Synthesis and crystal structure of the lanthanum cyanurate complex La[H2N3C3O3]3 · 8.5 H2O

Abstract Single crystals of La[H2N3C3O3]3 · 8.5 H2O were obtained from stoichiometric amounts of as-precipitated La(OH)3 with cyanuric acid (CYA) [H3N3C3O3]3 in a boiling aqueous solution, followed by slow cooling and evaporation of water under ambient conditions. According to the X-ray structure analysis of the colorless and transparent crystals, La[H2N3C3O3]3 · 8.5 H2O adopts the triclinic space group P1 (no. 1) and exhibits the unit-cell parameters a = 987.24(7), b = 1110.97(8), c = 1179.81(9) pm, α = 113.716(2), β = 97.053(2), γ = 101.502(2)° for Z = 2. The CYA is singly deprotonated to give monoanions [H2N3C3O3]– which are O,N-coordinated to the La3+ cations. These dihdrogencyanurate anions are assembled in ribbons with two crystallographically different La3+ cations coordinating to either one or two different ligands, respectively. The coordination sphere of the La3+ cations is comprised of water molecules, and interstitial water molecules fill the dead volume of the crystals. The anionic ribbons are stacked to maximize the contact between the six-membered rings, showing distances of about 330 pm.

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Synthese und Kristallstruktur von Triphenyltelluroniumsulfid / Synthesis and Crystal Structure of Triphenyltelluroniumsulfide

Zeitschrift für Naturforschung B ◽

10.1515/znb-1994-1208 ◽

1994 ◽

Vol 49 (12) ◽

pp. 1654-1658 ◽

Cited By ~ 2

Author(s):

Markus Wieber ◽

Stefan Lang ◽

Stefan Rohse ◽

Ralph Habersack ◽

Christian Burschka

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Title Compound ◽

Spectroscopic Characterization ◽

Unit Cell ◽

X Ray Diffraction ◽

Triclinic Space Group ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Cell Parameters

The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P1) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, α = 77.67(3)°, β = 82.18(2)°, γ = 66.00(2)° (V = 1766(1) × 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two molecules of CH2Cl2 per unit cell.

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Pentafluoro[(4-methyl-1,4-bisazoniacy clohex-1 -yl)methy 1] germanate Hydrate: Synthesis and Crystal Structure of a Zwitterionic λ6Ge-Germanate with a GeF5C Framework

Zeitschrift für Naturforschung B ◽

10.1515/znb-1998-5-607 ◽

1998 ◽

Vol 53 (5-6) ◽

pp. 535-539 ◽

Cited By ~ 6

Author(s):

Reinhold Tacke ◽

Joachim Heermann ◽

Melanie Pülm

Keyword(s):

Molar Ratio ◽

Water Molecules ◽

Crystal Data ◽

X Ray Diffraction ◽

Coordination Polyhedra ◽

Triclinic Space Group ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Distorted Octahedra ◽

Positively Charged

Abstract The zwitterionic (molecular) λ6Ge-germanate pentafluoro[(4-methyl-1,4-bisazoniacyclohexl-yl)methyl]germanate (5) was synthesized by reaction of 1-methyl-4-[(trimethoxygermyl) methyl]piperazine (8) with HF (molar ratio 1:5) in a mixture of water and ethanol at 0 °C and isolated as the hydrate 5 · H2O. The zwitterion 5 is characterized by the presence of a hexacoordinate (formally twofold negatively charged) germanium atom and two tetracoordinate (formally positively charged) nitrogen atoms. Compound 5 · H2O was structurally characterized by single-crystal X-ray diffraction. Crystal data are as follows: C6H17F5GeN2O , triclinic space group P1̄ (no. 2), a = 7.5228(11) Å, b = 12.174(2) Å, c = 12.3041(14) Å, α = 73.74(2)°, β = 82.44(2)°, γ = 74.762(10)°, V = 1041.7(2) Å3, T = 173(2) K, Z = 4, R1 = 0.0227. There are one pair each of crystallographically independent zwitterions 5 and water molecules in the asymmetric unit, the structures of the zwitterions being very similar. Their coordination polyhedra around the germanium atoms are slightly distorted octahedra.

