Syntheses and Crystal Structures of the Solid Solution Sr4OBr2.89(2)Cl3.11(2) and the Elusive Ba2OBr2

2011 ◽  
Vol 66 (10) ◽  
pp. 1000-1004
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Solid Solution ◽  
Solid State ◽  
Single Crystals ◽  
Crystal Structures ◽  
Solid State Reactions ◽  
Molar Ratio ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters

Transparent and colorless single crystals of the compounds Sr4OBr2.89(2)Cl3.11(2) and Ba2OBr2 were obtained by solid-state reactions of SrCl2, SrBr2 and SrO (3 : 3 : 2 molar ratio) or by using an excess of BaO together with BaBr2 and Ba as a flux with the molar ratio 3 : 2 : 2, respectively. Ba2OBr2 crystals are isopointal to K2ZnO2 adopting the orthorhombic space group Ibam (no. 72, Z = 4) with the cell parameters a = 7247.44(10), b = 1297.76(20) and c = 657.43(10) pm. Sr4OBr2.89(2)Cl3.11(2) is isotypic to Ba4OCl6 (or isopointal to K6ZnO4) and crystallizes in the hexagonal space group P63mc (no. 186, Z = 2) with the cell parameters a = 982.20(4) and c = 750.41(7) pm.

Alkaline Earth Metal Oxyhalides Revisited – Syntheses and Crystal Structures of Sr4OBr6, Ba4OBr6 and Ba2OI2

2008 ◽  
Vol 63 (5) ◽  
pp. 519-524 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Solid State ◽  
Single Crystals ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Ternary Systems ◽  
Solid State Reactions ◽  
Alkaline Earth Metal ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters

Single crystals of the compounds Ca4OCl6, Sr4OBr6, Ba4OBr6, and Ba2OI2 were obtained by solid-state reactions. The crystals of Ba2OI2 are transparent and colorless and isopointal to K2ZnO2 adopting the orthorhombic space group Ibam (no. 72, Z = 4) with the cell parameters a = 747.20(9), b = 1392.02(18), and c = 678.12(9) pm. Sr4OBr6 and Ba4OBr6 are isotypic to Ba4OCl6 (or isopointal to K6ZnO4) and crystallize in the hexagonal space group P63mc (no. 186, Z = 2) exhibiting the cell parameters a = 982.20(4) and c = 750.41(7) pm for Sr4OBr6 and a = 1030.10(2) and c = 785.92(4) pm for Ba4OBr6. In the ternary systems Ca-O-X (X = Cl, Br or I) the only compound found other than the starting materials was the already known Ca4OCl6 which is also isotypic to Ba4OCl6 crystallizing in the hexagonal space group P63mc (no. 186, Z = 2) with the cell parameters a = 903.30(6) and c = 683.27(8) pm.

Zum Mineral Johillerit verwandte Oxovanadate RbCd4V3O12 und TlCd4V3O12 / Oxovanadates RbCd4V3O12 and TlCd4V3 O12 Related to the Mineral Johillerite

1997 ◽  
Vol 52 (5) ◽  
pp. 663-668 ◽  
Author(s):  
B. Mertens ◽  
Hk. Müller-Buschbaum
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystals ◽  
Solid State Reactions ◽  
Space Group ◽  
Related Compounds

Abstract Single crystals of I RbCd4V3O12 and TlCd4V3O12 II have been prepared by solid state reactions in closed iron tubes. The compounds crystallize closely related to the Johillerite structure in the space group C62h- C2/c with I: a = 13.058(3); b - 13.528(3), c = 7 .0 6 0 (2 )Å , β = 114.88(2)°; II: a = 12.999(6), b = 13.527(7), c = 7.055(3) Å , β = 114.88(4)°, Z = 4. Special features are the loss of Cu2+ in order to gain an additional Cd2+ position. The crystal structure is discussed with respect to related compounds of the Johillerite type.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Die Kristallstrukturen von MesSn(Cl)Me2 und Mes2SnCl2 / The Crystal Structures of MesSn(Cl)Me2 and Mes2SnCl2

1998 ◽  
Vol 53 (4) ◽  
pp. 503-506 ◽  
Author(s):  
Thomas Kräuter ◽  
Bernhard Neumüller
Keyword(s):  
Solid State ◽  
Single Crystals ◽  
Crystal Structures ◽  
Space Group ◽  
State 1

Single crystals of MesSn(Cl)Me2 (1) and Mes2SnCl2 (2) were obtained by the reactions of MesGaCl2 with Me3SnF and Mes3SnF, respectively. 1 and 2 are monomeric molecules in the solid state. 1: space group P21/n, Z = 4. lattice dimensions at -70°C: a = 1202,3(1), b = 739,1(1), c = 1441,3(1) pm , β = 102,71(1)°, R1 = 0,0469; 2: space group Pbcn, Z = 4, lattice dimensions at -50°C: a = 1107,0(2), b = 949,9(1), c = 1729,8(2) pm, R1= 0,049.

