Tetrabutylammonium Salts of 2-Nitropropane, Cyclopentadiene and 9-Ethylfluorene: Crystal Structures and Use in Anionic Polymerization

1995 ◽  
Vol 50 (3) ◽  
pp. 415-422 ◽  
Author(s):  
Manfred T. Reetz ◽  
Stephan Hütte ◽  
Richard Goddard
Keyword(s):  
Anionic Polymerization ◽  
Room Temperature ◽  
Ion Pairs ◽  
Three Dimensional ◽  
Star Polymers ◽  
X Ray ◽  
Dimensional Network ◽  
Acidic Compounds ◽  
Cyclopentadienyl Anion ◽  
Special Case

Reaction of the CH-acidic compounds 2-nitropropane, cyclopentadiene and 9-ethylfluorene with HON (nBu)4 affords the corresponding tetrabutylammonium salts in crystalline form, which have been characterized by X -ray structure analysis. The nitrostabilized salt is not a “naked ” anion (real carbanion). Rather, the α-methylene entities of the N+(nBu)4 cations form relatively strong hydrogen bonds with the O -atom s of the nitronateanion, forming dimers in a three-dimensional network. In solution dimers in the form of supramolecular ion pairs exist. In contrast, the cyclopentadienyl anion appears to be a real carbanion, since anion and cation do not interact with one another via H -bonding. The structure of the N+(nBu)4 salt of the 9-ethylfluorenyl anion is a special case in that closer contacts between cation and anion occur, which may be indicative of unusual [CH ··· C]- bonding. All three salts function as initiators in the metal-free anionic polymerization of acrylates and methacrylates at room temperature. In the case of tetrabutylammoniumcyclopentadienide, star polymers are formed.

Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaamino-1-oxo- 1λ5 ,3λ5-diphosphaz-2-en, (NH2)2(O)P-N=P(NH2)3 / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ5, 3λ5-diphosphaz-2-ene, (NH2)2(O)P-N=P(NH2)3

1996 ◽  
Vol 51 (8) ◽  
pp. 1079-1083 ◽  
Author(s):  
N. Stock ◽  
W. Schnick
Keyword(s):  
Crystal Structure ◽  
Thermal Properties ◽  
Room Temperature ◽  
Three Dimensional ◽  
Intermolecular Hydrogen Bonding ◽  
Structure And Properties ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Ray Methods

Coarse crystalline (NH2)2(O)P-N=P(NH2)3 is obtained from a NH3 saturated CH2Cl2 suspension of (NH2)2(O)P-N=P(NH2)3 NH4Cl at room temperature. (NH2)2(O)P-N=P(NH2)3·NH4Cl is synthesized by slow addition of Cl2(O)P-N=PCl3 to a solution of NH3 in CH2Cl2 at -78 °C. Excess NH4Cl is removed by treatment with HNEt2 followed by extraction with CH2Cl2. The crystal structure of (NH2)2(O)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, β = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H···N ≥ 313 pm. N-H···O ≥ 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C.

Structure and optical non-linearity of PbO.2B2O3

1996 ◽  
Vol 52 (2) ◽  
pp. 260-265 ◽  
Author(s):  
D. L. Corker ◽  
A. M. Glazer
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Asymmetric Distribution ◽  
X Ray Diffraction ◽  
Acta Cryst ◽  
X Ray ◽  
Dimensional Network ◽  
Non Linear ◽  
Linear Optical ◽  
Atomic Coordinates

The crystal structure of lead tetraborate, PbO.2B2O3, has been refined using single-crystal X-ray diffraction data (Mo Kα radiation, λ = 0.71069 Å). Crystal data at room temperature: Mr = 362.43, orthorhombic, P21 nm (C 7 2v ), a = 4.251 (2), b = 4.463 (3), c = 10.860 (3) Å, V = 206.04 Å3 with Z = 2, μ = 402.6 cm−1, Dx = 5.88 Mg m−3, F(000) = 316, final R = 0.022, wR = 0.025 over 655 reflections with I > 2.5σ(I). Atomic coordinates are in general agreement with those previously reported for the isostructural compound, SrO.2B2O3, by Perloff & Block [Acta Cryst. (1966), 20, 274–279]. All the borons are tetrahedrally coordinated with a three-dimensional network formed from O atoms that are common to either two or three tetrahedra. The tetrahedra show deformation because the B—O bonds involving the two-coordinated O atoms are much shorter than those involved with three-coordinated O atoms. The Pb atoms are situated in empty tunnels running along [010] left by the network of tetrahedra. The Pb atoms display a highly asymmetric distribution of Pb—O bonding, with the five shortest bonds covering the range 2.483 (5)–2.664 (5) Å, being all situated to one side of the Pb atom. Preliminary investigations of the non-linear optical behaviour of lead tetraborate are also discussed. The results indicate that doping with barium should lead to a new non-linear optical material that is both phase-matchable and has a high optical non-linearity.

