The crystal structure of tedhadleyite, Hg2+Hg101+O4l2(Cl,Br)2, from the Clear Creek Claim, San Benito County, California

2009 ◽  
Vol 73 (2) ◽  
pp. 227-234 ◽  
Author(s):  
M. A. Cooper ◽  
F. C. Hawthorne
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
The Other ◽  
Covalent Bonds ◽  
Pass Through

AbstractThe crystal structure of tedhadleyite, ideally Hg2+Hg101+O4l2(Cl,Br)2,triclinic, AĪ, a 7.0147(5), b 11.8508(7), c 12.5985(8) Å, α 115.583(5), β 82.575(2), γ 100.619(2)º, V 927.0(2) Å3, Z = 2,was solved by direct methods and refined to an R1 index of 4.5% for 2677 unique reflections. There are six symmetrically distinct Hg sites in tedhadleyite: Hg(1) is occupied by Hg2+ and Hg(2–6) are occupied by Hg+ that forms three [Hg–Hg]2+ dimers with Hg–Hg separations between 2.527 and 2.556 Å. These [Hg–Hg]2+ dimers have strong covalent bonds to O atoms,forming pseudo-linear O–Hg–Hg–O arrangements,and weak bonds to halogen and O atoms at high angles to the dimer axis. The [O–Hg–Hg-O] groups share anions to form four-membered square rings of composition [Hg8O4] that link along [100] via [O–Hg–Hg-O] groups and along [001] via [O–Hg–O] groups, forming rectangular rings of composition [Hg14O8]. The rings form a corrugated layer that interweaves with a symmetrically related layer whereby the [O–Hg(6)–Hg(6)–O] linking groups of one layer pass through the centres of the square [Hg8O4] rings of the other layer to form [Hg11O4] complex slabs parallel to (010) that link through Hg-I and Hg-Br,Cl bonds.

The crystal structure and chemistry of mereheadite

2009 ◽  
Vol 73 (1) ◽  
pp. 103-117 ◽  
Author(s):  
S. V. Krivovichev ◽  
R. Turner ◽  
M. RumseY ◽  
O. I. Siidra ◽  
C. A. Kirk
Keyword(s):  
Crystal Structure ◽  
Lead Oxide ◽  
Direct Methods ◽  
Structural Formula ◽  
The Other ◽  
Naturally Occurring ◽  
Pb Ions ◽  
Oriented Parallel ◽  
Crystal Structure And Chemistry ◽  
The Ideal

The crystal structure of mereheadite (monoclinic, Cm, a = 17.372(1), b = 27.9419(19), c = 10.6661(6) Å, β = 93.152(5)°, V = 5169.6(5) Å3) has been solved by direct methods and refined to R1 = 0.058 for 6279 unique observed reflections. The structure consists of alternating Pb–O/OH blocks and Pb–Cl sheets oriented parallel toth e (201) plane and belongs toth e 1:1 type of lead oxide halides with PbO blocks. It contains 30 symmetrically independent Pb positions, 28 of which belong to the PbO blocks, whilst two positions (Pb12 and Pb16) are located within the tetragonal sheets of the Cl– anions. Mereheadite is thus the first naturally occurring lead oxychloride mineral with inter-layer Pb ions. The coordination configurations of the Pb atoms of the PbO blocks are distorted versions of the square antiprism. In one half of the coordination hemisphere, they are coordinated by hard O2– and OH– anions whose number varies from three to four, whereas the other coordination hemisphere invariably consists of four soft Cl– anions located at the vertices of a distorted square. The Pb12 and Pb16 atoms in between the PbO blocks have an almost planar square coordination of four Cl– anions. These PbCl4 squares are complemented by triangular TO3 groups (T = B, C) so that a sevenfold coordination is achieved. The Pb–O/OH block in mereheadite can be obtained from the ideal PbO block by the following list of procedures: (1) removal of some PbO4 groups that results in the formation of square-shaped vacancies; (2) insertion of TO3 groups into these vacancies; (3) removal of some Pb atoms (that correspond to the Pb1A and Pb2A sites), thus transforming coordination of associated O sites from tetrahedral OPb4 tot riangular OHPb3; and (4) replacement of two O2– anions by one OH– anion with twofold coordination; this results in formation of the 1×2 elongated rectangular vacancy. The structural formula that can be derived on the basis of the results of single-crystal structure determination is Pb47O24(OH)13Cl25(BO3)2(CO3). Welch et al. (1998) proposed the formula Pb2O(OH)Cl for mereheadite, which assumes that neither borate nor carbonate is an essential constituent of mereheadite and their presence in the mineral is due to disordered replacements of Cl– anions. However, our study demonstrates that this is not the case, as BO3 and CO3 groups have well-defined structural positions confined in the vacancies of the Pb–O/OH blocks and are therefore essential constituents. Our results also show that mereheadite is not a polymorph of blixite, but is in fact related to symesite. Symesite thus becomes the baseline member of a group of structurallyrelated minerals.

