Lewis-base adducts of Group 1 metal(I) compounds. III. Synthesis and crystal structures of the 1 : 1 adducts of silver(I) iodide with triethylamine, 2- and 3-methylpyridine and quinoline

1983 ◽  
Vol 36 (9) ◽  
pp. 1851 ◽  
Author(s):  
PC Healy ◽  
NK Mills ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Unit Cell ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray ◽  
Group 1

The crystal structures of the title compounds have been determined at 295(1) K by single-crystal X-ray diffraction methods. For [AgI(Et3N)] (1), the unit cell is tetragonal, P42/nmc, a 13.202(6),c 11.654(8) �; the structure was refined to a residual of 0.077 for 589 independent 'observed' reflections, and is isostructural with the 'pseudo-cubane' triethylphosphine and triethylarsineanalogues with two tetrameric units in the cell. For [AgI(2-MeC5H4N)] (2), the cell is orthorhombic,P212121, a 16.63(1), b 10.797(9), c 4.570(4) �, Z 4; a residual of 0.030 was obtained for 770 independent 'observed' reflections. For [AgI(3-MeC5H4N)] (3), the cell is monoclinic, P21/n, a 19.57(2), b 4.633(3), c 9.355(7) �, β 90.85(7)�, Z 4, a residual of 0.038 being obtained for 1382 independent 'observed' reflections. For [AgI(C9H7N)](4), the unit cell is monoclinic, P21/n, a 12.964(9), b 16.84(2), c 4.454(4) �, β 97.10(7)�, Z 4, a residual of 0.040 being obtained for 660 'observed' independent reflections. For compounds (2)-(4), the observed structures are all 'stairpolymers'; the structures of (2) and (3) are quite similar, but that of (4) exhibits significant differences.

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.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Structural Study of the Disordered RECd6 Quasicrystal Approximants (RE = Tb, Ho, Er, Tm and Lu)

2006 ◽  
Vol 61 (6) ◽  
pp. 644-649 ◽  
Author(s):  
Shu Ying Piao ◽  
Cesar P. Gömez ◽  
Sven Lidin
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Structural Study ◽  
Diffraction Data ◽  
Unit Cell Dimension ◽  
Unit Cell ◽  
Cell Dimension ◽  
X Ray Diffraction ◽  
X Ray ◽  
Different Types

The crystal structures of approximants RECd6 (RE = Tb, Ho, Er, Tm and Lu) have been refined from single crystal X-ray diffraction data. This work is a continuation of a previous study of MCd6 approximants [1] in which the different types of disorder of the central Cd4 tetrahedra located in the dodecahedral cavities were examined. The structures of the title compounds are all similar to GdCd6 and disorder was observed in all these compounds. There is a correlation between the anisotropic displacement parameter and the unit cell dimension

scholarly journals Synthesis, Characterization and Biological Studies of Ether–Based Ferrocenyl Amides and their Organic Analogues

Crystals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 480
Author(s):  
Sana Waseem Abbasi ◽  
Naveed Zafar Ali ◽  
Martin Etter ◽  
Muhammad Shabbir ◽  
Zareen Akhter ◽  
...  
Keyword(s):  
Single Crystal ◽  
Cell Volume ◽  
Crystal Structures ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Spectral Studies ◽  
Scavenging Activity ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Ferrocenyl amides (FB1-FB13) and their organic analogues (BZ1-BZ13) were prepared by a low-temperature condensation method. Ferrocenyl amides were synthesised using 4-ferrocenylbenzoyl chloride and ether-based amines and diamines. Benzoyl chloride was used to synthesise organic analogues by reacting with various amines. The synthesised compounds were characterised by elemental, spectroscopic (FT-IR and NMR) and single crystal X-ray diffraction methods. Crystal structures of the representative organic analogues (BZ2 and BZ6) were solved by single crystal X-ray diffraction. BZ2 crystallises in the triclinic space group P 1 ¯ with a unit cell volume of V = 1056.6(3) Å3 and with two formula units per unit cell. Whereas BZ6 assembles in the orthorhombic space group Pbca with four formula units per unit cell and a unit cell volume of V = 1354.7(2) Å3. Spectral studies confirmed the presence of amide linkages in the synthesised compound with a strong N—H·····O=C hydrogen bonding network established between amide groups of neighbouring molecular scaffolds further stabilising the molecular stacking in accordance with the archetypal crystal structures. The bioactive nature of each compound was assessed by DPPH (2,2-diphenyl-1-picrylhydrazyl) free radical scavenging activity, hydrogen peroxide scavenging activity and total antioxidant activity. Antidiabetic, anticholinesterase enzyme inhibition tests, as well as antibacterial activities, were performed showing significant biological activity for ferrocenyl amides as compared to their organic analogues.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXIX. Crystal Structures of Bis(Pyridine-4-carbonitrile)silver(I) Nitrate and Bis(4-benzoylpyridine)Silver(I) Nitrate Monohydrate

