Combined neutron powder and X-ray single-crystal diffraction refinement of the atomic structure and hydrogen bonding of goslarite (ZnSO4·7H2O)

2005 ◽  
Vol 69 (3) ◽  
pp. 259-271 ◽  
Author(s):  
J. L. Anderson ◽  
R. C. Peterson ◽  
I. P. Swainson
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Atomic Structure ◽  
Data Sets ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
Future Studies ◽  
X Ray ◽  
Hydration And Dehydration ◽  
Phase Relationships

AbstractThe atomic structure of synthetic, deuterated goslarite (ZnSO4·7D2O), a = 11.8176(6) Å, b = 12.0755(7) Å, c = 6.8270(4)Å, space group P212121, Z = 4, has been refined in a combined neutron powder diffraction and X-ray single-crystal data refinement to wRp 1.92%, Rp 1.45% and R(F2) 12.66% for the neutron powder data contribution and R(F2) 8.72% for the X-ray single-crystal data contribution. Both data sets were necessary to achieve the best overall fit agreement in the Rietveld refinement and reasonable geometry within structural units. The results of this study confirm that the H-bonding scheme for goslarite is the same as that of the other epsomite group minerals. Small but significant variations of the Zn–O bond lengths can be attributed to details of the H bonds to the O atoms of the Zn octahedra. This investigation of the atomic structure and hydrogen bonding of goslarite is groundwork for future studies into phase relationships and the mechanisms of hydration and dehydration in the ZnSO4–H2O system.

D'ansite-(Mn), Na21Mn2+(SO4)10Cl3 and d'ansite-(Fe), Na21Fe2+(SO4)10Cl3, two new minerals from volcanic fumaroles

2012 ◽  
Vol 76 (7) ◽  
pp. 2773-2783 ◽  
Author(s):  
F. Demartin ◽  
I. Campostrini ◽  
C. Castellano ◽  
C. M. Gramaccioli ◽  
M. Russo
Keyword(s):  
Single Crystal ◽  
Empirical Formula ◽  
Energy Dispersive Spectrometry ◽  
Chemical Analyses ◽  
Crystal Data ◽  
Unit Cell Parameters ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Fossa Crater

AbstractThe new minerals d'ansite-(Mn), Na21Mn2+(SO4)10Cl3, and d'ansite-(Fe), Na21Fe2+(SO4)10Cl3, occur as encrustations in fumaroles at Vesuvius, Naples, Italy and La Fossa crater, Vulcano, Aeolian Islands, Italy, respectively. Both minerals are cubic and crystallize in space group I3d. D'ansite-(Mn) forms colourless translucent tristetrahedral crystals up to 0.2 mm on edge; d'ansite-(Fe) forms aggregates of colourless to white complex isometric crystals of about the same size. Chemical analyses obtained by energy-dispersive spectrometry on an electron microprobe gave the following mean compositions: d'ansite-(Mn), Na2O 39.37, MnO 3.46, MgO 0.13, SO3 49.99, Cl 6.36, O=Cl–1.44, total 97.87 wt.%, corresponding to an empirical formula, on the basis of 43 anions, of Na20.61 (Mn2+0.79Mg0.05)Σ0.84S10.13O40.09Cl2.91; and d'ansite-(Fe), Na2O 39.12, FeO 4.18, MgO 0.12, SO3 49.91, Cl 6.81, O=Cl –1.54, total 98.60 wt.%, corresponding to an empirical formula of Na20.42(Fe2+0.94Mg0.05)Σ0.99S10.08O39.89Cl3.11. The six strongest reflections in the X-ray powder diffraction pattern of d'ansite-(Fe) [listed as dobs(Å) (I) (hkl)] are as follows: 2.807(100)(044), 2.570(37)(235), 1.714(29)(129), 3.384(27)(233), 3.113(26)(134), 2.108(15)(237). The unit-cell parameters obtained from single-crystal data are 15.9291(9) and 15.882(3) Å for d'ansite-(Mn) and d'ansite-(Fe), respectively. The structure of both minerals was refined, using single-crystal diffraction data, to final R parameters of 0.0309 and 0.0336 on reflections with I > 2σ(I). The structure contains three independent Na sites, one of which is partially occupied by Mn2+ or Fe2+, two independent sulfate anions and one chlorine site.

