Ivashkevich, LS Lyakhov, AS Selevich, AE
Ilieva, D Lesnikovich, AL
The crystal structure Of Y2P4O13 from X-ray powder diffraction data
ZEITSCHRIFT FUR KRISTALLOGRAPHIE, 217, 2002, 605-608.
The crystal structure Of Y2P4O13 has been determined. from X-ray powder
diffraction data. Y2P4O13 crystallizes in the orthorhombic
space group
C222(1) (No. 20) with a = 17.2817(7) Angstrom, b = 6.9823(4)
Angstrom,
c = 8.5391(3) Angstrom, V = 1030.38(8) Angstrom(3), and
Z = 4. The
structure has been solved by direct methods using EXPO
program and
refined by FULLPROF package. The final R-Bragg value was
9.1%. The
tetraphosphate anion has the point group 2 symmetry. The
yttrium atom
is seven-coordinated forming strongly distorted octahedron
with one
bifurcated vertex. There are infinite chains of oxygen-bridged
ittrium
atoms miming parallel to the b axis and linked together
by the
tetraphosphate anions with formation of three-dimensional
network.
TREOR
2002-2
Filaretov, AA Zhizhin, MG Olenev, AV
Gurkin, AA Bobylev, AP
Lazoryak, BI Danilov, VP Komissarova,
LN
Hydrothermal synthesis, structures, and properties: Indium hydrogen
phosphates (MIn)-In-I(HPO4)(2) (M-I = K, Rb, and NH4)
RUSSIAN JOURNAL OF INORGANIC CHEMISTRY 47, 2002, 1773-1789.
Mixed hydrogen phosphates KIn(HPO4)(2) (I), beta(2)-RbIn(HPO4)(2) (II),
and (NH4)In(HPO4)(2) (III) were prepared in the In2O3-MH2PO4-H3PO4-HF,
In2O3-M2CO3-H3PO4-HF (where M = K or Rb), and In2O3(NH4)Cl-H3PO4
systems under hydrothermal conditions (200degreesC, 20
atm, 96 h). The
phosphates were characterized by IR and Raman spectroscopy,
thermal
analysis, and electron probe microanalysis. The structure
of compound
II was established by single-crystal X-ray diffraction
analysis. The
crystal structures of compounds I and III were determined
by the
Rietveld method. All compounds crystallized in the monoclinic
system
(space group P2(1)/c, Z= 4); a = 9.6232(1) Angstrom, b
= 8.2573(1)
Angstrom, c = 9.4571(1) Angstrom, beta = 115.72(1)degrees,
R-p =
0.0465, R-wp = 0.0619 for I; a = 9.705(2) Angstrom, b
= 8.367(2)
Angstrom, c = 9.528(2) Angstrom, beta = 116.60(3)degrees,
R-1 = 0.0503,
wR(2) = 0.1464 for II; a = 9.6651(1) Angstrom, b = 8.2763(1)
Angstrom,
c = 9.5964(1) Angstrom, beta = 116.146(1)degrees, R-p
= 0.0380, R-wp =
0.0553 for III. The structures of indium hydrogen phosphates
can be
described as a mixed framework {In[HPO4](2)}(3infinity)(-)
of octahedra
and tetrahedra. Large cavities in the framework are occupied
by
monovalent cations. Second-harmonic-generation measurements
demonstrated that the crystal structures of compounds
I-III have a
center of symmetry.
TREOR
2002-3
Zhang, QA Nakamura, Y Oikawa, K
Kamiyama, T Akiba, E
New alkaline earth aluminum hydride with one-dimensional zigzag chains
of [AlH6]: Synthesis and crystal structure of BaAlH5
INORGANIC CHEMISTRY 41, 2002, 6941-6943.
The title hydride and its deuteride were successfully synthesized.
The
crystal structure of the deuteride was determined by time-of-flight
neutron powder diffraction. BaAlD5 crystallizes with a
new orthorhombic
structure in space group Pna2(1) (No. 33), cell parameters
a = 9.194(1)
Angstrom, b = 7.0403(9) Angstrom, and c = 5.1061(6) Angstrom,
Z = 4.
BaAlH5 is the first example that contains one-dimensional
zigzag chains
of [AlH6] along the crystallographic c axis.
TREOR
2002-4
Cunin, F Deudon, C Favier, F Mula,
B Pascal, JL
First anhydrous gold perchlorato complex: ClO2Au(CIO4)(4). Synthesis
and molecular and crystal structure analysis
INORGANIC CHEMISTRY 41, 2002, 4173-4178.
Chlorine trioxide, Cl2O6, reacts with Au metal, AuCl3, or HAuCl4.nH(2)O
to yield the well-defined chloryl salt, ClO2.Au(ClO4)(4).
The crystal
and molecular structure of ClO2Au(CIO4)(4) was solved
by a Rietveld
analysis of powder X-ray diffraction data. The salt crystallizes
in a
monoclinic cell, space group C2/c, with cell parameters
a = 15.074(5),
b = 5.2944(2), and c = 22.2020(2) Angstrom and beta =
128.325(2). The
structure displays discrete ClO2+ ions lying in channels
formed by
Au(CIO4)(4)(-) stacks. Au is located in a distorted square
planar
environment: Au-O = 1.87 and 2.06 Angstrom. [ClO4] groups
are
monodentate with ClOb = 1.53 and ClOt = 1.39 Angstrom
(mean distances;
O-b, oxygen bonded to Au; O-t, free terminal oxygen).
A full
vibrational study of the Au(ClO4)(4)(-) anion is supported
by DFT
calculations.
TREOR
2002-5
Filaretov, AA Zhizhin, MG Komissarova, LN
Danilov, VP Chernyshev, VV Lazoryak, BI
Synthesis and structure of the new ammonium indium phosphate
(NH4)In(OH)PO4
JOURNAL OF SOLID STATE CHEMISTRY 166, 2002, 362-368.
A new ammonium indium phosphate (NH4)In(OH)PO4 was prepared by
hydrothermal reaction in the In2O3-NH4H2PO4-NH3/OH system
(T =
200degreesC, autogenous pressure, 7 days). The formula
(NH4)In(OH)PO4
was determined on the basis of chemical and thermal analysis
(TG/DSC),
X-ray powder diffraction and IR-spectroscopy. (NH4)In(OH)PO4
crystallizes in the tetragonal system with space group
P4(3)2(1)2 (No.
96), a - 9.4232(1) Angstrom, 11. 1 766(1) Angstrom, V
= 992.45(2)
Angstrom(3); Z= 8. The crystal structure was refined by
the Rietveld
method (R-w = 6.35%, R-p = 5.10%). The second-harmonic
generation study
confirmed that structure of (NH4)In(OH)PO4 does not have
a center of
symmetry. The cis-InO4(OH)(2) octahedra form helical chains,
parallel
to the c-axis. The In-O-In bonds are nearly equidistant.
The chains are
interconnected by phosphate tetrahedra and create tunnels
containing
the NH4+ ions along the c-axis. (NH4)In(OH)PO4 is isostructural
with
RbIn(OH)PO4.
TREOR
2002-6
Kubota, Y Honda, T Plevert, J Yamashita,
T Okubo, T Sugi, Y
Synthesis of a new molecular sieve using DABCO-based
structure-directing agent
CATALYSIS TODAY 74, 2002, 271-279.
A new 1,4-diazabicyclo[2.2.2]octane (DABCO)-based quaternary ammonium
compound is designed, synthesized, and used as structure-directing
agent (SDA) for molecular sieve synthesis. Several
1,1'-alkylenedi(4-aza-1-azonia-2,5-dimethyl-bicyclo [2.2.2]
octane)
type SDAs are used in all-silica synthesis mixtures. Among
the SDAs
tested, the use of 1, 1'-butylenedi-(4-aza-1-azonia-2,5
5-dimethylbicyclo[2.2.2]octane) gives a new phase (GUS-1),
whereas the
use of other SDAs gives zeolite beta ((*)BEA), ZSM-12
(MTW), and ZSM-5
(MR). The GUS-1 is indexed in the orthorhombic crystal
class with
refined lattice constants a = 16.4206(4) Angstrom, b =
20.0540(4)
Angstrom and c = 5.0464(1) Angstrom. The crystalline architecture
of
GUS-1 shows the same [001] projection of the framework
as that of
mordenite (MOR), and is characterized by a one-dimensional
12-membered
ring channel system that is closely related to the channels
of ZSM-12.
The GUS-1 is stable to heat upon calcination at 700 degreesC
in air.
The calcined material exhibits adsorption capacity that
is comparable
to typical large-pore one-dimensional microporous silicates.
The
behavior of the SDA during synthesis is also discussed.
TREOR
2002-7
Jensen, TR Hazell, RG Christensen, AN
Hanson, JC
Hydrothermal synthesis of lithium zinc phosphates: Structural
investigation of twinned alpha-Li4Zn(PO4)(2) and a high
temperature
polymorph beta-Li4Zn(PO4)(2)
JOURNAL OF SOLID STATE CHEMISTRY 166, 2002, 341-351.
