Coordination preferences of the alkali cations sodium and caesium in the mixed-cationic Zintl ammoniate Cs3.2Na0.8Ge9·5.3NH3

2014 ◽  
Vol 70 (11) ◽  
pp. 1036-1039 ◽  
Author(s):  
Stefanie Gärtner ◽  
Christof Suchentrunk ◽  
Nikolaus Korber
Keyword(s):  
Monoclinic Space Group ◽  
Alkali Cations ◽  
Space Group ◽  
Mixed Cation ◽  
Coordination Behaviour ◽  
Cation Sites

The involvement of two different alkali cations in the nonagermanide ammoniate Cs3.2Na0.8Ge9·5.3NH3[tricaesium sodium nonagermanide–ammonia (1/5.3)] provides insights into the coordination behaviour of ammonia towards sodium and caesium cations within one compound and represents the first mixed-cationic solvate structure of nonagermanide tetraanions. The compound crystallizes in the monoclinic space groupP21/mand, with the presence of pseudomerohedral twinning, mixed-cation sites and disordering of the nonagermanide cage anions, features a combination of crystallographic challenges which could all be resolved during the refinement.

Novel and Disparate Hydrogen-Bonding Associations in 13-Amino-6-hydroxy-13-methyl-1,4,8,11-tetraazacyclotetradecane Tetrahydrochloride Monohydrate

2005 ◽  
Vol 58 (1) ◽  
pp. 60 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Yang Kim ◽  
Young Hoon Lee ◽  
Gareth L. Nealon ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Water Molecule ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Space Group ◽  
Cation Sites ◽  
L 13 ◽  
Hydrogen Bonded

The title compound crystallizes in the monoclinic space group Pn with two independent [LH4]Cl4·H2O formula units (L = 13-amino-6-hydroxy-13-methyl-1,4,8,11-tetraazacyclotetradecane) in the asymmetric unit. Despite pseudo-symmetry, these two units exhibit subtle and interesting differences in their hydrogen-bonded association by the interchange of the water molecule site with one of the chloride anions. Although a pentamine, L crystallizes as a tetrahydrochloride in which the tetracation has a conformation similar to that of tetraprotonated cyclam (1,4,8,11-tetraazacyclotetradecane), despite a different pattern of protonation sites. Difficulties in purification are perpetuated in the crystal, the minor isomeric component co-crystallizing in one of the cation sites.

Darstellung und Kristallstruktur von Na4Ga2S5. Ein Thiogallat mit -Zweier-Doppelketten / Preparation and Crystal Structure of Na4Ga2S5. A Thiogallate with --zweier-Double Chains

1992 ◽  
Vol 47 (7) ◽  
pp. 937-941 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Alkali Cations ◽  
Space Group ◽  
Distorted Octahedral ◽  
New Type

Transparent single crystals of Na4Ga2S5 were obtained from a melt of Na2S, Ga and S. Na4Ga2S5 is monoclinic, space group P21/c with a = 7.967(1), b = 6.133(2), c = 19.852(9) Å, β = 91.61(2)°, Ζ = 4. Its crystal structure was refined to a conventional R of 0.033 for 1150 observed reflections.The structure of Na4Ga2S5 is of a new type. It is characterized by infinite ribbon like thiogallate anions, -, which are built up by GaS4-tetrahedra (mean Ga-S bond length 2.28 A) sharing apices and edges. The four crystallographically independent alkali cations are coordinated to six sulphur atoms in distorted octahedral configurations.

Kristallstrukturen der Alkalimetall-Thiosulfate A2S2O3 nH2O (A/n = K/0, K/⅓ , Rb=1) / Crystal Structures of the Alkali Thiosulfates A2S2O3 · nH2O (A/n = K/0, K/⅓ , Rb=1)

2013 ◽  
Vol 68 (4) ◽  
pp. 323-337 ◽  
Author(s):  
Anna J. Lehner ◽  
Lisa V. Schindler ◽  
Caroline Röhr
Keyword(s):  
Crystal Structures ◽  
Complex Structure ◽  
Partial Molar Volumes ◽  
Double Layers ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Orthorhombic Unit Cell ◽  
Alkali Cations ◽  
Experimental Conditions ◽  
Space Group

