Synthese von zweikernigen Triazenido- und Pentaazadienidokomplexen des einwertigen Silbers. Kristallstruktur von [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Py, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Py / Dimeric Triazenido and Pentaazadienido Complexes of Monovalent Silver. Synthesis and Structure of [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Pyridine, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Pyridine

1989 ◽  
Vol 44 (7) ◽  
pp. 778-785 ◽  
Author(s):  
Edmund Hartmann ◽  
Raimund Schmid ◽  
Joachim Strähle
Keyword(s):  
Unit Cell ◽  
Dinuclear Complexes ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bridging Ligand ◽  
Orange Yellow ◽  
Ag Contact ◽  
Saturated Solutions

[Ag(MeOC6H4N3C6H4OMe)]2 (1) is formed in THF from AgNO3 , and the triazenide anion, as obtained from the corresponding triazene and Na. 1 crystallizes from pyridine in the form of orange-yellow , air stable crystals with the com position 1·2/3 C5H5N: space group P 1̅ with a = 1468.0(5), b = 1514.1(6), c - 1316.1(3) pm, a = 113.45(3)°, β = 1 1 4 .8 1 (2 )°, γ = 66.78(3)°, Z - 3. The triazenide ion functions as a bridging ligand forming planar (AgN3)2 heterocycles. The unit cell contains two symmetry-independent dinuclear complexes, one of which is centrosymmetrical. The short Ag -Ag distances of 268.0 and 269.8 pm suggest Ag -Ag bonding. The pentaazadienido complexes Ag(RN5R) with R = p -MeO - C6H4 (2), p -EtO - C6H4 (3), p-Cl -C6H4 (4), p -F -C6H4 (5), are obtained from saturated solutions of the pentaazadiene in conc. NH3 and AgNO3 , as explosive, red precipitates which are stable in air. Crystals of 2 and 3 · C5H5N are obtained from pyridine. 2 crystallizes in the monoclinic space group P21/c: a - 583.7(6), b = 1705.1(9), c = 1489.6(9) pm. β = 96.2(1)°, Z = 2; 3 · C5H5N is triclinic (space group P 1̅) with a = 1160.4(4). b = 1671.0(6), c = 509.0(1) pm. a = 97.51(2)°, β = 97.36(2)°, γ = 81.51(3)°, Z = 1. The complexes 2 and 3 are dinuclear with the pentaazadienide ion as a (N1)-η1,(N5)-η1 bridging ligand in 2 and a (N1)-η1, (N3)-η1 bridging ligand in 3. The bridging mode in 3 results in a short Ag -Ag contact of 283.44 pm. The Ag -N distances range from 210.8 to 215.7 pm in 1 and from 215.0 to 220 pm in (2) and (3).

NTO Polymorphs

1992 ◽  
Vol 296 ◽  
Author(s):  
Kien-yin Lee ◽  
Richard Giloxdi
Keyword(s):  
Crystal Structure ◽  
Cell Density ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Monoclinic Form ◽  
Network Of Hydrogen Bonds ◽  
Air Bag ◽  
Ray Methods

AbstractNTO is an explosive of current interest. It has been evaluated as an insensitive component to replace RDX in the bomb fill, and as a major ingredient for the auto air bag system. The crystal structure of the β from of NTO has been determined by single-crystal X-ray methods. The unit cell is monoclinic, space group P21/c, with a = 9.326, b = 5.515, c = 9.107 Å, β = 100.77°. There are four molecules in the cell, density 1.878 g/cm3. Infinite extension of H-bonding in two-dimensional sheets occurs in the monoclinic form. Bond lengths and angles all have normal values.Efforts have been made to determine the crystal structure of α-NTO. However, a structure refined only to R = 17% was obtained, probably due to some kind of twinning about the crystal needle axis. The unit cell is triclinic, space group P1, with a = 5.12, b = 10.30, c = 17.9 Å, α = 106.7°, β= 97.7°, γ = 90.2°. There are eight molecules in the cell, density 1.92 g/cm3. Ribbons of NTO molecules formed by a relatively strong network of hydrogen bonds are observed. It was found that α-NTO is the stable, dominating form. A variety of techniques have been chosen to identify the two polymorphs.