The system LiOH:Zn(NO3)(2):H3PO4:H2O was investigated using
hydrothermal synthesis techniques in the temperature range
20degreesC <
T < 602degreesC and pressure range, 1 < p < 2.8
kbar, and the
crystallization fields of some lithium zinc orthophosphates
are
reported. Small crystals of a twinned lithium zinc phosphate,
alpha-Li(4)ZH(PO4)(2) were prepared and a structural investigation
was
performed using synchrotron X-ray diffraction: monoclinic,
space group
P2(1) /a, a = 8.096(2) Angstrom, b = 10.242(2) Angstrom,
c = 8.106(2)
Angstrom, beta = 104.73(3)degrees, V = 650.1(2) Angstrom(3)
and Z = 4.
The refinement gave R(F) = 0.042 and wR(F-2) = 0.068 based
on 968
independent reflections and 616 observed, F-o(2) > 3sigma(F-o(2))
(lambda = 0.9346(1) Angstrom). The cations are tetrahedrally
coordinated to oxygen, and the structure can be viewed
as layers of
regular ZnO4 and PO4 tetrahedra interconnected by more
distorted LiO4
tetrahedra. Thermal investigation using in situ powder
X-ray
diffraction in the temperature range 20degreesC < T
< 900degreesC was
performed. The reversible phase transition alpha --> Li4Zn(PO4)(2)
was
observed in agreement with previous investigations. A
powder pattern
measured at T = 900degreesC was indexed with a triclinic
unit cell:
space group, P (1) over bar, a = 5.173(3) Angstrom, b
= 7.97(1)
Angstrom, c = 9.92(1) Angstrom, alpha = 80.9(1)degrees,
beta =
126.8(1)degrees and gamma = 106.0(1)degrees, V = 319.8(7)
Angstrom(3)
and Z = 2. The linear thermal expansion of alpha- and
beta-Li4Zn(PO4)(2) are extracted from powder diffraction
data in the
temperature range RT to 900degreesC.
2002-8
Zhang, QA Nakamura, Y Oikawa, K
Kamiyama, T Akiba, E
Synthesis and crystal structure of Sr2AlH7: A new structural type of
alkaline earth aluminum hydride
INORGANIC CHEMISTRY 41, 2002, 6547-6549.
The title hydride and its deuteride were successfully synthesized.
The
heavy atom structure and hydrogen positions were determined
respectively by X-ray Powder diffraction and time-of-flight
neutron
powder diffraction, They crystallize with a new monoclinic
structure in
space group I2 (No. 5); cell parameters: a = 12.575(1)
Angstrom, b =
9.799(1) Angstrom, c = 7.9911(8) Angstrom, beta = 100,270(4)degrees
(hydride), a = 12.552(1) Angstrom, b = 9.7826(8) Angstrom,
c =
7.9816(7) Angstrom, beta = 100.286(4)degrees (deuteride),
Z = 8.
Sr2AlH7 is the first example that consists of isolated
[AlH6] units and
infinite one-dimensional twisted chains of edge-sharing
[HSr4]
tetrethedra along the crystallographic c axis.
2002-9
Kongshaug, KO Fjellvag, H
Coordination polymers constructed from paddle-wheel building units
JOURNAL OF SOLID STATE CHEMISTRY 166, 2002, 213-218.
The two structurally related coordination polymers [Cu(ndc)
(pyridine)], CPO-2-Cu, and [Zn(ndc)(3,4-lutidine)], CPO-2-Zn,
were
obtained by hydrothermal reactions between 2,6-naphthalenedicarboxylic
acid (ndc), pyridine and copper(II) nitrate (CPO-2-Cu)
and ndc,
3,4-lutidine and zinc(II) nitrate (CPO-2-Zn), respectively.
The
compounds are based on the binuclear paddle-wheel building
unit. In
both compounds these building units are connected into
2D sheets by
naphthalene rings. In the third dimension there are weaker
interactions
involving the axial ligands pyridine and 3,4-lutidine.
The sheets are
stacked so that large ID channels are formed into which
the axial
ligands protrude. The crystal structure of CPO-2-Cu was
solved from
synchrotron powder X-ray data, while the crystal structure
of CPO-2-Zn
was solved from conventional single-crystal X-ray data.
Crystal data
for CPO-2-Cu: Monoclinic space group C2/m (No. 12), a
= 10.2252(2), b =
19.0915(4), c = 8.0521(2)Angstrom, beta = 98.824(1)degrees,
V =
1553.30(7) Angstrom(3) and Z = 4. Crystal data for CPO-2-Zn:
Triclinic
space group P - 1 (No. 2), a = 7.540(1), b = 10.711(1),
c = 11.196(2)
Angstrom, alpha - 66.490(5)degrees, beta = 87.265(6)degrees,
chi =
88.470(6)degrees, V = 828.2(2)Angstrom(3) and Z = 2. The
thermal
properties of both compounds were investigated as well
as the magnetic
properties of CPO-2-Cu.
2002-10
Evans, IR Evans, JSO Howard, JAK
Variable temperature structural study of bismuth lead vanadate, BiPb2VO6
JOURNAL OF MATERIALS CHEMISTRY 12, 2002, 2648-2652.
At room temperature, monoclinic BiPb2VO6 is a polar,
noncentrosymmetric, second harmonic generation active
material and its
crystal structure is among the more complex to be solved
ab initio from
powder diffraction data. In its stability range, BiPb2VO6
also exists
in a high symmetry, orthorhombic form. Both phases have
been
structurally characterized by a combination of X-ray and
neutron
diffraction data. Their mutual relationship, as well as
that to the
known compounds of the BiM(2)AO(6) (M = Mg, Ca, Mn, Cu,
Zn, Pb and A =
P, V, As) family, has been established.
2002-11
Moussa, SM Fenton, RR Hunter, BA
Kennedy, BJ
Polymorphism and phase transitions in bis(glycinato) copper(II). A
powder diffraction study
AUSTRALIAN JOURNAL OF CHEMISTRY 55, 2002, 331-341.
Powder diffraction methods have been used to establish the structures
of four known polymorphs of bis(glycinato)copper(II).
The two
cis-modifications are orthorhombic, and the two trans-complexes
are
monoclinic. Refinements of the structures, including the
location of
the hydrogen/deuterium atoms have been achieved utilizing
Rietveld
analysis of powder data. The cis-monohydrate complex crystallizes
in
the space group P2(1)2(1)2(1) with lattice parameters
a 10.8053(3), b
5.2101(1), and c 13.4983(4) Angstrom. Upon dehydration,
contraction
along the a- and c- axes and elongation of the b-axis
is observed. The
anhydrous cis-complex also crystallizes in the space group
P212121 with
lattice parameters a 10.0673(7), b 5.3152(4), and c 13.212(1)
Angstrom.
The trans-hydrated complex crystallizes in the space group
I2/a with
lattice parameters a 14.8218(3), b 5.2321(1), and c 9.6408(2)
Angstrom,
and beta 87.243(1)degrees. Dehydration of the complex
affords the
anhydrous modification which crystallizes in the space
group P2(1)/c
with lattice parameters a 7.0831(6), b 5.1459(4), and
c 9.4431(9)
Angstrom, and beta 107.506(4)degrees. In all four modifications
a
network of hydrogen bonds stabilizes the complex. This
study
illustrates the current capabilities of powder diffraction
techniques.
2002-12
Landskron, K Huppertz, H Senker, A
Schnick, W
Multianvil synthesis, X-ray powder diffraction analysis, P-31-MAS-NMR,
and FTIR spektroscopy as well as material properties of
gamma-P3N5, a
high-pressure polymorph of binary phosphorus(V) nitride,
built up from
distorted PN5 square pyramids and PN4 tetrahedra
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE 628, 2002, 1465-1471.
The high-pressure phase gamma-P3N5 was synthesized at a pressure of
I I
GPa and a temperature of 1500 degreesC in a multianvil
apparatus.
Partially crystalline P3N5 has been used as a starting
material. The
crystal structure was solved by direct methods on the
basis of X-ray
powder diffraction data and it was refined by the Rietveld
method
(Imm2, a = 1287.21(4), b = 261.312(6), c 440.03(2) pm,
Z = 2, R-p =
0.073, wR(p) = 0.094, R-F = 0.048). gamma-phosphorus nitride
crystallizes in a three-dimensional network structure
built up from
corner sharing PN4 tetrahedra and trans-edge sharing distorted
PN5
square pyramids. In the P-31-MAS-NMR spectrum two sharp
isotropic
resonances with an intensity ratio of I : 2.02(5) are
observed at
-11.95(3) and -101.72(7) ppm, respectively The IR-spectroscopic
and
thermal properties of gamma-P3N5 are described. Measurement
of the
Vickers hardness resulted in a value of 9.7(21) GPa for
sintered
polycrystalline gamma-P3N5, which is significantly higher
than that for
the partially crystalline normal pressure modification
Of P3N5 (5.1(7)
GPa).
2002-13
Li, HM Ju, J Lin, JH
Synthesis and crystal structure of layered beryllium polyborate H2BeB4O8
CHINESE JOURNAL OF INORGANIC CHEMISTRY 18, 2002, 764-768.
A new layered beryllium polyborate H2Be4O8 was synthesized in molten
boric acid flux. It crystallizes in the monoclinic space
group P2(1)/n
with lattice constants a = 17.75640(15) Angstrom, b =4.2948(1)
Angstrom, c =7.1532(1) Angstrom, beta = 96. 8797 (9)degrees
and V =
541.574 (9) Angstrom(3). The crystal structure, determined
by powder
X-ray diffraction techniques, is composed of double three-membered
ring
unit [BeB4O11], which is further connected by corner-sharing
to form
two-dimensional layers. The two-dimensional layers are
stacked along
[100] direction and form three-dimensional structure via
hydrogen
bonding.