scholarly journals Synthesis, X-Ray Structure, and Characterization of a Complex Containing the Hexakis(urea)cobalt(II) Cation and Lattice Urea Molecules

2007 ◽  
Vol 2007 ◽  
pp. 1-7 ◽  
Author(s):  
Labrini Drakopoulou ◽  
Constantina Papatriantafyllopoulou ◽  
Aris Terzis ◽  
Spyros P. Perlepes ◽  
Evy Manessi-Zoupa ◽  
...  
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray ◽  
Lattice Constants ◽  
Dimensional Network ◽  
Different Types ◽  
Hydrogen Bonded

The 12: 1 reaction of urea (U) with CoI2in EtOH yielded the “clathrate-coordination” compound[CoU6]I2·4U (1). The complex crystallizes in the monoclinic space group P21/c. The lattice constants area= 9.844(4),b= 7.268(3),c= 24.12(1) Å, andβ=98.12(1)∘. The crystal structure determination demonstrates the existence of octahedral[CoU6]2+cations,I-counterions, and two different types (twoU1and twoU2) of hydrogen-bonded, lattice urea molecules. The[CoU6]2+cations and theU1lattice molecules form two-dimensional hydrogen-bonded layers which are parallel to theabplane. TheI-anions are placed above and below each layer, and are hydrogen bonded both toU1molecules and[CoU6]2+cations. EachU2molecule is connected to a[CoU6]2+cation through anN–H⋯Ohydrogen bond resulting in a three-dimensional network. Room temperature magnetic susceptibility and spectroscopic (solid-state UV/Vis, IR, Raman) data of1are discussed in terms of the nature of bonding and the known structure.

New Metal-Rich Compounds NblrSi, NblrGe, and TalrSi -Synthesis, Structure, and Magnetic Properties

2001 ◽  
Vol 56 (6) ◽  
pp. 463-468 ◽  
Author(s):  
Ratikanta Mishra ◽  
Rainer Pöttgen ◽  
Gunter Kotzyba
Keyword(s):  
Magnetic Properties ◽  
Silicon Germanium ◽  
High Frequency ◽  
Room Temperature ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Arc Melting ◽  
Dimensional Network ◽  
Pauli Paramagnetism

AbstractThe metal-rich intermetallic compounds NblrSi, NblrGe, and TalrSi were synthesized by arc-melting of the elements and subsequent annealing in glassy carbon crucibles in a high-frequency furnace. The three compounds were investigated by X-ray diffraction on powders and single crystals: TiNiSi type, Pnma, a = 641.27(3), b = 379.48(2), c = 727.70(3) pm, wR2 = 0.0773, 430 F2 values for NblrSi, a = 645.48(3), b = 389.21(2), c = 741.11(4) pm, wR2 = 0.0981, 297 F2 values for NblrGe, and a = 638.11(3), b = 378.69(2), c = 726.78(3) pm, wR2 = 0.0887, 290 F2 values for TalrSi with 20 variables for each refinement. The iridium and silicon (germanium) atoms form a three-dimensional network of puckered Ir3Si3 and Ir3Ge3 hexagons in which the niobium (tantalum) atoms fill larger cages. Magnetic susceptibility measurements on NblrSi and TalrSi indicate Pauli paramagnetism with room temperature susceptibilities of 0.30(5)·10-9 and 0.97(5)·10-9 m3/mol, respectively.

Syntheses, Structures and Photoluminescent Properties of the Two Novel Coordination Polymers [Cd(pydc)2(tu)]n and [Cd2(SO4)(nic)2(tu)1.5(H2O)2]n (pydc = Pyridine-2,3-dicarboxylate, nic = Nicotinate, tu = Thiourea)

2011 ◽  
Vol 66 (5) ◽  
pp. 459-464 ◽  
Author(s):  
Chao Xu ◽  
Sheng-Bo Liu ◽  
Taike Duan ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Hydrogen Bonds ◽  
Coordination Polymers ◽  
Room Temperature ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network

