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.

An Alternative Crystal Structure of Yb26B12O57 – X-Ray Structure Determination on Flux-synthesized Single Crystals

2014 ◽  
Vol 69 (3) ◽  
pp. 294-298 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Raman Spectra ◽  
Structure Determination ◽  
Title Compound ◽  
Lattice Parameters ◽  
Monoclinic Space Group ◽  
Subsequent Removal ◽  
Space Group ◽  
X Ray

Transparent and colorless single crystals of Yb26B12O57 were obtained by reacting Yb2O3 and B powder at 1000 °C in the presence of a KCl flux for 24 h in silica-jacketed Nb ampoules and subsequent removal of the flux by washing with water. Yb26B12O57 crystallizes in the monoclinic space group C2/m (no. 12, Z = 1) with the lattice parameters a = 2454:1(3), b = 357:78(4), c = 1426:7(2) pm and β = 115:111(6)°, and its structure differs slightly from that of a known compound with the same stoichiometry. Raman spectra of single crystals of the title compound were recorded and compared to those of known borate compounds

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.

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.

1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl2PN2CCl]3, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl2PN2CCl]3, Preparation, Spectra and Crystal Structure

1986 ◽  
Vol 41 (7) ◽  
pp. 839-844 ◽  
Author(s):  
H .-D. Hausen ◽  
G. Rajca ◽  
J. Weidlein
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Determination ◽  
Title Compound ◽  
Benzene Solution ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Low Symmetry

AbstractThe title compound, Cl2PN2CCl, has been synthesized by the reaction of PCl5 with Me3Si -N = C = N - SiMe3 (Me - CH3) in a 1:1 molar ratio. The colourless com pound is trimericin benzene solution and in the solid state and has a structure with a highly puckered 12-membered P3N6C3-ring skeleton of low symmetry. The X-ray structure determination shows a monoclinic space group P 21/a with 4 trimeric units per cell.

scholarly journals X-Ray crystal structure of [(?-H)Os2 (CO)4 (SnPh3)2 (?-HSnPh2) (?-dppf)] (dppf = 1,1´-bis (Diphenylphosphino) ferrocene

2014 ◽  
Vol 38 (1) ◽  
pp. 97-101
Author(s):  
Jagodish C Sarker ◽  
Md Saifur Rahman ◽  
Shariff E Kabir ◽  
Tasneem A Siddiquee
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Solid State ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Bimetallic Cluster ◽  
Space Group ◽  
X Ray ◽  
Academy Of Sciences

The solid-state molecular structure determination of the bimetallic osmium-tin compound [(?-H)Os2(CO)4(SnPh3)2(?-HSnPh2)(?-dppf)] (1) was carried out to determine the relative orientationof the coordinated ligands. Compound 1 crystallizes in the monoclinic space group P 21/c with a =22.366(7), b = 14.217(4), c = 25.213(8) Å, ? = 98.865(7)°, Z = 8 and V = 7921(4) Å3. It is a 34-electron bimetallic cluster with the Os-Os edge concomitantly bridged by a dppf and two HSnPh2 ligands DOI: http://dx.doi.org/10.3329/jbas.v38i1.20218 Journal of Bangladesh Academy of Sciences, Vol. 38, No. 1, 97-101, 2014

Preparations and the crystal structure of 3SbF3•4SbF5

1989 ◽  
Vol 67 (11) ◽  
pp. 2041-2046 ◽  
Author(s):  
John Fawcett ◽  
John H. Holloway ◽  
David R. Russell ◽  
Anthony J. Edwards ◽  
Khalaf I. Khallow
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Large Excess ◽  
Space Group ◽  
X Ray

3SbF3•4SbF5 has been prepared from the reaction of SbF3 with a large excess of SbF5 and from the reaction of WF5 with SbF5 in Genetron 113. An X-ray structure determination has shown that the compound crystallizes in the monoclinic space group P21/c with a = 8.547(10), b = 13.521(8), c = 19.551(12) Å, β = 100.3(1)°,Z = 4with the final residual indices of R = 0.0486 and Rw = 0.0526 for 4274 unique reflections. If only Sb—F distances of less than 2.1 Å are considered the structure can be viewed in terms of the arrangement (SbF2+)(SbF2+)(SbF6−)4. A Raman spectrum from single crystals of the compound is reported. Keywords: X-ray, structure, antimony, fluoride, Raman.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane / Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane

1980 ◽  
Vol 35 (8) ◽  
pp. 1015-1018 ◽  
Author(s):  
Werner Winter ◽  
Hanspeter Bühl ◽  
Herbert Meier
Keyword(s):  
General Formula ◽  
Structure Determination ◽  
Title Compound ◽  
Direct Methods ◽  
Spectroscopic Techniques ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Final Structure

Abstract Fragmentation of 1,2,3-thiadiazoles (1) leads to the compounds 5 - 8 with an increasing proportion of sulphur. Numerous structural possibilities exist for the products 7 with the general formula (R2C2)2S3. The number of proposals can be reduced by spectroscopic techniques, but the final structure determination is accomplished by an X-ray analysis of the title compound 7a. 7a crystallizes in the space group P21/c (Z = 4) with cell parameters of a = 9.714(1), b = 16.188(8), c = 9.149(2) Å and β = 98.93(1)°. The structure is solved by direct methods and refined to R = 0.053 with 1955 diffractometer data (I ≥ 2σ(I)). The trithiolane ring has a puckered conformation and the whole molecule shows nearly perfect C2-symmetry, which is not required crystallographically.

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.

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