scholarly journals Crystal Structure and Optical Properties of a Homometallic Heterotrinuclear Europium(III) Complex – a Cationic Eu(III) ion Coordinated by two [Eu(III)DOTA]- Complexes

2021 ◽  
Author(s):  
Maria Storm Thomsen ◽  
Ander Østergård Madsen ◽  
Thomas Just Sørensen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Coordination Number ◽  
Luminescence Spectroscopy ◽  
Data Sets ◽  
Complex Data ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
High Asymmetry ◽  
State Luminescence

The structure and solid state luminescence properties of a homometallic heterotrinuclear [Eu(μO)5(OH2)3][Eu(DOTA)(H2O)]2Cl crystal was determined and was found to have two sites: a free europium(III) ion and a [Eu(DOTA)(H2O)]- complex. The trinuclear compound crystallizes in a laminar structure in triclinic space group P. The crystal structure was determined using complex data treatment due to non-merohedric twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domain in order to obtain a reliable structure, which revealed the configuration of the europium(III) sites. In first site, the europium(III) 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate (Eu.DOTA) complex was found to adopt a capped twisted square antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the cationic europium(III) ion was found to be coordinated by three water molecules and five oxy groups from neighboring [Eu(DOTA)(H2O)]- complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP), and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in rate constant of luminescence was observed for Eu(III) in [Eu(DOTA)(H2O)]- in solid state luminescence spectroscopy measurements compared to in solution, which lead to investigations of single-crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]- in the [Eu(μO)5(OD2)3][Eu(DOTA)(D2O)]2Cl crystals<br>

scholarly journals Crystal Structure and Optical Properties of a Homometallic Heterotrinuclear Europium(III) Complex – a Cationic Eu(III) ion Coordinated by two [Eu(III)DOTA]- Complexes

2021 ◽  
Author(s):  
Maria Storm Thomsen ◽  
Ander Østergård Madsen ◽  
Thomas Just Sørensen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Coordination Number ◽  
Luminescence Spectroscopy ◽  
Data Sets ◽  
Complex Data ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
High Asymmetry ◽  
State Luminescence

The structure and solid state luminescence properties of a homometallic heterotrinuclear [Eu(μO)5(OH2)3][Eu(DOTA)(H2O)]2Cl crystal was determined and was found to have two sites: a free europium(III) ion and a [Eu(DOTA)(H2O)]- complex. The trinuclear compound crystallizes in a laminar structure in triclinic space group P. The crystal structure was determined using complex data treatment due to non-merohedric twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domain in order to obtain a reliable structure, which revealed the configuration of the europium(III) sites. In first site, the europium(III) 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate (Eu.DOTA) complex was found to adopt a capped twisted square antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the cationic europium(III) ion was found to be coordinated by three water molecules and five oxy groups from neighboring [Eu(DOTA)(H2O)]- complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP), and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in rate constant of luminescence was observed for Eu(III) in [Eu(DOTA)(H2O)]- in solid state luminescence spectroscopy measurements compared to in solution, which lead to investigations of single-crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]- in the [Eu(μO)5(OD2)3][Eu(DOTA)(D2O)]2Cl crystals<br>

scholarly journals Crystal Structure and Optical Properties of a Homometallic Heterotrinuclear Europium(III) Complex – a Cationic Eu(III) ion Coordinated by two [Eu(III)DOTA]- Complexes

2021 ◽  
Author(s):  
Maria Storm Thomsen ◽  
Ander Østergård Madsen ◽  
Thomas Just Sørensen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Coordination Number ◽  
Luminescence Spectroscopy ◽  
Data Sets ◽  
Complex Data ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
High Asymmetry ◽  
State Luminescence

The structure and solid state luminescence properties of a homometallic heterotrinuclear [Eu(μO)5(OH2)3][Eu(DOTA)(H2O)]2Cl crystal was determined and was found to have two sites: a free europium(III) ion and a [Eu(DOTA)(H2O)]- complex. The trinuclear compound crystallizes in a laminar structure in triclinic space group P. The crystal structure was determined using complex data treatment due to non-merohedric twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domain in order to obtain a reliable structure, which revealed the configuration of the europium(III) sites. In first site, the europium(III) 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate (Eu.DOTA) complex was found to adopt a capped twisted square antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the cationic europium(III) ion was found to be coordinated by three water molecules and five oxy groups from neighboring [Eu(DOTA)(H2O)]- complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP), and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in rate constant of luminescence was observed for Eu(III) in [Eu(DOTA)(H2O)]- in solid state luminescence spectroscopy measurements compared to in solution, which lead to investigations of single-crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]- in the [Eu(μO)5(OD2)3][Eu(DOTA)(D2O)]2Cl crystals<br>

