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1

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Synthesis and structure of tetrakis(2,6-dichlorophenoxide) bis(THF) uranium(IV) (2000)

Wilkerson, Marianne P. ; Burns, Carol J. ; Paine, Robert T. ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 7-10

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ISSN: 1572-8854

Keywords: crystal structure ; uranium (IV) ; dichlorophenoxide

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The reaction of UCl4 with KO-2,6-Cl2C6H3 in tetrahydrofuran results in the preparation of the title compound. The six-coordinate complex possesses pseudo-octahedral geometry about uranium, with U-O(phenoxide) bond lengths in the range 2.161(11) to 2.178(10) Å and U-O(THF) bond lengths of 2.467(10) and 2.475(11) Å. This complex crystallizes in the monoclinic space group P21/n (a = 11.169(2), b = 11.588(2), c = 35.119(5) Å, β = 92.11(1)°, V = 4542.2(13) Å3, and Z = 4).

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009594612946

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2

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Synthesis and crystal structure of hexakis(N-methylimidazole) iron(II) pyridine-2-sulfonate (2000)

García-Vázquez, José A. ; Romero, Jaime ; Sousa-Pedrares, Antonio ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 23-26

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ISSN: 1572-8854

Keywords: iron ; crystal structure ; synthesis ; N-methylimidazole

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The compound [Fe(C4H6N2)6][C5H4NSO3]2 crystallized in the monoclinic space group, P21/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, β = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C4H6N2)6]+2 hexacoordinated iron(II) cation and two C5H4NSO− 3 anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1i,N5i atoms are coplanar and the iron lies in this plane.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009537830693

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3

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Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol) (2000)

Zhang, Cun-Gen ; Leng, Yong-Jun ; Yan, De-Yue ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 35-38

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ISSN: 1572-8854

Keywords: copper(II) ; aminoalcoholato ; hydrogen bonding ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The copper complex, [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-μ2-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, α = 100.07(2), β = 104.33(3), γ = 72.79(2)°, V = 1471.8(7) Å3, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa− ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009542031602

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4

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Synthesis and crystal structure of manganese(III) hydroxyl-containing Schiff base complexes: [Mn(III)(Hvanpa)2]N3 (H2vanpa = 1−(3-hydroxysalicylaldeneamino)-3-hydroxypropane) (2000)

Zhang, Cungen ; Mei, Yamin ; Yan, Deyue

Springer

Journal of chemical crystallography 30 (2000), S. 39-42

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ISSN: 1572-8854

Keywords: manganese(III) ; Schiff base ; hydrogen bonding ; crystal structure ; Jahn-Teller distortion

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The manganese complex, [Mn(III)(Hvanpa)2]N3 has been prepared and the crystal structure determined using x-ray crystallography. The mononuclear complex has a six-coordinate octahedral geometry. The complex crystallizes in the monoclinic space group P21/c with a = 9.867(1), b = 13.316(2), c = 9.0110(1) Å, β = 107.870(1)°, V = 1126.8(2) Å3, and Z = 2. The Mn-O and Mn-N distances in the equatorial plane are in good agreement with those found for other manganese(III) Schiff base complexes. In the axial direction, the Mn-O distances of 2.274(2) Å is about 0.3 Å longer than those in the equatorial plane due to a Jahn-Teller distortion at the d4 manganese(III) center. In the crystal, each azido ion is linked through hydrogen bonding with two hydrogen atoms from the coordinate hydroxyl groups at the apical site.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009594015672

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5

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Preparation, characterization and crystal structure of an intermolecular compound based on H3PMo12O40·nH2O and diethylamine (2000)

Niu, Jing-Yang ; Wang, Jing-Ping ; Yan, Bo ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 43-48

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ISSN: 1572-8854

Keywords: molybodophosphoric acid ; crystal structure ; diethylamine

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract An intermolecular compound, H3PMo12O40·5(CH3CH2)2NH·H2O, between the heteropolymolybdate α-H3PMo12O40 and the organic substrate diethylamine, has been synthesized and characterized. Light yellow crystals of the title compound were crystallized from a mixed solvent of water and acetonitrile with formula H3PMo12O40·5(CH3CH2)2NH·H2O. Spectroscopic data support the presence of a sizable electronic interaction between the organic substrate and the inorganic anion in the solid state. The single crystal x-ray structure analysis of the title compound revealed that it crystallized in the triclinic system, space group P $$\overline 1$$ with a = 12.0786(13), b = 12.102(5), c = 21.416(3) Å, α = 94.87(2), β = 94.755(9), γ = 113.81(2)°, V = 2830.3(13) Å3, and Z = 2.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009546132511

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6

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Synthesis and crystal structure of K3Sb4BO13 (2000)