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An unexpected lanthanum chloride carbonate hydrate: synthesis, crystal structure, vibrational spectra and thermal degradation of LaCl[CO3]·3H2O

Zeitschrift für Naturforschung B ◽

10.1515/znb-2018-0111 ◽

2018 ◽

Vol 73 (9) ◽

pp. 661-667

Author(s):

Olaf Reckeweg ◽

Falk Lissner ◽

Björn Blaschkowski ◽

Armin Schulz ◽

Thomas Schleid

Keyword(s):

Aqueous Solutions ◽

Single Crystals ◽

Elevated Temperatures ◽

Water Molecules ◽

Orthorhombic Structure ◽

Ambient Conditions ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Tg Studies

AbstractMicrocrystalline powders of LaCl[CO3]·3H2O were precipitated and isolated from stoichiometric aqueous solutions of LaCl3·7H2O and Na2[CO3]·10H2O. This confirmed the surprising emergence of corresponding single crystals during a reaction of equimolar aqueous solutions of LaCl3·7H2O and Na[N3] under ambient conditions by the uptake of atmospheric CO2. According to the X-ray structure analysis of colorless, transparent and rectangular single-crystals, LaCl[CO3]·3H2O adopts an orthorhombic structure, space group Pbca with the unit-cell parameters a=856.82(5), b=1598.57(9) and c=967.68(6) pm for Z=8. The tenfold coordination polyhedron around La3+ consists of two monodentate as well as two bidentate [CO3]2− anions together with three oxygen atoms from coordinating water molecules and one chloride anion. According to DSC/TG studies and X-ray powder diffraction, LaCl[CO3]·3H2O loses first its water and then carbon dioxide under thermal treatment up to 900°C to leave LaOCl behind. Vibrational infrared and Raman spectra confirmed the presence of H2O and [CO3]2− in LaCl[CO3]·3H2O and its stepwise degradation at elevated temperatures.

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A Three-dimensional Manganese(II) 1,2,4-Benzenetricarboxylate Hydroxide Framework with Mn–O Inorganic Sheets: Hydrothermal Synthesis and Crystal Structure

Zeitschrift für Naturforschung B ◽

10.1515/znb-2008-1114 ◽

2008 ◽

Vol 63 (11) ◽

pp. 1339-1342 ◽

Cited By ~ 3

Author(s):

Shuxi Zhou ◽

Yanxiong Ke ◽

Hongliang Zou ◽

Tianhua Liu ◽

Fang Zhu ◽

...

Keyword(s):

Crystal Structure ◽

Hydrothermal Reaction ◽

Three Dimensional ◽

Transition Metal Ions ◽

X Ray Diffraction ◽

Triclinic Space Group ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Cell Parameters ◽

3D Framework

Abstract Utilizing unsymmetrical 1,2,4-benzenetricarboxylate (1,2,4-BTC) as a ligand, a complex [Mn2.5(1,2,4-BTC)- (OH)2(H2O)] was synthesized by hydrothermal reaction and characterized by single crystal X-ray diffraction. The coordination polymer crystallizes in the triclinic space group P1̅, with cell parameters a = 5.7702(5), b = 8.0269(6), c = 12.1378(9) Å, α = 88.000(1)°, β = 81.493(1)◦, γ = 88.569(1)°, and Z = 2. In the the crystal, there are Mn- O-Mn sheets which are further connected through the 1,2,4-BTC ligands into a 3D framework, which is rare in the coordination chemistry originating from transition metal ions and unsymmetrical polycarboxylates.

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Synthesis and molecular structure of a novel barium arylspiroboronate ester

Open Chemistry ◽

10.2478/s11532-011-0017-7 ◽

2011 ◽

Vol 9 (3) ◽

pp. 386-390 ◽

Cited By ~ 1

Author(s):

Nathan Halcovitch ◽

Michael Geier ◽

Christopher Vogels ◽

Andreas Decken ◽

Stephen Westcott

Keyword(s):