Crystal structure and optical properties of a two-sited EuIII compound: an EuIII ion coordinated by two [EuIII(DOTA)]− complexes (DOTA is 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate)

2021 ◽  
Vol 77 (7) ◽  
Author(s):  
Maria Storm Thomsen ◽  
Anders Ø. Madsen ◽  
Thomas Just Sørensen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Coordination Number ◽  
Luminescence Spectroscopy ◽  
Data Sets ◽  
Complex Data ◽  
Triclinic Space Group ◽  
High Asymmetry ◽  
State Luminescence ◽  
The Eu

The structure and solid-state luminescence properties of an EuIII compound with two different lanthanide sites, [Eu(μ-O)5(OH)(H2O)2][Eu(DOTA)(H2O)]2 (DOTA is 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate, C16H24N4O8), were determined. The compound crystallizes in a laminar structure in the triclinic space group P\overline{1}, where the two sites are a free europium(III) ion and an [Eu(DOTA)(H2O)]− complex. The crystal structure was determined using complex data treatment due to nonmerohedral twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domains in order to obtain a reliable structure. In the first site, the [Eu(DOTA)(H2O)]− complex was found to adopt a capped twisted square-antiprismatic (cTSAP) conformation, where a capping water molecule increased the coordination number of the europium(III) site to nine (CN = 9). In the second site, the europium(III) ion was found to be coordinated by two water molecules, one hydroxide group and five oxide groups from neighbouring [Eu(DOTA)(H2O)]− complexes. The coordination geometry of this site was found to be a compressed square antiprism (SAP) and the coordination number of the europium(III) ion was found to be eight (CN = 8). A large increase in the rate constant of luminescence was observed for EuIII in [Eu(DOTA)(H2O)]− in solid-state luminescence spectroscopy measurements compared to in solution, which led to investigations of single crystals in deuterated media to exclude additional effects of quenching. We conclude that the most probable cause of the decrease in the observed luminescence lifetimes is the high asymmetry of the coordination environment of [Eu(DOTA)(D2O)]− in the [Eu(μ-O)5(OD)(D2O)2][Eu(DOTA)(D2O)]2 crystals.

scholarly journals A new zinc(II) supramolecular square: Synthesis, crystal structure, thermal behavior and luminescence

2015 ◽  
Vol 80 (10) ◽  
pp. 1289-1295
Author(s):  
Xiu-Yan Wang ◽  
Zhong-Yu Zhao ◽  
Qian Han ◽  
Miao Yu ◽  
De-Yu Kong
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Thermal Behavior ◽  
Luminescence Property ◽  
Room Temperature ◽  
Hydrothermal Condition ◽  
Stacking Interactions ◽  
Triclinic Space Group ◽  
Four Corners ◽  
State Luminescence

A new square-shaped Zn(II) complex, namely, [Zn4(L)4(phen)4]?6H2O (1) (L = 2-hydroxynicotinate and phen = 1,10- phenanthroline), has been synthesized under hydrothermal condition. The crystal of 1 belongs to triclinic, space group P -1 with a = 10.773(2) ?, b = 12.641(3) ?, c = 13.573(3) ?, ? = 107.44(3)?, ? = 102.66(3)?, ? = 93.89(3)?, C72H56N12O18Zn4, Mr = 1638.77, V = 1702.8(6) ?3 , Z = 1, Dc = 1.598 g/cm3 , S = 1.045, ?(MoK?) = 1.475 mm-1 , F(000) = 836, R = 0.0472 and wR = 0.0919. In 1, four L ligands bridge four Zn(II) atoms to form a square-shaped structure, where four phen ligands are respectively located on four corners of the square. The ?-? stacking interactions extend the adjacent squares into a 1D supramolecular chain. The thermal behavior of 1 has been characterized. Moreover, its solid state luminescence property has been studied at room temperature.

