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

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.

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

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.

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

2005 ◽  
Vol 60 (11) ◽  
pp. 1149-1157 ◽  
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.

Analysis of an industrial production suspension ofBacillus lentussubtilisin crystals by powder diffraction: a powerful quality-control tool

2014 ◽  
Vol 70 (4) ◽  
pp. 1115-1123 ◽  
Author(s):  
Christian G. Frankaer ◽  
Olga V. Moroz ◽  
Johan P. Turkenburg ◽  
Stein I. Aspmo ◽  
Majbritt Thymark ◽  
...  
Keyword(s):  
Quality Control ◽  
Single Crystals ◽  
Powder Diffraction ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Quality Control Tool ◽  
Control Tool

A microcrystalline suspension ofBacillus lentussubtilisin (Savinase) produced during industrial large-scale production was analysed by X-ray powder diffraction (XRPD) and X-ray single-crystal diffraction (MX). XRPD established that the bulk microcrystal sample representative of the entire production suspension corresponded to space groupP212121, with unit-cell parametersa= 47.65,b= 62.43,c= 75.74 Å, equivalent to those for a known orthorhombic crystal form (PDB entry 1ndq). MX using synchrotron beamlines at the Diamond Light Source with beam dimensions of 20 × 20 µm was subsequently used to study the largest crystals present in the suspension, with diffraction data being collected from two single crystals (∼20 × 20 × 60 µm) to resolutions of 1.40 and 1.57 Å, respectively. Both structures also belonged to space groupP212121, but were quite distinct from the dominant form identified by XRPD, with unit-cell parametersa= 53.04,b = 57.55,c= 71.37 Å anda= 52.72,b= 57.13,c= 65.86 Å, respectively, and refined toR= 10.8% andRfree= 15.5% and toR= 14.1% andRfree= 18.0%, respectively. They are also different from any of the forms previously reported in the PDB. A controlled crystallization experiment with a highly purified Savinase sample allowed the growth of single crystals of the form identified by XRPD; their structure was solved and refined to a resolution of 1.17 Å with anRof 9.2% and anRfreeof 11.8%. Thus, there are at least three polymorphs present in the production suspension, albeit with the 1ndq-like microcrystals predominating. It is shown how the two techniques can provide invaluable and complementary information for such a production suspension and it is proposed that XRPD provides an excellent quality-control tool for such suspensions.

The Crystal Structures of the Diastereoisomers (+)589-(Λ-δ-δ)-cis-Bis(ethylenediamine)dinitrocobalt(III)Hydrogen-D-tartrate Monohydrate and (-)589-(Λ-λ-λ)-cis-Bis(ethylenediamine)dinitrocobalt(III) Hydrogen-D-tartrate Dihydrate

1988 ◽  
Vol 41 (9) ◽  
pp. 1305 ◽  
Author(s):  
JM Frederiksen ◽  
E Horn ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Layer Structure ◽  
Three Dimensional ◽  
Water Molecules ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Tartrate Anion

The crystal structures of the diastereoisomers formed between the hydrogen-D-tartrate anion and the cations (+)-(Λ-[Co(en)2(NO2)2]+ (1) and (-)-(Δ)-[Co(en)2(NO2)2]+ (2) have been determined by three-dimensional X-ray analysis. The crystal structures are comprised of octahedrally coordinated cobalt atoms, hydrogentartrate anions and water molecules interconnected by a complex hydrogen bonding network. In (1), columns of complex parallel to a 21 screw axis along a, are linked via hydrogen bonding contacts to a total of six chains of 'head-to-tail' hydrogentartrate strands. In contrast, in (2) the chains of hydrogentartrate anions associate with each other to form well defined 'walls' which sandwich hydrogen-bonded columns of complex cations such that the structure may be thought of as a layer structure of hydrogentartrate anions and complex cations. Crystals of both compounds are orthorhombic, space group P212121 with Z = 4, unit cell parameters for (1): a 7.670(1), b 12.160(1), c 18.028(1)Ǻ, V 1681.4 Ǻ3 and for (2): a 7.735(2), b 8.505(5), c 26.846(9) Ǻ, V 1766 1 Ǻ3. The structures were each refined by a full-matrix least-squares procedure to final R 0.026, Rw 0.027 for 1764 reflections with I ≥ 2.5σ(I) for (1) and R 0.065, Rw 0.073 for 1322 reflections for (2).

