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The crystal structure of sodium tricyanomethanide Na[C(CN)3] has been confirmed by Rietveld refinement of X-ray powder diffraction data. Additionally, Raman and IR spectra of the title compound have been recorded exhibiting spectra in good agreement with those of other tricyanomethanides. Despite Na[C(CN)3] and K[C(CN)3] crystallizing both in the triclinic space group P 1 ‾ $\overline{1}$ (no. 2), with seemingly similar unit cell parameters, it is demonstrated that they are clearly not isotypic compounds. [ABSTRACT FROM AUTHOR]

The title compound, [Co(NCS)2(C6H7NO)]n or Co(NCS)2(2-methylpyridine N-oxide), was prepared by the reaction of Co(NCS)2 and 2-methylpyridine N-oxide in methanol. All crystals obtained by this procedure show reticular pseudo-merohedric twinning, but after recrystallization, one crystal was found that had a minor component with only a very few overlapping reflections. The asymmetric unit consists of one CoII cation, two thiocyanate anions and one 2-methylpyridine N-oxide coligand in general positions. The CoII cations are octahedrally coordinated by two O-bonding 2-methylpyridine N-oxide ligands, as well as two S- and two N-bonding thiocyanate anions, and are connected via μ-1,3(N,S)-bridging thiocyanate anions into chains that are linked by μ-1,1(O,O) bridging coligands into layers. No pronounced directional intermolecular interactions are observed between the layers. The 2-methylpyridine coligand is disordered over two orientations and was refined using a split model with restraints. Powder X-ray diffraction (PXRD) indicates that a pure sample was obtained and IR spectroscopy confirms that bridging thiocyanate anions are present. Thermogravimetry and differential thermoanalysis (TG-DTA) shows one poorly resolved mass loss in the TG curve that is accompanied by an exothermic and an endothermic signal in the DTA curve, which indicate the decomposition of the 2-methylpyridine N-oxide coligands.

The reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions and four 3-cyanopyridine ligands. The complexes are arranged in columns along the crystallographic c-axis direction and are linked by weak C—H...N interactions. In 2, the asymmetric unit consists of one iron cation on a center of inversion as well as one thiocyanate anion, one 3-cyanopyridine ligand, one water ligand and one 3-cyanopyridine solvate molecule in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions, two cyanopyridine ligands and two water ligands. O—H...N and C—H...S hydrogen bonding is observed between the water ligands and the solvent 3-cyanopyridine molecules. In the crystal structure, alternating layers of the iron complexes and the solvated 3-cyanopyridine molecules are observed. Powder X-ray (PXRD) investigations reveal that both compounds were obtained as pure phases and from IR spectroscopic measurements conclusions on the coordination mode of the thiocanate anions and the cyanogroup were made. Thermogravimetric (TG) and differential thermoanalysis (DTA) of 1 indicate the formation of a compound with the composition {[Fe(NCS)2]3(C6H4N2)4}n that is isotypic to the corresponding Cd compound already reported in the literature. TG/DTA of 2 show several mass losses. The first mass loss corresponds to the removal of the two water ligands leading to the formation of 1, which transforms into {[Fe(NCS)2]3(C6H4N2)4}n, upon further heating.

The title compound, [Co(NCS)2(C6H7NO)]n or Co(NCS)2(2-methylpyridine Noxide), was prepared by the reaction of Co(NCS)2 and 2-methylpyridine Noxide in methanol. All crystals obtained by this procedure show reticular pseudo-merohedric twinning, but after recrystallization, one crystal was found that had a minor component with only a very few overlapping reflections. The asymmetric unit consists of one CoII cation, two thiocyanate anions and one 2-methylpyridine N-oxide coligand in general positions. The CoII cations are octahedrally coordinated by two O-bonding 2-methylpyridine N-oxide ligands, as well as two S- and two N-bonding thiocyanate anions, and are connected via μ-1,3(N,S)-bridging thiocyanate anions into chains that are linked by μ-1,1(O, O) bridging coligands into layers. No pronounced directional intermolecular interactions are observed between the layers. The 2-methylpyridine coligand is disordered over two orientations and was refined using a split model with restraints. Powder X-ray diffraction (PXRD) indicates that a pure sample was obtained and IR spectroscopy confirms that bridging thiocyanate anions are present. Thermogravimetry and differential thermoanalysis (TG-DTA) shows one poorly resolved mass loss in the TG curve that is accompanied by an exothermic and an endothermic signal in the DTA curve, which indicate the decomposition of the 2-methylpyridine N-oxide coligands. [ABSTRACT FROM AUTHOR]