Structure and stereochemistry in 'f-block' complexes of high coordination number. VII. The [M(unidentate X)2(unidentate Y)6] system: Crystal structure of hexaaquadichloroeuropium(III) chloride (a redetermination)

1983 ◽  
Vol 36 (3) ◽  
pp. 477 ◽  
Author(s):  
DL Kepert ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Coordination Number ◽  
Title Compound ◽  
Chlorine Atoms ◽  
Coordination Environment ◽  
Twofold Axis ◽  
High Coordination Number ◽  
Europium Atom ◽  
High Coordination

The crystal structure of the title compound [EuCl2(OH2)2]Cl ('europium trichloride hexahydrate') has been redetermined from single-crystal diffractometer data at 295 K and refined to a residual of 0.040 for 1094 independent 'observed' reflections. Crystals are monoclinic, P2/n, a 9.659(3), b 6.529(2), c 7.936(4) �, β 93.67(4)�, Z 2. The europium atom lies on a crystallographic twofold axis, which passes between the two planes of a square-antiprismatic coordination environment in which the two chlorine atoms, on opposite faces, lie cis to each other. Eu-O distances range from 2.401(6) to 2.431(5) �; Eu-Cl is 2.774(2) �.

Eine unerwartete Synthese des Triphenyphosphazenium-chlorids, [(C6H5)3PNH2]+CI– und eine Neubestimmung seiner Kristallstruktur / An Unaspected Synthesis of Triphenylphosphazenium Chloride, [(C6H5)3PNH2]+Cl– , and a Redeterm ination of its Crystal Structure

1996 ◽  
Vol 51 (6) ◽  
pp. 865-868 ◽  
Author(s):  
H. Vogt ◽  
A. Fischer ◽  
P. G. Jones
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group

Abstract Triphenylphosphazenium chloride has been prepared by the reaction of triphenylphosphine with trimethylsilylazide in impure, wet dichloromethane. Yields are improved as stoichiometric quantities of water are added. Colourless crystals are obtained by recrystallization from the same solvent. The crystals are triclinic, space group P1̅, Z=2, a = 894,6(3), b - 979,8(3), c = 1142,9(4) pm, α = 107,27(3), β = 93,70(3), y = 92,97(3)°. In the solid state the compound exists as [(C6H5)3PNH2]+ cations, and Cl- anions. Dimeric units are formed by H-bonding. The crystal structure contains one molecule CH2Cl2 per one molecule (C6H5)3PNH2Cl. The cation has a slightly irregular tetrahedral geometry around the P-atom with a relatively short P-N bond

Solvothermal self-assembly of Cd2+ coordination polymers with supramolecular networks involving N-donor ligands and aromatic dicarboxylates: synthesis, crystal structure and photoluminescence studies

2017 ◽  
Vol 46 (11) ◽  
pp. 3623-3630 ◽  
Author(s):  
Yadagiri Rachuri ◽  
Bhavesh Parmar ◽  
Kamal Kumar Bisht ◽  
Eringathodi Suresh
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Coordination Polymers ◽  
Self Assembly ◽  
Luminescence Quenching ◽  
Donor Ligands ◽  
Supramolecular Networks ◽  
Photoluminescence Studies ◽  
State Luminescence

Structural, solid state luminescence of Cd(ii) coordination polymers and detection of acetone by CP1via luminescence quenching have been discussed.

Cyclothiazeno-oxo-diazidowoIframat(VI) Die Kristallstruktur von (AsPh4)2[W(N3S2)(O)(N3)2]2 / Cyclothiazeno Oxodiazidotungstate(VI) The Crystal Structure of (AsPh4)2[W(N3S2)(O)(N3)2]2

1985 ◽  
Vol 40 (12) ◽  
pp. 1626-1630 ◽  
Author(s):  
Heribert Wadle ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Ring System ◽  
Crystal Data ◽  
Improved Method ◽  
Silver Azide ◽  
Tungsten Atom ◽  
Triclinic Space Group

