Phase-transformation-induced twinning of an iron(III) calix[4]pyrrolidine complex

2014 ◽  
Vol 70 (7) ◽  
pp. 644-649 ◽  
Author(s):  
Guillaume Journot ◽  
Reinhard Neier ◽  
Helen Stoeckli-Evans
Keyword(s):  
Phase Transformation ◽  
Title Compound ◽  
Macrocyclic Ligand ◽  
Reduced Form ◽  
Slow Phase ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Monoclinic Form ◽  
Independent Molecules ◽  
The Individual

The title compound, tetrachlorido-1κCl;2κ3Cl-(2,2,7,7,12,12,17,17-octamethyl-21,22,23,24-tetraazapentacyclo[16.2.1.13,6.18,11.113,16]tetracosane-1κ4N,N′,N′′,N′′′)-μ2-oxido-diiron(III), [Fe2Cl4O(C28H52N4)], undergoes a slow phase transformation atca173 K from monoclinic space groupP21/n, denoted form (I), to the maximal non-isomorphic subgroup, triclinic space groupP\overline{1}, denoted form (II), which is accompanied by nonmerohedral twinning [twin fractions of 0.693 (4) and 0.307 (4)]. The transformation was found to be reversible, as on raising the temperature the crystal reverted to monoclinic form (I). In the asymmetric unit of form (I),Z′ = 1, while in form (II),Z′ = 2, with a very small reduction (ca1.8%) in the unit-cell volume. The two independent molecules (AandB) in form (II) are related by a pseudo-twofold screw axis along thebaxis. The molecular overlay of moleculeAon moleculeBhas an r.m.s. deviation of 0.353 Å, with the largest distance between two equivalent atoms being 1.202 Å. The reaction of calix[4]pyrrolidine, the fully reduced form ofmeso-octamethylporphyrinogen, with FeCl3gave a red–brown solid that was recrystallized from ethanol in air, resulting in the formation of the title compound. In both forms, (I) and (II), the FeIIIatoms are coordinated to the macrocyclic ligand and have distorted octahedral FeN4OCl coordination spheres. These FeIIIatoms lie out of the mean plane of the four N atoms, displaced towards the O atom of the [OFeCl3] unit by 0.2265 (5) Å in form (I), and by 0.2210 (14) and 0.2089 (14) Å, respectively, in the two independent molecules (AandB) of form (II). The geometry of the [OFeCl3] units are similar, with each FeIIIatom having a tetrahedral coordination sphere. The NH H atoms are directed below the planes of the macrocycles and are hydrogen bonded to the coordinated Cl−ions. There are also intramolecular C—H...Cl hydrogen bonds present in both (I) and (II). In form (I), there are no significant intermolecular interactions present. In form (II), the individual molecules are arranged in alternate layers parallel to theacplane. TheBmolecules are linked by a C—H...Cl hydrogen bond, forming chains along [100].

scholarly journals (1S,2R,8R)-11-Amino-2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodec-10-en-9-one

IUCrData ◽  
2017 ◽  
Vol 2 (2) ◽  
Author(s):  
Mustapha Ait Elhad ◽  
Ahmed Benharref ◽  
Lahcen El Ammari ◽  
Mohamed Saadi ◽  
Abdelouahd Oukhrib ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
Asymmetric Unit ◽  
Space Group ◽  
Axis Direction ◽  
Compound C ◽  
Independent Molecules

The title compound, C16H23Cl2NO, crystallizes in the monoclinic space groupP21with two independent molecules (AandB) in the asymmetric unit. They have essentially the same conformation. Each molecule is built up from fused six- and seven-membered rings and an additional three-membered ring. The six-membered ring has an envelope conformation, with the C atom belonging to the three-membered ring forming the flap, while the seven-membered ring displays a boat conformation. In the crystal, molecules are linked into chains propagating along thea-axis direction by N—H...O hydrogen bonds.

