Synthesis and solid-state molecular structures of bis- and mono-nitrosobenzene complexes of ruthenium porphyrins

2002 ◽  
Vol 80 (9) ◽  
pp. 1252-1258 ◽  
Author(s):  
Jonghyuk Lee ◽  
Brendan Twamley ◽  
George B Richter-Addo
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Ir Spectra ◽  
Single Crystal ◽  
Binding Mode ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Parallel Arrangement ◽  
Ruthenium Porphyrin

Bis-nitrosobenzene complexes of the form (por)Ru(PhNO)2 (por = TPP, TTP; TPP = tetraphenylporphyrinato dianion, TTP = tetratolylporphyrinato dianion) have been prepared in good yields from the reaction of the (por)Ru(CO) precursor with excess PhNO in dichloromethane. The IR spectra of the complexes (as KBr pellets) displayed new bands at ~1348 cm–1, due to υNO. The solid-state molecular structure of (TPP)Ru(PhNO)2 was determined by single-crystal X-ray diffraction, and revealed that the PhNO ligands are bound to the Ru center via the N-binding mode. Reactions of the (por)Ru(PhNO)2 complexes with excess 1-methylimidazole gave the mono-nitrosobenzene complexes (por)Ru(PhNO)(1-MeIm). The IR spectra revealed a lowering of υNO in these mononitrosobenzene derivatives by ~27 cm–1, a feature consistent with the replacement of one π-acid PhNO ligand with the more basic 1-MeIm ligand. The solid-state molecular structure of (TPP)Ru(PhNO)(1-MeIm) reveals, in addition to the N-binding of the PhNO ligand, an essentially parallel arrangement of the C-N-O (of PhNO) and imidazole planes; this is in contrast with the (TPP)Ru(PhNO)2 complex, in which the C-N-O planes (of PhNO) are essentially perpendicular.Key words: nitroso, X-ray, ruthenium, porphyrin, imidazole.

On Attempts to Synthesize Lanthanide Complexes of the Dianionic Fluorenyl-alkoxo Ligand [C13H8-cyclo-C6H10-O]2-. Crystal Structure of (C13H9-cyclo-C6H10-O)LaI2(DME)2

2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectra ◽  
Single Crystal ◽  
Lanthanide Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.

Molecular structures of various alkyldichlorosilanes in the solid state

2017 ◽  
Vol 46 (27) ◽  
pp. 8875-8882
Author(s):  
Jörg Wagler ◽  
Robert Gericke
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray

A series of organodichlorosilanes RR′SiCl2 (R,R′ = (CH2)3; (CH2)4; (CH2)5; Me,Me; Me,H; Me,Cl) was studied by single-crystal X-ray diffraction analyses.

Synthesis and Crystal Structures of Dimethylsilylene-Bridged (Amidocyclopentadienyl)dichlorotitanium(IV) Complexes with Various Substituents on the Cyclopentadienyl Ligand

2001 ◽  
Vol 66 (4) ◽  
pp. 605-620 ◽  
Author(s):  
Jaroslav Zemánek ◽  
Petr Štěpnička ◽  
Karla Fejfarová ◽  
Róbert Gyepes ◽  
Ivana Císařová ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Single Crystal ◽  
Spectral Methods ◽  
Nmr Spectra ◽  
Bulky Substituent ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cyclopentadienyl Ligand

(Amidocyclopentadienyl)dichlorotitanium(IV) complexes of the general formula [TiCl2{η5:η1(N)-C5(1-SiMe2Nt-Bu-2,3,4-Me3-5-R)}], where R = H (6b), Ph (6c), 4-fluorophenyl (6d) and 1-methylallyl (6e) were synthesized and characterized by spectral methods. Solid-state structure of [TiCl2{η5:η1(N)-C5Me4(SiMe2Nt-Bu)}] (6a) and 6d determined by single-crystal X-ray diffraction showed that variation of the ring substituent R has only a negligible effect on the molecular structure of the complexes. The NMR spectra indicate that motion of the bulky substituent R in compounds 6c, 6d and 6e is hindered below ca 50 °C.

Kristall- und Molekülstruktur von As2P2S7/ Crystal and Molecular Structure of As2P2S7

1984 ◽  
Vol 39 (8) ◽  
pp. 1088-1091 ◽  
Author(s):  
Wolfgang Hönle ◽  
Claus Wibbelmann ◽  
Wolfgang Brockner
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Group V ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of As2P2S7 has been determined by single crystal X-ray diffraction (space group V 21/c; Z = 4; a = 1174.6(16) pm; b = 823.9(7) pm; c = 1140.1(10) pm; β - 94.43(9)°; R = 0.073. The molecule is isosteric to P4S7 and possesses C2v symmetry. Mean bond lengths are: d (As-As) = 250.9 pm; d (As-S ) = 225.7 pm; d(P - S) = 208.3 pm and d(P = S) = 193.2 pm. The observed As -As bond length agrees well with spectroscopic results

scholarly journals Synthesis of Bis(Carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) and Attempt of Synthesis of Gadolinium Bis(Dicarbollide)

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1321
Author(s):  
Yasunobu Asawa ◽  
Aleksandra V. Arsent’eva ◽  
Sergey A. Anufriev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
X Ray Diffraction ◽  
Stable Conformation ◽  
Acyl Chlorides ◽  
X Ray ◽  
Cesium Fluoride ◽  
The Stability

Bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) were prepared by the reactions of the corresponding carboranyl acyl chlorides with ethylenediamine. Crystal molecular structure of 1,1′-μ-(CH2NH(O)C-1,2-C2B10H11)2 was determined by single crystal X-ray diffraction. Treatment of bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 with ammonium or cesium fluoride results in partial deboronation of the ortho-carborane cages to the nido-carborane ones with formation of [7,7′(8′)-μ-(CH2NH(O)C(CH2)n-7,8-C2B9H11)2]2−. The attempted reaction of [7,7′(8′)-μ-(CH2NH(O)CCH2-7,8-C2B9H11)2]2− with GdCl3 in 1,2-dimethoxy- ethane did not give the expected metallacarborane. The stability of different conformations of Gd-containing metallacarboranes has been estimated by quantum-chemical calculations using [3,3-μ-DME-3,3′-Gd(1,2-C2B9H11)2]− as a model. It was found that in the most stable conformation the CH groups of the dicarbollide ligands are in anti,anti-orientation with respect to the DME ligand, while any rotation of the dicarbollide ligand reduces the stability of the system. This makes it possible to rationalize the design of carborane ligands for the synthesis of gadolinium metallacarboranes on their base.

1,2-Hydroboration of Alkyn-1-yldichlorosilanes using Triethylborane

2008 ◽  
Vol 63 (11) ◽  
pp. 1267-1275 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Ezzat Khan ◽  
Wolfgang Milius
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Hydrogen Transfer ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ethyl Group ◽  
Nmr Data

Abstract Triethylborane, BEt3, can act as a 1,2-hydroborating reagent towards alkyn-1-ylsilanes, depending on the nature of the silane. A mechanism is proposed invoking hydrogen transfer from the β -carbon of one ethyl group, quite different from the 1,2-hydroboration mechanism using tri-n-propylborane, BnPr3. The structure of the products has been confirmed by comparison with that obtained using 9-borabicyclo[3.3.1]nonane, 9-BBN, as a well established 1,2-hydroborating reagent. All products have been characterized by a consistent set of NMR data (1H, 11B, 13C and 29Si NMR). The molecular structure of (Z)-1-dichlorosilyl-1-[9-(9-borabicyclo[3.3.1]nonyl)]-2-phenylethene has been determined by single crystal X-ray diffraction.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

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