Molecular Structure ◽

Direct Methods ◽

Water Molecules ◽

X Ray Diffraction ◽

Triclinic Space Group ◽

X Ray ◽

Cell Parameters ◽

Barium Atom ◽

Single Oxygen ◽

Bonding Mode

AbstractThe compound barium bis{bis-(4,6-di-tert-butyl[1,2-benzenediolato(2-)-O,O′]borate)} has been prepared by the addition of 3,5-di-tert-butylcatechol to a solution of boric acid and Ba(OH)2 and characterized by a single crystal X-ray diffraction study. The title compound crystallized in the triclinic space group P-1, with cell parameters a = 13.280(2) Å, b = 15.755(3) Å, and c = 16.980(3) Å, α = 71.691(2)o, β = 79.528(3)o, γ = 80.741(3)o, Z = 1, and V = 3296.1(10) Å3. The structure was solved by direct methods and refined to a final R = 0.0459 for 14370 reflections with I > 2σ(I). One of the arylspiroboronate ester counterions is bound to the barium atom in a rare example of the η1 bonding mode via a single oxygen of one of the catecholato groups. The coordination sphere around the barium is complemented by four molecules of water, one molecule of acetone and two bridging water molecules, connecting to an adjacent barium atom.

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Structural Study of a new Compound Based on Acid 1,4-Cyclohexanedicarboxylic (1,4-CDC)

JOURNAL OF ADVANCES IN CHEMISTRY ◽

10.24297/jac.v6i1.969 ◽

2010 ◽

Vol 6 (1) ◽

pp. 891-896

Author(s):

Manel Halouani ◽

M. Dammak ◽

N. Audebrand ◽

L. Ktari

Keyword(s):

Aqueous Solution ◽

Water Molecules ◽

Carboxyl Group ◽

X Ray Diffraction ◽

Compound I ◽

Unit Cell Parameters ◽

Monoclinic System ◽

X Ray ◽

Cell Parameters ◽

Cyclohexanedicarboxylic Acid

One nickel 1,4-cyclohexanedicarboxylate coordination polymers, Ni2 [(O10C6H4)(COO)2].2H2O (I), was hydrothermally synthesized from an aqueous solution of Ni (NO3)2.6H2O, (1,4-CDC) (1,4-CDC = 1,4-cyclohexanedicarboxylic acid) and tetramethylammonium nitrate. Compound (I) crystallizes in the monoclinic system with the C2/m space group. The unit cell parameters are a = 20.1160 (16) Å, b = 9.9387 (10) Å, c = 6.3672 (6) Å, β = 97.007 (3) (°), V= 1263.5 (2) (Å3) and Dx= 1.751g/cm3. The refinement converged into R= 0.036 and RW = 0.092. The structure, determined by single crystal X-ray diffraction, consists of two nickel atoms Ni (1) and Ni (2). Lots of ways of which is surrounded by six oxygen atoms, a carboxyl group and two water molecules.

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Synthesis and crystal structure of (Ag,Pd)22Se6

Powder Diffraction ◽

10.1017/s0885715612000929 ◽

2013 ◽

Vol 28 (1) ◽

pp. 13-17 ◽

Cited By ~ 1

Author(s):

F. Laufek ◽

A. Vymazalová ◽

D.A. Chareev ◽

A.V. Kristavchuk ◽

J. Drahokoupil ◽

...

Keyword(s):

Crystal Structure ◽

Diffraction Data ◽

Glass Tube ◽

Structure Type ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Cell Parameters ◽

Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

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Growth defects and infrared spectra analysis of CePO4single crystals

Journal of Applied Crystallography ◽

10.1107/s0021889805017528 ◽

2005 ◽

Vol 38 (4) ◽

pp. 675-677 ◽

Cited By ~ 11

Author(s):

Kunpeng Wang ◽

Jianxiu Zhang ◽

Jiyang Wang ◽

Changshui Fang ◽

Wentao Yu ◽

...