Zýkait z dolu Lehnschafter u Mikulova v Krušných horách (Česká republika) - popis a Ramanova spektroskopie

2021 ◽  
Vol 29 (2) ◽  
pp. 241-248
Author(s):  
Jiří Sejkora ◽  
Roman Gramblička
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Czech Republic ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Water Molecules ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters

The zýkaite samples were found at abandoned Lehnschafter mine near Mikulov in the Krušné hory Mts. (Czech Republic). It occurs as irregular white to light greenish rounded to spherical aggregates up to 1.5 cm in size composed of tiny acicular crystals up to 5 - 10 μm in length. Its empirical formula can be expressed as (Fe3.79Al0.02)Σ3.81[(AsO4)2.66(PO4)0.20(SiO4)0.07]Σ2.93 (SO4)1.07(OH)0.44·15H2O (mean of 3 spot analyzes; on the basis of As+P+S+Si = 4 apfu).Zýkaite is probably monoclinic, with the unit-cell parameters refined from X-ray powder diffraction data: a 21.195(8), b 7.052(2), c 36.518(17) Å, β 91.07(2)° and V 5458(2) Å3. Raman spectroscopy documented the presence of both (AsO4)3- and (SO4)2- units in the crystal structure of zýkaite. Multiple Raman bands connected with vibrations of water molecules and (AsO4)3- groups indicate the presence of more structurally non-equivalent these groups in the crystal stucture of zýkaite.

Flurlite, Zn3Mn2+Fe3+(PO4)3(OH)2·9H2O, a new mineral from the Hagendorf Süd pegmatite, Bavaria, with a schoonerite-related structure

2015 ◽  
Vol 79 (5) ◽  
pp. 1175-1184 ◽  
Author(s):  
I. E. Grey ◽  
E. Keck ◽  
W. G. Mumme ◽  
A. Pring ◽  
C. M. Macrae ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Layer Structure ◽  
New Mineral ◽  
Water Molecules ◽  
Unit Cell Parameters ◽  
Calculated Density ◽  
X Ray ◽  
Cell Parameters ◽  
Bright Orange ◽  
Edge Sharing Octahedra

AbstractFlurlite, ideally Zn3Mn2+Fe3+(PO4)3(OH)2·9H2O, is a new mineral from the Hagendorf-Süd pegmatite, Hagendorf, Oberpfalz, Bavaria, Germany. Flurlite occurs as ultrathin (<1 μm) translucent platelets that form characteristic twisted accordion-like aggregates. The colour varies from bright orange red to dark maroon red. Cleavage is perfect parallel to (001). The mineral occurs on mitridatite and is closely associated with plimerite. Other associated minerals are beraunite, schoonerite, parascholzite, robertsite and altered phosphophyllite. The calculated density of flurlite is 2.84 g cm–3. It is optically biaxial (–), α = 1.60(1), β= 1.65(1) and γ = 1.68(1), with weak dispersion and parallel extinction, X ≈ c, Y ≈ a, Z ≈ b. Pleochroism is weak, with colours: X = pale yellow, Y = pale orange, Z = orange brown. Electron microprobe analyses (average of seven) with FeO and Fe2O3 apportioned and H2O calculated on structural grounds, gave ZnO 25.4, MnO 5.28, MgO 0.52, FeO 7.40, Fe2O3 10.3, P2O5 27.2, H2O 23.1, total 99.2 wt.%. The empirical formula, based on 3 P a.p.f.u. is Zn2.5Mn2+0.6Fe2+0.8Mg0.1Fe3+(PO4)3(OH)2·9H2O. Flurlite is monoclinic, P21/m, with the unit-cell parameters (at 100 K) of a = 6.3710(13), b = 11.020(2), c = 13.016(3) Å, β = 99.34 (3)°. The strongest lines in the X-ray powder diffraction pattern are [dobs in Å(I) (hkl)] 12.900(100)(001); 8.375(10)(011); 6.072(14)(101); 5.567(8)(012); 4.297(21)(003); 2.763(35)(040). Flurlite (R1 = 0.057 for 995 F > 4σ(F)) has a heteropolyhedral layer structure, with layers parallel to (001) and with water molecules packing between the layers. The slab-like layers contain two types of polyhedral chains running parallel to [100]: (a) chains of edge-sharing octahedra containing predominantly Zn and (b) chains in which Fe3+-centred octahedra share their apices with dimers comprising Zn-centred trigonal bipyramids sharing an edge with PO4 tetrahedra. The two types of chains are interconnected by corner-sharing along [010]. A second type of PO4 tetrahedron connects the chains to MnO2(H2O)4 octahedra along [010] to complete the structure of the (001) slabs. Flurlite has the same stoichiometry as schoonerite, but with dominant Zn rather than Fe2+ in the edge-shared chains. Schoonerite has a similar heteropolyhedral layer structure with the same layer dimensions 6.4 × 11.1 Å. The different symmetry (orthorhombic, Pmab) for schoonerite reflects a different topology of the layers.