scholarly journals 4-(4-Hydroxyphenyl)-2,2,4-trimethyl-7,8-benzothiachroman, a fused-ring counterpart ofthia-Dianin's compound

2017 ◽  
Vol 73 (11) ◽  
pp. 1662-1665 ◽  
Author(s):  
Christopher S. Frampton ◽  
Joseph J. McKendrick ◽  
David D. MacNicol
Keyword(s):  
Hydrogen Bond ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Methyl Group ◽  
Space Group ◽  
Compound C ◽  
Fused Ring ◽  
Phenolic Group ◽  
Independent Molecules ◽  
Dianin's Compound

The title compound, C22H22OS [systematic name: 4-(1,3,3-trimethyl-2,3-dihydro-1H-4-thiaphenanthren-1-yl)phenol], crystallizes unsolvated from nitromethane as colourless prisms (m.p. 425–427 K) in the polar monoclinic space groupIawithZ′ = 2 (moleculesAandB). Both independent molecules possess a very similarproximalconformation, this referring to the juxtaposition of the 4-hydroxyphenyl substituent with respect to thesyn-related methyl group. In the crystal, moleculeAis linked to moleculeBby an O—H...O hydrogen bond. In turn, moleculeBexhibits a weak O—H...π interaction with the phenolic group of moleculeArelated bya-glide symmetry. Together, these lead to [100] chains.

A New Host Lattice Built of the Werner-Type Copper(I,II) Cyanide Complex Involving a Macrocyclic Ligand

1998 ◽  
Vol 63 (5) ◽  
pp. 622-627 ◽  
Author(s):  
Hidetaka Yuge ◽  
Takayoshi Soma ◽  
Takeshi Ken Miyamoto
Keyword(s):  
Macrocyclic Ligand ◽  
Host Lattice ◽  
Macrocyclic Complex ◽  
Monoclinic Space Group ◽  
Cyanide Complex ◽  
New Host ◽  
Space Group

Crystals of a new clathrate [CuII(hmtd)CuI(CN)3]·CH2Cl2 were afforded from a Me2CO-EtOH-CH2Cl2 solution of a macrocyclic complex CuII(hmtd)CuI(CN)3·2 H2O (hmtd = 5,7,7,12,14,14-hexamethyl- 1,4,8,11-tetraazacyclotetradeca- 4,11-diene). It crystallizes in the monoclinic space group P21/n, a = 7.936(5), b = 18.717(4), c = 17.783(6) Å, β = 98.55(4)°, Z = 4, R = 0.0558 for 1 870 reflections. Unprecedentedly, only one of the three nitrogen-ends of a CuI(CN)3 moiety is coordinated to the square-pyramidal Cu(II) center. The guest CH2Cl2 molecules are captured in the channel between the potlid-shaped [CuII(hmtd)CuI(CN)3] molecules.

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

Crystal and molecular structure of di-o-anisylketone

1985 ◽  
Vol 63 (12) ◽  
pp. 3374-3377 ◽  
Author(s):  
C. Faerman ◽  
S. C. Nyburg ◽  
G. Punte ◽  
B. E. Rivero ◽  
A. A. Vitale ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Compound C ◽  
Twist Conformation ◽  
Oxygen Atoms

The crystal and molecular structure of the title compound, C15H14O3, is described. Crystals are monoclinic, space group P21/n, a = 9.893(5), b = 10.719(5), c = 12.136(3) Å, β = 90.56(3)°. The molecule has a twist conformation and interactions between oxygen atoms of the methoxyl groups are thought to play some part in this.