Two novel cadmium coordination polymers, [Cd(pydc)2(tu)]n (1) and [Cd2(SO4)(nic)2(tu)1.5 - (H2O)2]n (2) (pydc = pyridine-2,3-dicarboxylate, nic = nicotinate, tu = thiourea), have been synthesized under hydrothermal conditions and structurally characterized by X-ray diffraction analysis. 1 is a one-dimensional ladder coordination polymer in a two-dimensional network formed by hydrogen bonds. 2 consists of two kinds of Cd(II) centers in different coordination environments connected via nicotinate and sulfate to form a two-dimensional grid network integrated in a three-dimensional framework generated by hydrogen bonds. 2 shows intense fluorescent emission in the solid state at room temperature

scholarly journals 4-(3-Chlorophenyl)-1-(3-chloropropyl)piperazin-1-ium chloride redetermined at 100 K

IUCrData ◽  
2016 ◽  
Vol 1 (2) ◽  
Author(s):  
Muzzaffar Ahmad Bhat ◽  
Sanjay K. Srivastava ◽  
Pooja Sharma ◽  
Ambika Chopra ◽  
Ray J. Butcher
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Ion Pairs ◽  
Three Dimensional ◽  
Chair Conformation ◽  
Temperature Data ◽  
Acta Cryst ◽  
Piperazine Ring ◽  
Dimensional Network

The crystal structure of the title salt, C13H19Cl2N2+·Cl−, has been reported previously [Homrighausen & Krause Bauer (2002).Acta Cryst.E58, o1395–o1396] based on room-temperature data, where it was found to contain a disordered chloropropyl group. We now present the structure at 100 K in which the chloropropyl group is ordered. The piperazine ring adopts a chair conformation with the exocyclic N—C bonds in equatorial orientations. The dihedral angle between the piperazine ring (all atoms) and the benzene ring is 28.47 (5)°. The chloropropyl group has an extended conformation [N—C—C—C = −177.25 (8) ° and C—C—C—Cl = 174.23 (7)°]. In the crystal, charge-assisted N—H...Cl hydrogen bonds link the cation and anion into ion pairs. Numerous weak C—H...Cl interactions link the ion pairs into a three-dimensional network. Short Cl...Cl contacts [3.2419 (4) Å] are also observed.

Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. III 2/4-Nitrophenoxides of Univalent Heavy Metals

1998 ◽  
Vol 51 (8) ◽  
pp. 735 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Closed Shell ◽  
Two Dimensional ◽  
Nitrogen Base ◽  
Coinage Metal ◽  
Aromatic Carbon ◽  
X Ray ◽  
Dimensional Network ◽  
Oxygen Atoms

Room-temperature single-crystal X-ray studies are recorded for 2- and 4-nitrophenoxide salts of silver(I) and thallium(I), M(2-np) and Tl(4-np) (anhydrous), and Ag(4-np).H2O. Ag(2-np) is monoclinic, P21/c, a 9·012(4), b 5·743(5), c 12·594(5) Å, β 104·34(4)°, Z = 4; conventional R on |F| was 0·042 for No 1378 independent ‘observed’ (I > 3σ(I)) reflections. Tl(2-np) is monoclinic, C2/c, a 27·250(3), b 3·712(1), c 15·147(3) Å, β 114·41(1)°, Z = 8, R 0·025 for No 1346. Ag(4-np).H2O is monoclinic, P21/a, a 5·613(6), b 13·191(7), c 9·844(5) Å, β 92·50(6)°, Z = 4, R 0 ·033 for No 622. Tl(4-np) is tetragonal, I 41/a, a 18·037(8), c 8·979(8) Å, Z = 16, R 0·043 for No 924. An acid salt of the latter, Tl(4-np).(4-npH)3, triclinic, P-1, a 11·861(8), b 11·45(1), c 11· 423(1) Å, α 114·00(6), β 109·78(5), γ 96·87(7)°, Z = 2, R 0·042 for No 3814, is isomorphous with its rubidium analogue. These comprise a novel array of structures: although the structures of the silver(I) complexes are two-dimensional sheets with familiar head-tail connecting ligands, a strong silver-aromatic carbon interaction is found in Ag(2-np) (Ag–C 2·496(5) Å). Tl(2-np) and Tl(4-np) both present unusual forms related to the stair-polymer and cubane adducts found in 1 : 1 coinage metal(I)/halide-unidentate nitrogen base adducts; Tl(2-np) is a double-stranded stair-polymer array, with the phenoxide oxygen atoms incorporated in the stair and the nitro oxygen atoms linking successive thallium atoms. The structure of Tl(4-np) is based on a tetranuclear cubane motif of -4 symmetry, [Tl(O-phenoxide)]4, these being linked into a three-dimensional network by further Tl · · · O-nitro interactions from adjacent units. The structure of silver(I) picrate monohydrate, isomorphous with its sodium counterpart, is also recorded: monoclinic, C 2/m, a 12·818(7), b 20·208(8), c 3· 741(1) Å, β 88·25(3)°, Z = 4, R 0·047 for No 1042, void of any significant Ag · · · C contacts.

