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) � ].

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

The Preparation and Crystal Structure of 2-Phenoxypropenoic Acid

1992 ◽  
Vol 45 (12) ◽  
pp. 2061 ◽  
Author(s):  
M Campbell ◽  
MJ Mcleish ◽  
DE Lynch ◽  
G Smith ◽  
KA Byriel ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Benzene Ring ◽  
Dihedral Angle ◽  
Side Chain ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Carboxylic Acid Groups ◽  
A Cell ◽  
Ray Methods

The potential herbicide 2-phenoxypropenoic acid has been synthesized, and its structure has been determined by X-ray methods and refined to a residual R 0.068 for 564 observed reflections. Crystals are orthorhombic, space group Pbca with Z 8 in a cell of dimensions a 5.6547(9), b 9.263(2), c 31.76(1) � . The carboxylic acid groups form centrosymmetric hydrogen-bonded cyclic dimers [O…O 2.62(1) � ], while the oxypropenoic acid side chain is essentially planar but inclined to the plane of the benzene ring [dihedral angle 71.5(7)°].

Crystal structure of 9-Oxofluorene-4-carboxylic acid

1981 ◽  
Vol 34 (5) ◽  
pp. 1143 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
A Cell

The crystal structure of 9-oxofluorene-4-carboxylic acid has been determined by direct methods using three-dimensional X-ray diffraction data, and refined to R0·068 for 1323 'observed' reflections. Crystals are monoclinic, space group P21/c with 24 in a cell of dimensions a 3·843(3), b 7·986(5), c 3269(2) �, β 96·64(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O···O 2·642(3) �] with the plane of the carboxylic acid making an angle of 26·5� with that of the 9-oxofluorene group. Stacks of molecules form down the a axis with 3.843 �. separation.

Molecular Cocrystals of Carboxylic Acids. XII. Structures of the 1 : 1 Adducts of 4-Nitrobenzoic Acid and 3,5-Dinitrobenzoic Acid With N,N'-Bis(1-methylethyl)-6-methylthio-1,3,5-triazine-2,4-diamine (Prometryn)

1993 ◽  
Vol 46 (6) ◽  
pp. 921 ◽  
Author(s):  
DE Lynch ◽  
G Smith ◽  
KA Byriel ◽  
CHL Kennard
Keyword(s):  
Carboxylic Acid ◽  
Acid Group ◽  
Side Chain ◽  
Monoclinic Space Group ◽  
Carboxylic Acid Group ◽  
Triazine Herbicide ◽  
X Ray ◽  
Nitrobenzoic Acid ◽  
A Cell ◽  
Ray Methods

Two 1:1 molecular adducts of the s- triazine herbicide prometryn [N,N′- bis (1-methylethyl)-6-methylthio-1,3,5-triazine-2,4-diamine] with 4-nitrobenzoic acid, [(C7H4NO4)-(C10H20N5S)+.H2O] (1), and with 3,5-dinitrobenzoic acid, [(C7H3N2O6)-(C10H20N5S)+] (2), have been prepared and characterized. The structure of (1) has been determined by X-ray methods and refined to a residual R 0.055 for 2072 observed reflections. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 7.191(4), b 28.359(8), c 10.990(6) Ǻ, β 104.75(3)°. The carboxylic acid group protonates a nitrogen of the triazine ring and is involved in a cyclic hydrogen-bonding association with this and with a secondary amine of the side chain [N…O, 2.76, 2.78(1)Ǻ], while the second amine is associated with the lattice water [N…O, 2.90(1)Ǻ]. Spectroscopic methods have been used to confirm the similarity of the molecular associations involving the carboxylic acid groups of the aromatic acids and prometryn in both (1) and (2).

The Crystal Structure of KIO3.HIO3

1971 ◽  
Vol 49 (3) ◽  
pp. 468-476 ◽  
Author(s):  
Lilian Y. Y. Chan ◽  
F. W. B. Einstein
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Potassium Hydrogen ◽  
A Cell ◽  
Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

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.

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

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.

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.

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.

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