Co-reporter:Daniele C. Menezes, Geraldo M. de Lima, James L. Wardell, Jessica Gomez-Banderas, William T.A. Harrison
Journal of Organometallic Chemistry 2017 Volume 848(Volume 848) pp:
Publication Date(Web):15 October 2017
DOI:10.1016/j.jorganchem.2017.08.011
•New types of amidotehyl tin complexes are presented.•Ligand disproportionation and trans-esterification reactions occur.•New insights into polymorphism and hydrolytic stability are offered.The syntheses, spectroscopic data and crystal structures of (H2NCOCH2CH2-C)(R2NCS2-S,S′)3Sn (1), (H2NCOCH2CH2-C,O)2SnCl2 (triclinic polymorph) (2), (H2NCOCH2CH2-C,O)(2-H2NCOC6H4S-O,S)SnCl2 (3) and Sn(C11H9N2O2)Cl3 (4) are reported. The tin atom in compound 1 (R = Et) is coordinated by three chelating dithiocarbamate anions and a C-bound non-chelating amidoethyl ligand to generate a SnS6C pentagonal-bipyramidal coordination polyhedron. Compound 2, which features SnC2O2Cl2 octahedra, was crystallised from mixed solvents (ethanol and water) and complements the two known monoclinic forms. Compound 3 arose unexpectedly due to ligand disproportionation of the tin starting material and a “trans-esterification” reaction of the starting ligand: distorted SnCSO2Cl2 octahedra are seen in the crystal structure. Compound 4 arose from another ligand disproportionation reaction and features neutral complex molecules with N2OCl3 donor sets coordinating to the octahedral tin atoms.Download high-res image (133KB)Download full-size image
Co-reporter:M. J. Plater;B. M. De Silva;M. R. St. J. Foreman
Journal of Structural Chemistry 2016 Volume 57( Issue 6) pp:1169-1175
Publication Date(Web):2016 November
DOI:10.1134/S0022476616060160
The syntheses and crystal structures of two one-dimensional coordination polymers, [Mn(C5HO2F6)2(C16H20N2)]n (1) and [Mn(C5HO2F6)2(C20H20N2)]n (2), are described, where C5HO2F6− is the hexafluoro acetylacetonate anion, C16H20N2 is 1,6-bis(4-pyridyl)-hexane, and C20H20N2 is 1,4-bis[2-(3-pyridyl)ethyl]-benzene. In both phases, the metal ion lies on a crystallographic twofold axis and is coordinated by two chelating C5HO2F6− anions and two bridging bipyridyl ligands to generate a cis-MnN2O4 octahedron. The bridging ligands, which are completed by crystallographic inversion symmetry in both compounds, connect the metal nodes into zigzag [20 1 ] chains in 1 and contorted [001] chains in 2. Intrachain C–H•••O interactions occur in 1 but not in 2, which may be correlated with the relative orientations of the ligands. Crystal data: 1, C26H22F12MnN2O4, Mr = 709.40, monoclinic, C2/c (No. 15), a = 9.3475(2) Å, b = 16.6547(3) Å, c = 18.3649(4) Å, β = 91.1135(8)°, V = 2858.50(10) Å3, Z = 4, R(F) = 0.030, wR(F2) = 0.075. 2, C30H22F12MnN2O4, Mr = 757.44, monoclinic, C2/c (No. 15), a = 19.9198(2) Å, b = 10.6459(2) Å, c = 16.8185(3) Å, β = 119.8344(8)°, V = 3093.91(9) Å3, Z = 4, R(F) = 0.032, wR(F2) = 0.078.
Co-reporter:Muhammad Nadeem Akhtar
Transition Metal Chemistry 2016 Volume 41( Issue 3) pp:325-330
Publication Date(Web):2016 April
DOI:10.1007/s11243-016-0025-8
The synthesis, crystal structure and biological properties of [Co(edtp)Cl)]·NO3·H2O are described, where edtp is N,N,N′,N′-tetrakis(2-hydroxypropyl) ethylenediamine. The Co2+ ion is coordinated by the N,N′,O,O′,O″-pentadentate edtp ligand and a chloride to generate a distorted CoClN2O3 octahedron. The complex exhibits moderate antithrombolytic activity (38 % screened by hemolytic assay) against clots developed by bovine blood and negligible cytotoxicity (5 %) against bovine erythrocytes. Conversely, very high bacterial biofilm inhibition (90 %) was recorded against both Gram-positive and Gram-negative bacterial species.