Herein, the Hirshfeld surfaces analysis of the crystalline methylone hydrochloride was performed in order to analyze NH⋯Cl, CH⋯Cl, and CH⋯O intermolecular interactions and study the formation of the NН2+–Cl− salt fragment in methylone hydrochloride crystal. There are two isomeric dimers with parallel and side-by-side orientation extracted from the crystal packing to model the IR spectrum of the crystalline methylone hydrochloride within the framework of density functional theory (DFT) and B3LYP/6-31G(d,p) method. We have assigned and interpreted all observed IR bands in the experimental spectrum of the 3,4-methylenedioxymethcathinone hydrochloride standard crystal sample that is important for forensic-medical examination. It was shown that intermolecular interactions between the NН2+ and Cl− ionic moieties occur in crystalline samples that confirm the presence of the ionized form of the methylone hydrochloride compound with the NН2+Cl− fragment. [ABSTRACT FROM AUTHOR]

Natisite, a natural tetragonal (P4/nmm) modification of Na2TiSiO5 = Na2TiO(SiO4) is an abundant indicator mineral of relatively low-temperature (no higher than 300–350°C) peralkaline (hyperagpaitic) hydrothermal assemblages in the Lovozero and Khibiny alkaline plutons, Kola Peninsula, Russia. The proportion of natisite in hypersodic (with Na K) hydrothermal veins in Lovozero and in the hydrothermally altered zones of potassium-rich pegmatites in Khibiny is up to 30 and 10 vol %, respectively; i.e., natisite can be a rock-forming mineral and the major Ti concentrator in the rock. In Lovozero, natisite is a primary mineral crystallized from hydrothermal solution, whereas in Khibiny, natisite is secondary: it predominantly occurs as pseudomorphs after earlier Ti minerals, namely, ilmenite, titanite, aenigmatite, lamprophyllite and rinkite. The chemical composition of natisite is rather stable, close to Na2TiSiO5. A very bright blue to bluish white fluorescence in shortwave ultraviolet light (λ = 245 nm) is an important identification feature of natisite. The crystal structure of natisite was first solved for a natural sample (Mt. Rasvumchorr, Khibiny), R1 = 1.97%. A comparative study of natisite and other titanosilicates with tetragonal pyramids TiO5 revealed a distinct negative correlation between the length of an essentially covalent Ti–O bond in the titanyl group and the frequency of its stretching vibrations in the IR spectrum. [ABSTRACT FROM AUTHOR]

Mononuclear and dinuclear dioxidomolybdenum(VI) complexes of an aroylhydrazone are prepared and their experimental results are correlated by theoretical studies [Display omitted] Four dioxidomolybdenum(VI) complexes, [MoO 2 (L)] 2 ·H 2 O (1), [MoO 2 (L)(py)] (2), [MoO 2 (L)(3-pic)]·H 2 O (3) and [MoO 2 (L)(4-pic)] (4) of a dibasic tridentate ONO donor aroylhydrazone, H 2 L (where H 2 L = 3-methoxy-2-hydroxybenzaldehyde-2-furoic acid hydrazone) have been synthesized and well characterized. The stoichiometric reaction of aroylhydrazone with MoO 2 (acac) 2 in methanolic medium yielded phenoxobridged binuclear complex 1 whereas monomeric complexes, 2 , 3 and 4 were formed as a result of incorporating different monodentate heterocyclic bases. The tridentate aroylhydrazone coordinates to the MoO 2 2+ core through phenolate oxygen, azomethine nitrogen and iminolate oxygen atoms. Single crystal XRD studies established the coordination geometry of mononuclear dioxidomolybdenum(VI) complexes as distorted octahedron. The crystal structures and various solid state interactions were also investigated here. DFT investigations were conducted to explore the reactivity parameters of the studied aroylhydrazone and complexes. Furthermore, molecular docking analyses unveiled the superior putative binding energy of the investigated compounds in contrast to cisplatin. These findings were particularly pronounced in relation to the selected target proteins, which are indicative of their potential efficacy against lung and breast cancer cell lines. [ABSTRACT FROM AUTHOR]

