As-As 242.9(1) pm). In accordance with the crystallographically imposed symmetry 2/m, the molecules adopt antiperiplanar conformation. Their crystal structures are closely related to those of the homologues tetramethyldistibane 3 [1] and -dibismuthane 4 [3]. As found for the latter compounds, the E -E units (E = P, As) are also aligned in linear chains, but the intermolecular E···E contacts (P···P 381/As···As 370 pm) do not allow any extended interaction between molecules, which otherwise would result in thermochromic effects.

The synthesis, and molecular and crystal structure of diphenyl(2-oxidonaphthylmethyl-iminoacetato)tin(IV)

1996 ◽  
Vol 74 (11) ◽  
pp. 2041-2047 ◽  
Author(s):  
Frank. E. Smith ◽  
Lian Ee Khoo ◽  
Ngoh Khang Goh ◽  
Rosemary C. Hynes ◽  
George Eng
Keyword(s):  
Crystal Structure ◽  
Elemental Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

The new diorganotin complex ((C6H5)2Sn(OC10H6CH=NCH2COO)) was prepared and characterized by 1H NMR, IR, elemental analysis, and a single crystal X-ray diffraction study. The crystals are monoclinic, space group P21/a with a = 16.9167(9) Å, b = 19.1276(16) Å, c = 26.538(2) Å, β = 100.534(6)°, V = 8442.5(11) Å3, Z = 16, and Dcalc = 1.574 Mg m−3. The final discrepancy factors are RF = 0.030, and RW = 0.021 for 6524 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.12 Å and 2.09 Å and the equatorial Sn—N bond of 2.14 Å are among the shortest found in related complexes. Key words: diorganotin(IV), bicycloazastannoxide, trigonal bipyramidal, antitumour.

scholarly journals Synthesis, crystal structure and computational chemistry research of a Zinc(II) complex: [Zn(Pt)(Biim)2]

2012 ◽  
Vol 77 (2) ◽  
pp. 177-185
Author(s):  
Fei Teng ◽  
Nan Jiang ◽  
Zhonghui Wang ◽  
Yuncheng Cui ◽  
Jiajun Wang
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Computational Chemistry ◽  
Elemental Analysis ◽  
Phthalic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chemistry Research ◽  
Metal Organic

The title metal-organic coordination complex [Zn(pt)(Biim)2] (pt=phthalic acid, benzene-1,2-dicarboxylate, Biim=2,2'-biimidazole) 1 has been obtained by using hydrothermal synthesis and characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/n with a = 8.5466(15) ?, b = 11.760(2) ?, c = 20.829(4) ?, ? = 95.56(2)?, V = 2083.5(6) ?3, Mr =497.78, Dc = 1.587 g/cm3, ?(MoK?) = 1.226 mm?1, F(000) = 1016, Z = 4, the final R = 0.0564 and wR = 0.1851 for 3656 observed reflections (I > 2?(I)). The elemental analysis, IR, TG and the theoretical calculation were also investigated.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.

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.

The Influence of the Axial Ligands of a Series of Platinum(IV) Anti-Cancer Complexes on Their Reduction to Platinum(II) and Reaction With DNA

1995 ◽  
Vol 48 (4) ◽  
pp. 793 ◽  
Author(s):  
LT Ellis ◽  
HM Er ◽  
TW Hambley
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reduction Potentials ◽  
Axial Ligands ◽  
Carboxylate Anions ◽  
Anti Cancer ◽  
Molecular Modelling Studies ◽  
Modelling Studies

The electrochemical reduction and DNA binding have been studied for a series of platinum(IV) complexes with Cl-, OH-, and carboxylate anions as the axial ligands ; [Pt(en)Cl4], [Pt(en)Cl2(OH)2], and [Pt(en)Cl2(OC(O)R)2], R = CH3, CH2CH3, CH2CH2CH3. Cathodic reduction potentials vary by more than 650 mV with the tetrachloro complex reduced most readily and the dihydroxo least readily. The binding of the complexes correlates with the reduction potentials with the more readily reduced complexes binding more readily to DNA. The influence of the reducing agent glutathione on platinum binding to DNA was found to depend on whether it was added before or after Pt/DNA incubation. The results are consistent with octahedral platinum(IV) binding monofunctionally to DNA, and molecular modelling studies have been used to confirm that this is sterically feasible. The crystal structure of [Pt(en)Cl2(OC(O)CH3)2] has been determined by X-ray diffraction methods and refined to R = 0.028 (977 F). The crystals are monoclinic, space group C2/c, a 15.569(6), b 8.104(1), c 13.188(1) Ǻ, β 136.38(2)°.

Synthesis of an Unprecedented H-stitched Binuclear Crystal Structure Based on Selective Fluorescence Recognition of Zn2+ in Newly Synthesized Schiff Base Ligand with DFT and Imaging Application in Living Cells

2021 ◽  
Author(s):  
SOUMYA SUNDAR MATI ◽  
Dr. SAUGATA KONAR ◽  
BOBY SAMAI
Keyword(s):  
Crystal Structure ◽  
Schiff Base ◽  
Elemental Analysis ◽  
Schiff Base Ligand ◽  
Binuclear Complex ◽  
Living Cells ◽  
X Ray Diffraction ◽  
Schiff Base Ligands ◽  
X Ray ◽  
Imaging Application

A zinc coordinated rare binuclear complex was synthesised and characterized by elemental analysis and single-crystal X-ray diffraction. Two mononuclear units formed by two Schiff base ligands 2-((2-(pyrimidin-2-yl)hydrazono)methyl)phenol (PHP) coordinated with...

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