The potassium and rubidium thiosulfates (hydrates) considered in this work were originally obtained as by-products during several syntheses of mixed sulfido=oxido metallates. The interesting complexity of their structural chemistry has motivated us to investigate them in detail. The crystal structures of all title compounds have been determined using single-crystal X-ray data. The structure of the anhydrous potassium thiosulfate K2S2O3 (monoclinic, space group P21/c, a=1010.15(14), b=910.65(12), c=1329.4(2) pm, b =111.984(11)º, Z =8, R1=0.0665) exhibits two crystallographically different thiosulfate anions, overall coordinated by 9=10 potassium cations. Their packing in the structure leads to a complex structure with a pseudo orthorhombic unit cell. The structure of the anhydrous salt is discussed in comparison with the known even more complicated 1=3 hydrate K2S2O3·1/3H2O (monoclinic, space group P21/c, a=938.27(6), b=602.83(4), c=3096.0(2) pm, b =98.415(6)º, Z =12, R1=0.0327). Under the chosen experimental conditions, rubidium forms the monohydrate Rb2S2O3 ·H2O, which also crystallizes with a new, in this case less complex structure (monoclinic, space group C2/m, a=1061.4(1), b=567.92(4), c=1096.4(1) pm, b =97.40(1)º, Z =4, R1=0.0734). Its thiosulfate ions form double layers of equally oriented tetrahedral units. The bond lengths and angles of the thiosulfate ions in all title compounds and in the sodium salts used for comparison vary only very slightly (dS-S =199.8 - 203.0 pm, dS-O =144.8 - 147.4 pm), and the deviation from the ideal C3v symmetry is very small, despite their complex packing. The overall coordination number of the thiosulfate ions by the alkali cations (and water molecules) increases systematically with the ionic radius of the counter cations and the amount of water molecules. For all known alkali thiosulfates, both the conventional and the calculated effective coordination numbers (ECoN) of the alkali cations as well as the partial molar volumes of the cations and the water molecules are compared and discussed.

A New Host Lattice Built of the Werner-Type Copper(I,II) Cyanide Complex Involving a Macrocyclic Ligand

1998 ◽  
Vol 63 (5) ◽  
pp. 622-627 ◽  
Author(s):  
Hidetaka Yuge ◽  
Takayoshi Soma ◽  
Takeshi Ken Miyamoto
Keyword(s):  
Macrocyclic Ligand ◽  
Host Lattice ◽  
Macrocyclic Complex ◽  
Monoclinic Space Group ◽  
Cyanide Complex ◽  
New Host ◽  
Space Group

Crystals of a new clathrate [CuII(hmtd)CuI(CN)3]·CH2Cl2 were afforded from a Me2CO-EtOH-CH2Cl2 solution of a macrocyclic complex CuII(hmtd)CuI(CN)3·2 H2O (hmtd = 5,7,7,12,14,14-hexamethyl- 1,4,8,11-tetraazacyclotetradeca- 4,11-diene). It crystallizes in the monoclinic space group P21/n, a = 7.936(5), b = 18.717(4), c = 17.783(6) Å, β = 98.55(4)°, Z = 4, R = 0.0558 for 1 870 reflections. Unprecedentedly, only one of the three nitrogen-ends of a CuI(CN)3 moiety is coordinated to the square-pyramidal Cu(II) center. The guest CH2Cl2 molecules are captured in the channel between the potlid-shaped [CuII(hmtd)CuI(CN)3] molecules.

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

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

New mixed-valent alkali chain sulfido ferrates A1+x[FeS2] (A = K, Rb, Cs; x = 0.333–0.787)

2020 ◽  
Vol 235 (8-9) ◽  
pp. 275-290
Author(s):  
Michael Schwarz ◽  
Pirmin Stüble ◽  
Katharina Köhler ◽  
Caroline Röhr
Keyword(s):  
Alkali Metal ◽  
General Structure ◽  
Variable Number ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Modulated Structure ◽  
Space Group ◽  
X Ray ◽  
Local Coordination ◽  
Natural Pyrite