Co-reporter:Muhammad Kaleem Khosa;Paul T. Wood;Simon M. Humphrey
Acta Crystallographica Section C 2016 Volume 72( Issue 1) pp:63-67
Publication Date(Web):
DOI:10.1107/S205322961502330X
Compounds containing copper(I) are of interest for their role in biological processes. The nature of short (< ∼3.2 Å) Cu...Cu contacts within these compounds has been debated, being either described as weakly attractive (bonding) `cuprophilic' interactions, or simply as short metal–metal distances constrained by ligand geometry or largely ionic in nature. The title three-dimensional Cu+-containing coordination polymer, [Cu3(C7H7N2O2)Cl2]n, was formed from the in situ reduction of CuCl2 in the presence of 3,5-diaminobenzoic acid and KOH under hydrothermal conditions. Its complex crystal structure contains ten distinct CuI atoms, two of which lie on crystallographic inversion centres. The copper coordination geometries include near-linear CuOCl and CuN2, T-shaped CuOCl2 and distorted tetrahedral CuOCl3 groups. Each CuI atom is also associated with two adjacent metal atoms, with Cu...Cu distances varying from 2.7350 (14) to 3.2142 (13) Å; if all these are regarded as `cuprophilic' interactions, then infinite [01] zigzag chains of CuI atoms occur in the crystal. The structure is consolidated by N—H...Cl hydrogen bonds.
Co-reporter:Thais C. M. Nogueira;Alessra C. Pinheiro;James L. Wardell;Marcus V. N. de Souza;Jordan P. Abberley ;William T A Harrison
Acta Crystallographica Section C 2015 Volume 71( Issue 8) pp:647-652
Publication Date(Web):
DOI:10.1107/S2053229615012450
Oxazolidin-2-ones are widely used as protective groups for 1,2-amino alcohols and chiral derivatives are employed as chiral auxiliaries. The crystal structures of four differently substituted oxazolidinecarbohydrazides, namely N′-[(E)-benzylidene]-N-methyl-2-oxo-1,3-oxazolidine-4-carbohydrazide, C12H12N3O3, (I), N′-[(E)-2-chlorobenzylidene]-N-methyl-2-oxo-1,3-oxazolidine-4-carbohydrazide, C12H12ClN3O3, (II), (4S)-N′-[(E)-4-chlorobenzylidene]-N-methyl-2-oxo-1,3-oxazolidine-4-carbohydrazide, C12H12ClN3O3, (III), and (4S)-N′-[(E)-2,6-dichlorobenzylidene]-N,3-dimethyl-2-oxo-1,3-oxazolidine-4-carbohydrazide, C13H13Cl2N3O3, (IV), show that an unexpected mild-condition racemization from the chiral starting materials has occurred in (I) and (II). In the extended structures, the centrosymmetric phases, which each crystallize with two molecules (A and B) in the asymmetric unit, form A+B dimers linked by pairs of N—H...O hydrogen bonds, albeit with different O-atom acceptors. One dimer is composed of one molecule with an S configuration for its stereogenic centre and the other with an R configuration, and possesses approximate local inversion symmetry. The other dimer consists of either R,R or S,S pairs and possesses approximate local twofold symmetry. In the chiral structure, N—H...O hydrogen bonds link the molecules into C(5) chains, with adjacent molecules related by a 21 screw axis. A wide variety of weak interactions, including C—H...O, C—H...Cl, C—H...π and π–π stacking interactions, occur in these structures, but there is little conformity between them.