2002-14 ???
Bock, H Hinz-Hubner, D Ruschewitz, U
Naumann, D
Structure of bis(pentafluorophenyl)xenon, Xe(C6F5)(2)
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION 41, 2002, 448-450.
2002-15
Grins, J Esmaeilzadeh, S Hull, S
Structure and ionic conductivity of Bi6Cr2O15, a new structure type
containing (Bi12O14)(n)(8n+) columns and CrO42- tetrahedra
JOURNAL OF SOLID STATE CHEMISTRY 163, 2002, 144-150.
Powder samples of the Cr6+-containing compound Bi6Cr2O15 were prepared
by solid state reaction of Bi2O3 and Cr2O3 in air at 650degreesC.
The
structure was solved and refined using high-resolution
neutron powder
diffraction data in space group Ccc2, with anisotropic
thermal
displacement parameters a = 12.30184(5), h = 19.87492(7),
and c =
5.88162(2) Angstrom, V= 1438.0 Angstrom(3), and 126 variables
to R-F =
1.8%. Bi6Cr2O15 exhibits a new structure type that contains
(Bi12O14)(n)(8n+) columns, of the kind previously found
only for phases
isotypic with Bi13MO4VO34. Each column is surrounded by
eight CrO42-
tetrahedra. The ionic conductivity of Bi6Cr2O15 was determined
by
impedance measurements to be 3.5 X 10(-5) (Omega cm)(-1)
at
600degreesC.
2002-16
Solovyov, LA Zaikovskii, VI Shmakov, AN
Belousov, OV Ryoo, R
Framework characterization of mesostructured carbon CMK-1 by X-ray
powder diffraction and electron microscopy
JOURNAL OF PHYSICAL CHEMISTRY B 106, 2002, 12198-12202.
The model of structure and structural transformation of the
mesostructured carbon material CMK-1 was established by
X-ray powder
diffraction (XRD) and transmission electron microscopy
(TEM)
investigations. The investigations showed that the enantiomeric
carbon
subframeworks formed within the pores of the MCM48 mesoporous
template
used for the material synthesis displaced with respect
to one another
without significant distortions after the dissolution
of the silica
wall of the template. The model proposed agrees well with
TEM images
observed. The XRD structural modeling of CMK- I done using
the
continuous density function technique allowed perfect
fit of the
calculated to the experimental powder diffraction pattern
and provided
geometric characteristics of the material texture. The
structural
characteristics obtained agreed fairly well with TEM analysis
and with
previously reported adsorption data.
2002-17
Solovyov, LA Shmakov, AN Zaikovskii, VI
Joo, SH Ryoo, R
Detailed structure of the hexagonally packed mesostructured carbon
material CMK-3
CARBON 40, 2002, 2477-2481.
Detailed investigation of the ordered mesoporous CMK-3 carbon using
XRD
structural modeling based on the continuous electron density
representation and the Rietveld technique allowed deriving
comprehensive and consistent information on the material
anatomy. The
electron density distribution map agrees with carbon 'bridges',
which
seem to be attributed to the material interconnecting
carbon nanorods
in the CMK-3 mesostructure. These carbon 'bridges' are
supposed to be
derived from former complementary mesopores of the SBA-15
template
used.
2002-18
James, M Watson, JN
The synthesis and crystal structure of doped uranium brannerite phases
U1-xMxTi2O6 (M=Ca2+, La3+, and Gd3+)
JOURNAL OF SOLID STATE CHEMISTRY 165, 2002, 261-265.
Doped uranium brannerite phases (U1-xMxTi2O6; M = Ca2+, La3+ and Gd3+;
x < 0.5) were synthesized at 1400degreesC; the range
of solid solution
was found to vary depending on whether sintering took
place in argon or
air. Powder X-ray diffraction revealed that these phases
crystallized
to form monoclinic (C2/m) structures. In particular, the
crystal
structures of U0.74Ca0.26Ti2O6 (1) (a = 9.8008(2); b =
3.7276(1); c =
6.8745(1); beta = 118.38(1); V = 220.97(1); Z = 2; R-P
= 7.3%; R-B =
4.6%) and U0.55La0.45Ti2O6 (2) (a = 9.8002(7); b = 3.7510(3);
c =
6.9990(5); beta = 118.37(4); V = 226.40(3); Z = 2; R-P
= 4.5%; R-B =
2.9%) were refined from powder neutron diffraction data,
revealing
planes of corner and edge-sharing TiO6 octahedra separated
by 8-fold
coordinate U/M atoms. The oxygen sites within these structures
were
found to be fully occupied, confirming that the doping
of lower valence
M atoms occurs in conjunction with the oxidation of U(IV)
to U(V).
2002-19 ???
AU Gover, RKB Withers, ND Allen, S
Withers, RL Evans, JSO
Structure and phase transitions of SnP2O7
JOURNAL OF SOLID STATE CHEMISTRY 166, 2002, 42-48.
SnP2O7 is a member of the ZrP2O7 family of materials, several of which
show unusual thermal expansion behavior over certain temperature
ranges
and which show a number of displacive phase transitions
on cooling from
high temperature. Here we describe the structural properties
of SnP2O7
from 100 to 1243K as determined by X-ray and neutron powder
diffraction. These studies reveal that SnP2O7 shows two
phase
transitions in this temperature range. At room temperature
the material
has a pseudo-cubic 3 X 3 X 3 superstructure. Electron
diffraction
studies show that the symmetry of this structure is P2(1)3
or lower. On
warming to similar to 560 K it undergoes a phase transition
to a
structure in which the subcell reflections show a triclinic
distortion;
above 830 K the subcell reflections show a rhombohedral
distortion.
Significant hysteresis in cell parameters is observed
between heating
and cooling. The structure of SnP2O7 is discussed with
references to
other members of the AM(2)O(7) family of materials.
2002-20
Toraya, H Yamazaki, S
Simulated annealing structure solution of a new phase of dicalcium
silicate Ca2SiO4 and the mechanism of structural changes
from
alpha-dicalcium silicate hydrate to alpha(L)'-dicalcium
silicate via
the new phase
ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE 58, 2002, 613-621.
A new phase of dicalcium silicate (Ca2SiO4) was formed by heating
alpha-dicalcium silicate hydrate [alpha-Ca-2 (SiO4H)OH
= alpha-C-2 SH]
at temperatures of similar to663-763 K, and it was transformed
into
alpha'(L)-Ca2SiO4 (= alpha'(L)-C2S) above similar to1193
K. The crystal
structure of the new phase (hereafter called x-C2S) has
been determined
by simulated annealing and refined by the Rietveld method
using
synchrotron radiation powder diffraction data. The structure
consists
of isolated SiO4 tetrahedra and a three-dimensional CaOn
polyhedral
network, forming a new structural type of dicalcium silicate.
A
structural change from alpha-C2SH to x-C2S is compelled
by large
displacements of SiO4 tetrahedra, accompanied by dehydration,
in the
direction perpendicular to the two-dimensional Ca(O,OH)(n)
polyhedral
network in alpha-C2SH. With increasing temperature, sizes
of CaOn
polyhedra in x-C2S become too large to confine Ca atoms
at the sixfold
to eightfold coordination sites. Then the structure of
alpha-C2S is
transformed into alpha'(L)-C2S, having eightfold to tenfold
coordination sites for the Ca atoms.
2002-21
Harris, KDM Johnston, RL Turner, GW
Tedesco, E Cheung, EY Kariuki, BM
Recent advances in the opportunities for solving molecular crystal
structures directly from powder diffraction data
MOLECULAR CRYSTALS AND LIQUID CRYSTALS 389, 2002, 123-129.
For those solids that can be prepared only as microcrystalline powders,
and are not suitable for investigation by single crystal
diffraction
methods, it is necessary to carry out structure determination
using
powder diffraction data. Here we highlight recent developments
in the
opportunities for solving molecular crystal structures
from powder
diffraction data, focusing on a direct-space strategy
in which a
hypersurface based on the powder profile R-factor R-wp
is searched
using a Genetic Algorithm. Recent fundamental developments
are
described, and the application of the method is illustrated
by the
structure determination of two oligopeptide materials.
2002-22
Kaduk, JA
Use of the Inorganic Crystal Structure Database as a problem solving
tool
ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE 58, 2002, 370-379.
The information in the Inorganic Crystal Structure Database (ICSD)
can
be used to determine the structures of new compounds by
analogy; this
database is thus a useful tool for practical problem solving.
A model
for the structure of (NH4)Fe(CO3)(OH)(2) [Cmcm, a = 6.6154
(6), b =
12.0639 (10), c = 6.0263 (5) Angstrom, Z = 4] was found
by searching
the ICSD for compounds with C-centered orthorhombic cells
and
containing C, H, N and O.
[Al(H2O)(6)](2)[Al(H2O)(5)(SO4)](2)-(H3O)(2)(SO4)(5) [P
(1) over bar, a
= 12.5881 (5), b = 13.0726 (5), c = 7.3354 (2) Angstrom,
alpha =
108.162 (2), beta = 70.536 (2), gamma = 112.658 (2)degrees,
Z = 1] is
isostructural to a Cr compound of the same stoichiometry,
which was
located by searching on the formula type ANX = A4B7X52.