1987 ◽  
Vol 40 (9) ◽  
pp. 1603 ◽  
Author(s):  
S Gotsis ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Silver Atoms ◽  
Close Contacts

The crystal structures of the title compounds, [Ag(C6H4N2),] (NO3), (I), and [Ag(C12H9NO)2] (NO3).H2O, (2), have been determined by single-crystal X-ray diffraction methods at ~295 K, being refined by full-matrix least-squares methods to residuals of 0.042 and 0.044 for 1814 and 3434 independent 'observed' reflections respectively. Crystals of (1) and (2) are triclinic P1; for (1) a, 27.954(7), b 6.354(2), c 3.710(1)�, α 87.55(3), β 86.21(2), γ 89.35(2)�, Z 2; for (2), a 17.036(5), b 8.691(3), c 7.849(3) �, α � 107.74(2), β 97 53(2), γ 91 .11(2)�, Z 2. In both structures the formulation is basically a linearly coordinated complex cation/anion as shown above: in (I), Ag-N are 2.214(4), 2.203(4) � with N-Ag-N, 162.2(2)"; in (2), Ag-N are 2.146(3), 2.147(3) �, N-Ag-N, 175.3(1)�. The shortest Ag-O contact is found in (1) at 2.693(4)�. No close contacts are found between the silver atoms and cyano or ketonic ligand substituents.

Crystal structures of (S)- and (R,S)-2,2′-bipyridine-3,3′-dicarboxylic acid 1,1′-dioxides and of their barium salts: absolute configuration and molecular distortion enforced by supramolecular self-assembly

1997 ◽  
Vol 212 (3) ◽  
Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  
Keyword(s):  
Single Crystal ◽  
Dicarboxylic Acid ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Self Assembly ◽  
Barium Salt ◽  
X Ray Diffraction ◽  
X Ray

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(

Lewis-base adducts of Group 1B metal(I) compounds. VII. Synthesis and structures of the 1 : 1 adducts of copper(I) halides with N,N,N',N'-tetramethyletlrylenediamine

1984 ◽  
Vol 37 (11) ◽  
pp. 2207 ◽  
Author(s):  
LM Engelhardt ◽  
RI Papasergio ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray

1 : 1 adducts of N,N,N',N'-tetramethylethylenediamine ('tmeda') with copper(1) chloride, bromide and iodide have been synthesized and the structures of the solid iodide and chloride derivatives established by single-crystal X-ray diffraction methods. The iodide,(1),is monoclinic, P21/c, a 12.370(5), b 12.119(5), c 15.36(1) �, β 109.16(5)�, Z = 4 dimers; the residual R was 0.067 for 1240 'observed' reflections. The complex is a ��'-diiodobridged dimer (tmeda)CuI2Cu(tmeda); thedistance between the pair of four-coordinate copper atoms is very short [2.566(4) A]. The bromide is isomorphous with the iodide. The chloride, (2), is monoclinic, P21/n, a 14.477(3), b 15.063(3),c 9.326(2) �, β 96.99(2)�, Z = 4 formula units; R was 0.055 for No = 1195. The complex is ionic [Cu(tmeda)2]+ [CuCl2]-.