Crystal and molecular structure of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]octane

1976 ◽  
Vol 54 (20) ◽  
pp. 3142-3151 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
H. Becker
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Boron Atom ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
The Other ◽  
Full Matrix ◽  
Atom Bond ◽  
Tetrahedral Boron

Crystals of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]-octane are monoclinic, a = 22.323(1), b = 9.555(1), c = 16.0027(6) Å, β = 109.055(4)°, Z = 8, space group C2/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.048 and Rw of 0.066 for 2629 reflections with I ≥ 3σ(I). The central part of the molecule consists of two fused five-membered rings. One of them is a familiar BOCCN ring while the other is a novel and nearly planar BOBON ring containing one tetrahedral boron atom and one trigonal planar boron atom. Bond lengths are: O—B, 1.337(2)–1.467(2), N—B, 1.692(2), O—N, 1.440(2), O—C, 1.426(2), N—C, 1.513(2), B—C, 1.557(2) and 1.599(2), C(sp3)—C(sp3), 1.520(2)–1.530(2), C—C(ar), 1.372(4)–1.407(2), N—H, 0.89(2), mean C(ar)—H, 0.97(1), and mean C(sp3)—H, 1.01(1) Å. The crystal structure consists of discrete molecules each linked to two others by N—H … O hydrogen bonds (N … O = 2.853(2) Å).

Advances in theEXPO2009systematic decomposition procedure: an atom-matching-based figure of merit

2011 ◽  
Vol 44 (3) ◽  
pp. 448-453 ◽  
Author(s):  
Angela Altomare ◽  
Corrado Cuocci ◽  
Carmelo Giacovazzo ◽  
Anna Moliterni ◽  
Rosanna Rizzi
Keyword(s):  
Crystal Structure ◽  
Figure Of Merit ◽  
Bragg Reflection ◽  
Direct Methods ◽  
The Other ◽  
Correct Solution ◽  
Powder Diffraction Data ◽  
Decomposition Procedure ◽  
Integrated Intensities

Ab initiocrystal structure determination from powder diffraction data is not yet a straightforward process: it is strongly disrupted by the low quality of the estimated Bragg reflection intensities. In a two-stage method the integrated intensities calculated from a powder pattern are immediately submitted to direct methods to obtain phases. The larger the accuracy of the integrated intensities, the more efficient the phasing process. A systematic decomposition procedure was introduced in theEXPO2004program to improve the efficiency of the phasing process. The disadvantage of this approach is that a large number of feasible trial structures are generated, among which the correct solution must be recognized. A new procedure is described aiming at introducing strategies to reduce the total number of trials to explore by defining an appropriate figure of merit able to regroup trial structures into different batches, each element of a batch sharing a high percentage of atoms with the other elements of the same batch. The new figure of merit, implemented in an updated version ofEXPO2009, is able to discriminate non-solutions from promising trials, corresponding to incomplete or rough models which evolve, after refinement, into the correct solution.

scholarly journals Crystal Structure of Triclinic Colchiceine Hemihydrate

1985 ◽  
Vol 38 (3) ◽  
pp. 413 ◽  
Author(s):  
Maureen F Mackay ◽  
James D Morrison ◽  
Jacqueline M Gulbis
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
The Other ◽  
Water Molecules ◽  
Space Group

Triclinic crystals of colchiceine hemihydrate, C21H23N06.!H20, belong to the space group PI with a 8 .211(1), b 8�361(1), c16 �898(2) A, a 92 �35(1)", J3 93 �93(1)", l' 121�35(1)" and Z 2. The structure was solved by direct methods and successive difference syntheses with diffractometer data measured with CuKa radiation. Refinement converged at R 0�053 for 2798 observed reflections. The two tautomers, one of the isoco1chiceine and the other of the colchiceine form, exist as independent entities in the crystal; the angles between the normals to the plane of the benzene and troponoid rings are 44�5(4)" and 51� 5(5)" respectively. The hydroxyl and N-acetyl groups are oriented to form channels along the a-axis which accommodate the water molecules.