Suitable models
for MgCl2(H2O)(4) [P2(1)/c, a = 5.9001 (9), b = 7.2709
(7), c = 8.4199
(7) Angstrom, beta = 111.007 (15)degrees, Z = 2], MgCl2(H2O)(2)
[C2/m,
a = 7.3886 (29), b = 8.5498 (24), c = 3.6488 (17) Angstrom,
beta =
98.96 (3)degrees, Z = 2], and MgCl2(H2O) [Pnma, a = 8.899
(7), b =
3.6339 (20), c = 11.398 (8) Angstrom, Z = 4] were located
by combining
searches on chemistry and formula type. Quantum-chemical
calculations
were performed on all five structures to locate the H-atom
positions
and to obtain quantitative understanding of the hydrogen
bonding
important in all the structures.
2002-23
Metastable NaYF4 fluorite at high pressures
and high temperatures
Grzechnik-A; Bouvier-P; Crichton-WA; Farina-L; Kohler-J
SOLID-STATE-SCIENCES. JUL 2002; 4 (7) : 895-899
The new polymorph is of the gagarinite-type (P6(3)/m. Z = 1) with partially
ordered cations, the formula being Na1.5Y1.5F6.
Crystal structure of [VOCl2(H2O)(C6H8O2)(2)]
from powder diffraction data
Lasocha-W; Grybos-R
JOURNAL-OF-MOLECULAR-STRUCTURE. NOV 6 2002; 641 (2-3) : 153-157
aquadichlorobis(2-hydroxy-3-methyl-2-cyclopenten-1-one) oxovanadium(IV)-VO6Cl2Cl2H18
was solved by powder diffraction method. Space group C2/c(15),
Ab initio structure solution of the polymer
electrolyte poly(ethylene oxide)(3): LiAsF6
Martin-Litas-I; Andreev-YG; Bruce-PG
CHEMISTRY-OF-MATERIALS. MAY 2002; 14 (5) : 2166-2170
PEO3:LiAsF6 has been determined ab initio from X-ray and neutron powder
diffraction data using a simulated annealing approach in direct crystallographic
space.
Crystal structure and morphology of the NdSr2RuCu2Oy
compound
Vecchione-A; Gombos-M; Pace-S; Marchese-L; Cerrato-G; Tedesco-C; Stephens-PW;
Noce-C
EUROPEAN-PHYSICAL-JOURNAL-B. MAR 2002; 26 (1) : 51-55
NdSr2RuCu2Oy,. The crystal structure of this material has been determined
by a combined high-resolution electron microscopy, selected area electron
diffraction and high-resolution X-ray powder diffraction study.
Synthesis, characterization and structure determination
of two novel layered aluminophosphates templated by 2-methylpiperazine
Tuel-A; Gramlich-V; Baerlocher-C
MICROPOROUS-AND-MESOPOROUS-MATERIALS. NOV 2002; 56 (2) : 119-130
(C5N2H14)(3)(H2O)(10) \ [Al6P8O32(H2O)(2)], P3 (no. 143) and (C5N2H14)(4.5)(H2O)(2.5)
\ [Al9P12O48], P2(1)/c
Tetraaryl biphenyl diamine hole transport materials:
a structural study utilizing both single crystal and high resolution powder
diffraction
Kennedy-AR; Smith-WE; Tackley-DR; David-WIF; Shankland-K; Brown-B;
Teat-SJ
JOURNAL-OF-MATERIALS-CHEMISTRY. 2002; 12 (2) : 168-172
The crystal structure of TPD-4, is derived from high resolution powder
diffraction techniques.
A new anion conductive bismuth-vanadium oxyfluoride
Akopjan-AV; Serov-TV; Dolgikh-VA; Ardaschnikova-EI; Lightfoot-P
JOURNAL-OF-MATERIALS-CHEMISTRY. 2002; 12 (5) : 1490-1494
Bi2VO5F0.7 , has been determined from powder X-ray and neutron diffraction
data, I4mm,
Structure elucidation of a novel aluminum methylphosphonate,
Al-3(CH3PO3)2 .O.(OH)(3), through a combination of X-ray powder diffraction,
solid-state NMR spectroscopy, and computational energy minimization
Edgar-M; Carter-VJ; Grewal-P; Sawers-LJ; Sastre-E; Tunstall-DP; Cox-PA;
Lightfoot-P; Wright-PA
CHEMISTRY-OF-MATERIALS. AUG 2002; 14 (8) : 3432-3439
Al-3(CH3PO3)(2).O.(OH)(3), direct methods crystallographic programs
tailored to X-ray powder diffraction. Pmnb
Synthesis and structure of fluoride-containing
GeO2 analogues of zeolite double four-ring building units
Villaescusa-LA; Lightfoot-P; Morris-RE
CHEMICAL-COMMUNICATIONS. 2002; (19) : 2220-2221
Double four-membered ring (D4R) anionic building units [Ge8O12(OH)(8)F](-)
have been synthesised hydrothermally and their structures solved from powder
X-ray diffraction.
Structure-property correlations in the new
ferroelectric Bi5PbTi3O14Cl and related layered oxyhalide intergrowth phases
Kusainova-AM; Stefanovich-SY; Irvine-JTS; Lightfoot-P
JOURNAL-OF-MATERIALS-CHEMISTRY. 2002; 12 (12) : 3413-3418
X-ray mapping in heterocyclic design: VI. X-ray
diffraction study of 3-(isonicotinoyl)-2-oxooxazolo[3,2-a]pyridine and
the product of its hydrolysis
Rybakov-VB; Babaev-EV; Pasichnichenko-KY; Sonneveld-EJ
CRYSTALLOGRAPHY-REPORTS. JAN-FEB 2002; 47 (1) : 69-74
3-(isonicotinoyl)-2-oxooxazolo[3,2-a]pyridine, C13H8N2O3, (1) is determined
by X-ray powder diffraction analysis. Pna2(1). The structure is solved
by the grid search procedure and refined by the Reitveld method
Structure of haloform intercalated C-60 and
its influence on superconductive properties
Dinnebier-RE; Gunnarsson-O; Brumm-H; Koch-E; Stephens-PW; Huq-A; Jansen-M
SCIENCE-. APR 5 2002; 296 (5565) : 109-113
Crystal structure of K-2[C2O6] - First proof
of existence and constitution of a peroxodicarbonate ion
Dinnebier-RE; Vensky-S; Stephens-PW; Jansen-M
ANGEWANDTE-CHEMIE-INTERNATIONAL-EDITION. 2002; 41 (11) : 1922-1924,1817
Reversible dimerization of C-60 molecules in
the crystal structure of the bis(arene)chromium fulleride [Cr(C7H8)](2)C-60
Honnerscheid-A; Dinnebier-R; Jansen-M
ACTA-CRYSTALLOGRAPHICA-SECTION-B-STRUCTURAL-SCIENCE. JUN 2002; 58 Part
3 Special Iss. 2 : 482-488
The structure of the blue luminescent delta-phase
of tris(8-hydroxyquinoline)aluminium(III) (Alq(3))
Colle-M; Dinnebier-RE; Brutting-W
CHEMICAL-COMMUNICATIONS. 2002; (23) : 2908-2909
Quinoline N-oxide dihydrate from powder data
Ivashevskaja-SN; Aleshina-LA; Andreev-VP; Nizhnik-YP; Chernyshev-VV
ACTA-CRYSTALLOGRAPHICA-SECTION-E-STRUCTURE-REPORTS-ONLINE. AUG 2002;
58 Part 8 : o920-o922
The structure of quinoline N-oxide dihydrate, C9H7NO.2H(2)O, has been
determined from X-ray powder diffraction data, using grid search technique
and a bond-restrained Rietveld refinement.
Synthesis and crystal structure of new double
indium phosphates (M3In)-In-I(PO4)(2) (M-I = K and Rb)
Zhizhin-MG; Filaretov-AA; Olenev-AV; Chernyshev-VV; Spiridonov-FM;
Komissarova-LN
CRYSTALLOGRAPHY-REPORTS. SEP-OCT 2002; 47 (5) : 773-782
K3In(PO4)(2) is solved using the Patterson function and refined
by the Rietveld method.
Bis(mu-quinoline N-oxide-kappa O-2 : O)bis[dichloro-copper(II)],
a powder diffraction study
Ivashevskaja-SN; Aleshina-LA; Andreev-VP; Nizhnik-YP; Chernyshev-VV
ACTA-CRYSTALLOGRAPHICA-SECTION-E-STRUCTURE-REPORTS-ONLINE. DEC 2002;
58 Part 12 : M721-M723
The crystal structure of the title compound, [ Cu2Cl4( C9H7NO) (2)],
has been determined from powder diffraction data.
Structure solution of a novel aluminium methylphosphonate
using a new simulated annealing program and powder X-ray diffraction data
Edgar-M; Carter-VJ; Tunstall-DP; Grewal-P; Favre-Nicolin-V; Cox-PA;
Lightfoot-P; Wright-PA
CHEMICAL-COMMUNICATIONS. 2002; (8) : 808-809
Al-2(CH3PO3)(3), has been solved from laboratory X-ray powder diffraction
data by simulated annealing of five independent structural sub-units.