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

scholarly journals Crystal structures of two novel iron isocyanides from the reaction of 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate(−1)

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
William W. Brennessel ◽  
John E. Ellis
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Tridentate Ligand ◽  
Reductive Cyclization ◽  
X Ray Diffraction ◽  
X Ray

The reaction of the [K(18-crown-6)(thf)2]1+ (thf is tetrahydrofuran) salt of bis(anthracene)ferrate(−1), or [Fe(C14H10)2]−, with 2,6-dimethylphenyl isocyanide (CNXyl) in thf resulted in the formation of two new iron isocyanide complexes, namely, [(1,2,3,4-η)-anthracene]tris(2,6-dimethylphenyl isocyanide)iron, [Fe(C14H10)(C9H9N)3] or [Fe(1,2,3,4-η-C14H10)(CNXyl)3], and {5,6-bis(2,6-dimethylanilino)-3-(2,6-dimethylphenyl)-1,2,7-tris[(2,6-dimethylphenyl)imino]-3-azoniahept-3-ene-1,4,7-triido}tris(2,6-dimethylphenyl isocyanide)iron tetrahydrofuran disolvate, [Fe(C54H56N6)(C9H9N)3]·2C4H8O or [Fe(C54H56N6)(CNXyl)3]·2C4H8O, which were characterized by single-crystal X-ray diffraction. The former is likely an intermediate along the path to the known homoleptic [Fe(CNXyl)5], while the latter contains a tridentate ligand that is formed from the `coupling' of six CNXyl ligands. A third crystal structure from this reaction, (7-methylindol-1-ido-κN)(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6 O)potassium, [K(C9H8N)(C12H24O6)] or [K(C9H8N)(18-crown-6)], contains a 7-methylindol-1-ide anion, in which one CNXyl ligand has shed a proton during its reductive cyclization.

The structures of marialite (Me6) and meionite (Me93) in space groups P42/n and I4/m, and the absence of phase transitions in the scapolite series

2011 ◽  
Vol 26 (2) ◽  
pp. 119-125 ◽  
Author(s):  
Sytle M. Antao ◽  
Ishmael Hassan
Keyword(s):  
Phase Transitions ◽  
High Resolution ◽  
Crystal Structures ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Space Groups ◽  
Cell Parameters ◽  
The Mean

The crystal structures of marialite (Me6) from Badakhshan, Afghanistan and meionite (Me93) from Mt. Vesuvius, Italy were obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinements. Their structures were refined in space groups I4/m and P42/n, and similar results were obtained. The Me6 sample has a formula Ca0.24Na3.37K0.24[Al3.16Si8.84O24]Cl0.84(CO3)0.15, and its unit-cell parameters are a=12.047555(7), c=7.563210(6) Å, and V=1097.751(1) Å3. The average ⟨T1-O⟩ distances are 1.599(1) Å in I4/m and 1.600(2) Å in P42/n, indicating that the T1 site contains only Si atoms. In P42/n, the average distances of ⟨T2-O⟩=1.655(2) and ⟨T3-O⟩=1.664(2) Å are distinct and are not equal to each other. However, the mean ⟨T2,3-O⟩=1.659(2) Å in P42/n and is identical to the ⟨T2′-O⟩=1.659(1) Å in I4/m. The ⟨M-O⟩ [7]=2.754(1) Å (M site is coordinated to seven framework O atoms) and M-A=2.914(1) Å; these distances are identical in both space groups. The Me93 sample has a formula of Na0.29Ca3.76[Al5.54Si6.46O24]Cl0.05(SO4)0.02(CO3)0.93, and its unit-cell parameters are a=12.19882(1), c=7.576954(8) Å, and V=1127.535(2) Å3. A similar examination of the Me93 sample also shows that both space groups give similar results; however, the C–O distance is more reasonable in P42/n than in I4/m. Refining the scapolite structure near Me0 or Me100 in I4/m forces the T2 and T3 sites (both with multiplicity 8 in P42/n) to be equivalent and form the T2′ site (with multiplicity 16 in I4/m), but ⟨T2-O⟩ is not equal to ⟨T3-O⟩ in P42/n. Using different space groups for different regions across the series implies phase transitions, which do not occur in the scapolite series.

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