The chemical composition, crystal structure, and infrared (IR) spectrum of a hydrated CO3-bearing analog of manganoeudialyte from alkali pegmatites of the Konder pluton (Khabarovsk krai) are studied. The chemical composition of the mineral corresponds to the formula N[Na6.94H2O5.13(Y,REE)0.58. Pb0.31K0.28Ba0.08]13.32M1[Ca5.09Sr0.89]5.98M2[Mn1.523+Ti0.21Mg0.04Fe0.033+Al0.02]1.82M3(Si1.16Nb0.47)1.63 M4(Si)0.50. Z[Zr3.04Hf0.03]3.07(Si3O9)2(Si9O27)2(CO3)0.28 X[(H2O)4.45OH0.04Cl0.03]4.52. The IR spectrum contains the following lines (s, strong; sh, shoulder): 455s, 475s, 655, 740s, 925s, 977s, 1010s, 1145, 1420sh, 1504, 1650, 2970sh, 3240sh, 3480 cm-1. The crystal structure is refined in the R3¯m spatial group, a = 14.243(3), c = 30.371(6) Å, and V = 5336(2) Å for 1393 independent reflections (|Fo| > 4σF with a similarity factor R1 of 6.5%. The deficit in Na and Cl, the presence of Pb and Ba, and the high degree of hydration of the mineral indicates postcrystallization ion-exchange processes typical of hydrothermal alteration of aegirine-albite rocks of the Konder pluton. [ABSTRACT FROM AUTHOR]

The title complex Cd/4-(phosphonomethyl) benzoic acid 4-HOOCC6H14CH2PO3(H3BCP) with 1,10-phenanthroline has been hydrothermally synthesized directly as [Cd3(BCP)2(phen)]·H2O 1 (phen = 1,10-phenanthroline). The crystal structure was determined by single-crystal X-ray diffraction with the following data: triclinic P-1. The complex is a two-dimensional layer structure. Interestingly, the one-dimensional cluster chain is composed of the novel repeated La4 cluster units connected by two Cd3 ions. The adjacent cluster chains link to be 2D layer structure by the coordination interaction of oxygen atoms of the carboxyl with the Cd3 ions of the adjacent chains. It is worthy of mentioning that IR, photo-luminescent and solid UV-Vis spectrum are employed in order to explore the structural characteristics. [ABSTRACT FROM AUTHOR]

The structure of levofloxacinium 2-thiobarbiturate trihydrate LevoH2+Htba-·3H2O (I) (LevoH is levofloxacin, H2tba is 2-thiobarbituric acid) is determined (CIF file CCDC No. 1547466); its thermal decomposition and IR spectrum are studied. The crystals of I are triclinic: a = 8.670(1) Å, b = 9.605(1) Å, c = 15.786(2) Å, α = 89.144(5)°, β = 88.279(5)°, γ = 76.068(5)°, V = 1275.4(3) Å3, space group P1, Z = 2. The unit cell of I contains two LevoH2+ ions, two Htba- ions, and six H2O molecules. The absolute structure of the crystal and the configuration of the chiral center in a levofloxacin molecule S are determined. Experiments for generating the second optical harmonics gave a positive result. Intermolecular hydrogen bonds (HBs) N-H···O and O-H···O in I form a bilayer system along the ab diagonal with hydrophilic moieties within a layer and hydrophobic moieties directed outward. The structure is stabilized by multiple HBs and the π-π interaction between the Htba-and LevoH2+ ions and between the LevoH2+ ions. [ABSTRACT FROM AUTHOR]

The complex (2,2′‐biquinoline‐κ2N,N′)(carbamoylcyanonitrosomethanide‐κ2N,O)chloridocopper(II) acetonitrile monosolvate, [Cu(C3H2N3O2)Cl(C18H12N2)]·CH3CN or [Cu(ccnm)Cl(biq)]·acn (acn is acetonitrile, biq is 2,2′‐biquinoline and ccnm is carbamoylcyanonitrosomethanide), (I), was prepared as a result of nucleophilic addition of water to the dicyanonitrosomethanide ion in the presence of CuII and biq. IR spectroscopy confirmed the presence of ccnm, biq and acn in (I). The solid‐state structure consists of the neutral complex containing ccnm and biq ligands, coordinated to the CuII atom in a bidendate chelating manner, and a chloride ligand, resulting in a distorted tetragonal pyramidal coordination of CuII. The asymmetric unit is supplemented by one molecule of solvated acn which, along with the nitrile group of ccnm, serves as an acceptor in intermolecular hydrogen bonding, creating infinite chains along the b axis. Magnetic measurements revealed a paramagnetic behaviour with a very small Weiss temperature Θ = −0.32 K and high anisotropy of the g tensor (gx = 2.036, gy = 2.120 and gz = 2.205). [ABSTRACT FROM AUTHOR]