X-ray structures of adducts of 1,2,5-triphenylphosphole with dimethyl acetylenedicarboxylate: a confirmation, a revision, and a new structure

1993 ◽  
Vol 71 (11) ◽  
pp. 1873-1889 ◽  
Author(s):  
Martin B. Hocking ◽  
Francies W. Van Der Voort Maarschalk
Keyword(s):  
Amorphous Material ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Dimethyl Acetylenedicarboxylate ◽  
Orthorhombic Space Group ◽  
Polymeric Product ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Refinement

Dimethyl acetylenedicarboxylate was reacted with 1,2,5-triphenylphosphole under mild conditions, and four products isolated. Regardless of conditions used, every preparation gave low yields of dimethyl 3,6-diphenylphthalate coincident with loss of the phosphorus bridge. NMR data and X-ray crystal structures are provided for a yellow, and a red, 2:1 adduct. The yellow adduct, tetramethyl 1,6,7-triphenyl-6-phospha(V)-tricyclo[7.3.1.01,9]nona-3,5,7-triene-2,3,4,5-tetracarboxylate 6, crystallized in the triclinic space group [Formula: see text] (No. 2) with two molecules in the unit cell. Refinement (a = 11.259(1) Å, b = 12.947(3) Å, c = 13.784(3) Å, α = 112.25(2)°, β = 103.44(1)°, and γ = 101.80(1)°) converged at R = 0.0453 (Rw = 0.0453) for 537 parameters using 2880 reflections with I > 2σ(I). The red adduct, trimethyl 1,2,5-triphenylphosphoranylidene-4-methoxycyclopent-2-ene-5-one-2,3,4-tricarboxylate, an exocyclic phosphorane 8, crystallized in the monoclinic space group P21/c (No. 14) with four molecules in the unit cell. Refinement of this structure (a = 13.233(5) Å, b = 15.712(5) Å, c = 17.191(7) Å, α = 90°, β = 110.35(4)°, and γ = 90°) converged at R = 0.0916 (Rw = 0.0937) for 400 parameters using 2052 reflections with I > 2.5σ(I). Small amounts of a white or buff amorphous material, which could represent a polymeric product from the lost phosphorus bridge, were also obtained. Thermal rearrangement of the yellow adduct gave a colourless 6,5,3 tricyclic isomer 11, possibly via the isomeric cyclopropyl derivative 15 or the nine-membered phosphonin 7. The structure of 11 was confirmed by mild oxidation of the colourless rearrangement product to its P-oxide. This product, tetramethyl 2,3,6-triphenyl-2-phosphatricyclo[6.1.01,8.05,9]-2-oxonona-3,6-diene-1,7,8,9-tetracarboxylate 12, was also colourless. It crystallized in the orthorhombic space group Pbc21 (No. 29) with four pairs of molecules in the unit cell. Refinement of this structure (a = 8.918(1) Å, b = 22.605(4) Å, and c = 30.169(6) Å) converged at R = 0.0747 (Rw = 0.0757) for 321 parameters using 3255 reflections with I > 3σ(I). Unequivocal structures for these adducts and derivatives finally confirms, and establishes further understanding of, the complex reactions of the triphenylphosphole with dimethyl acetylenedicarboxylate.