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

Orthoborate Halides with the Formula (M+II)5(BO3)3X: Syntheses, Crystal Structures and Raman Spectra of Eu5(BO3)3Cl and Ba5(BO3)3X (X = Cl, Br)

2011 ◽  
Vol 66 (4) ◽  
pp. 359-365 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Raman Spectra ◽  
Direct Synthesis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Incremental Volume

Single crystals of Eu5(BO3)3Cl were obtained by serendipity by reacting Eu2O3 and Mg with B2O3 at 1300 K in the presence of an NaCl melt for 13 h in silica-jacketed Nb ampoules. Ba5(BO3)3X (X = Cl, Br) crystals were formed by direct synthesis from appropriate amounts of Ba(OH)2, H3BO3 and the respective barium halide (hydrate) in alumina crucibles kept in the open atmosphere at 1300 K for 13 h. The crystal structures of the title compounds were determined with single-crystal X-ray diffraction. All compounds crystallize isotypically to Sr5(BO3)3Cl in the orthorhombic space group C2221 (no. 20, Z = 4) with the lattice parameters a = 1000.34(7), b = 1419.00(9), c = 739.48(5) pm for Eu5(BO3)3Cl, a = 1045.49(5), b = 1487.89(8), c = 787.01(4) pm for Ba5(BO3)3Cl, and a = 1048.76(7), b = 1481.13(9) and c = 801.22(5) pm for Ba5(BO3)3Br. The Raman spectra of all compounds were acquired and are presented and compared to literature data. The incremental volume of the orthoborate (BO3)3− anion has been determined and is compared to the Biltz volume

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Crystal Structures of Cyclosporin Derivatives: O-Acetyl-(4R)-4-(E-2-butyl)-4,N-dimethyl-L-threonyl-cyclosporin A and O-Acetyl-(4R)-4-[E-2-(4-bromobutyl)]-4,N-dimethyl-L-threonyl-cyclosporin A

1999 ◽  
Vol 64 (1) ◽  
pp. 89-98 ◽  
Author(s):  
Bohumil Kratochvíl ◽  
Alexandr Jegorov ◽  
Svetlana Pakhomova ◽  
Michal Hušák ◽  
Petr Bulej ◽  
...  
Keyword(s):  
Solid State ◽  
Cyclosporin A ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The structures of O-acetyl-(4R)-4-(E-2-butyl)-4,N-dimethyl-L-threonyl-cyclosporin A (1) and O-acetyl-(4R)-4-[E-2-(4-bromobutyl)]-4,N-dimethyl-L-threonyl-cyclosporin A (2) were determined by X-ray diffraction methods and compared with the structure of related cyclosporins. In contrast to expectation, neither the acetylation nor the subsequent bromination of 1 affects the conformation and packing of cyclosporins in the solid state. Both compounds are isomorphous and crystallize in the orthorhombic space group P212121 with a = 12.936(2) Å, b = 15.590(2) Å, c = 36.280(3) Å, and a = 12.916(3) Å, b = 15.675(4) Å, c = 36.715(7) Å, for 1 and 2, respectively.

Cs3NdSi8O19 und Cs6Nd2Si21O48: Zwei cäsiumhaltige Oxosilicate des Neodyms im Vergleich / Cs3NdSi8O19 and Cs6Nd2Si21O48: Two Caesium-containing Oxosilicates of Neodymium in Comparison

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1329-1338 ◽  
Author(s):  
Marion C. Schäfer ◽  
Thomas Schleid
Keyword(s):  
Solid State ◽  
Coordination Sphere ◽  
Quaternary System ◽  
Three Dimensional ◽  
Single Layer ◽  
Solid State Reactions ◽  
Double Layers ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
First Case

