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.

scholarly journals The crystal structure of alstonite, BaCa(CO3)2: an extraordinary example of ‘hidden’ complex twinning in large single crystals

2020 ◽  
Vol 84 (5) ◽  
pp. 699-704
Author(s):  
Luca Bindi ◽  
Andrew C. Roberts ◽  
Cristian Biagioni
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Determinations

AbstractAlstonite, BaCa(CO3)2, is a mineral described almost two centuries ago. It is widespread in Nature and forms magnificent cm-sized crystals. Notwithstanding, its crystal structure was still unknown. Here, we report the crystal-structure determination of the mineral and discuss it in relationship to other polymorphs of BaCa(CO3)2. Alstonite is trigonal, space group P31m, with unit-cell parameters a = 17.4360(6), c = 6.1295(2) Å, V = 1613.80(9) Å3 and Z = 12. The crystal structure was solved and refined to R1 = 0.0727 on the basis of 4515 reflections with Fo > 4σ(Fo) and 195 refined parameters. Alstonite is formed by the alternation, along c, of Ba-dominant and Ca-dominant layers, separated by CO3 groups parallel to {0001}. The main take-home message is to show that not all structure determinations of minerals/compounds can be solved routinely. Some crystals, even large ones displaying excellent diffraction quality, can be twinned in complex ways, thus making their study a crystallographic challenge.

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

Synthesis, vibrational spectra and single-crystal structure determination of lithium tricyanomethanide Li[C(CN)3]

2018 ◽  
Vol 73 (3-4) ◽  
pp. 225-229
Author(s):  
Olaf Reckeweg ◽  
Maurice Conrad ◽  
Armin Schulz ◽  
Francis J. DiSalvo ◽  
Thomas Schleid
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Metathesis Reaction ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Related Compounds

AbstractThe long-elusive structure of lithium tricyanomethanide Li[C(CN)3] has been determined on the basis of material synthesized via a metathesis reaction of Ag[C(CN)3] with LiCl in water driven by AgCl precipitation and subsequently recrystallization from methanol. Li[C(CN)3] crystallizes in the non-centrosymmetric orthorhombic space groupIma2 with the unit-cell parametersa=751.06(4),b=1059.75(6) andc=563.27(3) pm adopting a unique structure with planar [C(CN)3]−anions exhibiting nearly ideal trigonal planarD3hsymmetry. The Li+cations are coordinated by five independent tricyanomethanide anions forming a distorted square pyramid with Li–N distances between 202 and 249 pm. The vibrational frequencies were also determined and along with other properties of Li[C(CN)3] compared with those of related compounds.

Syntheses, single-crystal structure determination, and Raman spectra of Rb[C(CN)3] and Cs[C(CN)3]

2015 ◽  
Vol 70 (2) ◽  
pp. 151-154 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Single Crystals ◽  
Raman Spectra ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Cell Parameters ◽  
Ethanol Yields

AbstractExtracting residues of an aqueous solutions containing equimolar amounts of K[C(CN)3] and RbF or CsF, respectively, with absolute ethanol, yields triangular, transparent colorless crystals of Rb[C(CN)3] and Cs[C(CN)3] after the ethanol was allowed to evaporate. The compounds are isotypic and crystallize isopointal to calcite in space group R3̅c (no. 167) with the cell parameters a=809.9(1) and c=1461.3(3) pm and a=843.29(9) and c=1459.9(2) pm, respectively. Single crystals were used to record the Raman spectra of the title compounds.

The Constituents of Marine Sponges. V. The Isolation From Chelonaplysilla violacea (Dendroceratida) of Aplyviolene and Other Diterpenes, and the Determination of the Crystal Structure of Aplyviolene

1990 ◽  
Vol 43 (11) ◽  
pp. 1861 ◽  
Author(s):  
TW Hambley ◽  
A Poiner ◽  
WC Taylor
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Marine Sponge ◽  
Marine Sponges ◽  
Spectroscopic Methods ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Deep Violet

From the deep violet, encrusting marine sponge Chelonaplysilla violacea, two rearranged spongian diterpenes, aplyviolene, (1R*,1′S*,3?aR*,5R*,6R*,8R*,8′aS*)-3-oxo-8-(1′,4′,4′-trimethyl-8′-methylenedecahydroazulen-1′-yl)-2,7-dioxabicyclo[3.2.1]oct-6-yl acetate (1), the acetoxy derivative, aplyviolacene (2), (5R*,8S*,9S*,10R*,13S*,14R* ,15S*,16R*)-spongian-15,16-diyl diacetate (3) and (5R*,8S*,9S*,10R*,13S*,14R*)-spongian-16-one (4) were isolated. The structures were determined by spectroscopic methods, and the structure of aplyviolene was confirmed by a single-crystal X-ray determination. The crystal structure was refined to a residual of 0.036 for 1125 independent observed reflections. The crystals were orthorhombic, space group P212121 with a 8.098(1), b 11.628(1), c 21.774(3)Ǻ.