AbstractFour new mixed-valent chain alkali metal (A) sulfido ferrates of the general structure family ${A}_{1+x}\left[{\text{Fe}}_{x}^{\text{II}}{\text{Fe}}_{1-x}^{\text{III}}{\text{S}}_{2}\right]$ were synthesized in the form of tiny green-metallic needles from nearly stoichiometric melts reacting elemental potassium with natural pyrite (A = K) or previously prepared Rb2S/Cs2S2 with elemental iron and sulfur (A = Rb/Cs). The crystal structures of the compounds were determined by means of single crystal X-ray diffraction: In the (3+1)D modulated structure of K7.15[FeS2]4 (space group Ccce(00σ3)0s0, a = 1363.87(5), b = 2487.23(13), c = 583.47(3) pm, q = 0,0,0.444, R1 = 0.055/0.148, x = 0.787), a position modulation of the two crystallographically different undulated ${}_{\infty }{}^{1}\left[{\text{FeS}}_{4/2}\right]$ tetrahedra chains and the surrounding K cations is associated with an occupation modulation of one of the three potassium sites. In the case of the new monoclinic rubidium ferrate Rb4[FeS2]3 (x = $\frac{1}{3}$; space group P21/c, a = 1640.49(12), b = 1191.94(9), c = 743.33(6) pm, β = 94.759(4)°, Z = 4, R1 = 0.1184) the undulation of the tetrahedra chain is commensurate, the repetition unit consists of six tetrahedra. In the second new Rb ferrate, Rb7[FeS2]5 (x = 0.4; monoclinic, space group C2/c, K7[FeS2]5-type; a = 2833.9(2), b = 1197.36(9), c = 744.63(6) pm, β = 103.233(4)°, Z = 4, R1 = 0.1474) and its isotypic mixed Rb/Cs-analog Rb3.6Cs3.4[FeS2]5 (a = 2843.57(5), b = 1226.47(2), c = 759.890(10) pm, β = 103.7170(9)°, R1 = 0.0376) the chain buckling leads to a further increased repetition unit of 10 tetrahedra. For all mixed-valent ferrates, the Fe–S bond lengths continuously increase with the amount (x) of Fe(II). The buckling of the chains is controlled through the local coordination of the S atoms by the variable number of A cations of different sizes.

Crystal and Molecular Structure of the Copper(I)-thiolate-selenide Complex [Ph4P][Cu(SeS2CNC4H8)(S2CN2C4H8)] with an Unusual Se-S Bond

1999 ◽  
Vol 54 (10) ◽  
pp. 1313-1317 ◽  
Author(s):  
Qianfeng Zhang ◽  
Jinxi Chen ◽  
Maochun Hong ◽  
Xinquan Xin ◽  
Hoong-Kun Fun
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
A Cell

Reaction of a DMF solution of Cu(S2CNC4H8) with [Ph4P]2[WSe4] affords [Ph4P]2[WSe4- (CuS2CNC4H8)3] (1) and [Ph4P][Cu(SeS2CNC4H )(S2CN2C4H8)] (2) in which a Se atom from the decomposition of the WSe42- anion has reacted with the pyrrolidyldithiocarbamate (C4H8dtc) ligand anion to form the new ligand anion SeS2CNC4H8⊖. Complex 2 crystallizes with four formula units in the monoclinic space group P21/c in a cell of dimensions a = 10.5824(2), b = 18.7575(3), c = 18.3268(4) Å and ß = 109.0980(10)°. 6055 independent reflections above background were measured with a diffractometer and the structure was refined anisotropically to R =0.073. The anion contains a three-coordinated copper(I) atom. The C4H8dtc⊖ ligand is bonded to the Cu+ cation in a terminal fashion, while SeS2CNC4H8⊖ chelates the Cu+ cation. The Se-S bond length is 2.231 (4) Å.

Zur Kenntnis von EuBeGd2O5 mit einem Beitrag über Phasen der Zusammensetzung M1-xM′xBeLn2O5: Ca0,4Sr0,6BeSm2O5, Ba0,25Ca0,75BeNd2O5 und Ba0,36Sr0,64BeNd2O5 / On EuBeGd2O5 and on Phases of the Composition M1-xM′xBeLn2O5: Ca0,4Sr0,6BeSm2O5, Ba0,25Ca0,75BeNd2O5 and Ba0,36Sr0,64BeNd2O5

1994 ◽  
Vol 49 (7) ◽  
pp. 919-922 ◽  
Author(s):  
Hk. Müller-Buschbaum ◽  
S. Frenzen
Keyword(s):  
Single Crystals ◽  
Plasma Torch ◽  
Monoclinic Space Group ◽  
Orthorhombic Symmetry ◽  
Laser Technique ◽  
Space Group

Abstract Single crystals of (I): EuBeGd2O5, (II): Ca0,4Sr0,6BeSm2O5, (III): Ba0,25Ca0,75BeNd2O5 and (IV): Ba0.36Sr0.64BeNd2O5 were prepared by (I): plasma torch and (II)-(IV ): CO2-LASER technique. X-Rayo investigations lead to (I) monoclinic (space group C52h-P21/c, a = 7.126, b = 6.457, c = 9.394 Å , β = 90.40°) and (II)-(IV) orthorhombic symmetry (D162h-Pnma). (II: a = 9.454, b = 7.142, c = 6.490 Å; III: a = 9.508, b = 7.188, c = 6.531 Å; IV: a = 9.642, b = 7.295, c = 6.614 Å). In contrary to the phases M1-xM′xBeLn2O5, EuBeGd2O5 is characterized by an ordered distribution of Eu2+ and Gd3+ inside of the Kagomé network.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

Sign in / Sign up

Export Citation Format

Share Document