Ftini, Mohamed Mongi ; Haddad, Amor ; Jouini, Tahar

Springer

Journal of chemical crystallography 30 (2000), S. 53-53

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ISSN: 1572-8854

Keywords: boroantimonate ; borate ; antimonate ; crystal structure ; 49

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract K3Sb4BO13, Mr = 823.11 g.mol−1, crystallizes in the triclinic system, space group P $$\overline 1$$ , Z = 2. The lattice parameters are a = 7.133(1) Å, b = 7.232(1) Å, c = 13.259(2) Å, α = 82.00 (1)°, β = 99.77(1)° and γ = 117.08(1)°, V = 598.7(2) Å3, Dx = 4.566 Mg m−3. The final R index and weighted Rw index are 0.0251 and 0.0623, respectively. The three-dimensional network of the title compound is constituted by layers (Sb3O9)n, similar to that of hexagonal bronze of Magneli. These layers are linked together, in the c direction, alternatively by edge-sharing pairs of SbO6 octahedra and BO3 triangles. This framework has interconnected tunnels, running approximately along the a and b directions, in which the K+ ions are located.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1009598116581

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7

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Crystal structure of a (25R)-2α,3α-epoxy-5α-spirostan-6, 23-dione hemi-ethyl acetate solvate (2000)

Morales, Angel Dago ; Novoa de Armas, Héctor ; Blaton, Norbert M. ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 693-697

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ISSN: 1572-8854

Keywords: brassinosteroids ; steroids ; natural products ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The compound (25R)-2α,3α-epoxy-5α-spirostan-6,23-dione, crystallizes as a hemi-ethyl acetate solvate, having two host molecules of similar conformation per molecule of ethyl acetate, in the asymmetric unit. The O atom of the epoxy group is α-oriented. The presence of the epoxy group disturbs the chair conformation in the ring A of the steroidal nucleus. Ring A has a C5α,C10β half-chair conformation. The six-membered rings B, C, and F have chair conformation as expected. The D ring adopts a C14α-envelope conformation and the E ring is midway between a C22α,O3β half-chair and a C22α-envelope conformations. The A/B, B/C, and C/D ring junctions are trans. Crystal data: C27H38O5·1/2C4H8O2, Monoclinic, space group P21, a = 7.7363(18) b = 28.769(12) c = 12.038(6) Å, β = 90.88(5), V = 2679.0(10) Å3, Z = 4. The packing of the molecules is assumed to be dictated by van der Waals interactions and by intermolecular C—H ··· O hydrogen bonds.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1012277425969

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8

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X-ray crystal structure of trans-bis(monoethanolamine) bis(saccharinato)nickel(II) (2000)

Andac, Omer ; Topcu, Yildiray ; Yilmaz, Veysel T. ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 767-771

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ISSN: 1572-8854

Keywords: saccharin ; monoethanolamine ; nickel(II) complex ; hydrogen bonding ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The crystal structure of trans-bis(monoethanolamine)bis(saccharinato)nickel(II), [Ni(C7H4NO3S)2(C2H7NO)2], has been determined from X-ray diffraction data. The metal complex is monoclinic, with a = 11.0555(5), b = 8.9103(4), c = 11.3890(5) Å, β = 105.0230(10)°, Z = 2, and space group P21/c . The structure consists of individual molecules. Two monoethanolamine molecules and two saccharinate anions coordinate the nickel atom forming a distorted octahedron. The monoethanolamine molecules act as a bidentate ligand and form five-membered trans chelate rings, which constitute the plane of the coordination octahedron, while two saccharinate ions behave as a monodentate ligand occupying the axial positions. Intermolecular hydrogen bonds link the molecules to form a three-dimensional infinite structure.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1013292406687

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9

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Crystal structure of 2,2,3-trimethyl-3-(2′,4′,5′-tricyanophenyl) cyclopentyl-1-acetic acid, methyl ester, C20H21N3O2 (2000)

Bovio, Bruna ; Locchi, Stelio

Springer

Journal of chemical crystallography 30 (2000), S. 589-592

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ISSN: 1572-8854

Keywords: Phenylcyclopentaneacetate derivative ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract The title compound crystallizes in space group P21/n, with a = 14.600(2), b = 7.091(2), c = 18.211(5) Å, and β = 103.67(2)°. Owing to the centric space group, both C(1) and C(3) chiral centers are either R or S. The acetate group is equatorial, the H(1) and the methyl group at C(3) are axial and reciprocally trans.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1011358327087

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10

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The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)] (2000)

Zhang, Jin-Nan ; Huang, Hui ; Li, Qi ; [et al.]

Springer

Journal of chemical crystallography 30 (2000), S. 737-741

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ISSN: 1572-8854

Keywords: crystal structure ; asymmetric synthesis ; spiro-cyclopropane derivatives

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences , Physics

Notes: Abstract Crystal structure of C41H53O7Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P212121, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1012254312765

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