A New Copper (II) Complex with the N,N'-Bis(antipyryl-4-methyl)-piperazine (BAMP) Ligand: [Cu(BAMP)](ClO4)2

2002 ◽  
Vol 57 (12) ◽  
pp. 1454-1460 ◽  
Author(s):  
Otilia Costișor ◽  
Ramona Tudose ◽  
Ingo Pantenburg ◽  
Gerd Meyer

The synthesis of the Mannich base N,N’-bis(antipyryl-4-methyl)-piperazine (BAMP) (1), its crystal structure as well as the synthesis and the crystal structure of the copper complex Cu(BAMP)(ClO4)2 (2) are reported. C28H34N6O2 ∙ 4H2O (BAMP ∙ 4H2O) crystallizes with triclinic symmetry, space group P1̄, lattice parameters: a = 704,9(2), b = 983,4(2), c = 1198,9(3) pm, α = 68,72°, β = 73,62°, γ = 78,49°. The copper-complex Cu(BAMP)(ClO4)2 crystallizes with tetragonal symmetry, space group P42/n, lattice parameters: a = 2295,1(3), c = 1412,2(2) pm. The copper(II) atom is five-coordinate by the two nitrogen atoms belonging to the piperazine ring and the oxygen atoms of the antipyrinemoieties. The geometry of the copper(II) atom can be described as a square-based pyramid with the N2O2 donor atoms of BAMP forming the basal plane and an oxygen atom of the neighbouring complex molecule occupying the apical position. BAMP acts as a tetradentate ligand, which incorporates a piperazine-fused ring. The structural parameters illustrate well the reinforcing effect exerted by the double “straps” of the piperazine molecule.

1994 ◽  
Vol 49 (3) ◽  
pp. 355-359 ◽  
Author(s):  
F.-D. Martin ◽  
H. Müller-Buschbaum

Abstract Single crystals of KBaCuV2O7Cl have been prepared by a flux technique and investigated by X-ray analysis. The compound crystallizes with tetragonal symmetry, space group C24v-P4 bm, a = 8.8581, c = 5.4711 Å, Z = 2. The crystal structure shows Cu2+ within a one sided strongly distorted CuO4Cl2 octahedron. The copper ion is shifted towards the nearer Cl- neighbour to form a CuO4Cl square pyramid. Two VO4 tetrahedra are connected to give stretched V2O7 double tetrahedra, and linked in planes via the oxygen corners of the CuO4Cl pyramids. The crystal structure and the structure of the complex BaO8Cl2 polyhedron are discussed.


1997 ◽  
Vol 52 (5) ◽  
pp. 553-556 ◽  
Author(s):  
O. Sfreddo ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of Ba13Dy8Zn4Pt4O37 have been prepared by reaction of mixtures of BaCO3, ZnO and DyO3 at temperatures up to 1225 °C using platinum crucibles. X-ray investigations led to a new crystal structure with tetragonal symmetry, space group C4h5-I4/m, a = 18.659(7), c = 5.734(2) Å, Z = 2. The structure is characterized by PtO6 and BaO6 octahedra as well as by tetragonal ZnO5 pyramids and single capped trigonal prisms of oxygen around dysprosium. The remaining barium positions show coordination numbers of nine and ten. The crystal structure has large ∞1[(PtDy4O)6)4] polyhedra tunnels. Considering the ∞1[Ln4O16]20- polyhedra groups some parts of the structure show similarities to BaZnLn2O5, Ba5Zn4Ln8O21 and Ba2Ln2ZnPtO8.


1997 ◽  
Vol 52 (9) ◽  
pp. 1067-1071 ◽  
Author(s):  
O. Sfreddo ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of Ba17Dy16Zn8Pt4O57 (I), Ba17Ho16Zn8Pt4O57 (II), Ba17Er16Zn8Pt4O57 (III) and Ba17YZn8Pt4O57 (IV) have been prepared by high temperature reactions using platinum crucibles. X-ray investigations led to tetragonal symmetry, space group C54h - I4/m, (I) - (IV): a = 22.905(1), 22.840(1), 22.795(1), 22.848(1) Å and c = 5.728(1), 5.722(1), 5.700(1), 5.709(1) Å,Z = 2. The crystal structure is characterized by small square, medium-sized quadrangular and large rectangular tunnels, which are filled by oxygen, barium and zinc. The polyhedra network is discussed with respect to the network of compounds of the Ba13Dy8Zn4Pt4O37 type.


