Synthesis and Structures of Bis- and Tris-(triphenylarsine)gold(I) Iodides

2020 ◽  
Vol 73 (6) ◽  
pp. 497
Author(s):  
Graham A. Bowmaker ◽  
Peter C. Healy ◽  
Alexandre N. Sobolev ◽  
Allan H. White
Keyword(s):  
Crystalline Phase ◽  
Structural Parameters ◽  
X Ray Diffraction ◽  
Coinage Metal ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
Triclinic Phase ◽  
Yield Trends ◽  
Metal Ligand

The title compounds [(Ph3As)2AuI] and [(Ph3As)3AuI] have been crystallized from equimolar solutions of Bu4NAuI2 and AsPh3 in dimethylformamide and structurally characterized by single crystal X-ray diffraction studies. [(Ph3As)2AuI] crystallizes in space group C2/c, Z 4, and is isomorphous with other [(Ph3E)2MX] (MX=coinage metal(i) salt) arrays, with the Au–I bond being disposed on a crystallographic 2-axis: Au–I, As 2.7008(2), 2.4337(2) Å, As–Au–As, I 125.736(8)°, 117.132(4)° (153K). [(Ph3As)3AuI] crystallizes as a triclinic phase in space group , Z 4, and is isomorphous with [(Ph3Sb)3CuI] and [(Ph3P)3AgI]: Au–As 2.4847–2.5049(10), Au–I 2.8518(8), 2.8597(7) Å with As–Au–As, I 109.67(3)–115.97(3)°, 101.33(2)–106.85(3)°. A second ‘[(Ph3As)3AuI]’ product was obtained as a co-crystalline phase in space group P21/n containing [(Ph3As)3AuI], and [(Ph3As)2AuI] accompanied by an additional unbound Ph3As molecule, i.e. [(Ph3As)3AuI]·[(Ph3As)2AuI·Ph3As], with structural parameters closely similar to those for the corresponding separate [(Ph3As)3AuI] and [(Ph3As)2AuI] complexes described above. Comparison of the bond lengths for these and related complexes show that they are generally consistent with the ‘gold is smaller than silver’ phenomenon caused by relativistic orbital contraction effects in gold, but the results also show that the magnitude of this effect is dependent on the nature of the metal–ligand bonds involved, and on changes in the metal coordination environment, which can in some circumstances yield trends in which the effect on particular bonds is partially masked or even reversed.

The Crystal and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

scholarly journals Structure determination and phase transition behaviour of dimethyl sulfate

2006 ◽  
Vol 62 (2) ◽  
pp. 280-286 ◽  
Author(s):  
Richard M. Ibberson ◽  
Mark T. F. Telling ◽  
Simon Parsons
Keyword(s):  
Phase Transition ◽  
Dimethyl Sulfate ◽  
Monoclinic Structure ◽  
Orthorhombic Structure ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
First Order ◽  
Transition Behaviour

The crystal structures of phase I and phase II of dimethyl sulfate, (CH3O)2SO2, have been determined using complementary high-resolution neutron powder and single-crystal X-ray diffraction techniques. Below its melting point of 241 K dimethyl sulfate crystallizes in an orthorhombic structure (I) in the space group Fdd2. On cooling below ∼175 K the crystal transforms to a monoclinic structure (II) in the space group I2/a. The molecule is located on a twofold axis (Z′ = 1/2) in both structures. The phase transition is of first order with strong hysteresis. The phase transition results in changes to both the intra- and the intermolecular coordination environment.

scholarly journals Zirconium tetrachloride revisited

2018 ◽  
Vol 74 (3) ◽  
pp. 307-311
Author(s):  
Rosendo Borjas Nevarez ◽  
Samundeeswari Mariappan Balasekaran ◽  
Eunja Kim ◽  
Philippe Weck ◽  
Frederic Poineau
Keyword(s):  
Phase Transformation ◽  
Single Crystal ◽  
Structural Parameters ◽  
X Ray Diffraction ◽  
Zirconium Tetrachloride ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Temperature Range ◽  
Crystallographic Study

Zirconium tetrachloride, ZrCl4, is a strategic material with wide-ranging applications. Until now, only one crystallographic study on ZrCl4has been reported [Krebs (1970).Z. Anorg. Allg. Chem.378, 263–272] and that was more than 40 years ago. The compound used for the previous determination was prepared from ZrO2and Cl2–CCl4, and single-crystal X-ray diffraction (SCXRD) studies on ZrCl4obtained from Zr metal have not yet been reported. In this context, we prepared ZrCl4from the reaction of Zr metal and Cl2gas in a sealed tube and investigated its structure at 100, 150, 200, 250, and 300 K. At 300 K, the SCXRD analysis indicates that ZrCl4crystallizes in the orthorhombic space groupPca21[a= 6.262 (9),b= 7.402 (11),c= 12.039 (17) Å, andV= 558.0 (14) Å3] and consists of infinite zigzag chains of edge-sharing ZrCl6octahedra. This chain motif is similar to that observed previously in ZrCl4, but the structural parameters and space group differ. In the temperature range 100–300 K, no phase transformation was identified, while elongation of intra-chain Zr...Zr [3.950 (1) Å at 100 K and 3.968 (5) Å at 300 K] and inter-chain Cl...Cl [3.630 (3) Å at 100 K and 3.687 (9) Å at 300 K] distances occurred.