Die Röntgenstrukturanalyse der Pyrrolide (CH3)2Al - C4H3NCH3 und (CH3)2Ga - N(CCH3)4 / The X-Ray Structure Determination of the Pyrrolides (CH3)2Al - C4H3NCH3 and (CH3)2Ga - N(CCH3)4

1994 ◽  
Vol 49 (3) ◽  
pp. 430-433 ◽  
Author(s):  
Hans-Dieter Hausen ◽  
Jochen Tödtmann ◽  
Johann Weidlein
Keyword(s):  
Structure Determination ◽  
Unit Cell ◽  
Lattice Parameters ◽  
Metal Ring ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

AbstractN-M ethyl-2-dimethylaluminium pyrrolide, (CH3)2Al -C4H3NCH3, crystallizes in the triclinic space group P1̄ with the lattice constants a = 700.5(1), b = 725.9(1), c = 886.8(1) pm, α = 67.69(1)°, β = 70.99(1)°, γ = 88.48(1)°, and Z = 2. This compound is isotypic with the gallium homologue [1], the shortest metal-ring contact between the two molecules of one unit cell decreases to 228.6 pm. N-dimethylgallium tetramethylpyrrolide has been synthesized from Li-N (CCH3)4 and (CH3)2GaCl. This “π-associate” crystallizes in the monoclinic space group P21/c with the lattice parameters a = 989.9(2), b = 1305.4(3), c = 878.3(2) pm, β - 112.73(1)° and 4 units per cell. Again two centrosymmetrically orientated molecules form a dimer by short (224.0 pm) intermolecular “Ga - πC ” contacts but the structure differs significant from the structure of the indium homologue [1].

Structures and phase transition of three isomers of 1-phenylindolin-2-one derivatives: 6-chloro-1-phenylindolin-2-one, 4-chloro-1-phenylindolin-2-one and 1-(3-chlorophenyl)indolin-2-one

2018 ◽  
Vol 74 (12) ◽  
pp. 1750-1758
Author(s):  
Bing Wang ◽  
Qi Fang
Keyword(s):  
Phase Transition ◽  
Low Temperature ◽  
Phenyl Ring ◽  
Density Functional ◽  
Room Temperature ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Functional Theory ◽  
Triclinic Space Group ◽  
Space Group

Three 1-phenylindolin-2-one derivatives, namely 6-chloro-1-phenylindolin-2-one (A), 4-chloro-1-phenylindolin-2-one (B) and 1-(3-chlorophenyl)indolin-2-one (C), all C14H10ClNO, have been synthesized and the structures of these compounds at room temperature (A RT, B RT and C RT) and low temperature (A LT, B LT and C LT) have been determined. Crystal A at 295 K (A RT) crystallized in the monoclinic space group P21/c and the phenyl ring of the unique molecule exhibits disorder over two positions. At low temperature, the disorder disappeared and crystal A at 90 K (A LT) crystallized in the triclinic space group P\overline{1} with a doubled unit-cell volume and four molecules in the asymmetric unit. Density functional theory (DFT) calculations revealed a low oscillation barrier (0.24 kcal mol−1) of the phenyl ring of molecule A and the phase transition from the P21/c structure to the P\overline{1} structure can be interpreted in terms of the freezing out of the two conformations at low temperature. Crystal B retains space group P21/c in the temperature range from 100 to 297 K. A kind of obtuse-cell to acute-cell change can be recognized; if the unit cell of B LT at 100 K is set to be a standard obtuse cell [β = 90.341 (2)°] and the cell is kept untransformed in the course of temperature changing, the cell of B RT at 297 K was found to be acute [β = 89.288 (2)°]. The molecules in structure C are packed in layers, with C—H...O hydrogen bonds between neighbouring layers.