Solid-state and solution phase reactivity of
10-hydroxy-10,9-boroxophenanthrene: a model building block for self-assembly
processes
Greig-LM; Kariuki-BM; Habershon-S; Spencer-N; Johnston-RL; Harris-KDM;
Philp-D
NEW-JOURNAL-OF-CHEMISTRY. 2002; 26 (6) : 701-710
Structure of compounds E(SnMe3)(4) (E = Si,
Ge) as seen by high-resolution X-ray powder diffraction and solid-state
NMR
Dinnebier-RE; Bernatowicz-P; Helluy-X; Sebald-A; Wunschel-M; Fitch-A;
van-Smaalen-S
ACTA-CRYSTALLOGRAPHICA-SECTION-B-STRUCTURAL-SCIENCE. FEB 2002; 58 Part
1 : 52-61
Decomposition of silver carbonate; the crystal
structure of two high-temperature modifications of Ag2CO3
Norby-P; Dinnebier-R; Fitch-AN
INORGANIC-CHEMISTRY. JUL 15 2002; 41 (14) : 3628-3637
Ag2CO3 the structures of the two high-temperature phases were
determined by direct methods and refined using the Rietveld method:
Crystal structures of hydrofluorocarbons from
powder X-ray diffraction data: HFC-134a and HFC-152a
Brunelli-M; Fitch-AN
ZEITSCHRIFT-FUR-KRISTALLOGRAPHIE. 2002; 217 (7-8) : 395-400
1,1,1,2-tetrafluoroethane (HFC-134a) and 1,2-difluoroethane (HFC-152a)
were solved by autoindexing, intensity extraction and direct methods with
the EXPO program, and refined via the Rietveld method. P2(1)/c, and
Pc.
Synthesis and characterization of new lamellar
templated titanium(IV) phosphates with perforated layers: MIL-28(n) or
Ti3O2X2(HPO4)(x)(PO4)(y).(N2CnH2n+6)(z).(H2O)(2) (n=2, 3; x=0, 2; y=4,2;
z=3,2; X = F, OH)
Serre-C; Taulelle-F; Ferey-G
CHEMISTRY-OF-MATERIALS. MAR 2002; 14 (3) : 998-1003
MIL-28(3) or [Ti3O2(OH)(2)(HPO4)(2)(PO4)(2)].(NH3-(CH2)(3)-NH3)(2).(H2O)(2)
has been determined ab initio from powder diffraction data and was refined
in the orthorhombic space group Fm2m
Two chain gallium fluorodiphosphates: synthesis,
structure solution, and their transient presence during the hydrothermal
crystallisation of a microporous gallium fluorophosphate
Millange-F; Walton-RI; Guillou-N; Loiseau-T; O'-Hare-D; Ferey-G
CHEMICAL-COMMUNICATIONS. 2002; (8) : 826-827
Two novel gallium fluorodiphosphates have been isolated and their structures
solved ab initio from powder X-ray diffraction data
The first 3-D ferrimagnetic nickel fumarate
with an open framework: [Ni-3(OH)(2)(O2C-C2H2-CO2)(H2O)(4)].2H(2)O
Guillou-N; Pastre-S; Livage-C; Ferey-G
CHEMICAL-COMMUNICATIONS. 2002; (20) 2358-2359
A three-dimensional nickel fumarate has been isolated by hydrothermal
reaction and its structure solved from powder X-ray diffraction
Structure of C-15-, C-17- and C-19-mono-acid
beta-triacylglycerols
Helmholdt-RB; Peschar-R; Schenk-H
ACTA-CRYSTALLOGRAPHICA-SECTION-B-STRUCTURAL-SCIENCE. FEB 2002; 58 Part
1 134-139
beta-1,2,3-tris(pentadecanoyl)glycerol (beta-C15C15C15), beta-1,2,3-tris(heptadecanoyl)glycerol
(beta-C17C17C17) and beta-1,2,3-tris(nonadecanoyl)glycerol (beta-C19C19C19)
have been determined from high-resolution X-ray powder diffraction data.
Grid search .
Spin crossover in hexakis(1-(2-chloroethyl)-tetrazole)iron(II)
complexes; synthesis and magnetic properties
Stassen-AF; Dova-E; Ensling-R; Schenk-H; Gutlich-P; Haasnoot-JG; Reedijk-J
INORGANICA-CHIMICA-ACTA. JUN 27 2002; 335 61-68
[Fe(teec)6](BF4)2 has been determined using X-ray synchrotron powder
diffraction.
The crystal structure of the decomposition
product NH4HC2O4 from powder diffraction data
Audebrand-N; Louer-D
ZEITSCHRIFT-FUR-KRISTALLOGRAPHIE. 2002; 217 (1) 35-40
NH4HC2O4, P2(1)/c,
New open-framework ammonium and amine cadmium
zirconium oxalates with helical structures
Jeanneau-E; Audebrand-N; Louer-D
CHEMISTRY-OF-MATERIALS. MAR 2002; 14 (3) 1187-1194
2[NH4](+)[CdZr(C2O4)(4)](2-) . 3.9H(2)O, P6(4)22 ; II, [C2N2H10](2+)[CdZr(C2O4)(4)](2-).4.4H(2)O,
P3(1)12 (no. 151).
Very large breathing effect in the first nanoporous
chromium(III)-based solids - MIL-53 or Cr-III(OH). {O2C-C6H4-CO2} {HO2C-C6H4-CO2H}(x)
H2Oy
Serre-C; Millange-F; Thouvenot-C; Nogues-M; Marsolier-G; Louer-D; Ferey-G
JOURNAL-OF-THE-AMERICAN-CHEMICAL-SOCIETY. NOV 13 2002; 124 (45)
13519-13526
MIL-53as , Pnam ; MIL-53ht , Imcm ; MIL-53It , C2/c
Building layered structures from hydrogen bonded
molecular units and 1D metal phosphonate chains: synthesis, characterization
and crystal structures of N,N '-dimethyl-N,N '-ethylenediamine-bis(methylenephosphonic
acid), its Ni(II) and Pb(II) complexes
Mao-JG; Wang-ZK; Clearfield-A
JOURNAL-OF-THE-CHEMICAL-SOCIETY-DALTON-TRANSACTIONS. 2002; (24)
: 4541-4546
The diphosphonic acid, N,N'-dimethyl-N,N'-ethylenediamine-bis(methylenephosphonic
acid) (H4L) 1, along with its Ni(II) and Pb(II) complexes, have been synthesized
and structurally determined.
The role of deprotonation of the ligand on
the structures of metal phosphonates: synthesis, characterization and crystal
structures of two new metal diphosphonates with a 1D double chain and a
2D layer structure
Mao-JG; Wang-Z; Clearfield-A
JOURNAL-OF-THE-CHEMICAL-SOCIETY-DALTON-TRANSACTIONS. 2002; (23)
: 4457-4463
Reactions of N-methyl-iminobis(methylenephosphonic acid), CH3N(CH2PO3H2)(2),
(H4L) with divalent metal nitrates in aqueous solution afforded two new
metal diphosphonates with different structures. Zn(H2L)(H2O) (1) ;
Cd(H3L)(2).2H(2)O (2).
New lead inorganic-organic hybrid microporous
and layered materials: Synthesis, properties, and crystal structures
Mao-JG; Wang-ZK; Clearfield-A
INORGANIC-CHEMISTRY. NOV 18 2002; 41 (23) : 6106-6111
Two new lead(II) phosphonates, namely, Pb-2{PMIDA}.1.5H(2)O (1) (H(4)PMIDA
= H2O3PCH2N(CH2CO2H)(2)) and Pb(H2L) (2) (H4L = CH3N(CH2PO3H2)(2)), have
been synthesized
Hydrothermal synthesis, characterization and
crystal structures of two new zinc(II) phosphonates: Zn-2[(O3PCH2)(2)NHCH2CO2]
and Zn-2[HO3PCH2NH(CH2PO3)(2)]
Mao-JG; Wang-ZK; Clearfield-A
NEW-JOURNAL-OF-CHEMISTRY. 2002; 26 (8) : 1010-1014
Zn-2[(O3PCH2)(2)NHCH2CO2] (complex 1) is hexagonal, P6(1),
Zn-2[HO3PCH2NH(CH2PO3)(2)] (complex 2) is also hexagonal, P6(1)
Synthesis and crystal structures of copper(II)
diphosphonatoalkanes: C-4 and C-5
Arnold-DI; Ouyang-X; Clearfield-A
CHEMISTRY-OF-MATERIALS. MAY 2002; 14 (5) : 2020-2027
Cu-2[(O3PC4H8PO3)(H2O)].2H(2)O (1) and Cu-2[(O-3-PC5H10PO3)(H2O)(2)].2.8H(2)O
(2), have been synthesized and their crystal structures solved from X-ray
powder data.
