The solid-state structure of bis(pentafluorophenyl)zinc

1998 ◽  
Vol 76 (5) ◽  
pp. 513-517 ◽  
Author(s):  
Yimin Sun ◽  
Warren E Piers ◽  
Masood Parvez
Keyword(s):  
Crystal Structure ◽  
Diethyl Ether ◽  
Benzene Solution ◽  
Close Contact ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray ◽  
Anhydrous Zncl ◽  
Ring Centroid ◽  
Linear Geometry

Using the published method of Wiedenbruch, bis(pentafluorophenyl)zinc, 1, was prepared from anhydrous ZnCl2 and 2 equiv. of LiC6F5 in diethyl ether. Base-free 1 was obtained in 60-65% yield by repeated distillation of the initially formed bis(diethyl) ether adduct of 1. The X-ray quality crystals of 1 were obtained from benzene solution. The molecular structure of 1 revealed a near linear geometry for the two-coordinate zinc center (C(1)-Zn-C(7) = 172.6(2)°), typical of monomeric ZnR2 derivatives. In the crystal structure, stacking interactions between C6F5 rings on adjacent molecules is a dominant motif, with ring centroid to ring centroid distances of 3.503 and 3.563 Å observed. A weak intermolecular C-F ...Zn interaction between F(2) and an adjacent zinc center, as judged by the close contact of 2.849(2) Å, also appears to be an important aspect of the crystal structure. Compound 1 is an effective but nonselective C6F5 transfer agent to BCl3; 1: monoclinic, space group P21/n, a = 11.902(2) Å, b = 7.732(2) Å, c = 13.735(2) Å, β = 110.58(1)°, V = 1183.4(4) Å3, Z = 4, R = 0.048, Rw = 0.069.Key words: organozinc complex, pentafluorophenyl transfer agent.

1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl2PN2CCl]3, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl2PN2CCl]3, Preparation, Spectra and Crystal Structure

1986 ◽  
Vol 41 (7) ◽  
pp. 839-844 ◽  
Author(s):  
H .-D. Hausen ◽  
G. Rajca ◽  
J. Weidlein
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Determination ◽  
Title Compound ◽  
Benzene Solution ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Low Symmetry

AbstractThe title compound, Cl2PN2CCl, has been synthesized by the reaction of PCl5 with Me3Si -N = C = N - SiMe3 (Me - CH3) in a 1:1 molar ratio. The colourless com pound is trimericin benzene solution and in the solid state and has a structure with a highly puckered 12-membered P3N6C3-ring skeleton of low symmetry. The X-ray structure determination shows a monoclinic space group P 21/a with 4 trimeric units per cell.

Synthesis and Crystal Structure of 5,10,15,20-Tetrakis(3,5-dinitrophenyl)porphyrin

1998 ◽  
Vol 02 (05) ◽  
pp. 391-396 ◽  
Author(s):  
P. BHYRAPPA ◽  
K. S. SUSLICK
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Data ◽  
Crystal Structure Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

The synthesis, characterization and crystal structure of the octanitro-substituted porphyrin 5,10,15,20-tetrakis(3,5-dinitrophenyl)porphyrin, H 2 T (3,5- DNP ) P , are described. The solid state structure has two porphyrins in the unit cell with eight pyridine solvates and is made up from columnar arrays of the porphyrins. X-ray crystal structure data: monoclinic, space group P1 21/n1, a = 14.9996(9) Å, b = 8.2489(5) Å, c = 24.818(2) Å, α = 90 °, β = 104.172(1) °, γ = 90 °, V = 2977.3(3) Å3, dcalc = 1.440 g m-3, Z = 2.

Synthesis and Solid-state Structure of 2,2,2ʹ,2ʹ -(Tetrahydroxymethyl)- dibutylether (Di-TMP), an Environmentally Benign Polymer Crosslinker and High-potential Additive for Lubricants

2012 ◽  
Vol 67 (2) ◽  
pp. 181-184
Author(s):  
Guido D. Frey ◽  
Rian D. Dewhurst ◽  
Eberhardt Herdtweck
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Environmentally Benign ◽  
Monoclinic Space Group ◽  
Spectroscopic Methods ◽  
Two Dimensional ◽  
State Structure ◽  
X Ray ◽  
Trimethylol Propane

The crystal structure of the industrially relevant tetrahydroxy ether 2,2,2ʹ,2ʹ-(tetrahydroxymethyl)-dibutylether (technically known as di(trimethylol)propane, Di-TMP; C12H26O5) was determined from single-crystal X-ray data at 123 K: monoclinic, space group C2/c (no. 15), a = 20.1202(13), b = 5.8169(4), c = 13.0323(8) Å, β = 114.296(3)°, V = 1390.17(16) Å3 and Z = 4. The adjacent molecules assemble into a two-dimensional framework in the solid state, linked by two intermolecular O-H...O hydrogen bonds. The compound is characterized via spectroscopic methods and mass spectrometry.

A study on α-RuCl3 crystal structure by scanning tunneling microscopy

1989 ◽  
Vol 47 ◽  
pp. 30-31
Author(s):  
H.-J. Cantow ◽  
H. Hillebrecht ◽  
S. Magonov ◽  
H. W. Rotter ◽  
G. Thiele
Keyword(s):  
Crystal Structure ◽  
Density Distribution ◽  
Scanning Tunneling Microscopy ◽  
Electron Density ◽  
Structure Determination ◽  
Electron Density Distribution ◽  
Scanning Tunneling ◽  
Monoclinic Space Group ◽  
Tunneling Microscopy ◽  
X Ray

From X-ray analysis, the conclusions are drawn from averaged molecular informations. Thus, limitations are caused when analyzing systems whose symmetry is reduced due to interatomic interactions. In contrast, scanning tunneling microscopy (STM) directly images atomic scale surface electron density distribution, with a resolution up to fractions of Angstrom units. The crucial point is the correlation between the electron density distribution and the localization of individual atoms, which is reasonable in many cases. Thus, the use of STM images for crystal structure determination may be permitted. We tried to apply RuCl3 - a layered material with semiconductive properties - for such STM studies. From the X-ray analysis it has been assumed that α-form of this compound crystallizes in the monoclinic space group C2/m (AICI3 type). The chlorine atoms form an almost undistorted cubic closed package while Ru occupies 2/3 of the octahedral holes in every second layer building up a plane hexagon net (graphite net). Idealizing the arrangement of the chlorines a hexagonal symmetry would be expected. X-ray structure determination of isotypic compounds e.g. IrBr3 leads only to averaged positions of the metal atoms as there exist extended stacking faults of the metal layers.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

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)°.

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

A 35-year-old mystery solved: a facile synthetic route and structural confirmation of tetrachlorobis(diethyl ether)tungsten(IV)

2021 ◽  
Vol 77 (4) ◽  
Author(s):  
Thomas E. Shaw ◽  
Alfred P. Sattelberger ◽  
Titel Jurca
Keyword(s):  
Crystal Structure ◽  
Diethyl Ether ◽  
Thermal Instability ◽  
Room Temperature ◽  
Surface Characteristics ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
Synthetic Route ◽  
X Ray ◽  
Elemental Analyses

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O) x , has been in doubt since 1985. Initially postulated as the bis-adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono-ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis-adduct. Here, we report the room-temperature X-ray crystal structure and Hirshfeld surface characteristics of trans-tetrachloridobis(diethyl ether)tungsten(IV), trans-WCl4(Et2O)2 or trans-[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.

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