1994 ◽  
Vol 49 (11) ◽  
pp. 1459-1462 ◽  
Author(s):  
F.-D. Martin ◽  
Hk. Müller-Buschbaum

Single crystals of K4CuV5O15Cl were prepared by crystallization from the melt. The yellow brown crystals show tetragonal symmetry, space group C14-P4, a = 8.8690, c = 5.4196 Å, Z = 1. K4CuV5O15Cl is strongly related to KBaCuV2O7Cl and K2V3O8. V(1) shows V2O7 double tetrahedra connected by square VO5 and CuO4Cl pyramids. The crystal structure is discussed with respect to the related compounds.


1996 ◽  
Vol 51 (4) ◽  
pp. 493-497 ◽  
Author(s):  
S. Münchau ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of K4CdV5O15Cl have been prepared by crystallization from melts. The yellow crystals show tetragonal symmetry, space group C14-P4, a = 9.097(1), c = 5.331(2) Å, Z = 1. K4CdV5O15Cl belongs to the K4CuV5O3Cl type. V (l) forms V2O7 double tetrahedra connected by square V(2)O5 pyramids and CdO4Cl2 octahedra. The crystal structure is dis­cussed with respect to the isotypic compound K4CuV5O15Cl considering a short V(2)-O distance indicative of a vanadinyl group.


Author(s):  
Takaharu Araki

AbstractAn approach to structure determination for a crystal from component crystals in equal volume fractions, the most difficult case to the solution, is outlined with precautions for stepwise initialization. Proper selection of a crystal geometrical symmetry space group from a corresponding twin anti-symmetry space group and interpretation of a Patterson space are indispensable prerequisite for the solution. Observations unique to the case are briefly described in a sequence of Patterson synthesis, Fourier approach and least-squares refinement for efficient interpretation and processing.


1995 ◽  
Vol 50 (2) ◽  
pp. 252-256 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of AgKCu3Mo4O16 have been prepared by crystallization from melts and investigated by X-ray diffractometer techniques. This compound crystallizes with monoclinic symmetry, space group C2h5 - P21/c, a = 5.056(1), b = 14.546(4), c = 19.858(9) Å, β = 86.64(5)°, Z = 4. The crystal structure of AgKCu3Mo4O16 is closely related to K2Cu3Mo4O16 showing ribbons of edge-sharing CuO6 and AgO7 polyhedra. The ribbons are linked by tetrahedrally coordinated molybdenum and K2O10 groups. Another kind of MoO4 tetrahedra occupies the cavities inside the ribbons. The crystal structure and the coordination of silver, copper, potassium and molybdenum by oxygen are discussed with respect to K2Cu3Mo4O16.


1996 ◽  
Vol 51 (4) ◽  
pp. 469-472 ◽  
Author(s):  
D. Frerichs ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of Zn2.28Mg0.72(AsO4)2 have been prepared by CO2 LASER techniques. The compound crystallizes with monoclinic symmetry space group C52h-P21/n and the lattice parameters a = 5.292(2), b = 8.450(3), c = 7.737(3) Å , β = 96.33(3)°, Z = 2. Zn2.28Mg0.72(AsO4)2 is isotypic to β-Zn3(AsO4)2. The formation of the β-Zn3(AsO4)2 struc­ture instead of other possible orthoarsenates is discussed.


1995 ◽  
Vol 50 (4) ◽  
pp. 585-588 ◽  
Author(s):  
S. Frenzen ◽  
Hk. Müller-Buschbaum

Single crystals of Ba9Ru3.2Mn5.8O27 have been prepared by flux techniques. X-ray four circle diffractometer measurements led to trigonal (rhombohedral) symmetry, space group D53d - R3̄̄̄m , a = 5.7043(5), c = 21.255(4) Å , Z = 1. This phase is isotypic to BaRuO3. The crystal structure and the occupation of the M3O12 triple octahedra by ruthenium and manganese are discussed with respect to other oxides containing M3O12 groups in an ordered and disordered way.


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