Structure of Ce2Pt6Ga15: interplanar disorder from the Ce2Ga3 layers

1996 ◽  
Vol 52 (4) ◽  
pp. 580-585 ◽  
Author(s):  
G. H. Kwei ◽  
A. C. Lawson ◽  
A. C. Larson ◽  
B. Morosin ◽  
E. M. Larson ◽  
...  
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Diffraction Data ◽  
Diffuse Scattering ◽  
Heavy Fermion ◽  
Neutron Diffraction Data ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
A Cell

The structure of the heavy fermion compound Ce2Pt6Ga15 has been determined from neutron powder and X-ray/neutron single-crystal diffraction. Examination of symmetry equivalence among the single-crystal data, as well as the good fit of the powder data to the final structural arrangement, with all the atoms on symmetry sites, suggests that the correct space group is P63/mmc. The structure is unusual in that Ce layers have 1/3 of the Ce atoms replaced by groups of three Ga atoms; distances between atoms in these planes suggest this substitution must occur in a concerted fashion. The refined occupancies lead to a stoichiometry near Ce2Pt6Ga15, consistent with such an arrangement. In addition, single-crystal neutron diffraction data show columns of weak diffuse scattering along the <001> axes, suggesting disorder arising from a lack of registration of successive Ce2Ga3 layers (lying half a cell length or 8.27 Å apart along z) and a 3 × 3 × 1 supercell. This disorder is very likely responsible for the low resistance ratio of approximately unity measured for single-crystal samples.

Crystal Structure of 3-Indolepropionic Acid

2013 ◽  
Vol 454 ◽  
pp. 272-275
Author(s):  
Li Hua Wang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Ethanol Solution ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
One Dimensional ◽  
X Ray

The crystals of 3-indolepropionic acid have been obtained by evaporation from ethanol solution. The crystal structure of the 3-indolepropionic acid was determined by X-ray single crystal diffraction analysis. The crystal data for 3-indolepropionic acid: monoclinic, space group P2(1)/c, a = 14.3592(8) Å, b = 5.2446(2) Å, c = 12.3518(6) Å, V = 926.96(8) Å3, Z = 4, Mr = 189.21, De = 1.356 g/cm3, T = 298(2) K, F (000) = 400, R = 0.0435 and wR = 0.1010. The compound forms one-dimensional chained structure through hydrogen bonds and π-π interaction.

scholarly journals Crystal structure of 2-[2-(pyridin-3-yl)diazen-1-yl]aniline

2018 ◽  
Vol 74 (7) ◽  
pp. 1013-1016
Author(s):  
Morten K. Peters ◽  
Christian Näther ◽  
Rainer Herges
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Crystalline Phase ◽  
Title Compound ◽  
Molecular Packing ◽  
Crystal Data ◽  
X Ray ◽  
Compound C

The crystal structure of the title compound, C11H10N4, comprises molecules in a trans conformation for which all the atoms are located in general positions. The six-membered rings are coplanar and this arrangement might be stabilized by intramolecular N—H...N hydrogen bonding. In the crystal, the molecules are linked into helical chains parallel to the b axis via N—H...N hydrogen bonding. The molecular packing shows a herringbone-like pattern along the a axis. Comparison of the X-ray powder diffraction with that calculated from single crystal data proves that a pure crystalline phase was obtained and UV–Vis measurements reveal that only the trans isomer is present.

scholarly journals Combined X-ray and neutron single-crystal diffraction in diamond anvil cells

2020 ◽  
Vol 53 (1) ◽  
pp. 9-14 ◽  
Author(s):  
Andrzej Grzechnik ◽  
Martin Meven ◽  
Carsten Paulmann ◽  
Karen Friese
Keyword(s):  
High Pressure ◽  
Data Processing ◽  
Single Crystal ◽  
Diamond Anvil Cell ◽  
Crystal Data ◽  
Structural Refinement ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Diamond Anvil ◽  
First Time

It is shown that it is possible to perform combined X-ray and neutron single-crystal studies in the same diamond anvil cell (DAC). A modified Merrill–Bassett DAC equipped with an inflatable membrane filled with He gas has been developed. It can be used on laboratory X-ray and synchrotron diffractometers as well as on neutron instruments. The data processing procedures and a joint structural refinement of the high-pressure synchrotron and neutron single-crystal data are presented and discussed for the first time.

Structure characterization with neutron powder data of LaGaO3 and NdGaO3 based on X-ray single-crystal data: evidence for an inversion center

1996 ◽  
Vol 211 (12) ◽  
Author(s):  
W. Marti ◽  
P. Fischer ◽  
J. Schefer ◽  
F. Kubel
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Structure Characterization ◽  
Inversion Center ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
X Ray

AbstractFrom neutron powder diffraction intensities it is often problematic to distinguish between centrosymmetry and non-centrosymmetry. X-ray single crystal diffraction may be more accurate. In this paper we compare refinement results of crystal structures on the basis of neutron powder data of orthorhombic NdGaO

Crystal structures of dihydroquercetin 3-acetate and dihydroquercetin 3,3'4',7-tetraacetate: hydrogen bonding in 5-hydroxyflavanones