Metall-Komplexe mit S4N4 -Liganden: Die Strukturen von zwei Komplexen der Zusammensetzung [TiCl4(S4N4)]2 / Metal Complexes with S4N4 Ligands: The Structures of Two Complexes of Composition [TiCl4(S4N4)]2

1988 ◽  
Vol 43 (4) ◽  
pp. 467-471 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl
Keyword(s):  
Crystal Structure ◽  
Metal Complexes ◽  
Dinuclear Complexes ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Bridging Ligands ◽  
Space Group ◽  
Slow Reaction ◽  
Orange Yellow ◽  
Monodentate Ligands

AbstractSlow reaction of TiCl4 with S4N4 in CH2Cl2/CCl4 produces a mixture of two crystalline dinuclear complexes of composition [TiCl4(S4N4)]2. Crystal data for the orange-yellow α-isomer: mono­clinic, space group P21/n with a = 11.608(3) Å. b = 8.304(3) Å, c = 10.938(5) Å, β = 101.06(4)° and Z = 2. Crystal data for the red-brown β-isomer: monoclinic, space group P21/c with a = 11.220(2) Å, b = 13.868(2) Å, c = 14.839(4) Å, β = 106.18(2)° and Z = 4. Crystal structure analyses reveal that the S4N4 molecules in the α-form act as 1,3-N,N′-bonded bridging ligands and in the β-form as N-bonded monodentate ligands.

Metal complexes of dicamba: the crystal and molecular structures of dicamba(3,6-Dichloro-2-methoxybenzoic acid) and catena-μ-Aqua-diaquabis(3,6-dichloro-2-methoxybenzoato)zinc(II) dihydrate

1983 ◽  
Vol 36 (11) ◽  
pp. 2175 ◽  
Author(s):  
G Smith ◽  
EJ O'Reilly ◽  
CHL Kennard
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bridging Ligand ◽  
Methoxy Groups ◽  
A Cell ◽  
Methoxybenzoic Acid

The crystal structures of the herbicide, dicamba (3,6-dichloro-2-methoxybenzoic acid) and the zinc(II) complex of this acid, {[Zn(dicamba)2(H2O)3].2H2O}}n (1), have been determined from X-ray diffraction data and refined by least squares to final residuals of 0.034 and 0.043 respectively. Dicamba is triclinic, space group P1, Z 2 with a cell a 7.232(1), b 7.971(1), c 9.050(3) �, α 102.76(3), β 91.33(3), γ 110.38(1)�, while (1) is monoclinic, space group P21/n, Z 4 with a cell a 10.467(1), b 8.135(3), c 28.079(2) �, β 96.497(7)�. Dicamba forms hydrogen-bonded cyclic dimers [O---O, 2.655(7) �] with the carboxyl and the methoxy groups synclinal to the benzene ring. The dicamba ligands retain their conformation in the ZnII complex and are cis-related and unidentate [Zn-0,2.083,2.095(4) �]. Three of the waters are coordinated [Zn-0, 2.036, 2.055, 2.099(4) �] with one of these also acting as a bridging ligand between the octahedral zinc centres [Zn-0, 2.326(4) �], giving a 'linear' polymer structure [Zn-0-Zn bridge angle, 133.6(3)�]. The MnII and CoII complexes of dicamba [(2) and (3)] have been confirmed as isomorphous and isostructural with the ZnII analogue.

scholarly journals Synthesis and molecular structure of biologically significant bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) complexes with chloride and dichloridoaurate counter-ions

2019 ◽  
Vol 75 (4) ◽  
pp. 462-468 ◽  
Author(s):  
Jayaraman Selvakumar ◽  
Meredith H. Miles ◽  
David A. Grossie ◽  
Kuppuswamy Arumugam
Keyword(s):  
Crystal Lattice ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Counter Anion ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
Average Value ◽  
Counter Ions