The preparation and crystal structure of pentaiodinium hexafluoroantimonate(V) containing I153+

1979 ◽  
Vol 57 (9) ◽  
pp. 968-973 ◽  
Author(s):  
Jack Passmore ◽  
Peter Taylor ◽  
Tom Whidden ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Multiple Solution ◽  
The Other ◽  
Full Matrix ◽  
Space Group ◽  
Bond Angles

Crystalline pentaiodinium hexafluoroantimonate was prepared by the reaction of I2 and SbF5 in AsF3. The crystals were triclinic, a = 8.295(4) Å, b = 15.61(1) Å, c = 8.390(4) Å, α = 81.49(4)°, β = 110.02(4)°, γ = 85.06(4)°, Z = 3, space group [Formula: see text]. The structure was solved by multiple-solution direct methods and Fourier syntheses and refined by full-matrix and blocked-matrix least-squares procedures to a final R of 0.062 and Rw of 0.090 for 2229 reflections with I ≥ 3σ(I). The two crystallographically independent planar, bent I5+ chains (one centrosymmetric, the other essentially centrosymmetric), each have two collinear central bonds of 2.899(2) Å (× 2); 2.896(2), and 2.920(2) Å, bond angles 180° and 178.7(6)°, respectively, and two shorter terminal bonds of 2.680(3) Å (× 2); 2.666(3) and 2.698(2) Å, with bond angles between central and terminal bonds of 94.53(6)° (× 2); 93.86(7) and 93.17(7)°, respectively. Three I5+ units are joined by a weak (3.416(3) Å) interaction to form what may be regarded as an I153+ unit. The SbF6− anions are approximately octahedral.

Ag13I4(AsO4)3: Synthesis, Crystal Structure and Ionic Conductivity

2009 ◽  
Vol 64 (8) ◽  
pp. 891-895 ◽  
Author(s):  
Dragan Pitzschke ◽  
Jan Curda ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
The Other ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
Stoichiometric Mixture ◽  
Single Crystal Diffraction ◽  
Ion Conductor ◽  
Partial Structures ◽  
First Time

Ruby-red single crystals of Ag13I4(AsO4)3 were prepared for the first time by reacting a stoichiometric mixture of Ag2O, AgI and As2O3 at elevated oxygen pressure of 120 MPa and at a temperature of 350 ◦C. The polyhedral crystals belong to the monoclinic space group P21/m with a = 9.247(1), b = 7.152(1), c = 17.674(2) Å , β = 91.492(2)◦, and Z = 2. The structure is fully ordered and was solved by Direct Methods, and refined on single crystal diffraction data (10376 observed reflections, R1 = 3.28 %). The crystal structure is built up of two two-dimensional interlocked partial structures, one consisting of silver and iodine ions, the other of silver and arsenate(V) ions. The slabs extend in the ac plane, and the Ag-I framework is linked to the AsO43− units by Ag-O contacts. The silver-oxygen interactions perturb the tetrahedron of the arsenate group, resulting in As-O distances ranging from 1.670 to 1.697 Å, and angles varying from 107.3 to 112.1◦. Pure Ag13I4(AsO4)3 is a solid ion conductor with a r. t. conductivity of 6.4×10−6 Ω−1 cm−1 at 30 ◦C. The activation energy for silver ion conduction is 0.41 eV in the temperature range from 30 to 130 ◦C

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

PHASE TRANSITION IN LAYERED PEROVSKITE LIKE MANGANATE Ca3Mn2O7 UNDER HIGH PRESSURE

2001 ◽  
Vol 15 (18) ◽  
pp. 2491-2497 ◽  
Author(s):  
J. L. ZHU ◽  
L. C. CHEN ◽  
R. C. YU ◽  
F. Y. LI ◽  
J. LIU ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Diamond Anvil Cell ◽  
The Other ◽  
Layered Perovskite ◽  
X Ray Diffraction ◽  
Two Phase ◽  
X Ray ◽  
Diamond Anvil