Abstract A new, improved method of synthesis for the cyclothiazeno complex AsPh4[WCl4(N3S2)] consists of the reaction of Na2WO4 with molten trithiazyl chloride (NSCl)3 followed by treatment with AsPh4Cl in CH2C12. Through the reaction with silver azide suspended in CH2C12 in the presence of moisture, black crystalline (AsPh4)2[W(N3S2)(O)(N3)2]2 is obtained. Its IR spectrum and its crystal structure are reported. Crystal data: triclinic, space group P1̄, Z = 1, a - 1018.3, b = 1107.8, c = 1379.1 pm; a = 91.11°, β = 106.74°, γ = 113.91°. Structure determination with 3219 observed reflexions, R = 0.061. The structure consists of AsPh4+ cations arranged to form (AsPh4+)2 pairs and of dimeric anions [W(N3S2)(O)(N3)2]2⊖ in which the tungsten atom s are members of planar cyclothiazeno rings WN3S2 with WN bond lengths of 186 and 222 pm. The oxygen atoms are in positions trans to the longer of these bonds. One of the N atoms of each cyclothiazeno ring is involved in the dimerization resulting in a centrosymmetric W2N2 ring. The azido groups are situated above and below the ring system and complete the coordination number of six for the W atoms with WN distances of 208 and 212 pm

Hloušekite, (Ni,Co)Cu4(AsO4)2(AsO3OH)2(H2O)9, a new member of the lindackerite supergroup from Jáchymov, Czech Republic

2014 ◽  
Vol 78 (5) ◽  
pp. 1341-1353 ◽  
Author(s):  
J. Plášil ◽  
J. Sejkora ◽  
R. Škoda ◽  
M. Novák ◽  
A. V. Kasatkin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Czech Republic ◽  
X Ray Diffraction ◽  
Calculated Density ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
Xrd Pattern ◽  
Mohs Hardness ◽  
The Difference ◽  
Pale Green

AbstractHloušekite, (Ni,Co)Cu4(AsO4)2(AsO3OH)2(H2O)9, is a new supergene arsenate mineral from the Geister vein (Rovnost mine), Jáchymov (St Joachimsthal), Western Bohemia, Czech Republic. It was found along with veselovský ite, pradetite, lavendulan, arsenolite, babánekite and gypsum on the surface of strongly altered ore fragments containing dominant tennantite and chalcopyrite. Hloušekite forms thin, lath-like crystals, locally elongated reaching up to 3 mm across. It is transparent, has a pale green colour with vitreous lustre, has a greyish-white streak and it is very brittle with an uneven fracture. It does not fluoresce under shortwave or longwave ultraviolet radiation. Cleavage on {010} is perfect; the Mohs hardness is 2–3. The calculated density is 3.295 g cm–3. Hloušekite is optically biaxial with α’ = 1.653(2) and γ’ = 1.73. The estimated optical orientation is γ’ vs. elongation (c) = 14(1)°. In larger grains it is weakly to moderately pleochroic (α = colourless, γ = pale green to green). Hloušekite is triclinic, space group P1̄ , a = 6.4010(6), b = 8.0041(6), c = 10.3969(14) Å , α = 85.824(8), β = 79.873(9), γ = 84.655(7)° and V = 521.23(10) Å3, with Z = 1, a:b:c = 0.800:1:1.299. The eight strongest lines in the powder X-ray diffraction (XRD) pattern [d in Å (I)(hkl)] are 10.211(100)(001), 7.974(9)(010), 3.984(6)(020), 3.656(5)(11̄2), 3.631(5)(02̄ 1), 3.241(5)(022), 3.145(5)(200) and 3.006(5)(210). Chemical analysis by electron microprobe yielded MgO 0.20, FeO 0.10, NiO 5.79, CoO1.80, CuO29.53, ZnO 0.66, Al2O3 0.14, P2O5 0.11, As2O5 45.01, H2O 17.71 (calc.), for a total of 101.05 wt.%. The resulting empirical formula, calculated by stoichiometry (9H2O + 2OH), obtained from the crystal structure, is (Ni0.79Co0.25)Σ1.04(Cu3.78Zn0.08Mg0.05Al0.03Fe0.01)Σ3.95 (AsO4 )1.98(PO4 )0.02(AsO3OH)2.00(H2O)9.00 . The ideal endmember formula , NiCu4(AsO4)2(AsO3OH)2(H2O)9.00, requires NiO7.23, CuO30.81, As2O5 44.51, H2O17.45, total 100.00 wt.%. The crystal structure of hloušekite was solved by charge flipping from single-crystal XRD data and refined to R1 = 0.0599 for 1441 reflections with [Iobs > 3σ(I)]. Hloušekite is a new member of the lindackerite group (also including lindackerite, pradetite and veselovský ite) of the lindackerite supergroup. The ondrušite group of the lindackerite supergroup includes ondrušite, chudobaite, geigerite and klajite. The establishment of these two groups reflects the difference between the crystal structures of their members, mainly in the coordination environment of the Me cations.

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