Formation and Structural Characterization of [RuCl2(CO)2(SPh2)2], [RuCl2(CO)3(OH2)], and [Ru(OH2)6][RuCl3(CO)3]2 · 2H2O

2003 ◽  
Vol 58 (10) ◽  
pp. 959-964 ◽  
Author(s):  
Marjaana Taimisto ◽  
Raija Oilunkaniemi ◽  
Risto S. Laitinen ◽  
Markku Ahlgrén
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Three Dimensional ◽  
Temperature Reaction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimensional Network ◽  
Moderate Yield

While the room temperature reaction of [RuCl2(CO)3]2 and Ph2S in tetrahydrofuran in air affords [RuCl2(CO)2(SPh2)2] (1) in moderate yield, that in dichloromethane results in the formation of a mixture of [RuCl2(CO)3(H2O)] (2) and [Ru(H2O)6][RuCl3(CO)3]2·2H2O (3). Very small amounts of 1 are produced only upon prolonged reflux of the reagents. All compounds were characterized by X-ray crystallography. 1 crystallizes as discrete octahedral cis(CO), cis(Cl), trans(Ph2S) complexes, which are joined into stacks by weak H···Cl hydrogen bonds. 2 is also composed of discrete octahedral complexes. Four hydrogen bonds involving aqua and chlorido ligands link two complexes into a dimer. The structure of 3 consists of octahedral hexaaquaruthenium cations and two tricarbonyltrichloridoruthenate anions. The water of crystallization is involved in hydrogen bonding between the cations and anions resulting in the formation of a continuous three-dimensional network.

scholarly journals 1,3,4-Tri-O-acetyl-2-N-(trifluoroacetyl)-β-L-fucose

2014 ◽  
Vol 70 (2) ◽  
pp. o134-o135
Author(s):  
David C. McCutcheon ◽  
Peter Norris ◽  
Matthias Zeller
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Three Dimensional ◽  
Chair Conformation ◽  
X Ray ◽  
Compound C ◽  
Product Mixture ◽  
Dimensional Network ◽  
Graph Set

The title compound, C14H18F3NO8, was produced through conjugation of 1,3,4-tri-O-acetyl-2-azidodeoxy-α,β-L-fucose with trifluoroacetyl chloride in the presence of bis(diphenylphosphino)ethane in tetrahydrofuran at room temperature. The X-ray crystal structure reveals that the β-anomer of the product mixture crystallizes from ethyl acetate/hexanes. The compound exists in a typical chair conformation with the maximum possible number of substituents, four out of five, located in the sterically preferred equatorial positions. The major directional force facilitating packing of the molecules are N—H...O hydrogen bonds involving the amide moieties of neighboring molecules, which connect molecules stacked along thea-axis direction into infinite strands with aC11(4) graph-set motif. Formation of the strands is assisted by a number of weaker C—H...O interactions involving the methine and methyl H atoms. These strands are connected through further C—H...O and C—H...F interactions into a three dimensional network

Synthesis, Crystal Structure, Magnetic, Thermal and Fluorescent Properties of [Co(H2O)4(nia)2](suc)·(H2suc)

2010 ◽  
Vol 65 (6) ◽  
pp. 695-700 ◽  
Author(s):  
Selcuk Demir ◽  
Veysel T. Yilmaz ◽  
Jerzy Mroziński ◽  
Tadeusz Lis ◽  
Małgorzata Hołyńska
Keyword(s):  
Room Temperature ◽  
Complex Cation ◽  
Three Dimensional ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
Fluorescent Properties ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral

A new cobalt(II) complex, [Co(H2O)4(nia)2](suc)·(H2suc) [nicotinamide = nia, succinate = suc2−], has been synthesized and characterized by elemental analysis, IR, TG-DTA and single-crystal X-ray diffraction. It contains [Co(H2O)4(nia)2]2+ complex cations, uncoordinated suc2− anios and H2suc species. In the complex cation the cobalt(II) ion is coordinated by four aqua and two nia ligands in a distorted octahedral geometry. The suc2− dianion acts as a counter-ion, while H2suc is present as a molecule of solvation. A three-dimensional network is formed by O-H· · ·O and N-H· · ·O hydrogen bonds. The title complex exhibits luminescence in the solid state at room temperature. The magnetism of the complex was studied over the temperature range 1.8 - 300 K.

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