In situ high pressure energy dispersive X-ray diffraction measurements on layered perovskite-like manganate Ca 3 Mn 2 O 7 under pressures up to 35 GPa have been performed by using diamond anvil cell with synchrotron radiation. The results show that the structure of layered perovskite-like manganate Ca 3 Mn 2 O 7 is unstable under pressure due to the easy compression of NaCl-type blocks. The structure of Ca 3 Mn 2 O 7 underwent two phase transitions under pressures in the range of 0~35 GPa. One was at about 1.3 GPa with the crystal structure changing from tetragonal to orthorhombic. The other was at about 9.5 GPa with the crystal structure changing from orthorhombic back to another tetragonal.

A new three-dimensional anionic cadmium(II) dicyanamide network

2014 ◽  
Vol 70 (11) ◽  
pp. 1054-1056 ◽  
Author(s):  
Qiang Li ◽  
Hui-Ting Wang
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Unit Cell Volume ◽  
Three Dimensional ◽  
Building Blocks ◽  
The Other ◽  
Dimensional Structure ◽  
Cadmium Nitrate ◽  
Nitrate Tetrahydrate ◽  
Anionic Framework

A new cadmium dicyanamide complex, poly[tetramethylphosphonium [μ-chlorido-di-μ-dicyanamido-κ4N1:N5-cadmium(II)]], [(CH3)4P][Cd(NCNCN)2Cl], was synthesized by the reaction of tetramethylphosphonium chloride, cadmium nitrate tetrahydrate and sodium dicyanamide in aqueous solution. In the crystal structure, each CdIIatom is octahedrally coordinated by four terminal N atoms from four anionic dicyanamide (dca) ligands and by two chloride ligands. The dicyanamide ligands play two different roles in the building up of the structure; one role results in the formation of [Cd(dca)Cl]2building blocks, while the other links the building blocks into a three-dimensional structure. The anionic framework exhibits a solvent-accessible void of 673.8 Å3, amounting to 47.44% of the total unit-cell volume. The cavities in the network are occupied by pairs of tetramethylphosphonium cations.

scholarly journals The crystal structure of szenicsite, Cu3MoO4(OH)4

1998 ◽  
Vol 62 (04) ◽  
pp. 461-469 ◽  
Author(s):  
Peter C. Burns
Keyword(s):  
Crystal Structure ◽  
Goodness Of Fit ◽  
Direct Methods ◽  
Ligand Field ◽  
Area Detector ◽  
Vertex Sharing ◽  
Distorted Octahedral ◽  
Jahn Teller ◽  
Jahn Teller Effect ◽  
Least Squares Techniques

Abstract The crystal structure of szenicsite, Cu3MoO4(OH)4, orthorhombic, a = 8.5201(8), b = 12.545(1), c = 6.0794(6) Å, V = 649.8(2) Å3, space group Pnnm, Z = 4, has been solved by direct methods and refined by least-squares techniques to an agreement index (R) of 3.34% and a goodness-of-fit (S) of 1.11 for 686 unique observed [|F| ⩾ 4σF] reflections collected using graphite-monochromated Mo-Kα X-radiation and a CCD area detector. The structure contains three unique Cu2+ positions that are each coordinated by six anions in distorted octahedral arrangements; the distortions of the octahedra are due to the Jahn-Teller effect associated with a d 9 metal in an octahedral ligand-field. The single unique Mo6+ position is tetrahedrally coordinated by four O2− anions. The Cu2+ϕ6 (ϕ: unspecified ligand) octahedra share trans edges to form rutile-like chains, three of which join by the sharing of octahedral edges to form triple chains that are parallel to [001]. The MoO4 tetrahedra are linked to either side of the triple chain of Cu2+ϕ6 octahedra by the sharing of two vertices per tetrahedron, and the resulting chains are cross-linked through tetrahedral-octahedral vertex sharing to form a framework structure. The structure of szenicsite is closely related to that of antlerite, Cu3SO4(OH)4, which contains similar triple chains of edge-sharing Cu2+ϕ6 octahedra.

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