The Preparation and Crystal Structure of Ammonium Bis[citrato(3-)]cuprate(II)

1991 ◽  
Vol 44 (10) ◽  
pp. 1495 ◽  
Author(s):  
RC Bott ◽  
DS Sagatys ◽  
DE Lynch ◽  
G Smith ◽  
CHL Kennard ◽  
...  

The copper(II) complex with citric acid (NH4)4 [Cu(C6H5O7)2] has been prepared, and its structure determined by X-ray diffraction, giving a residual R 0.035 for 1208 observed reflections. Crystals are monoclinic, space group P21/c with Z 2 in a cell of dimensions a 8.755(3), b 13.185(4), c 9.364(2)Ǻ, β 113.73(2)°. The complex is a centrosymmetric six-coordinate monomer which is isomorphous with ammonium zinc(II) citrate. However, the Cu-O(hydroxyl) bonds [2.341(3)Ǻ] show Jahn-Teller distortion relative to the Cu-O(carboxyl) bonds [1.969(3) and 1.977(3)Ǻ].

1981 ◽  
Vol 34 (5) ◽  
pp. 1143 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar

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.


1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.


2002 ◽  
Vol 57 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Beatriz S. Parajón-Costaa ◽  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Eduardo E Castellano

The crystal structure of [Cu(sac)2(nic)2(H2O)] (sac = saccharinate anion; nic = nicotinamide) has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c with Z = 4 and the Cu(II) ion presents a CuN4O square pyramidal coordination. Some comparisons with related structures are made and the most important features of its IR spectrum were also discussed.


1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)


2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.


1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.


1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard

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.


1983 ◽  
Vol 36 (5) ◽  
pp. 1043 ◽  
Author(s):  
RM Carman ◽  
E Horn ◽  
CHL Kennard ◽  
G Smith ◽  
MR Snow ◽  
...  

The crystal structure of (1S,3S,4R)-1,3,8-tribromo-p-menthan-2-one has been determined from X-ray diffraction data and refined to a final residual of 0.075 for 635 'observed' reflections. Crystals are orthorhombic, of space group P212121 with four molecules in a cell of dimensions a 15.248(3), b 12.189(3), c 7.201(2) �. The analysis confirms that the molecule exists in a distorted twist-boat conformation.


1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae

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.


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