Co-reporter:S. Hussain;I. U. Khan;W. T. A. Harrison;M. N. Tahir
Journal of Structural Chemistry 2015 Volume 56( Issue 5) pp:934-941
Publication Date(Web):2015 September
DOI:10.1134/S0022476615050169
The synthesis, crystal structures, and characterization (IR, TGA/DSC) of [Nd(C5H6O4)(H2O)4]•Cl (1) and [Pr(C5H6O4)(C5H7O4)(H2O)]•H2O (2) are described. Compound 1 is a one-dimensional coordination polymer containing double chains incorporating pairs of edge-sharing NdO9 polyhedra linked by glutarate dianions. A network of O–H…O and O–H…Cl hydrogen bonds helps to consolidate the structure. Compound 2 is a three-dimensional coordination polymer incorporating chains of edge-sharing PrO10 polyhedra. Its glutarate ion adopts an extended conformation, whereas its hydrogen glutarate ion takes on a twisted conformation. O–H…O hydrogen bonds are seen in the crystal structure, which features small channels occupied by water molecules. Crystal data: 1, C5H14ClNdO8, Mr = 381.85, monoclinic, P21/c (No. 14), a = 8.9763(6) Å, b = 15.9277(11) Å, c = 8.8690(6) Å, β = 112.090(2)°, V = 1174.94(14) Å3, Z = 4, R(F) = 0.016, wR(F2) = 0.037. 2, C10H17O10Pr, Mr = 438.15, orthorhombic, Pbca (No. 61), a = 16.3030(7) Å, b = 8.6714(4) Å, c = 19.3899(8) Å, V = 2741.1(2) Å3, Z = 8, R(F) = 0.020, wR(F2) = 0.050.
Co-reporter:Magnus G. Johnston
European Journal of Inorganic Chemistry 2011 Volume 2011( Issue 19) pp:2967-2974
Publication Date(Web):
DOI:10.1002/ejic.201100344
Abstract
The syntheses and characterisation of a new family of isostructural mixed-metal selenites based on the zemannite-type framework are described. These BaM2(SeO3)3·3H2O phases are built up from three-dimensional networks of MO6 (M = Co, Ni, Mn, Mg) octahedra and SeO3 pyramids. The octahedral groups form isolated M2O9 face-sharing pairs, which are linked by the selenite anions into a three-dimensional anionic framework. The framework encapsulates one-dimensional 12-ring channels occupied by the barium cations and water molecules. There are two types of channels: in one, the cations and water molecules are well ordered, and the channels are fully occupied; in the other, the same species are disordered, and the channels are partially occupied. There is little if any evidence of zeolitic reversible de/rehydration and cation ion-exchange behaviour for these materials.
Co-reporter:Raj Pal Sharma, Ajnesh Singh, Paloth Venugopalan, William T.A. Harrison
Journal of Molecular Structure 2011 Volume 994(1–3) pp:6-12
Publication Date(Web):17 May 2011
DOI:10.1016/j.molstruc.2011.02.040
In an effort to utilize the cationic cobalt(III) complex as a binding agent for fluoroanions, the reaction of carbonatobis(1,10-phenanthroline)cobalt(III) chloride with sodium tetrafluoroborate and sodium hexafluorophosphate in water (1:1 M ratio) leads to the formation of [Co(phen)2CO3]BF4 (1) and [Co(phen)2CO3]PF6·3H2O (2). These cobalt(III) complex salts have been characterized by elemental analyses, spectroscopic techniques (multinuclear NMR, UV/Visible and FT-IR), solubility product and conductance measurements. X-ray structure determination of these complex salts revealed the presence of ionic structures i.e., one complex cation [Co(phen)2CO3]+ and one BF4- anion in 1 and one complex cation [Co(phen)2CO3]+, one PF6- anion and three water molecules of crystallisation in 2. The packings in both complex salts are stabilized by CH⋯F, CH⋯O(carbonato) hydrogen bonds and anion⋯π interactions beside electrostatic forces of attraction. In addition to these non-covalent interactions, OH⋯O(water) and π–π stacking interactions are also observed in 2. The formation of complex salts of definite composition with tetrafluoroborate and hexafluorophosphate ions suggest that [Co(phen)2CO3]+ may be used as binding agent for weakly coordinating fluoroanions i.e. BF4- and PF6-.
