<i>SIR92</i>: a powerful direct methods package

Altomare, Angelina; Cascarano, G.; Giacovazzo, Carmelo; Guagliardi, Antonietta; Camalli, Mercedes; Burla, Maria Cristina; Polidori, Giampiero

doi:10.1107/s0108767378098402

Cited by 28 publications

(31 citation statements)

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“…All calculations were performed using the teXsan crystallographic software package. The structure was solved by direct methods and expanded using Fourier techniques …”

Section: Methodsmentioning

confidence: 99%

Iron Complexes Containing the Tripodal Tetraphosphine Ligand P(CH₂CH₂PMe₂)₃

et al. 1997

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The preparation and characterization of iron(II) complexes containing the tripodal tetraphosphine ligand tris[2-(dimethylphosphino)ethyl]phosphine, P(CH(2)CH(2)PMe(2))(3) (PP(3), 1), are reported. The complex FeCl(2)(PP(3)) (2) was formed by the reaction of PP(3) with anhydrous iron(II) chloride. The complexes FeHCl(PP(3)) (3) and FeH(2)(PP(3)) (4) were formed by the reaction of 2 with lithium aluminum hydride. Likewise, the complexes FeMeCl(PP(3)) (5) and FeMe(2)(PP(3)) (6) were formed by the reaction of 2 with methyllithium or dimethylmagnesium. Reaction of 2 with CO afforded a mixture of isomeric carbonyl chloride complexes [Fe(CO)Cl(PP(3))](+) (7 and 8). Reaction of 2 with PPh(3) afforded [Fe(PPh(3))Cl(PP(3))](+) (9). The air-sensitive complexes 2-9 were characterized by multinuclear NMR spectroscopy, and 9 was characterized by X-ray crystallography. Crystals of 9 (BPh(4) salt), C(54)H(65)BClFeP(5), M 971.09, are monoclinic, space group P2(1)/c, a = 13.246(3) Å, b = 30.314(2) Å, c = 14.338(2) Å, beta = 100.92(2) degrees, Z = 4; R = 0.058.

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“…All calculations were performed using the teXsan crystallographic software package. The structure was solved by direct methods and expanded using Fourier techniques …”

Section: Methodsmentioning

confidence: 99%

Iron Complexes Containing the Tripodal Tetraphosphine Ligand P(CH₂CH₂PMe₂)₃

et al. 1997

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“…For both compounds, data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 and SAINT (Bruker, 2004); data reduction: SAINT and XPREP (Bruker, 2004); program(s) used to solve structure: SIR92 (Altomare et al, 1992); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Bruno et al, 2002); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).…”

Section: Computing Detailsmentioning

confidence: 99%

Hydrogen-bonded assemblies in the molecular crystals of 2,2′-thiodiacetic acid with ethylenediamine ando-phenylenediamine

Gomathi

Theivarasu

2017

Acta Crystallogr C Struct Chem

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Carboxylate molecular crystals have been of interest due to the presence of hydrogen bonding, which plays a significant role in chemical and crystal engineering, as well as in supramolecular chemistry. Acid-base adducts possess hydrogen bonds which increase the thermal and mechanical stability of the crystal. 2,2'-Thiodiacetic acid (Tda) is a versatile ligand that has been widely explored, employing its multidendate and chelating coordination abilities with many metals; however, charge-transfer complexes of thiodiacetic acid have not been reported. Two salts, namely ethylenediaminium 2,2'-thiodiacetate, CHN·CHOS, denoted Tdaen, and 2-aminoanilinium 2-(carboxymethylsulfanyl)acetate, CHN·CHOS, denoted Tdaophen, were synthesized and characterized by IR, H andC NMR spectroscopies, and single-crystal X-ray diffraction. In these salts, Tda reacts with the aliphatic (ethylenediamine) and aromatic (o-phenylenediamine) diamines, and deprotonates them to form anions with different valencies and different supramolecular networks. In Tdaen, the divalent Tda anions form one-dimensional linear supramolecular chains and these are extended into a three-dimensional sandwich-type supramolecular network by interaction with the ethylenediaminium cations. However, in Tdaophen, the monovalent Tda anions form one-dimensional zigzag supramolecular chains, which are extended into a three-dimensional supramolecular network by interaction with the 2-aminoanilinium cations. Thus, both three-dimensional structures display different ring motifs. The structures of these diamines, which are influenced by hydrogen-bonded assemblies in the molecular crystals, are discussed in detail.

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“…The structures were solved by direct methods using SIR 92 program. 15 The re®nements of structures were performed by full matrix least squares method (CRYSTAN 6.3). The parameters were re®ned adopting anisotropic temperature factors for non-hydrogen atoms of the donor molecules.…”

Section: Measurementsmentioning

confidence: 99%