Coordination compounds of indium. Part 43. Indium(III) derivatives of benzenethiol, and the crystal structure of tetraphenylphosphonium bromotris(benzenethiolato)- indate(III), Ph4P[BrIn(SPh)3]

1987 ◽  
Vol 65 (4) ◽  
pp. 804-809 ◽  
Author(s):  
Raj K. Chadha ◽  
Peter C. Hayes ◽  
Hassan E. Mabrouk ◽  
Dennis G. Tuck
Keyword(s):  
Crystal Structure ◽  
Lewis Acid ◽  
Vibrational Spectra ◽  
Coordination Compounds ◽  
Monoclinic Space Group ◽  
Tetrahedral Symmetry ◽  
X Ray ◽  
Cell Dimensions ◽  
Derivatives Of ◽  
Ray Methods

In(SPh)3 is readily prepared by the reaction of InCl3 and NaSPh in methanol. The compound is a Lewis acid, forming 1:1 adducts with 2,2′-bipyridine, 1,10-phenanthroline, N,N,N′,N′-tetramethylethanediamine, bis(diphenylphosphino)ethane, and dimethylsulphoxide, and 1:2 adducts with pyridine, trimethylamine, and triphenylphosphine. Reaction with R4NX (X = Cl, Br, I) or similar salts gives R4N[XIn(SPh)3] salts, which are 1:1 electrolytes. The structure of Ph4P[BrIn(SPh)3] has been determined by X-ray methods. The crystals are monoclinic, space group P21/c, with cell dimensions a = 9.964(3) Å, b = 13.477(3) Å, c = 30.359(7) Å, α = 98.30(2)°, Z = 4, R = 0.0622 for 2924 unique observed reflections. The anion has distorted tetrahedral symmetry in the InBrS3 kernel, with In—Br = 2.527(2) Å, and In—S(av) = 2.450 Å. The vibrational spectra of In(SPh)3 and its derivatives in the region 500–200 cm−1 are discussed.

Studies on Crown Ether Complexes. XXXI. Synthesis, Properties and Structure of the Complexes of Lighter Lanthanide Nitrates With (Z)-2,3-Diphenyl-1,4,7,10,13-pentaoxacyclopentadec-2-ene (Stilbeno-15-crown-5)

1993 ◽  
Vol 46 (11) ◽  
pp. 1817 ◽  
Author(s):  
TB Lu ◽  
N Tang ◽  
MY Tan ◽  
Y Liu ◽  
KB Yu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Conductivity Measurements ◽  
X Ray ◽  
Elemental Analyses ◽  
Crown Ether Complexes ◽  
Synthesis Properties ◽  
Lanthanide Nitrates ◽  
Ray Methods

Complexes of the lighter lanthanide nitrates with stilbeno-15-crown-5 (L) have been prepared in ethyl acetate. These new complexes with the general formula Ln (NO3)3.L.H2O ( Ln = La, Ce , Pr, Nd ) have been characterized by means of elemental analyses, i.r . spectra, 1H n.m.r. spectra and conductivity measurements. The crystal structure of La(NO3)3.L has been determined by X-ray methods, and refined to a residual R 0.0513 for 4937 independent reflections with I ≥ 1.5σ(I). It crystallizes in the monoclinic space group P21/a with a 16.090(5), b 15.654(8), c 22.687(2) Ǻ, β 93.96(4)°, V 5700(4)Ǻ3, and Z 8. There are two independent La(NO3)3.L monomers in one asymmetric unit; in each the coordination number is 11.

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

The Crystal Structure of Acifluorfen {5-[2-Chloro-4-(trifluoromethyl)-phenoxy]-2-nitrobenzoic Acid}

1987 ◽  
Vol 40 (6) ◽  
pp. 1131 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
T Hari
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Phenyl Ring ◽  
Acid Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Carboxylic Acid Group ◽  
X Ray ◽  
Nitrobenzoic Acid ◽  
Cell Dimensions

The crystal structure of the herbicide acifluorfen (5-[(2-chloro-4-trifluoromethyl)]phenoxy-2- nitrobenzoic acid] has been determined by X-ray diffraction and refined to a residual of 0.051for 1124 observed reflections. Crystals are monoclinic, space group C2/c with cell dimensions a 26.848(7), b 8 .O29(2), c 19 .Ol4(6) �, ,R l34.72(2)� and Z 8. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O---0, 2.637(7) �] with the carboxylic acid group and the phenoxy group synclinally related to the first phenyl ring while the nitro substituent isessentially coplanar with the ring.