1999 ◽  
Vol 77 (8) ◽  
pp. 1436-1443 ◽  
Author(s):  
Eberhard Kiehlmann ◽  
Kumar Biradha ◽  
Konstantin V Domasevitch ◽  
Michael J Zaworotko
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Crystal Packing ◽  
Heterocyclic Ring ◽  
Molecular Structures ◽  
Crystal Data ◽  
Aromatic Rings ◽  
X Ray

The molecular structures of dihydroquercetin 3-acetate 3 and dihydroquercetin 3,3',4',7-tetraacetate 4 were determined by single crystal X-ray analysis. Comparison of their crystal data with those of 16 known 5-hydroxyflavanones shows intramolecular O(5)-H···O(4)=C hydrogen bonding, preference for nearly perpendicular orientation of the two aromatic rings and preferred sofa conformation of the heterocyclic ring. The major stabilizing force in the crystal packing pattern of 3 is intermolecular hydrogen bonding.Key words: crystal structure, dihydroquercetin, flavanones, hydrogen bonding.

Hydrogen bonding in hydroxypyridium salts

2018 ◽  
Vol 233 (7) ◽  
pp. 501-506
Author(s):  
Andrei V. Mironov ◽  
Victor A. Tafeenko ◽  
Dmitrii Yu. Grebenkin ◽  
Alexander E. Oblezov
Keyword(s):  
Hydrogen Bonding ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Nitrate Anion ◽  
Single Crystal Diffraction ◽  
Space Group ◽  
X Ray ◽  
Unit Cells

Abstract The crystal structures of 6-methyl-2-ethyl-3-hydroxypyridiniun nitrate (C8H12NO)NO3 (I) and fumarate (C8H12NO)2C4H2O4 (II) were solved and refined from X-ray single crystal diffraction data (CuKα, (I) a=4.6477(2), b=14.5906(9), c=14.5551(8) Å, β=99.100(4)°, space group P21/c, Z=4, Rp/Rwp=0.033/0.047; (II) a=8.8293(3), b=13.4268(5), c=8.3893(3) Å, β=96.303(3)°, space group P21/c, Z=2, Rp/Rwp= 0.034/0.049). Both structures are built of infinite chains along ac diagonal of the unit cells formed by hydrogen bonding between the hydroxypyridium cation and the corresponding anion. Each fumarate anion is linked to four hydroxypyridium cations while nitrate anion is connected with two hydroxypyridium cations only leaving one oxygen atom in the nitrogen group isolated.

scholarly journals Accurate molecular structures and hydrogen bonding in two polymorphs of ortho-acetamidobenzamide by single-crystal neutron diffraction

2006 ◽  
Vol 62 (5) ◽  
pp. 926-930 ◽  
Author(s):  
Charlotte K. Leech ◽  
Sarah A. Barnett ◽  
Kenneth Shankland ◽  
Matthias Gutmann ◽  
Chick C. Wilson
Keyword(s):  
Hydrogen Bonding ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Molecular Structures ◽  
Full Description ◽  
Single Crystal Diffraction ◽  
Comprehensive Description ◽  
Torsion Angles ◽  
X Ray ◽  
Bonding Scheme

The structures of both known forms of the polymorphic material ortho-acetamidobenzamide, C9H10N2O2, have been determined by low-temperature neutron single-crystal diffraction. Neutron diffraction allows the full description of the H-atom positions in this molecular material, which is vital in benchmarking related crystal-structure predictions. Significant conformational differences are indicated by a number of the torsion angles involving H atoms when compared with previous X-ray studies. A comprehensive description of the hydrogen-bonding scheme in both polymorphs is given.

Synthesis and Crystal Structure of 1-(2R,3S,4R,5R)-3-fluoro-4-hydroxy-5-(hydroxymethyl)tetrahydrofuran-2-yl)-5-iodopyrimidine-2,4(1H,3H)-dione

2014 ◽  
Vol 997 ◽  
pp. 196-199
Author(s):  
Wei Li ◽  
Qiang Xiao ◽  
Ru Chun Yang
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Nmr Spectra ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

The title compound, 1-(2R,3S,4R,5R)-3-fluoro-4-hydroxy-5-(hydroxymethyl) tetrahydrofuran-2-yl)-5-iodopyrimidine-2,4(1H,3H)-dione , C9H10FIN2O5, as potential drugs for anti-tumor, anti-viral have been synthesized and characterized by NMR spectra. Meanwhile, the crystal of 2b was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P2(1),a= 9.0832(11) Ǻ,b= 5.4332(7) Ǻ,c= 12.2464(15) Ǻ,β= 107.809(4)°,V= 575.41(12) Ǻ3,Z= 2,F(000) = 360,Dx= 2.148 Mg m-3,μ= 2.813 mm-1,R= 0.014 andwR= 0.056 for 1988 independent reflections (Rint= 0.0209) and 1932 observed ones (I > 2σ (I)).

Sign in / Sign up

Export Citation Format

Share Document