Intermediate Products of the Reaction of (4,4,9,9-Tetramethyl-5,8-diazadodecane-2,11-dione dihydrazone)nickel(II) With Butane-2,3-dione; the Structure of cis-Aqua(3,4,7,9,9,14,14,16-octamethyl-1,2,5,6,10,13-hexaazacyclohexadeca-1(16),4,6-tien-3-Ol)nickel(II) Perchlorate Trihydrate

1994 ◽  
Vol 47 (10) ◽  
pp. 1885 ◽  
Author(s):  
NF Curtis ◽  
AR Davis ◽  
FWB Einstein
Keyword(s):  
Water Molecule ◽  
Hydroxy Group ◽  
Secondary Amine ◽  
Macrocyclic Ligand ◽  
Equilibrium Mixture ◽  
Monoclinic Space Group ◽  
Amine Nitrogen ◽  
Space Group ◽  
X Ray ◽  
Intermediate Products

Intermediate products have been isolated from the reaction of (4,4,9,9-tetramethyl-5,8-diazadodecane-2,11-dione dihydrazone )nickel(II) perchlorate with butane-2,3-dione which finally yields the macrocyclic product (3,4,7,9,9,14,14,16-octamethyl-1,2,5,6,10,13-hexaazacyclohexa-deca-2,4,6,16-tetraene)nickel(II) perchlorate , [Ni( omht )] (ClO4)2. An initial violet product is assigned a structure with the macrocyclic ligand 3-acetyl-3,6,8,8,13,13,15-heptamethyl-1,2,4,5,9,12-hexaazacyclopentadeca-5,15-diene. In water this converts into an equilibrium mixture of the tautomeric cations blue cis-aqua(3,4,7,9,9,14,14,16-octamethyl-1,2,5,6,10,13-hexaazacyclohexadeca-1(16),4,6-trien-3-ol)nickel(II), cis-[Ni(L2)(H2O)]2+, and orange (3,6,8,- 8,13,13-hexamethyl-4,5,9,12-tetraazahexadeca-3,5-diene-2,15-dione 15-hydrazone)nickel(II), [Ni(L3)]2+. The rates at 25°C of the forward and reverse reactions of this tautomerism, and of the slower conversion of the equilibrium mixture to [Ni( omht )](ClO4)2, are reported. The structure of cis -[Ni(L2)(H2O)](ClO4)2.3H2O has been determined by X-ray diffractometry (monoclinic, space group P21/n, a 9.694(8), b 19.218(14), c 16.652(9) Ǻ, β 94.88(1)°, R 0.079 for 3254 reflections). This has NiII in octahedral coordination by secondary amine nitrogen atoms 10 and 13, hydrazone nitrogen atoms 1 and 6, and the carbinolamine oxygen substituent at position 3 of the pentadentate macrocyclic ligand L2, with a water molecule coordinated cis to the hydroxy group. Compounds of the tautomeric cations [Ni(L2)]2+ and [Ni(L3)]2+ with coordinated thiocyanate, azide, nitrite, oxalate and acetate are described.

scholarly journals Metallorganische Verbindungen der Lanthanoide, 41 [1]. Die Kristall-und Molekülstruktur von (C5Me5)2HoCl(THF) / Organometallic Compounds of the Lanthanides, 41 [1]. The Crystal and Molecular Structure of (C5Me5)2HoCl(THF)

1988 ◽  
Vol 43 (3) ◽  
pp. 323-327 ◽  
Author(s):  
H. Schumann ◽  
J. Loebel ◽  
D. van der Helm ◽  
M. B. Hossain
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Organometallic Compounds ◽  
Asymmetric Unit ◽  
Space Group ◽  
X Ray ◽  
Independent Molecules

The title compound (1) is obtained as brownish crystals by reaction of HOCl3 with NaC5Me5 in tetrahydrofuran. The structure of 1, which has two slightly different independent molecules per asymmetric unit, has been elucidated by X-ray analysis. The crystals are triclinic with a = 1686.2(8) pm, b = 1816(1) pm, c = 846.5(4) pm, α = 92.02(7)°, β = 92.47(9)°, γ = 63.21(5)°, space group P1̄, D(calcd) = 1.560 g/cm3, and R = 0.0286, for 6219 observed reflections with I > 3σ(I).