Agardite-(Ce) from Clara Mine, Schwarzwald, Germany, has been investigated by means of electron microprobe analysis, single-crystal X-ray analysis, XANES spectroscopy and IR spectroscopy. Hexagonal unit-cell parameters are: a = 13.598(6), c = 5.954(3) Å; V = 953.5(2) Å3; space group P63/m. The structure has been solved and refined to final R1 = 3.87%, wR2 = 5.02 for 786 I > 3σ(I). Hydrogen atoms have been localized. The crystal-chemical formula is (Z = 2): A(1)(Ce0.82Ca0.14Sr0.04)Σ1.00A(2)(Ca0.03Ce0.02)Σ0.05 [Cu5.75(Fe3+, Mn)0.20]Σ5.95 [T(1)(AsO4)2.96T(2)(SbO4)0.04)]Σ3.00 (OH)5.96O0.04·3H2O. Hydrogen bonding in agardite-series minerals has been characterized for the first time. IR spectra of agardite-(Ce) and agardite-(Nd) from Lavrion used for comparison, as well as structural data indicate the presence of isolated H+ cations that do not form strong covalent bonds with coordinating O atoms. Agardite-(Ce) from Clara Mine forms epitaxial growths with the Sb-analogue of auriacusite. The latter mineral was characterized by EDS analyses; its typical empirical formulae are Ca0.06Ce0.04Fe3+1.06Cu0.89[(SbO4)0.58(AsO4)0.38(SiO4)0.04]Σ1.00(O,OH) and Ca0.075Ce0.04Fe3+0.93Cu0.97[(SbO4)0.59(AsO4)0.35(SiO4)0.06]Σ1.00(O,OH). The formation of uniaxial growths of the Sb-analogue of auriacusite and agardite-(Ce) is caused by the close values of their c parameters (for auriacusite s.s. c  =  5.9501(5) Å). Three-valence state of iron and five-valence of antimony in both minerals has been validated by means of Fe K- and Sb L2,3-edge XANES spectroscopy. [ABSTRACT FROM AUTHOR]

Crystal structure of orthorhombic γ-CdC 2 O 4 (sp.gr. Pmna , a = 7.3217(1), b = 6.0231(1), c = 9.2545(2) Å, V = 408.12(1) Å 3 , Z = 8, D x = 3.262 Μg·m −3 ) was solved from the powder diffraction pattern. Each metal atom in the structure is co-ordinated by seven oxygen atoms which belong to five oxalate-ions. Crystal packing containing the noticeable cavities in the [101] and [001] directions is not close and essentially differs from the known disordered α- and ordered β-modifications of transition metal oxalates. This modification seems to be meta-stable. It was found that spontaneous γ→β phase transition takes place for the γ-CdC 2 O 4 aged during 6 month in air. This transition may be accelerated via the heating of γ-CdC 2 O 4 with excessive amounts of oxalic acid. [ABSTRACT FROM AUTHOR]

FTIR spectroscopy is a powerful method to analyse materials and especially fiber structure. This technique is largely used to obtain quick information on the fiber composition and to detect possible transformations after physical and chemical treatments. Unlike other techniques, FTIR is a quick method which demands a reduced amount of fibers. Furthermore, it is a non destructive method especially for Attenuated Total Reflectance (ATR), and Near Infrared (NIR) spectroscopy which are nowadays widely used. In this work, FTIR spectrum of agave fiber has been thoroughly investigated. Because of its complexity, the spectrum was separated into two regions: CH and hydrogen bond stretching (>2500 cm −1 ) and “fingerprint” region (<2000 cm −1 ). A detailed study of intermolecular and intramolecular chains was made. Infrared ratios (Lateral Order Index, Total Crystallinity Index, and Hydrogen Bond Intensity) were used to study the crystallinity and the degree of regularity of agave fiber. [ABSTRACT FROM AUTHOR]