Synthesis and Crystal Structures of ATi[Nb6Cl18] Compounds (A = K, Rb, Cs, In, Tl)

2000 ◽  
Vol 55 (2) ◽  
pp. 139-144 ◽  
Author(s):  
A. Nägele ◽  
E. Anokhina ◽  
J. Sitar ◽  
H.-J. Meyer ◽  
A. Lachgar
Keyword(s):  
Structure Refinement ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Crystal System ◽  
Rhombohedral Crystal

Abstract New quaternary niobium cluster chlorides corresponding to the general formula ATi[Nb6Cl18] (A = K, Rb, Cs, In, Tl) have been synthesized in sealed quartz tubes at 720 °C, starting from stoichiometric amounts of NbCl5, niobium metal, TiCl3, and ACl (A = K, Rb, Cs), or In or Tl metals. The structures of RbTi[Nb6Cl18] and CsTi[Nb6Cl18] were determined using single­ crystal X-ray diffraction. RbTi[Nb6Cl18] crystallizes in the rhombohedral crystal system, space group R3̄ (no. 148), Z = 3, with lattice parameters: a = 9.163(4), c = 25.014(14) Å (hexagonal setting). The structure refinement converged to R1 = 0.044 and wR2 = 0.058 for all data. In this structure, discrete [Nb6Cl18]4-cluster units are linked by Rb+ and Ti3+ cations, located in a 12-coordinated anticubeoctahedral and octahedral chloride coordination environment, respectively. In contrast, CsTi[Nb6Cl18] crystallizes in the trigonal crystal system, space group P3̄1c (no. 163), Z = 2. The lattice parameters were determined to be a = 9.1075(6), c = 17.0017(8) Å. The structure refinement gives the reliability factors R1 = 0.029 and wR2 = 0.063 for all data. The structure is built up of discrete octahedral [Nb6Cl18]4- cluster units, linked by Cs+ and Ti3+ cations which are located in a distorted hexagonal antiprismatic and octahedral chloride coordination environment, respectively. The structures of the compounds ATi[Nb6Cl18] (A = K, In, Tl) were found to be isotypic with RbTi[Nb6Cl18], and their unit cell parameters were refined using X-ray powder diffraction analysis.

scholarly journals Crystal structures and comparisons of huntite aluminum borates REAl3(BO3)4 (RE = Tb, Dy and Ho)

2020 ◽  
Vol 76 (3) ◽  
pp. 339-343 ◽  
Author(s):  
Saehwa Chong ◽  
Brian J. Riley ◽  
Zayne J. Nelson ◽  
Samuel N. Perry
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Structural Parameters ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Slow Cooling ◽  
Spontaneous Crystallization ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Three huntite-type aluminoborates of stoichiometry REAl3(BO3)4 (RE = Tb, Dy and Ho), namely, terbium/dysprosium/holmium trialuminium tetrakis(borate), were synthesized by slow cooling within a K2Mo3O10 flux with spontaneous crystallization. The crystal structures were determined using single-crystal X-ray diffraction (SC-XRD) data. The synthesized borates are isostructural to the huntite [CaMg3(CO3)4] structure and crystallized within the trigonal R32 space group. The structural parameters were compared to literature data of other huntite REAl3(BO3)4 crystals within the R32 space group. All three borates fit well into the trends calculated from the literature data. The unit-cell parameters and volumes increase linearly with larger RE cations whereas the densities decrease. All of the crystals studied were refined as inversion twins.

Structural studies of dithiatetrazocines: X-ray crystal structures of the symmetric dithiatetrazocines p-XC6H4CN4S2CC6H4X [X = NO2, Br] and the first unsymmetric dithiatetrazocine, p-BrC6H4CN4S2CC6H4NO2

2002 ◽  
Vol 80 (11) ◽  
pp. 1507-1517 ◽  
Author(s):  
Andrew D Bond ◽  
Delia A Haynes ◽  
Jeremy M Rawson
Keyword(s):  
Intermolecular Interactions ◽  
Crystal Engineering ◽  
Molecular Electrostatic Potential ◽  
Monoclinic Space Group ◽  
Molecular Electrostatic Potentials ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Triclinic Phase