NTO Polymorphs

1992 ◽  
Vol 296 ◽  
Author(s):  
Kien-yin Lee ◽  
Richard Giloxdi
Keyword(s):  
Crystal Structure ◽  
Cell Density ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Monoclinic Form ◽  
Network Of Hydrogen Bonds ◽  
Air Bag ◽  
Ray Methods

AbstractNTO is an explosive of current interest. It has been evaluated as an insensitive component to replace RDX in the bomb fill, and as a major ingredient for the auto air bag system. The crystal structure of the β from of NTO has been determined by single-crystal X-ray methods. The unit cell is monoclinic, space group P21/c, with a = 9.326, b = 5.515, c = 9.107 Å, β = 100.77°. There are four molecules in the cell, density 1.878 g/cm3. Infinite extension of H-bonding in two-dimensional sheets occurs in the monoclinic form. Bond lengths and angles all have normal values.Efforts have been made to determine the crystal structure of α-NTO. However, a structure refined only to R = 17% was obtained, probably due to some kind of twinning about the crystal needle axis. The unit cell is triclinic, space group P1, with a = 5.12, b = 10.30, c = 17.9 Å, α = 106.7°, β= 97.7°, γ = 90.2°. There are eight molecules in the cell, density 1.92 g/cm3. Ribbons of NTO molecules formed by a relatively strong network of hydrogen bonds are observed. It was found that α-NTO is the stable, dominating form. A variety of techniques have been chosen to identify the two polymorphs.

Crystal data for the monoclinic form of the lanthanide molybdoperrhenates Ln(MoO4)(ReO4)

1981 ◽  
Vol 14 (6) ◽  
pp. 462-463
Author(s):  
D. Argelès ◽  
M. Quarton ◽  
J.-P. Silvestre
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Powder Diffraction Data ◽  
Space Group ◽  
Monoclinic Form ◽  
Cell Dimensions

Nd(MoO4) (ReO4) is monoclinic, space group P21/c; the cell dimensions are a = 6.169 (1), b = 9.822 (1), c = 13.139 (2) Å and β = 111.65 (1)°. The monoclinic compounds in the series Ln(MoO4) (ReO4), with Ln = Ce to Lu (Pm compound is not examined), are isotypic. Crystal parameters and powder diffraction data are given.

Irreversible single-crystal to polycrystal and reversible single-crystal to single-crystal phase transformations in cyanurates

2001 ◽  
Vol 57 (6) ◽  
pp. 791-799 ◽  
Author(s):  
Menahem Kaftory ◽  
Mark Botoshansky ◽  
Moshe Kapon ◽  
Vitaly Shteiman
Keyword(s):  
Phase Transformation ◽  
High Temperature ◽  
Low Temperature ◽  
Single Crystal ◽  
High Temperature Phase ◽  
Monoclinic Space Group ◽  
Temperature Phase ◽  
Space Group ◽  
Reversible Phase ◽  
Low Temperature Phase

4,6-Dimethoxy-3-methyldihydrotriazine-2-one (1) undergoes a single-crystal to single-crystal reversible phase transformation at 319 K. The low-temperature phase crystallizes in monoclinic space group P21/n with two crystallographically independent molecules in the asymmetric unit. The high-temperature phase is obtained by heating a single crystal of the low-temperature phase. This phase is orthorhombic, space group Pnma, with the molecules occupying a crystallographic mirror plane. The enthalpy of the transformation is 1.34 kJ mol−1. The small energy difference between the two phases and the minimal atomic movement facilitate the single-crystal to single-crystal reversible phase transformation with no destruction of the crystal lattice. On further heating, the high-temperature phase undergoes methyl rearrangement in the solid state. 2,4,6-Trimethoxy-1,3,5-triazine (3), on the other hand, undergoes an irreversible phase transformation from single-crystal to polycrystalline material at 340 K with an enthalpy of 3.9 kJ mol−1; upon further heating it melts and methyl rearrangement takes place.

Sign in / Sign up

Export Citation Format

Share Document