The structure (CIF file CCDC No. 1401886) of the hexaaqua- hexakis(2-thiobarbiturato)-disamarium [Sm(HO)(HTBA)] polymeric complex ( I), where HТВА is 2-thiobarbituric acid, is determined; its thermal decomposition and IR spectrum are studied. The crystals of I are monoclinic: a = 14.072(1) Å, b = 10.0842(6) Å, c = 15.323(1) Å, β = 110.408(2)°, V = 2037.9(2) Å, space group P2/ n, Z = 2. All three independent thiobarbiturate anions HTBA coordinate to Sm through oxygen atoms. To one of independent Sm ions six (two terminal and four bridging) HTBA ions and two water molecules are coordinated; the second is bonded with four bridging HTBA and four water molecules, forming square antiprisms. The bridging HТВА-anions arrange antiprisms in layers. The structure is stabilized by hydrogen bonds and a π-π interaction between the HТВА ions. The topology of the polymer network of I is analyzed. [ABSTRACT FROM AUTHOR]

Crystals of Hg2[N(CN)2]2 were grown by a slow diffusion-reaction between aqueous Hg2(NO3)2·2H2O and Na[N(CN)2]. Hg2[N(CN)2]2 adopts the triclinic space group P 1 ¯ (no. 2) with a = 3.7089(5), b = 6.4098(6), c = 8.150(6) Å, α = 81.575(6)°, β = 80.379(7)°, γ = 80.195(7)°, and Z = 1. Crystals of Tl[N(CN)2] were obtained from the reaction of TlBr with Ag[N(CN)2] in water. Single-crystal structure analyses evidence that Tl[N(CN)2] is isotypic to α-K[N(CN)2] and adopts the orthorhombic space group Pbcm (no. 57) with a = 8.5770(17), b = 6.4756(13), c = 7.2306(14) Å, and Z = 4. Regarding volume chemistry, the dicyanamide anion occupies ca. 44 cm3·mol−1, and so it corresponds to a large pseudohalide. The IR spectra of both compounds exhibit vibrational modes that are characteristic of the dicyanamide anion.

The reactions of 2,2'-pyridyl, (2-Py)C(O)C(O)(2-Py), with the Cd(II) compounds under various conditions are studied. The medium and nature of the anions exert a decisive effect on the compositions and structures of the formed cadmium complexes. The reaction of cadmium diacetate with 2,2'-pyridyl in an aqueous-alcohol medium in air affords coordination compound [Cd(Рic)(HO)] · HO ( I) (Pic is picolinate ion, COCHN), and its crystal structure is determined. The crystals are monoclinic: space group P2/ c, a = 7.499(1), b = 15.676(1), с = 12.719(1) Å, β = 94.79(1)°, V = 1490.0(2) Å3, Z = 4, ρ = 1.502 g/cm. The molecular packing of compound I is a supramolecular 3D framework consisting of discrete complexes [Cd(Pic)(HO)] linked by hydrogen bonds O-H...O. The coordination sphere of Cd contains two O atoms and two N atoms of the ligand and two water molecules. The coordination polyhedron of Cd is a distorted octahedron. [ABSTRACT FROM AUTHOR]

Lead and copper(I) chloride arsenite was found in the ancient metallurgic slag from the Vrissaki area, Lavrion district, Attikí Peninsula, Greece. Its chemical composition corresponds to the idealized formula Pb6Cu+(AsO3)2Cl7. The IR spectrum shows the presence of AsO33- anions and only a trace amount of O-H bonds. The crystal structure was solved by direct methods and refined to R(F) = 0.0304 based on 1778 unique reflections with I > 2σ(I). The compound is trigonal (rhombohedral), R¯3, a = 9.8691(2), c = 34.2028(13) Å, V = 2885.01(14) Å3, Z = 6. Two crystallographically nonequivalent As3+ cations occupy apexes of the AsO3 pyramids. Cu+ cation occupies an apex of the CuCl3 pyramid. The group [Cl3Cu-AsO3] is arranged along the c axis. Pb cations occupy two sites with seven- and eight-fold coordination. The crystal-chemical formula of the compound is Pb6(Cu+Cl3)(As3+O3)2Cl4. [ABSTRACT FROM AUTHOR]