In the quaternary system Cs / Nd / Si / O, two new representatives, the phyllo-oxosilicate Cs3NdSi8O19 and the tecto-oxosilicate Cs6Nd2Si21O48, were synthesized by CsF-flux-supported solid-state reactions between Nd2O3 and SiO2. The first one, Cs3NdSi8O19 (orthorhombic, Cmcm (no. 63), a = 705.74(5), b = 2712.85(19), c = 1163.72(8) pm, Z = 4), is not isotypic to the related scandium compound Cs3ScSi8O19. The [SiO4]4− tetrahedra (d(Si4+ -O2−) = 156 -163 pm) in the structure of Cs3NdSi8O19 are connected via common corners to form corrugated, loop-branched double layers containing four- and eight-membered rings in the (010) plane and eight-membered rings along [001]. Each of the eight-membered ellipses emerging along [100] is additionally loopbranched by two four-membered chains. The oxosilicate double layers are cross-linked by vertexsharing via otherwise isolated [NdO6]9− octahedra (d(Nd3+-O2-)= 232 - 234 pm) to build up a three-dimensional framework. Also in between the oxosilicate double layers, the (Cs1)+ cations are located on the 8 f site. Each of the octagonal channels along [001] hosts one (Cs3)+ and two (Cs2)+ cations, which both reside at only partially occupied sites (8g and 8 f , respectively) and disorder, because otherwise too short Cs+ ・ ・ ・ Cs+ distances would occur. The second compound, Cs6Nd2Si21O48, crystallizes also in an orthorhombic space group (Pmmn (no. 59), a = 2189.24(15), b = 731.92(5), c = 1593.61(11) pm, Z = 2). Starting from a loop-branched single layer containing five- and eight-membered rings, a three-dimensional framework of vertex-shared [SiO4]4− tetrahedra (d(Si4+-O2−) = 149 - 164 pm) built up, in which the Si-O distances range from 149 to 164 pm within a broad range. In certain cavities, one kind of Nd3+, but four kinds of Cs+ cations (here, all sites with full occupation) are embedded. Also surrounded by only six O2− anions just like in the first case, the Nd3+ cations (d(Nd3+-O2−) = 233 - 237 pm) exhibit an unusually small, but not unknown coordination sphere for this relatively large lanthanoid(III) cation

Insights into the van der Waals Radius of Low-Spin Ni(ii) fromMolecular Mechanics Studies and the Crystal Structures of [Ni(cis-cyclohexane-1,3-diamine)2]Cl2, [Ni{(R)-5,5,7-trimethyl-1,4-diazacycloheptane}2]Cl2·H2O and [Ni(5,7-dimethyl-1,4-diazacycloheptane)2](ClO4)2. Synthesis of 5,7-Dimethyl-1,4-diazacycloheptane and an Improved Synthesis of cis-Cyclohexane-1,3-diamine

2002 ◽  
Vol 55 (8) ◽  
pp. 523 ◽  
Author(s):  
V. P. Munk ◽  
S. T. Cham ◽  
R. R. Fenton ◽  
R. K. Hocking ◽  
T. W. Hambley
Keyword(s):  
Solid State ◽  
Molecular Mechanics ◽  
Crystal Structures ◽  
Van Der Waals ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
R Value ◽  
Shed Light

The structures of three bis(diamine)nickel(II) complexes, chosen to shed light on the van der Waals radius of nickel(II), are described. [Ni(cis-1,3-chxn)2]Cl2 (cis-1,3-chxn = cis-cyclohexane-1,3-diamine) crystallizes in the monoclinic space group P21/n, with a 6.397(2), b 16.463(4), c 7.229(2) Å, b 90.70(2)�, and its structure has been refined to an R value of 0.031 on 1214F. [Ni{(R)-tmdz}2]Cl2�H2O (tmdz = 5,5,7-trimethyl-1,4-diazacycloheptane) crystallizes in the orthorhombic space group P212121, with a 10.678(1), b 11.073(5), c 17.968(6) Å, and its structure has been refined to an R value of 0.031 on 1586F. [Ni(dmdz)2](ClO4)2 (dmdz = 5,7-dimethyl-1,4-diaza- cycloheptane) crystallizes in the monoclinic space group P21/n, with a 9.582(1), b 10.390(2), c 11.817(3) Å, β 96.19(2)�, and its structure has been refined to an R value of 0.059 on 817F. In all three structures, short Ni���H and Ni���C interactions, ranging from 2.37 to 2.61 Å and 2.99 to 3.03 Å, respectively, are observed. Using molecular mechanics modelling to reproduce these separations, we have arrived at a van der Waals radius of 1.35 Å for low-spin nickel(ii). Analysis of Ni���O contacts in the solid state leads to a van der Waals radius of about 1.26 Å, which is consistent with the molecular mechanics derived value since these are usually longer.

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