Co-reporter:Raj Pal Sharma, Ajnesh Singh, Paloth Venugopalan, William T.A. Harrison
Journal of Molecular Structure 2011 Volume 996(1–3) pp:82-89
Publication Date(Web):14 June 2011
DOI:10.1016/j.molstruc.2011.04.020
The syntheses, physical, spectroscopic characterizations and crystal structures of [Co(phen)2CO3]ClO3, [Co(phen)2CO3]BrO3·3.5H2O and [Co(phen)2CO3]IO4 are described (phen = 1,10-phenanthroline, C12H8N2). The crystal structures feature “synergistic” directional bonding interactions including cation-to-anion C–H⋯O(anion) bonds and anion-to-cation Cl⋯π and I–O⋯π bonds, as well as cation-to-cation C–H⋯O(carbonato) and π – π stacking interactions. The bromate structure also features distinctive O–H⋯O hydrogen bonding networks involving the water molecules. The facile formation of this series of complex salts with relatively small Ksp values suggests that the [Co(phen)2CO3]+ complex ion may be effective as a binding agent for oxo-anions containing halogen atoms(halates) in an aqueous environment.Highlights► Synthesis of three Co(III) complexes, [Co(phen)2CO3]ClO3, [Co(phen)2CO3] BrO3·3.5H2O and [Co(phen)2CO3]IO4. ► Synergistic cation-to-anion and anion-to-cation interactions. ► Non-covalent interactions C–H⋯O, O–H⋯O, I–O⋯π, Cl⋯π, π–π are playing crucial role in binding of anions.
Co-reporter:William T.A. Harrison, Ejaz, Islam Ullah Khan
Polyhedron 2011 30(13) pp: 2181-2185
Publication Date(Web):
DOI:10.1016/j.poly.2011.05.049
Co-reporter:Raj Pal Sharma, Anju Saini, Sukhjinder Singh, Paloth Venugopalan, William T.A. Harrison
Journal of Fluorine Chemistry 2010 Volume 131(Issue 4) pp:456-460
Publication Date(Web):April 2010
DOI:10.1016/j.jfluchem.2009.12.020
The syntheses, physical characterization and crystal structures of two new molecular copper(II) complexes of composition [Cu(C5H5N)2(C7F5O2)2] (1) and [Cu(C5H5N)2(C7F5O2)2(H2O)] (2) (C5H5N = py = pyridine and C7F5O2− = pfb = pentafluorobenzoate) are reported. Single-crystal X-ray structure determinations revealed that in 1, the Cu2+ ion, which lies on a crystallographic inversion centre, is coordinated to two py molecules and two oxygen atoms from two monodentate pfb anions, resulting in a trans-CuN2O2 square planar geometry. In 2, the Cu2+ ion is also coordinated to two py and two pfb species in addition to a water molecule in the apical site of a distorted CuN2O3 square pyramid. In the crystal packing, both 1 and 2 show segregated aromatic π–π stacking interactions in which (py + py) and (pfb + pfb) ring-pairings are seen, but no (py + pfb) pairings occur. Crystal data: 1: C24H10CuF10N2O4, Mr = 643.88, space group P1¯, a = 8.0777 (3) Å, b = 8.0937 (3) Å, c = 10.5045 (5) Å, α = 90.916 (3)°, β = 93.189 (2)°, γ = 118.245 (3)°, V = 603.36 (4) Å3, Z = 1. 2: C24H12CuF10N2O5, Mr = 661.90, space group P1¯, a = 7.5913 (5) Å, b = 15.6517 (6) Å, c = 21.1820 (14) Å, α = 95.697 (4)°, β = 94.506 (2)°, γ = 91.492 (4)°, V = 2495.2 (3) Å3, Z = 4.Two new copper(II)pentafluorobenzoate complexes with pyridine [Cu(py)2(pfb)2] (1) and [Cu(py)2(pfb)2(H2O)] (2) (where py = pyridine and pfb = pentafluorobenzoate) were isolated and structurally characterized. Detailed packing analysis of both complexes 1 and 2 show segregated aromatic π–π stacking interactions in which (py + py) and (pfb + pfb) ring-pairings are observed.