Synthesis, characterization, and crystal structures
of two divalent metal diphosphonates with a layered and a 3D network structure
Mao-JG; Wang-ZK; Clearfield-A
INORGANIC-CHEMISTRY. MAY 6 2002; 41 (9) : 2334-2340
Mn(H3L)(2).2H(2)O (complex 1) ,
Zn-3(HL)(2) (complex 2)
Critical role of diffraction simulation in
establishing the crystal and molecular structures of poly(biaryl
ether ketone)s
Aldred-PL; Colquhoun-HM; Williams-DJ; Blundell-DJ
MACROMOLECULES-. DEC 3 2002; 35 (25) 9420-9425
Molecular modeling and diffraction simulation studies of the biphenyl-based
poly(ether ketone)s [O-Ar-Ar-O-Ar-CO-Ar-Ar-CO-Ar-](n) (3) and [-O-Ar-Ar-CO
-Ar-](n) (4, Ar = 1,4-phenylene), coupled with data obtained from an oligomer
single-crystal study, have enabled their crystal and molecular structures
to be determined from X-ray powder data.
[Cu(imidazole)2(CO3)].H2O - an intermediate
in the formation of the copper bis-imidazolate polymer (blue phase),
N. Masciocchi, S. Bruni, E. Cariati, S. Galli, A. Sironi,
Zeit. Krist., (2002), 217, 131.
Alkyne oligomerization catalyzed by molybdenum(0)
complexes ,
G.A.Ardizzoia, S.Brenna, G.LaMonica, A.Maspero, N.Masciocchi,
J.Organomet.Chem., (2002), 649, 173.
Synthesis, structure and magnetism of homologous
series of polycrystalline cobalt alkane mono- and dicarboxylate soaps,
J.M.Rueff, N.Masciocchi, P.Rabu, A.Sironi, A.Skoulios,
Chem.Eur.J., (2002), 8, 1813.
The crystal structure of the organometallic
polymer [Pd{CH2C(O)Me}Cl]n, determined by X-ray powder diffraction methods,
N.Masciocchi, F.Ragaini, A.Sironi,
Organomet., 2002, 21, 3489.
X-ray Powder Diffraction Study of Organometallic
Polymers: [Ru(L)(CO)2]n (L = 2,2’-Bipyridine or 1,10 Phenanthroline),
N.Masciocchi, A. Sironi, S. Chardon-Noblat, A. Deronzier,
Organomet., 2002, 21, 4009.
One-dimensional polymers containing strictly
collinear metal ions: synthesis and XRPD characterization of homoleptic
binary metal pyrazolates,
N. Masciocchi, G.A. Ardizzoia, S. Brenna, G. LaMonica, A. Maspero,
S. Galli, A. Sironi,
Inorg.Chem. (2002) 41, 6080.
Preparation, Characterization and Structure
of Zirconium Fluoride Alkylamino- N,N-bis Methylphosphonates: a New Design
for Layered Zirconium Diphosphonates with a Poorly Hindered Interlayer
Region.
Costantino U; Nocchetti M; Vivani R.
J. Am. Chem. Soc., 124 (2002) 8428-8434.
ZrF(O3PCH2)(2)NHC5H11, F2(1)/c.
Crystal engineering on layered zirconium phosphonates.
Crystal structure (from X-ray powder data) and non-covalent interactions
on the layered zirconium compound of 4-[bis(phosphonomethyl)amino]butanoic
acid.
Vivani R; Costantino U; Nocchetti M.
J. Mater. Chem., 12 (2002) 3254-3260.
ZrHF(O3PCH2)(2) NHC3H6CO2, P2(1)/c
Powder diffraction study of the hydrogen bonds
in nitroxoline and its hydrochloride
Yatsenko AV, Paseshnichenko KA, Chernysshev VV,
Schenk H
Acta Cryst. C58 (2002) 019-021.
The solid state structures of potassium and
rubidium salicylate by high resolution X-ray powder diffraction
Dinnebier RE, Jelonek S, Sieler J, Stephens PW
Z. Anorg. Allg. Chem. 628 (2002) 363-368.
Structure prediction as a tool for solution
of the crystal structures of metallo-organic complexes using powder X-ray
diffraction data
Bond AD, Jones W
Acta Cryst. B58 (2002) 233-243.
One-dimensional spin chains from Cu-II ions
and 2,5-bis(pyrazol-1-y1)1,4-dihydroxybenzene
Dinnebier R, Lenner HW, Ding L, Shankland K,
David WIF, Stephens PW, Wagner M
Z. Anorg. Allg. Chem. 628 (2002)310-314.
Crystal structures of R-thiocamphor
Brunelli M, Fitch A, Mora AJ
Z. Kristallogr. 217 (2002) 83-87.
Synthesis and structure determination by ZEFSAII
of SSZ-55: A new high-silica, large-pore zeolite
Wu-MGG; Deem-MW; Elomari-SA; Medrud-RC; Zones-SI; Maesen-T; Kibby-C;
Chen-CY; Chan-IY
JOURNAL-OF-PHYSICAL-CHEMISTRY-B. JAN 17 2002; 106 (2) : 264-270
zeolite SSZ-55, Cmc21, The framework topology and symmetry of
SSZ-55 were determined by the Monte Carlo method ZEFSAII.
The crystal structure of 3-methyluracil from
X-ray powder diffraction data
Portalone,-G.; Ballirano,-P.; Maras,-A.
Journal-of-Molecular-Structure. 8 May 2002; 608(1): 35-9
3-methyluracil, Pbnm, conventional monochromatic X-ray powder
diffraction data, solved by direct methods
Synthesis, structure determination and properties
of MIL-53as and MIL-53ht: the first Cr-III hybrid inorganic-organic microporous
solids: Cr-III(OH).{O2C-C6H4-CO2}.{HO2C-C6H4-CO2H}(x)
Millange-F; Serre-C; Ferey-G
CHEMICAL-COMMUNICATIONS. 2002; (8) : 822-823
The first three-dimensional chromium(III) dicarboxylate compounds have
been isolated and their structures solved from powder X-ray diffraction
data.
Structure of nanocrystalline anatase solved
and refined from electron powder data
Weirich-TE; Winterer-M; Seifried-S; Mayer-J
ACTA-CRYSTALLOGRAPHICA-SECTION-A. JUL 2002; 58 Part 4 : 308-315
Energy-filtered Debye-Scherrer electron powder data have been successfully
employed to determine the structure of nanocrystalline anatase (TiO2).
The performed structure analysis includes determining the unit cell, space
group, solving the structure via direct methods from extracted intensities
and refining the structure using the Rietveld technique. The result of
the present study shows that the methods originally developed for determining
structures from X-ray powder data work equally well with data from electron
powder diffraction.
Supramol - a program for structure analysis
of intercalates using molecular simulations: the structure of VOPO4.C6H4O2
Koudelka-B; Capkova-P
JOURNAL-OF-MOLECULAR-MODELING. 2002; 8 (5) : 184-190
A method of structure analysis of intercalates has been developed that
uses a combination of molecular simulations with powder diffraction.
vanadyl phosphate intercalated with p-benzoquinone, I4/m,
the high temperature phase of vanadyl phosphate intercalated with dioxane,
C2/m
The crystal structure determination of the
crystalline layered silicic acid H-RUB-18
Borowski-M; Marler-B; Gies-H
ZEITSCHRIFT-FUR-KRISTALLOGRAPHIE. 2002; 217 (6) : 233-241
H-RUB-18 (chemical composition: Si4O7(OH)(2)) Crystal chemical
considerations and solid state NMR spectroscopy allowed to establish a
rough model of the structure which was optimized by forcefield molecular
dynamics (MD) simulations. A subsequent Rietveld refinement in space group
I4(1)/amd confirmed the model
Hydrothermal synthesis, structure determination
from powder data of a three-dimensional zirconium diphosphate with an exceptionally
high thermal stability: Zr(O3P-(CH2)-PO3) or MIL-57
Serre-C; Ferey-G
JOURNAL-OF-MATERIALS-CHEMISTRY. AUG 2002; 12 (8) : 2367-2369
Zr(O3P-(CH2)-PO3) or MIL-57 , P21/c, solved ab initio from laboratory
powder X-ray diffraction data.
Hydrothermal synthesis and X-ray powder structure
determination of a novel layered tin(IV) phosphate, Sn(HPO4)(2).(NH3)(0.4)(H2O)(0.6)
Roces-L; Khainakov-SA; Garcia-JR; Pertierra-P; Salvado-MA; Garcia-Granda-S
INORGANIC-CHEMISTRY-COMMUNICATIONS. SEP 2002; 5 (9) : 685-689
Sn(HPO4)(2) . (TH3)(0.4)(H2O)(0.6), R-3,
Hydrothermal synthesis, thermal behaviour and
structure determination from powder data of a porous three-dimensional
europium trimesate: Eu-3(H2O)(OH)(6)[C6H3(CO2)(3)]center dot 3H(2)O or
MIL-63
Serre-C; Ferey-G
JOURNAL-OF-MATERIALS-CHEMISTRY. 2002; 12 (10) : 3053-3057
MIL-63 or Eu -3(H2O)(OH)(6)[C6H3(CO2)(3)].3H(2)O, P21/n,
LiNa2AlF6: a powder structure solution
Kirik-SD; Zaitseva-JN; Yakimov-IS; Golovnev-NN
ACTA-CRYSTALLOGRAPHICA-SECTION-C-CRYSTAL-STRUCTURE-COMMUNICATIONS.