Oxidation of equimolar amounts of [p-BrC6H4CNSSN]Cl and [p-O2NC6H4CNSSN]Cl with elemental O2 in the presence of Ph3Sb in MeCN yields a mixture of the symmetric dithiatetrazocines, O2NC6H4CN4S2CC6H4NO2 (1) and BrC6H4CN4S2CC6H4Br (2) as well as the unsymmetrically substituted derivative BrC6H4CN4S2CC6H4NO2 (3). The structures of compounds 1–3 are determined by X-ray diffraction: 1 crystallizes in the monoclinic space group P21/c (a = 8.6397(4), b = 5.8359(4), c = 14.9767(11) Å, β = 92.088(4)°) with half a molecule in the asymmetric unit; 2 crystallizes in the triclinic space group P[Formula: see text] (a = 6.5330(5), b = 8.2084(6), c = 14.7264(9) Å, α = 84.483(4)°, β = 77.112(4)°, γ = 87.879(3)°); 3 was found to crystallize in two forms: recrystallization from CH2Cl2 at room temperature yielded a solvent-free, triclinic phase, space group P[Formula: see text] (a = 6.5060(9), b = 7.0739(9), c = 9.1164(8) Å, α = 81.860(3)°, β = 83.406(5)°, γ = 66.589(5)°), whereas cooling a solution to –5°C yielded a solvated form, 3·CH2Cl2, which crystallizes in the monoclinic space group P21/m (a = 6.179(1), b = 10.960(2), c = 13.884(3) Å, β = 92.69(3)°). The NO2···Br intermolecular interactions observed in the unsolvated structure of 3 are disrupted in the solvate structure; the CH2Cl2 molecule in the latter is aligned such that its molecular dipole interacts with both nitro and bromo groups, retaining a molecular chain motif. The structures are discussed in relation to their semi-empirically calculated molecular electrostatic potentials and calculations of intermolecular interactions using van der Waals forces combined with an electrostatic point charge model.Key words: dithiatetrazocine, crystal structure, crystal engineering, molecular electrostatic potential.

Synthesis, Structures and Magnetic Properties of 1D Cu(II)-NIT Radical Complex

2021 ◽  
Vol 13 (7) ◽  
pp. 1253-1258
Author(s):  
Cai-Wen Zhang ◽  
You-Juan Zhang ◽  
Jing Chen ◽  
Qing-Lun Wang
Keyword(s):  
Magnetic Properties ◽  
Single Crystal ◽  
Magnetic Interactions ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
Coordination Modes ◽  
Radical Complex ◽  
Ferromagnetic Interactions

ABSTRACTAn 1D Cu(II) complex, which formula is [Cu(hfac)2NITpPy]n (1) (NITpPy = 2-(4-pyridyl)-4,4,5,5-tetra-methylimidazoline-1-oxyl-3-oxide, hfac = hexafluoroacetylacetonate) has been synthesized and characterized by single crystal X-ray diffraction. The complex 1 crystallizes in the triclinic pī space group. Two adjacent Cu(II) ions with different coordination modes are bridged by NITpPy to form a magnetic zig-zag chain. In the built chains, the Cu(II) ions located in the CuO4N2 coordination environment and the >N–O–Cu(II)- O–N< hetero-spin clusters of the CuO6 units are alternately arranged, which lead to two different Cu-NITpPy magnetic interactions. The fit parameters (J1 = −3.56 cm−1 and J2 = 0.46 cm−1) indicate an antiferromagnetic and ferromagnetic interactions in the complex 1.

scholarly journals Structural and photoluminescent studies of non-centrosymmetric manganese(II) N-(2-pyridylmethyl)-(L)-alanine) dicyanamide

2019 ◽  
Vol 10 (3) ◽  
pp. 267-272
Author(s):  
Bridget Ndoye Ndosiri ◽  
Katia Nchimi Nono ◽  
Paboudam Gbambie Awawou ◽  
Emmanuel Ngwang Nfor ◽  
Aminou Mohamadou ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Octahedral Coordination ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray

The dinuclear compound, [Mn2(Pyala)2(Dca)2(H2O)]n·2H2O (1) (Pyala = N-(2-pyridylmethyl)-L-alanine and Dca = dicyanamide anion) has been synthesized and characterized by elemental analysis, IR and single crystal X-ray diffraction techniques. The crystal data for C22H26Mn2N10O6: orthorhombic, space group P212121 (no. 19), a = 10.3728(8) Å, b = 15.9780(12) Å, c = 16.3585(13) Å, V = 2711.2(4) Å3, Z = 4, T = 198(2) K, μ(MoKα) = 0.989 mm-1, Dcalc = 1.559 g/cm3, 129607 reflections measured (3.564° ≤ 2Θ ≤ 60.046°), 7923 unique (Rint = 0.0324, Rsigma = 0.0155) which were used in all calculations. The final R1 was 0.0169 (I > 2σ(I)) and wR2 was 0.0458 (all data). The obtained non-centrosymmetric dinuclear Mn(II) complex contains two unique Mn(II) cations with similar octahedral coordination environment. Photoluminescent measurements on the complex in the solid state show that it displays strong photoluminescence at 442 nm.

Crystal structure of an inclusion complex between chiral monoaza-15-crown-5 and S(–)-1-phenyl-ethyl ammonium percholorate

2003 ◽  
Vol 218 (5) ◽  
Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören
Keyword(s):  
Crystal Structure ◽  
Inclusion Complex ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
New Type

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

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