Diffraction-quality single crystals of two gold(I) complexes, namely bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) chloride benzene monosolvate, [Au(C29H26N2O2)2]Cl·C6H6or [(NQMes)2Au]Cl·C6H6,2, and bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) dichloridoaurate(I) dichloromethane disolvate, [Au(C29H26N2O2)2][AuCl2]·2CH2Cl2or [(NQMes)2Au][AuCl2]·2CH2Cl2,4, were isolated and studied with the aid of single-crystal X-ray diffraction analysis. Compound2crystallizes in a monoclinic space groupC2/cwith eight molecules in the unit cell, while compound4crystallizes in the triclinic space groupP\overline{1} with two molecules in the unit cell. The crystal lattice of compound2reveals C—H...Cl−interactions that are present throughout the entire structure representing head-to-tail contacts between the aromatic (C—H) hydrogens of naphthoquinone and Cl−counter-ions. Compound4stacks with the aid of short interactions between a naphthoquinone O atom of one molecule and the mesityl methyl group of another molecule along theaaxis, leading to a one-dimensional strand that is held together by strong π–η2interactions between the imidazolium backbone and the [AuCl2]−counter-ion. The bond angles defined by the AuIatom and two carbene C atoms [C(carbene)—Au—C(carbene)] in compounds2and4are nearly rectilinear, with an average value of ∼174.1 [2]°. Though2and4share the same cation, they differ in their counter-anion, which alters the crystal lattice of the two compounds. The knowledge gleaned from these studies is expected to be useful in understanding the molecular interactions of2and4under physiological conditions.

X-ray structures of triphenylphosphine and 1,2,5-triphenylphosphole products with dimethyl acetylenedicarboxylate tetramer

1994 ◽  
Vol 72 (12) ◽  
pp. 2428-2442 ◽  
Author(s):  
Martin B. Hocking ◽  
Frances W. van der Voort Maarschalk
Keyword(s):  
Triphenylphosphine Oxide ◽  
Previous Method ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Dimethyl Acetylenedicarboxylate ◽  
Polymeric Product ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Data

A tetramer of dimethyl acetylenedicarboxylate, tetramethyl 4-methoxy-5-[1,2,3-tris(methoxycarbonyl)-2-cyclopropen-1-yl]-7-oxabicyclo[2.2.1]hepta-2,5-diene-1,2,3,6-tetracarboxylate 3, was recovered from old stocks of the monomer, and was also prepared thermally from the monomer by a variation of a previous method. NMR data and an X-ray crystal structure were determined for a red 1:1 adduct of this ester with triphenylphosphine. This red adduct, tetramethyl 4-methoxy-5-[1,2,3-tris(carbomethoxy)-3-triphenylphosphoranylidenepropen-1-yl]-7-oxabicyclo[2.2.1]hepta-2,5-diene-1,2,3,6-tetracarboxylate 5, crystallized in the triclinic space group P1 (No. 2) with two molecules in the unit cell (a = 12.315(2) Å, b = 12.321(2) Å, c = 14.652(2) Å, α = 110.60(1)°, β = 90.62 (1)°, and γ = 103.22(1)°). Refinement converged at R = 0.0694 (Rw = 0.0986) for 542 parameters using 4714 reflections with I > 2σ(I). Triphenylphosphine oxide did not react with tetramer 3. Reaction of the tetramer of dimethyl acetylenedicarboxylate 3 with 1,2,5-triphenylphosphole gave an orange product with concomitant loss of a furan triester. NMR data confirmed that this was not a simple adduct, and examination of a crystal by X-ray established the structure as the dichloromethane complex of tetramethyl 1,9,10-triphenyl-1-phospha(V)tricyclo[5,2,1,05,10] deca-1,3,5,8-tetraene-2,3,4,6-tetracarboxylate 10. This orange product crystallized in the monoclinic space group P21/c (No. 14) with four molecules in the unit cell (a = 10.056(2) Å, b = 14.280(1) Å, c = 23.892(3) Å, α = 90.0°, β = 94.15(1)°, and γ = 90.0°). Refinement converged at R = 0.0683 (Rw = 0.0710) for 540 parameters using 3180 independent reflections with I > 3σ(I). The tetramer 3 did not react with 1,2,5-triphenylphosphole-1-oxide quickly, but after 9 months gave a white, probably polymeric, product.

scholarly journals The structure and conformation of 1-phenyl-2-methylcyclopropene-3-carboxylic acid and cis­2-(m-nitrophenyl)cyclopropanecarboxylic acid