Keyword(s):

Slow Cooling ◽

Spectra Analysis ◽

X Ray ◽

Cell Parameters ◽

Growth Defects ◽

Cooling Method ◽

Good Crystalline Quality ◽

Growth Habits ◽

Heterobimetallische 3d-4f-Komplexe mit Bis(1,2-dithiooxalato)nickelat(II) als planarem Brückenbaustein / Heterobimetallic 3d-4f-Complexes with Bis(1,2-dithiooxalato)nickelate(II) as Planar Bridging Block

Zeitschrift für Naturforschung B ◽

10.1515/znb-2005-1107 ◽

2005 ◽

Vol 60 (11) ◽

pp. 1149-1157 ◽

Cited By ~ 4

Author(s):

Matthias Siebold ◽

Alexandra Kelling ◽

Uwe Schilde ◽

Peter Strauch

Keyword(s):

Room Temperature ◽

Magnetic Moments ◽

Lanthanide Ions ◽

Water Molecules ◽

Unit Cell Parameters ◽

Ionic Radii ◽

X Ray ◽

Cell Parameters ◽

Heterobimetallic Complexes ◽

The Individual

Planar bis(1,2-dithiooxalato)nickelates(II) react in aqueous solutions of lanthanide ions to form pentanuclear, heterobimetallic complexes of the general composition [{Ln(H2O)n}2- {Ni(dto)2}3]・xH2O (Ln = Y3+, La3+, Ce3+, Pr3+, Nd3+, Sm3+, Eu3+, Gd3+, Tb3+, Dy3+, Ho3+, Er3+, Tm3+, Yb3+, Lu3+; n = 4 or 5; x = 9 - 12). With [{Nd(H2O)5}2{Ni(S2C2O2)2}3]・xH2O (x = 10 - 12) (1) and [{Er(H2O)4}2{Ni(S2C2O2)2}3]・xH2O (x = 9 - 10) (2) we were able to isolate two complexes of this series as single crystals, which were characterized by X-ray structure analysis. Depending on the individual ionic radii of the lanthanide ions, the compounds crystallize in two different crystal systems with the following unit cell parameters: 1, monoclinic in P21/c with a = 11.3987(13), b = 11.4878(8), c = 20.823(2) Å , β = 98.907(9)° and Z = 2; 2, triclinic in P1̅ with a = 10.5091(6), b = 11.0604(6), c = 11.2823(6) Å , α = 107.899(4)°, β = 91.436(4)°, γ = 112.918(4)° and Z = 1. The channels and cavities appearing in the packing of the molecules are occupied by uncoordinated water molecules. High magnetic moments up to 14.65 BM./f.u. have been observed at room temperature due to the combined moments of the individual lanthanide ions.

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Crystal Structures and Stability of Two Bipyridyl Complexes of Metal Chloroacetates

Zeitschrift für Naturforschung B ◽

10.1515/znb-2007-1007 ◽

2007 ◽

Vol 62 (10) ◽

pp. 1271-1276 ◽

Cited By ~ 4

Author(s):

Liang Chen ◽

Xian-Wen Wanga ◽

Jing-Zhong Chen ◽

Jian-Hong Liu

Keyword(s):

Binuclear Complexes ◽

Two Dimensional ◽

X Ray Diffraction ◽

Orthorhombic Space Group ◽

Reaction Conditions ◽

Triclinic Space Group ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

Dimensional Network

The complexes Mn(Cl3CCOO)2(4,4′-bpy) (1) and [Cu2(ClCH2COO)(2,2′-bpy)2(OH)(H2O)]-(NO3)2(2) (bpy = bipyridine) were generated under mild reaction conditions and characterized by IR spectra, thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), and single crystal X-ray diffraction. Compound 1 exhibits a two-dimensional network with octahedrally coordinated Mn(II) atoms linked by 4,4′-bpy ligands and Cl3COO− ligands. Compound 2 features a supramolecular structure of binuclear complexes, with edge-sharing five-coordinated square-pyramidal units bridged by the ClCH2COO− ligand, an OH− group and a water molecule. Complex 1 crystallizes in the orthorhombic space group Pbcn with cell parameters: a = 16.5390(17), b = 11.6396(17), c = 9.9181(12) Å, V = 1909.3(4) Å3, Z = 4, wR2 = 0.1576. Complex 2 crystallizes in the triclinic space group P1̅ with cell parameters: a = 7.6190(15), b = 11.151(2), c = 16.640(3) Å , α = 73.13(3), β = 80.89(3), γ = 74.51(3)°, V = 1298.73(4) Å3, Z = 2, wR2 = 0.1265.

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