The crystal structure of horse met-myoglobin - I. General features: the arrangement of the polypeptide chains

1950 ◽  
Vol 201 (1064) ◽  
pp. 62-89 ◽  
Keyword(s):  
Crystal Structure ◽  
Optical Properties ◽  
Real Space ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Vector Density ◽  
Molecular Weights ◽  
Plausible Model ◽  
Cell Dimensions ◽  
Polypeptide Chains

The preliminary results of an X-ray study of crystalline horse met-myoglobin are described. This protein crystallizes in the monoclinic space-group P2 1 with two molecules in general positions in the unit cell. The optical properties of the crystals show that the haem groups are parallel and lie approximately in the plane containing b and the internal bisector of β. a and c Patterson projections contain ridges of high vector density perpendicular to b and 15*4A apart; it is deduced that in real space the contents of the cell are arranged in pronounced layers of alternately high and low electron density, also perpendicular to b and 15*4 A apart. The b projections also exhibit rods of high vector density, 9*5 A apart and inclined at 20° to a . These rods are identified as the vector equivalents of the polypeptide chains, which thus run parallel to [20T] and 9*5 A apart. A Patterson projection along [20T] shows the rods well-resolved and in end-on view; by making certain plausible assumptions a Fourier projection has been made along the same direction. During shrinkage the cell dimensions change in such a way that the inter-chain distance alters very little; it is deduced that the molecules have flat sides parallel to (102) and that the liquid of crystallization is situated mainly on their [20T] faces. During shrinkage liquid is withdrawn and the molecules slide past one another along their flat sides. It is not possible to determine the whole shape of the molecule unequivocally; the most plausible model is a platelet built of four parallel co-planar lengths of chain each 54 A long (see figure 13). There are striking analogies between the structures of myoglobin and of horse haemoglobin. The type of chain folding seems to be the same in the two proteins, and probably the same as in a-keratin; and it may be that myoglobin has a structure analogous to that of one of the four layers of which haemoglobin is believed to be built up, the molecular weights of the two proteins being in the ratio 1:4.

Die Kristallstruktur von Di-μ-hydroxo-bis[aquotriamminkobalt(III)]-nitrat-2-Hydrat / The Crystal Structure of Di-μ-hydroxo-bis[aquotriamminecobalt (III)] - nitrate-2-hydrate

1971 ◽  
Vol 26 (10) ◽  
pp. 987-989 ◽  
Author(s):  
Karl Wieghardt
Keyword(s):  
Crystal Structure ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Spatial Behaviour ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Ray Methods

The crystal structure of Di-µ-hydroxy-bis [aquo-triamminecobalt (III)] nitrate-2-hydrate has been determined by x-ray diffraction using counter techniques. The compound crystallizes in the monoclinic space group C2h5-P21/n with a=9.444 (2), b=9.684 (3), c=10.736 (3) Å, β=90.1 (2)°, Z= 2. A total of 1765 independent reflections was used in solving the structure, which was refined to a conventional R1-factor of 0.047. It was not possible to distinguish by x-ray methods between the oxygen and nitrogen atoms of the NH3- and H2O molecules in the complex cation, because of their similarity in point of electrostatical and spatial behaviour.

Perchlorato, Nitrato, and Acetylacetonato Complexes of Copper(I). The Crystal and Molecular Structure of Perchloratobis(tricyclohexyiphosphine)Copper(I)

1975 ◽  
Vol 53 (13) ◽  
pp. 1949-1957 ◽  
Author(s):  
Roderic J. Restivo ◽  
Abraham Costin ◽  
George Ferguson ◽  
Arthur J. Carty
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Infrared Spectra ◽  
Copper Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Cell Dimensions

Copper(I) perchlorate, nitrate, and acetylacetonate complexes of the types Cu(triphos)ClO4 (triphos = CH3C(CH2PPh2)3), Cu(Cy3P)2ClO4 (Cy3P = P(C6H11)3), Cu(triphos)NO3, Cu(Cy3P)2(HFac)(HFac = hexafluoroacetylacetonate), and Cu (Cy3P)2(TtFac) (TtFac = thienyltrifluoroacetylacetonate) have been synthesized by reduction of the corresponding perchlorate, nitrate, and acetylacetonates with tertiary phosphines. Infrared spectra indicate the presence of monodentate perchlorate groups in Cu(triphos)ClO4 and in Cu(Cy3P)2ClO4 and the crystal structure of the latter has been determined by a three-dimensional X-ray analysis using diffractometer data. The crystals are monoclinic, space group C2/c, with cell dimensions a = 18.159(6), b = 9.493(2), c = 22.182(3) Å, and β = 95.41(2)° and four molecules per unit cell. The structure was refined by block-diagonal least squares methods to a final R of 0.051 for 2617 reflections using anisotropic thermal parameters for the nonhydrogen atoms. The structure consists of discrete Cu(Cy3P)2ClO4 molecules with symmetry C2 separated by normal van der Waals distances. The copper atom is three-coordinate and the perchlorate anion is monodentate but disordered over two sites. Principal dimensions include: Cu—P 2.262(1) Å, Cu—O 2.220(7) Å, [Formula: see text][Formula: see text] and 99.8(2)°, and [Formula: see text]