1983 ◽  
Vol 61 (1) ◽  
pp. 50-56 ◽  
Author(s):  
James D. Korp ◽  
Ivan Bernal ◽  
Richard Fuchs
Keyword(s):  
Carboxylic Acid ◽  
Phenyl Group ◽  
Carbonyl Oxygen ◽  
Membered Ring ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Carboxyl Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Cyclopropanecarboxylic Acid

The structures of cis-2-(m-nitrophenyl)cyclopropanecarboxylic acid (1) and 1-phenyl-2-methylcyclopropene-3-carboxylic acid (2) have been determined by X-ray methods. Crystals of 1 are triclinic, space group [Formula: see text], with a = 7.422, b = 8.615, c = 9.499 Å, α = 60.24, β = 63.76, γ = 71.36°, and two molecules in the unit cell. Crystals of 2 are monoclinic, space group P21/c, with four molecules in a unit cell of dimensions a = 9.345, b = 13.286, c = 8.187 Å, and β = 98.22°. The carboxyl group of 1 approaches the bisecting conformation. The phenyl group is 37° from this conformation, by contrast with the unhindered compound 2-(p-nitrophenyl) cyclopropyl methyl ketone. In 2 the carboxyl group bisects the three-membered ring, indicating that carbonyl-cyclopropene π interactions can occur if sterically allowed. The two rings are essentially coplanar, permitting maximum interaction of the phenyl group and the double bond. In both compounds, the carbonyl oxygen of the carboxyl is the nearer oxygen to the three-membered ring.

Studies of Some Cadmium(II) and Mercury(II) Complexes With Dicyclohexylphosphino-N-Phenylthioformamide, LH: Crystal and Molecular-Structures of [Cdl2(LH)]2, ([HgCl2(LH)]2.CH2Cl2) And HgCl2(LH)2

1986 ◽  
Vol 39 (4) ◽  
pp. 547 ◽  
Author(s):  
SW Cowan ◽  
D Dakternieks ◽  
RW Gable ◽  
BF Hoskins ◽  
CL Rolls ◽  
...  
Keyword(s):  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group ◽  
Mercury Compounds ◽  
Crystal And Molecular Structures ◽  
Tetrahedral Environment

The crystal and molecular structures of the title compounds, [CdI2(LH)]2, (1), [HgCl2(LH)]2.CH2Cl2(2), and HgCl2(LH)2(3)[where LH = dicyclohexylphosphino-N-phenyl-thioformamide,* (c-C6H11)2PC(S)N(H)Ph] have been determined by single-crystal X-ray diffraction techniques. Crystals of (1) are monoclinic, space group P21/n, a 13.051(2), b 10.183(1), c 18.106(1)Ǻ and β 101.55(8)° with Z 2; R and Rw were 0.047 and 0.044 respectively for 2320 unique, observed reflections. The unit cell contains two equivalent centrosymmetric, halogen-bridged cadmium dimers. Crystals of (2) are triclinic, space group Pī, with a 10.668(4), b 14.978(3), c 16.838(4)Ǻ, and α 111.80(2), β 101.03(2), γ 92.06(2)° with Z 2; R and Rw were 0.069 and 0.067 respectively for 3379 unique observed reflections. The structure shows two independent centrosymmetric halogen-bridged dimers within the unit cell. Crystals of (3) are monoclinic, space group C2/c, a 24.719(6), b 12.247(3), c 26.818(6) Ǻ, and β 94.62(2)° with Z 8; R and Rw were 0.075 and 0.071 respectively for 2698 unique, observed reflections. The structure shows the complex to be monomeric. In all three compounds the metal atom is in an approximately tetrahedral environment with the potentially multidentate ligand, LH, coordinating only through the phosphorus atom. The mercury compounds show a much larger deviation from ideal tetrahedral geometry than does the cadmium compound.

Sign in / Sign up

Export Citation Format

Share Document