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

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Olaf Reckeweg ◽  
Falk Lissner ◽  
Thomas Schleid
Keyword(s):  
Interstitial Water ◽  
Cyanuric Acid ◽  
Dead Volume ◽  
Water Molecules ◽  
Ambient Conditions ◽  
Slow Cooling ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters

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.

Crystal and X-Ray Powder Data for Three Orthovanadates M Th2 (VO4)3 (M = K, Rb, Cs)

1989 ◽  
Vol 4 (3) ◽  
pp. 165-167 ◽  
Author(s):  
A. Elfakir ◽  
J.P. Souron ◽  
M. Quartern
Keyword(s):  
Solid State ◽  
Single Crystals ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Solid State Reaction ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters

AbstractThree isotopic orthovanadates MTh2 (VO4)3 with M = K, Rb, Cs have been syndiesized by solid state reaction. Single crystals of K Th2 (VO4)3 and Rb Th2 (VO4)3 were obtained. These compounds are isotypic with the corresponding orthophosphates: monoclinic, space group C2/c, Z = 4. Unit-cell parameters for die diree compounds were determined. Powder diffraction data for each phase are reported.

Crystallization and preliminary crystallographic study of triple-helical DNA

2000 ◽  
Vol 56 (1) ◽  
pp. 104-105 ◽  
Author(s):  
Zong-Jin Han ◽  
Sangkee Rhee ◽  
Keliang Liu ◽  
H. Todd Miles ◽  
David R. Davies
Keyword(s):  
Single Crystals ◽  
Unit Cell ◽  
The Other ◽  
Diffusion Method ◽  
Triplex Dna ◽  
Asymmetric Unit ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Crystallographic Study

Single crystals of d(CTCCTSCCGCGCG)·d(CGCGCGGAG) have been grown by the vapor-diffusion method using 2-methyl-2,4-pentanediol as a precipitant. The crystals are tetragonal, space group P42, with unit-cell parameters a = b = 53.8, c = 43.1 Å, and diffract to 1.8 Å resolution at a synchrotron X-ray beamline. In the crystal, the asymmetric unit contains one copy of the construct. The two halves of the structure are related by non-crystallographic twofold symmetry. These observations are consistent with the conclusion that the sequences of the 12-mer and 9-mer oligonucleotides form a duplex DNA at one end and a triplex DNA at the other end.

Rietveld refinement of X-ray powder diffraction data of Ca0.925Ce0.075Mn0.9Fe0.1O3 polycrystalline material

2018 ◽  
Vol 33 (4) ◽  
pp. 303-305
Author(s):  
G. Murugesan ◽  
K. R. Nandan ◽  
S. Kalainathan
Keyword(s):  
Single Phase ◽  
Polycrystalline Material ◽  
General Structure ◽  
Sol Gel ◽  
Powder Diffraction Data ◽  
Orthorhombic Structure ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters

Polycrystalline Ca0.925Ce0.075Mn0.9Fe0.1O3 were prepared by sol-gel reaction at 1073 K. The compound was analyzed by a powder X-ray diffraction technique and found to be in single phase. The unit-cell parameters and atomic positions were refined using General Structure Analysis to an orthorhombic structure with space group Pnma (#62) a = 5.281 90 (33) Å, b = 7.4968 (45) Å, and c = 5.302 90 (32) Å.

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