NOV 2002; 58 Part 11 : I159-i160
LiNa2AlF6
Unexpected molecular structure
from laboratory powder diffraction data
Chernyshev-VV; Yatsenko-AV; Kuvshinov-AM;
Shevelev-SA
JOURNAL-OF-APPLIED-CRYSTALLOGRAPHY.
DEC 2002; 35 Part 6 : 669-673
2,4-dinitro-N-phenyl-6 -(phenylazo)benzamide,
(I),
N-(2-methoxyphenyl)-2-(2-methoxyphenylazo)-4,6
-dinitrobenzamide, (II), and
N-methyl-2,4-dinitro-N-phenyl-6-(phenylazo)
benzamide, (III),
were determined from low-resolution
laboratory powder diffraction data. - Based on the correct molecular structure
of (I), the crystal structures of ( II) and (III) were routinely solved
by the grid search technique.
Structure determination of the
anhydrous form of MIL-3K: a vanadodiphosphonate with a 3D hybrid framework
Kongshaug-KO; Riou-D
JOURNAL-OF-THE-CHEMICAL-SOCIETY-DALTON-TRANSACTIONS.
2002; (22) : 4152-4155
((KV2O3)-O-IV/V{O3P-(CH2)(2) -PO3} or MIL-3K(an)) , P-1,
determined from X-ray powder diffraction
Determination of the crystal
and magnetic structures of Rn+1Co3n+5B2n (n=1, 2, and 3; R=Pr, Nd,
and Dy)
Zlotea-C; Chacon-C; Isnard-O
JOURNAL-OF-APPLIED-PHYSICS. DEC 15 2002; 92 (12) : 7382-7388
Rn+1Co3n+5B2n compounds (R=Pr, Nd, and Dy; n=1,
2, and 3) have been studied by high-resolution powder neutron
diffraction and magnetization measurements.
C-H...O hydrogen bond mediated
chain reversal in a peptide containing a gamma-amino acid residue, determined
directly from powder X-ray diffraction data
Cheung-EY; McCabe-EE; Harris-KDM; Johnston-RL; Tedesco-E;
Raja-KMP; Balaram -P
ANGEWANDTE-CHEMIE-INTERNATIONAL-EDITION. 2002; 41 (3)
: 494-496
Three-dimensional structure determination
of N-(p-tolyl)-dodecylsulfonamide from powder diffraction data and validation
of structure using solid-state NMR spectroscopy
Rajeswaran-M; Blanton-TN; Zumbulyadis-N; Giesen-DJ; Conesa-Moratilla-C;
Misture-ST; Stephens-PW; Huq-A
JOURNAL-OF-THE-AMERICAN-CHEMICAL-SOCIETY. DEC 4 2002;
124 (48) : 14450-14459
N-(p-tolyl)-dodecylsulfonamide, P21/c, combination of
powder XRD data, several computational packages involving Monte Carlo simulations
and ab initio quantum mechanical calculations, and experimental solid-state
NMR chemical shifts.
Determination and Rietveld refinement
of the crystal structure of Li0.50Ni0.25TiO(PO4) from powder X-ray and
neutron diffraction
Manoun-B; El-Jazouli-A; Gravereau-P; Chaminade-JP; Bouree-F
POWDER-DIFFRACTION. DEC 2002; 17 (4) : 290-294
Li0.50Ni0.25TiO(PO4), P21/c, determined from conventional
X-ray and neutron powder diffraction data.
Synthesis, crystal structure
determination from X-ray powder diffractometry and vibrational spectroscopy
of the tricyanomelaminate monohydrates M-3[C6N9]center dot H2O (M = K,
Rb)
Irran-E; Jurgens-B; Schnick-W
SOLID-STATE-SCIENCES. OCT 2002; 4 (10) : 1305-1311
Rb-3n[C6N9].H2O, P1, synchrotron X-ray powder diffraction
data
Ab initio crystal structure determination
of Na2Si3O7 from conventional powder diffraction data
Kahlenberg-V; Marler-B; Acevedo-JCM; Patarin-J
SOLID-STATE-SCIENCES. OCT 2002; 4 (10) : 1285-1292
Na2Si3O7, P21/c, direct methods using integrated intensities
of conventional X-ray powder diffraction data
The crystal structure and magnetic
properties of the 1-dimensional dihalide -bridged polymers dichlorobis(thiazole)cobalt(II)
and bromobis(thiazole)-cobalt(II)
JAMES-M; HORVAT-J
The-Journal-of-physics-and-chemistry-of-solids. 2002;
63 (4) : 657-663
Co(thiazole)2X2 (X = Cl (1), Br(2)) C2/c,
Powder X-ray and neutron diffraction measurements were used for structural
determination.
Crystal and molecular structures
of poly(1,4-phenylenesulfone) and its trisulfone and tetrasulfone oligomers
COLQUHOUN-Howard-M; ALDRED-Peter-L; KOHNKE-Franz-H; HERBERTSON-Penelope-L;
BAXTER-Ian; WILLIAMS-David-J
Macromolecules-. 2002; 35 (5) : 1685-1690
poly(1,4-phenylenesulfone), [1,4-ArSO2]n (Ar = 1,4-phenylene),
and its tetrasulfone oligomer ArSO2ArSO2ArSO2ArSO2Ar
(Ar = phenyl or 1,4-phenylene)
from X-ray powder diffraction data interfaced to
molecular simulation and diffraction modeling.
Ab initio structure determination
of new boride CePt3B, a distorted variant of CaTiO3
SOLOGUB-O-L; HESTER-J-R; SALAMAKHA-P-S; LEROY-E; GODART-C
Journal-of-alloys-and-compounds. 2002; 337 (1-2) : 10-17
CePt3B, P4mm, from conventional and synchrotron radiation,
Ab initio structure determination
of a new compound, <beta>-SrGaBO4, from powder X-ray diffraction data
YANG-Z; LIANG-J-K; CHEN-X-L; CHEN-J-R
Journal-of-solid-state-chemistry. 2002; 165 (1) : 119-124
<beta>-SrGaBO4, P21212, powder X-ray diffraction data,
by direct methods.
Bridging the gap: structure determination
of the red polymorph of tetrahexylsexithiophene by Monte Carlo simulated
annealing, first -principles DFT calculations and Rietveld refinement
NEUMANN-Marcus-A; TEDESCO-Consiglia; DESTRI-Silvia; FERRO-Dino-R;
PORZIO -William
Journal-of-applied-crystallography. 2002; 35 (p.3) :
296-303
red polymorph of tetrahexylsexithiophene (THST), C2/m,
X-ray powder diffraction data by a direct-space Monte Carlo simulated-annealing
approach. First-principles density functional theory (DFT) calculations
are used to distinguish between three nearly identical solutions in the
space groups C2/m, C2 and P1
Two ammonium templated gallophosphates:
synthesis and structure determination from powder diffraction data of 2D
and 3D-GAPON
BONHOMME-Francois; THOMA-Steven-G; NENOFF-Tina-M
Microporous-and-mesoporous-materials. 2002; 53 (1-3)
: 87-96
[Ga(PO4)(OH)] [NH4] (2D-GAPON), P21/m
[Ga2(PO4)3]3+.3[NH4]+ (3D-GAPON), C2/c,
Synthetic hydrocerussite, 2PbCO3.Pb(OH)2,
by X-ray powder diffraction
MARTINETTO-Pauline; ANNE-Michel; DOORYHEE-Eric; WALTER-Philippe;
TSOUCARIS -Georges
Acta-crystallographica-Section-C-Crystal-structure-communications.
2002; 58 (p.6) : i82-i84
Pb3(CO3)2(OH)2], X-ray powder, Patterson function
X-ray powder structure determination
and thermal behavior of a new modification of Pb(II) selenite
LAHTINEN-Manu; VALKONEN-Jussi
Chemistry-of-materials. 2002; 14 (4) : 1812-1817
PbSeO3, P21/c, conventional X-ray powder diffraction
data. Direct methods and Rietveld refinement techniques were used for the
structure determination.
Two new three-dimensional vanadium(III)
and iron(III) phosphites templated by ethylenediamine: (C2H10N2)0.5[M(HPO3)2].
Ab initio structure determination, spectroscopic, and magnetic properties
FERNANDEZ-Sergio; MESA-Jose-L; PIZARRO-Jose-L; LEZAMA-Luis;
ARRIORTUA-Maria -I; ROJO-Teofilo
Chemistry-of-materials. 2002; 14 (5) : 2300-2307
(C2H10N2)0.5[V(HPO3)2], P2/c
Structure determination at room
temperature and phase transition studies above Tc in ABi4Ti4O15 (A
= Ba, Sr or Pb)
NALINI-G; GURU-ROW-T-N
Bulletin-of-Materials-Science. 2002; 25 (4) : 275-281
BaBi4Ti4O15, I4/mmm
SrBi4Ti4O15 and PbBi4Ti4O15, A21am.
Hydrothermal synthesis, structure
determination, and thermal behavior of new three-dimensional europium
terephthalates: MIL -51 LT, HT and MIL-52 or Eu2n(OH)x(H2O)y(O2C
-C6H4-CO2)z (n = III, III, II; x = 4, 0, 0; y = 2, 0, 0; z = 1, 1,
2)
SERRE-Christian; MILLANGE-Franck; MARROT-Jerome; FEREY-Gerard
Chemistry-of-materials. 2002; 14 (5) : 2409-2415
Three-dimensional europium terephthalates have been obtained
under hydrothermal conditions and their structures solved using either
X-ray powder diffraction or single-crystal data.