Synthesis and characterization of a disordered variant of KB5O7(OH)2

2015 ◽  
Vol 70 (9) ◽  
pp. 649-658 ◽  
Author(s):  
Teresa S. Ortner ◽  
Michael Schauperl ◽  
Klaus Wurst ◽  
Thomas S. Hofer ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Structure Determination ◽  
Molar Ratio ◽  
Potassium Cation ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group

AbstractThe potassium pentaborate KB5O7(OH)2 reported herein crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 904.8(2), b = 753.2(2), c = 1214.9(5) pm, β = 117.16(2)°, and V = 0.73663(5) nm3 (Z = 4). It is a disordered structural variant of an already known compound with the same composition (a = 766.90(3), b = 904.45(3), c = 1223.04(4) pm, β = 119.132(2)°, and V = 0.74101(5) nm3 (Z = 4)) reported by Wu in 2011. The disorder of the potassium cation in the single crystal structure determination of KB5O7(OH)2 presented here leads to a remarkably elongated a axis and a corresponding reduction of the length of the b axis in comparison to the ordered compound. The disordered variant was obtained through a hydrothermal synthesis from KNO3, B2O3, and Ce(NO3)3·6H2O with a molar ratio of 1:1:0.07.

Kristallstruktur von Cs2[B6H5(SCN)]/ Crystal Structure of Cs2[B6H5(SCN)]

1998 ◽  
Vol 53 (8) ◽  
pp. 816-818 ◽  
Author(s):  
W. Preetz ◽  
S. Zander ◽  
C. Bruhn
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Structure Determination ◽  
Deae Cellulose ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Abstract By reaction of [B6H6]2-with (SCN)2 in dichloromethane at -80 C° the thiocyanatohexaborate anion is formed and can be isolated by ion exchange chromatography on diethylaminoethyl (DEAE) cellulose. The X-ray structure determination of Cs2[B6H5(SCN)] (orthorhombic, space group Pbca with a = 9.506(5), b = 10.644(5), c = 21.857(5) Å, Z = 8) reveals that the SCN substituent is bonded via the S atom with the B-S distance of 1.885(9) Å and the B-S-C angle of 99.8(5)°. The SCN group is nearly linear (179.9(9)°).

The crystal structure of Cu2GeSe3 and the structure-types of the I2-IV-VI3 family of semiconducting compounds

2021 ◽  
Vol 77 (1) ◽  
pp. 158-167
Author(s):  
Analio Dugarte-Dugarte ◽  
Nahum Ramírez Pineda ◽  
Luis Nieves ◽  
José Antonio Henao ◽  
Graciela Díaz de Delgado ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Initial Report ◽  
Space Group ◽  
Cell Parameters ◽  
Semiconducting Compounds ◽  
Bond Valence Model

Almost 50 years after the initial report, the crystal structure of Cu2GeSe3, a I2-IV-VI3 semiconductor, has been revised using modern single-crystal X-ray diffraction data. The structure of this material can be properly described in the monoclinic space group Cc (No. 9) with unit-cell parameters a = 6.7703 (4) Å, b = 11.8624 (5) Å, c = 6.7705 (4) Å, β = 108.512 (6)°, V = 515.62 (5) Å3, Z = 4, rather than in the orthorhombic space group Imm2 (No. 44) with unit-cell parameters a = 11.860 (3), b = 3.960 (1), c = 5.485 (2) Å, V = 257.61 Å3, Z = 2, as originally proposed [Parthé & Garín (1971). Monatsh. Chem. 102, 1197–1208]. Contrary to what was observed in the orthorhombic structure, the distortions of the tetrahedra in the monoclinic structure are consistent with the distortions expected from considerations derived from the bond valence model. A brief revision of the structures reported for the I2-IV-VI3 family of semiconducting compounds (I: Cu, Ag; IV: Si, Ge, Sn; and VI: S, Se, Te) is also presented.

Molecular and crystal structure of a copper(II) complex of sildenafil

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Akhmatkhodja N. Yunuskhodjayev ◽  
Shokhista F. Iskandarova ◽  
Vahobjon Kh. Sabirov
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Piperazine Ring ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Abstract The crystal structure of a copper(II) complex of protonated sildenafil, CuCl3C22H31N6O4S⋅2H2O was studied by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with the unit cell parameters a = 15.4292(2), b = 9.06735(12), c = 21.1752(2) Å, V = 2945.48(7) Å3, Z = 4. The Cu atom is coordinated by the sildenafil ligand via the N2 atom of the pyrazolopyrimidine ring and by three chloride anions. Sildenafil is protonated at the methylated N6 atom of the piperazine ring and it is cation ligand with a 1+ charge.

Kristallstruktur von [Mo(Co)3(Ncme)(Srbu)]2 / Crystal Structure of [Mo(CO)3(NCMe)(S'Bu)]2

1998 ◽  
Vol 53 (3) ◽  
pp. 378-380
Author(s):  
Mike R. Kopp ◽  
Bernhard Neumüller
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Structure Determination ◽  
Space Group ◽  
X Ray

Abstract Single crystals of [Mo(CO)3(NCMe)(S′Bu)]2 (1) and [{Mo(CO)3}2{Mo(CO)2}{S′Bu}4] (2) were obtained by the reaction of [Mo(CO)3(NCMe)3] with [(PhCH2)2GaS′Bu]2 in 1,4-dio-xane. The X-ray structure determination of 1 showed the presence of a Mo2S2 four-membe-red ring with a Mo-Mo bond length of 296,7(1) pm. Space group Pbca, Z = 4, lattice dimen­sions at -80°C: a = 1588,2(3), b = 905,8(1), c = 1676,0(1) pm, R1 = 0,0555.

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