Co-reporter:Lucy A. Paton ;Dr. William T. A. Harrison
Angewandte Chemie International Edition 2010 Volume 49( Issue 42) pp:7684-7687
Publication Date(Web):
DOI:10.1002/anie.201003541
Co-reporter:Lucy A. Paton ;Dr. William T. A. Harrison
Angewandte Chemie 2010 Volume 122( Issue 42) pp:7850-7853
Publication Date(Web):
DOI:10.1002/ange.201003541
Co-reporter:Krishnan Srinivasan, Subbaiah Govindarajan, William T.A. Harrison
Inorganic Chemistry Communications 2009 Volume 12(Issue 7) pp:619-621
Publication Date(Web):July 2009
DOI:10.1016/j.inoche.2009.05.002
The syntheses and crystal structures of Zn(CH4N2O)2(H2O)2·2(NO3) (1) and Co(CH4N2O)2(H2O)2·2(NO3) (2), the first well-characterised metal complexes of formylhydrazine (fh), are described. In both compounds, the fh acts as an N,O-bidentate ligand in a centrosymmetric [M(fh)2(H2O)2]2+ cation, with charge balance supplied by nitrate counter ions. The packing for the two compounds are quite different: in 1, chains of [Zn(fh)2(H2O)2]2+ units are seen in the triclinic unit cell, whereas in the monoclinic structure of 2, sheets of cations occur. This might arise because the conformations of the five-membered chelate rings for the ligands are slightly different, with that for 2 showing a greater degree of puckering.The syntheses and crystal structures of Zn(CH4N2O)2·(H2O)2·2(NO3) (1) and Co(CH4N2O)2(H2O)2·2(NO3) (2), the first well-characterised metal complexes of formylhydrazine (fh), are described. In both compounds, the fh acts as an N,O-bidentate ligand in a centrosymmetric [M(fh)2(H2O)2]2+ cation, with charge balance supplied by nitrate counter ions. The packing for the two compounds are quite different: in 1, chains of [Zn(fh)2(H2O)2]2+ units are seen in the triclinic unit cell, whereas in the monoclinic structure of 2, sheets of cations occur. This might arise because the conformations of the five-membered chelate rings for the ligands are slightly different, with that for 2 showing a greater degree of puckering.
Co-reporter:Andrew S. Holtby, William T.A. Harrison, Veysel T. Yilmaz, Orhan Büyükgüngör
Solid State Sciences 2007 Volume 9(Issue 2) pp:149-154
Publication Date(Web):February 2007
DOI:10.1016/j.solidstatesciences.2006.11.001
The mild-condition syntheses, single-crystal structures and properties of H3N(CH2)5NH3·Zn3(HPO3)4 and β-H3N(CH2)6NH3·Zn3(HPO3)4 are reported. Both are constructed from (3,4)-nets of ZnO4 tetrahedra and HPO3 pyramids, sharing vertices to result in three-dimensional anionic open-frameworks. In both materials, the organic species interacts with the framework by way of N–H⋯O bonds. Crystal data: H3N(CH2)5NH3·Zn3(HPO3)4, Mr = 620.22, orthorhombic, Pccn (No. 56), a = 9.5364 (9) Å, b = 21.8015 (19) Å, c = 9.1118 (7) Å, V = 1894.4 (3) Å3, Z = 4, R(F) = 0.044, wR(F2) = 0.111. β-H3N(CH2)6NH3·Zn3(HPO3)4, Mr = 634.25, monoclinic, P21/n (No. 14), a = 8.7627 (1) Å, b = 13.8117 (2) Å, c = 16.6187 (3) Å, β = 92.680 (1)°, V = 2009.12 (5) Å3, Z = 4, R(F) = 0.072, wR(F2) = 0.187.