A structural study of polymorphism
in phenyl salicylate: determination of the crystal structure of a
meta-stable phase from X-ray powder diffraction data using a direct space
systematic search method
HAMMOND-R-B; JONES-M-J; ROBERTS-K-J; KUTZKE-H; KLAPPER-H
Zeitschrift-fur-Kristallographie. 2002; 217 (9) : 484-491
phenyl salicylate (salol), P21/n, Structure solution
was achieved by a procedure combining a computer based systematic
search method with a subsequent Rietveld refinement of experimental X-ray
powder diffraction data.
X-ray structural determination
of a multilayered magnetic dielectric ceramic Ba42Ti51Fe20O174 in the BaO-TiO2-Fe2O3
system
NASSIF-V-M; CARBONIO-R-E; HODEAU-J-L; DOORYHEE-E
Journal-of-solid-state-chemistry. 2002; 166 (2) : 400-414
(Ba42Ti51Fe20O174), C2/m, synchrotron X-ray powder
diffraction.
A new fluorite type compound
Pb5Bi17X5O43: synchrotron and neutron structure determination (X
= P) and conduction properties (X = P, V and As)
ROUSSEL-Pascal; GIRAUD-Sophie; SUARD-Emmanuelle; WIGNACOUN-Jean-Pierre;
STEINFINK-Hugo
Solid-state-sciences. 2002; 4 (9) : 1143-1152
Pb5Bi17P5O43, Im
Synthesis and ab initio structural determination
of a new pillared nickel diphosphonate: VSB-6 or Ni5.4(OH, F)4[O3P-(CH2)3
-PO3]2(H2O)1.4.1.2H3O
GUILLOU-Nathalie; QIUMING-GAO; NOGUES-Marc; CHEETHAM-Anthony-K; FEREY-Gerard
Solid-state-sciences. 2002; 4 (9) : 1179-1185
Ni5.4(OH,F)4[O3P -(CH2)3PO3]2(H2O)1.4.1.2H3O, Pmmn, from laboratory
X-ray powder diffraction data
Molecular, crystallographic and algorithmic
factors in structure determination from powder diffraction data by simulated
annealing
SHANKLAND-Kenneth; MCBRIDE-Lorraine; DAVID-William-I-F; SHANKLAND-Norman;
STEELED-Gerald
Journal-of-applied-crystallography. 2002; 35 (p.4) : 443-454
famotidine form B, P21/c, simulated annealing by DASH
Reaction of bis(trimethylsilylamino)dichlorosilane
with titanium tetrachloride - Synthesis and crystal structure of [mu -ClTiCl2N(SiMe3)SiCl2NH2](2)
Rannabauer-S; Bettenhausen-R; Schnick-W
ZEITSCHRIFT-FUR-ANORGANISCHE-UND-ALLGEMEINE-CHEMIE. FEB 2002; 628 (2)
: 373-376
[mu-ClTiCl2N(SiMe3)-SiCl2NH2](2) P21/n, the molecular structure
has been solved by X-ray powder diffraction methods and it could be confirmed
by single-crystal X -ray structure determination at -70degreesC.
Differential evolution: crystal structure determination
of a triclinic polymorph of adipamide from powder diffraction data.
Seaton CC, Tremayne M.
Chem Commun 2002:880–881.
The crystal structure of a previously unknown
triclinic polymorph of adipamide has been solved from laboratory X-ray
powder diffraction data using a new direct space global optimisation method
based on differential evolution.
Lead tartrate from X-ray powder diffraction
data
D. J. A. De Ridder, K. Goubitz, E. J. Sonneveld,
W. Molleman and H. Schenk
Acta Cryst. (2002). C58, 596-598
Pb^2+[middle dot]C[4]H[4]O[6]^2-
Crystal structure of the inclusion complex
of [beta]-cyclodextrin with mefenamic acid from high-resolution synchrotron
powder-diffraction data in combination with molecular-mechanics calculations
M. M. Pop, K. Goubitz, G. Borodi, M. Bogdan,
D. J. A. De Ridder, R. Peschar and H. Schenk
Acta Cryst. (2002). B58, 1036-1043
Structure determination from powder diffraction
data of a new layered ammonium lanthanum sulfate, beta-(NH4)La(SO4)2
P. Bénard-Rocherullé, H. Tronel
and D. Louër
Powder Diffraction 17 ( 2002) 210-217.
beta-(NH4)La(SO4)2, Pn,
DICVOL, LBM/EXPO, SHELXL97, FULLPROF
Terephthalate salts of dipositive cations
J. A. Kaduk
Acta Cryst. (2002). B58, 815-822
The structure of
a series of divalent metal terephthalate
salts was determined by applying Monte
Carlo simulated annealing techniques to X-ray powder data.
Structures of three substituted arenesulfonamides
from X-ray powder diffraction data using the differential evolution technique
M. Tremayne, C. C. Seaton and C. Glidewell
Acta Cryst. (2002). B58, 823-834
The crystal structures
of three substituted arenesulfonamides have
been solved from X-ray powder diffraction data using a new direct-space
structure solution method based on a differential evolution
algorithm.
The use of restraints in Rietveld refinement
of molecular compounds; a case study using the crystal structure determination
of tryptamine free base
H. Nowell, J. P. Attfield and J. C. Cole
Acta Cryst. (2002). B58, 835-840
tryptamine (C10H12N2), P212121, simulated annealing
Structure solution and refinement of tetracaine
hydrochloride from X-ray powder diffraction data
Nowell-H; Attfield-JP; Cole-JC; Cox-PJ; Shankland-K;
Maginn-SJ; Motherwell-WDS
NEW-JOURNAL-OF-CHEMISTRY. 2002; 26 (4) : 469-472
tetracaine hydrochloride ( C15H25N2O2+Cl-)
solved from synchrotron X-ray powder diffraction data using a direct-space
global optimisation method - nine torsional degrees of freedom in
the cation.
Crystal structure of Ca3(VO4)2 synthesized
at 11 GPa and 1373 K
A. Grzechnik
Solid State Sciences 4 (2002) 523-527.
Ca3(VO4)2, C2/m, 6 independent atoms, 11 atomic
coordinates refined
Programs :DICVOL91, EXPO, DM by EXPO, GSAS
Dichlorobis(2-methylquinoline N-oxide-[kappa]O)zinc(II)
from powder data
S. N. Ivashevskaja, L. A. Aleshina, V. P. Andreev,
Y. P. Nizhnik, V. V. Chernyshev and H. Schenk
Acta Cryst. C58 (2002) 300-301
[ZnCl2(C10H9NO)2]
Ab initio structure determination of
triphenyl phosphite by powder synchrotron X-ray diffraction
O. Hernandez, A. Hédoux, J. lefebvre,
Y. Guinet, M. Descamps, R. Papoular and O. Masson,
J. Appl. Cryst. 35 (2002) 212-219.
P(OC6H5)3, R-3, 22 non-hydrogen atoms,
6 torsion angles,
Programs : DICVOL, DASH, JANA2000
Failure by EXPO
The application of structure envelopes in structure
determination from powder diffraction data
S. Brenner, L.B. McCusker and C. Baerlocher,
J. Appl. Cryst. 35 (2002) 243-252.
C32N3O6H53 (tri-beta-peptide), P212121, 41 non-hydrogen
atoms, 17 torsion angles.
Programs : TREOR, DICVOL, EXTRACT, SayPerm, Safe
- simulated annealing -, Focus, XRS-82 .
Failure by EXPO
The crystal structure of Na3HP2O7 H2O from
X-ray powder diffraction data
L.S. Ivashkevich, K.A. Selevich, A.S. Lyakhov,
A.F. Selevich, Yu.I. Petrusevich
Zeitschrift für Kristallographie 217, (2002)
73-77.
Na3HP2O7 H2O, P21/n,
EXPO, FULLPROF
A tetragonal polymorph of caesium hydroxide
monohydrate, CsOH.H[2]O, from X-ray powder data
R. Cerny, V. Favre-Nicolin and B. Bertheville
Acta Cryst. (2002). C58, i31-i32
CsH3O2,
The crystal structure of the binary mixed valence
compound Bi(III)3Bi(V)O7 and isotypic Bi3SbO7 as determined by high resolution
X-ray and neutron powder diffraction
R.E. Dinnebier, R.M. Ibberson, H. Ehrenberg and
M. Jansen
J. Solid State Chem 163 (2002) 332-339.
Bi4O7, P-1, /
ITO, FULLPROF, EQUI, EXPO, , GSAS
Low-temperature crystal structure of S-camphor
solved from powder synchrotron X-ray diffraction data by simulated annealing
M. Brunelli, A.N. Fitch & A.J. Mora
J. Solid State Chem. 163 (2002) 253-258.
C10H160, P212121,
FZON, Expo failed, PowderSolve succeeded in locating
2 independent molecules, structure refined by WinMprof
Salts of aromatic carboxylates. The crystal
structures of nickel(II) and cobalt(II) 2,6-naphthalenedicarboxylate tetrahydrate
J. A. Kaduk and J. A. Hanko
accepted for publication in J. Applied Cryst
(2 compounds, 1 structure).