Die Kristallstruktur von PPh4[MoOCl4(OCHNMe2)] / The Crystal Structure of PPh4[MoOCl4(OCHNMe2)]

1986 ◽  
Vol 41 (4) ◽  
pp. 523-526 ◽  
Author(s):  
Dieter Fenske ◽  
Kay Jansen ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Carbon Tetrachloride ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Dimethyl Formamide ◽  
Structural Investigations ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Ray Methods

Green crystals of the title compound are formed in the reaction of (PPh4)2 [Mo2(O2C -Ph)4Cl2] ·2 CH2Cl2 with dimethyl formamide/carbon tetrachloride in the presence of water. According to the structural investigations by X-ray methods PPh4[MoCl4(O CHNMe2)] crystallizes orthorhombically in the space group C2221 with four formula units per unit cell (3132 observed, independent reflexions, R - 0.068). The cell dimensions are a = 792.1 pm, b = 1656.8 pm, c = 2211.3 pm. The structure consists of PPh4⊕ cations and anions [MoOCl4(OCHNMe2)]⊖, in which the coordination sphere of the molybdenum atom is of distorted octahedral geometry. The ligands are four equatorial chlorine atoms, one terminal O atom (Mo = O 165 pm) and the O atom of the dimethyl formamide molecule (MoO 232 pm). The IR spectrum is reported

Darstellung, 11B-NMR- und Schwingungsspektren von Aminohexahydro-closo-hexaborat(1–), [B6H6(NH2)]- sowie Kristallstruktur von Cs[B6H6(NH2)] · H2O / Preparation, 11B NMR and Vibrational Spectra of Aminohexahydro-closo-hexaborate(1–), [B6H6(NH2)]-, and the Crystal Structure of Cs[B6H6(NH2)] · H2O

1995 ◽  
Vol 50 (1) ◽  
pp. 11-14 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Nmr Spectra ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Aqueous Alkaline Solution ◽  
Nmr Spectrum ◽  
X Ray ◽  
11B Nmr ◽  
Ir And Raman

Aminohexahydro-closo-hexaborate(1–), Crystal Structure, 11B NMR Spectra, Vibrational SpectraBy reduction of [B6H5(NO2)]2- with Fe2+ in aqueous alkaline solution [B6H6(NH2)]- is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] · H2O has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) A, β = 100.168(6)°. The 11B NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N–H, B–H and B6 vibrations.

The Preparation and Crystal Structure of Polymeric Anhydrous Sodium Hydrogen o-Phenylenedioxydiacetate

1992 ◽  
Vol 45 (5) ◽  
pp. 947 ◽  
Author(s):  
RC Bott ◽  
DS Sagatys ◽  
DE Lynch ◽  
G Smith ◽  
CHL Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Sodium Hydrogen ◽  
Acid Proton ◽  
Axial Bond ◽  
A Cell ◽  
Ray Methods

The crystal structure of anhydrous sodium hydrogen o-phenylenedioxydiacetate , [Na2( Hbdda )2]n, has been determined by X-ray methods and refined to a residual R 0.031 for 1234 observed reflections. Crystals are monoclinic, space group C2/c with Z 4 in a cell of dimensions a 18.415(6), b 7.4667(7), c 16.354(7) � ,β112.61(2)�. The dimeric repeating unit has two centrosymmetrically related pentagonal pyramidal Na-O6 complex centres [Na-0, 2.272-2.439(2) � ] bridged by carboxylate oxygens. The pentagonal plane comprises four oxygens from the Hbdda ligand as well as one providing the bridging link. The axial bond gives the step-polymer link while the carboxylic acid proton is hydrogen bonded to a carboxylate oxygen of the inversion-related Hbdda ligand [O…O, 2.469(2) � ].

The construction and use of an X-ray goniometer. Crystal-structure of glyoxaline compounds (With Plate I.)

1926 ◽  
Vol 21 (112) ◽  
pp. 1-9 ◽  
Author(s):  
Gilbert Greenwood
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
X Ray ◽  
Derivatives Of ◽  
Ray Methods

In ordinary circumstances crystal-angles are measured by means of light reflected from the crystal-faces. In the partial or complete absence of faces the determination of axial ratios and angles may be impossible. In a recent investigation of certain derivatives of glyoxaline, an example of this was found. It was, in fact, the substance glyoxaline itself, which always occurred as long prisms having four faces in the prism-zone; the ends of the prisms were jagged and rough, and no siglls of optically reflecting-planes could be found on these ends. In such a case, X-ray methods of investigation are now available, and the problem in question is the determination of the dimensions of the unit-cell, not the complete X-ray inveatigation of the structure.

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