Co-reporter:John T. S. Irvine, Magnus G. Johnston and William T. A. Harrison
Dalton Transactions 2003 (Issue 13) pp:2641-2645
Publication Date(Web):2003/05/30
DOI:10.1039/B300573A
The hydrothermal and ceramic syntheses, single crystal structures and some properties of MnTe6O13, NiTe6O13 and CoTe6O13 are described. These isostructural phases [space group R
(No. 148) with a
≈ 10.2 Å and c
≈ 19 Å] contain a dense network of isolated MO6
(M = Mn, Ni, Co) octahedra, TeO4 folded squares and distorted TeO4+1 square-based pyramids, sharing vertices and edges by way of M–O–Te and Te–O–Te bonds. The TeIV lone pairs are directed into closed cavities formed from 18 Te-centred and 6 MO6 groupings. Magnetic susceptibility data for MnTe6O13 and CoTe6O13 show antiferromagnetic ordering at ca. 13 and 21 K, respectively, which must occur via a superexchange pathway.
Co-reporter:Rachel M. Yeates and William T. A. Harrison
Journal of Materials Chemistry A 2002 vol. 12(Issue 4) pp:1103-1106
Publication Date(Web):21 Feb 2002
DOI:10.1039/B110288E
Synthetic Na3Zn4O(AsO4)3·6H2O is built up from a three-dimensional network of vertex sharing ZnO4 and AsO4 tetrahedra with extra-framework sodium cations and water molecules completing the structure. Dehydration of Na3Zn4O(AsO4)3·6H2O results in a facile, irreversible, framework transformation to hexagonal NaZnAsO4. The title compound is a new member of the M3Zn4O(XO4)3·nH2O (M = univalent cation; X = P or As; n
= 3.5–6) family of open-framework phases. It is isostructural with its phosphate congener but the sodium coordination is subtly different for the two phases. Crystal data: Na3Zn4O(AsO4)3·6H2O, Mr
=
871.31, trigonal, R3c
(No. 161), a
= 10.9493 (5), c
= 26.7099 (13)
Å, V
= 2773.2 (2)
Å3, Z
= 6, R(F)
= 0.021, wR(F2)
= 0.042.
Co-reporter:William T.A. Harrison, Jennifer A. Rodgers, Mark L.F. Phillips, Tina M. Nenoff
Solid State Sciences 2002 Volume 4(Issue 7) pp:969-972
Publication Date(Web):June 2002
DOI:10.1016/S1293-2558(02)01340-7
The synthesis and structure of C2H7N4O·ZnPO4 (guanylurea zinc phosphate) are reported. The cationic [C2H7N4O]+ template was prepared in situ by the slow hydrolysis of the neutral 2-cyanoguanidine starting material. The resulting structure contains an unusual, unprotonated, zincophosphate layer topology as well as NH⋯O template-to-template hydrogen bonds which help to stabilize a “double sandwich” of templating cations between the inorganic sheets. Crystal data: C2H7N4O·ZnPO4, Mr=263.48, monoclinic, , b=5.0716(3), c=10.6005(7) Å, β=95.918(2)°, Z=4, V=729.7(1) Å3, R(F)=0.034, wR(F)=0.034.Graphic
Co-reporter:William T. A. Harrison, Mark L. F. Phillips, Tina M. Nenoff, Elizabeth J. MacLean, Simon J. Teat and Robert S. Maxwell
Dalton Transactions 2001 (Issue 5) pp:546-549
Publication Date(Web):15 Feb 2001
DOI:10.1039/B009641P
[CN3H6]2[Zn(CO3)2], the first organically templated open-framework carbonate has been synthesized hydrothermally and its single crystal structure and some properties have been determined. This phase is built up from a three-dimensional framework of vertex-linked ZnO4 and CO3 building units encapsulating the extra-framework guanidinium cations. Template-to-framework hydrogen bonding appears to play an important role in stabilizing the structure. The zincocarbonate framework shows a surprising similarity to those of known zinc phosphates and phosphites.
Co-reporter:William T. A. Harrison, Mark L. F. Phillips and Tina M. Nenoff
Dalton Transactions 2001 (Issue 17) pp:2459-2461
Publication Date(Web):09 Aug 2001
DOI:10.1039/B102007M
The solution-mediated synthesis and single crystal structure of (CN3H6)2·Zn(HPO3)2 are reported. This phase is built up from a three-dimensional framework of vertex-linked ZnO4 and HPO3 building units encapsulating the extra-framework guanidinium cations. The structure is stabilised by template-to-framework hydrogen bonding. The inorganic framework contains polyhedral 12-rings and shows a surprising similarity to those of some known organically-templated zinc phosphates.
Co-reporter:William T.A Harrison, Mark L.F Phillips, Tina M Nenoff
International Journal of Inorganic Materials 2001 Volume 3(Issue 7) pp:1033-1038
Publication Date(Web):November 2001
DOI:10.1016/S1466-6049(01)00076-9
The hydrothermal synthesis and single crystal structure of (CN4H7)2·Zn3(HPO3)4 are reported. This phase is built up from a network of vertex-linked ZnO4 and HPO3 building units encapsulating the extra-framework animoguanidinium cations. A new type of three-dimensional network for the inorganic component of the structure arises, which contains polyhedral 4-, 6-, 8-, 12- and 16-rings. There are close (∼3.6 Å), side-on, template–template contacts similar to those seen between pairs of guanidinium cations in molecular compounds. Crystal data: (CN4H7)2·Zn3(HPO3)4, Mr=666.30, monoclinic, space group P21/n (No. 14), a=10.2589 (4) Å, b=29.5851 (12) Å, c=13.7578 (5) Å, β=103.303 (1)°, V=4063.6 (5) Å3, Z=8, T=298 (2) K, R(F)=0.0399, wR(F2)=0.0792.
Co-reporter:Jennifer A. Rodgers and William T. A. Harrison
Journal of Materials Chemistry A 2000 vol. 10(Issue 12) pp:2853-2856
Publication Date(Web):08 Nov 2000
DOI:10.1039/B004994H
The solution-mediated synthesis, single crystal structure, and some properties of H3N(CH2)6NH3·Zn4(PO4)2(HPO4)2·3H2O, a novel organically-templated zinc phosphate containing 3-, 4-, 5-, 6- and 20-rings, are described. Vertex-linked ZnO4, PO4, and HPO4 building units self-assemble into a complex three-dimensional network incorporating extra-framework 1,6-diammoniohexane and water molecules. The organic species interacts with the framework by way of N–H⋯O hydrogen bonds. Previously unseen “trimers” of ZnO4 tetrahedra are a feature of the framework.
Co-reporter:Jennifer A. Rodgers and William T. A. Harrison
Chemical Communications 2000 (Issue 23) pp:2385-2386
Publication Date(Web):21 Nov 2000
DOI:10.1039/B007268K
[H2N(CH2)2NH2]
0.5·ZnHPO3 combines the structural features of
templated networks and coordination polymers.
Co-reporter:William T.A. Harrison, Mark L.F. Phillips, Xianhui Bu
Microporous and Mesoporous Materials 2000 Volume 39(1–2) pp:359-365
Publication Date(Web):September 2000
DOI:10.1016/S1387-1811(00)00213-4
The synthesis and crystal structure of caesium zinc arsenate hydrate, Cs3Zn4O(AsO4)3 · 4H2O, are described. This open-framework zincoarsenate, which is built up from a three-dimensional network of vertex-sharing ZnO4 and AsO4 tetrahedra, shows post-dehydration thermal stability to at least 600°C. A model involving merohedral rotational twinning about [0 0 1] was required to arrive at a satisfactory single-crystal structure solution. Crystal data: Cs3Zn4O(AsO4)3 · 4H2O, Mr=1165.05, tetragonal, space group , (no. 81), a=11.3099(2) Å, c=7.9216(2) Å, V=1013.28(4) Å3, Z=2, R(F)=3.90%, Rw(F)=4.81% (740 reflections with I>3σ(I), 81 parameters).
Co-reporter:William T. A. Harrison Dr.;Mark L. F. Phillips Dr.;Jesse Stanchfield;Tina M. Nenoff Dr.
Angewandte Chemie 2000 Volume 112(Issue 21) pp:
Publication Date(Web):27 OCT 2000
DOI:10.1002/1521-3757(20001103)112:21<3966::AID-ANGE3966>3.0.CO;2-M