Abstract: A crystal structure redetermination of the L-tryptophan picrate crystal previously studied by Ishida et al. (Chem. Pharm. Bull. 41 (1993) 433–438) showed that it comprises L-tryptophan L-tryptophanium dimeric cation, one picrate anion and picric acid. The O⋯O distance of the O–H⋯O hydrogen bond in the dimeric cation is equal to 2.470(6)Å. The infrared spectrum of the crystal was registered and analyzed. The infrared spectrum of the crystals contains a broad absorption band centered at ca. 1170cm−1, which is assigned to the stretching vibration of the O–H bond. [Copyright &y& Elsevier]

Abstract: Li3NaBaB6O12 was synthesized by high temperature solution method. It crystallizes in trigonal space group (No. 148) with lattice constants a = 9.462(9) Å, c = 18.71(3) Å, Z = 6. The crystal structure of Li3NaBaB6O12 is a three-dimensional (3D) network composed of the isolated twelve-membered cyclic B12O24 groups interconnected by NaO6, LiO4 and BaO9 polyhedra. Functional groups in the sample were identified by IR spectrum. Li3NaBaB6O12 exhibits a short UV cutoff edge below 190 nm. Band structures and density of states were calculated. [Copyright &y& Elsevier]

A one-dimensional cross-like chain coordination polymer, {[Zn2(4,4'-bipy)2(SO4)3(H2O)5][Zn(H2O)6]}n (1) (4,4'-bipy = 4,4'-bipyridine), has been prepared and characterized by infrared (IR) spectroscopy, elemental analysis, and single-crystal x-ray diffraction. The fluorescence properties of the polymer have also been determined. [ABSTRACT FROM AUTHOR]

Abstract: First mixed-ligand polyoxometalate complex of neptunium, K10.5H0.5[Np(BW11O39)(W5O18)]·15H2O, has been synthesized. Its structure has been determined using X-ray diffractometry and confirmed by electron and IR absorption spectroscopy. The structure consists of [Np(BW11O39)(W5O18)]11− anions, potassium cations and water molecules. The overall symmetry of the [Np(BW11O39)(W5O18)]11− anion can be approximated as C s . Two tetradentate ligands, [W5O18]6− and [BW11O39]9−, are connected to an Np atom through lacunary O atoms, so that a square antiprismatic surrounding of Np is formed. [Copyright &y& Elsevier]

Polymeric {[Cu( phen)][Pt(CN)]} compound ( phen = 1,10-phenanthroline) has been prepared under hydrothermal conditions using CuSO · 5HO, phen and K[Pt(CN)] · 3HO, and characterized by chemical analysis and IR spectroscopy. The X-ray structure analysis [ C2/ c, a = 6.6057(7), b = 19.747(2), c = 11.5891(13) Å, β = 91.723(10)°] has revealed that the coordination geometry of the Cu(II) atom, situated on a two-fold rotation axis, is tetragonally distorted octahedral. Two nitrogen donor atoms originate from one blocking phen ligand, chelate coordinated in the equatorial plane at the distance of 2.026(4) Å (2×). The remaining four coordination sites are occupied by the nitrogen atoms [Cu-N = 1.975(5) (2×) and 2.574(5) Å (2×)] of two pairs symmetrically related bridging cyanido groups. These link Cu(II) with Pt(II) atoms, which lie on symmetry centers and are coordinated by four C-bonded cyanido ligands in the square planar form. Thus infinite 2D wave-like net is formed in the ac plane stabilized by π-π interactions between the phen molecules. Graphical Abstract: Polymeric {[Cu( phen)][Pt(CN)]} ( phen = 1,10-phenanthroline) compound creates a wave-like 2D structural network stabilized by π-π interactions between the phen molecules.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

A novel metal-organic framework based on 6-methylpyridine-2,4-dicarboxylic acid N-oxide (MPDCO) ligand, [Co(MPDCO)(bix)(HO)] (bix = 1,4-bis(imidazol-1-ylmethyl)-benzene), has been prepared and structurally characterized. Single crystal X-ray analysis shows that it crystallizes in the monoclinic space group of P2/ n with four independent lattice parameters a = 10.269(2) Å, b = 10.462(2) Å, c = 15.875(4) Å, and β = 107.657(4)°, and it has four independent molecules in the unit cell ( Z = 4). A one-dimensional (1-D) helical chain was formed through the MPDCO spacer and Co centers along the a-axis. Then, these 1-D chains were further interconnected by the bidentate ligand bix to afford an infinite puckered 2-D herringbone framework with (6,3) topology. And a 3-D supramolecular network was formed through the strong intermolecular hydrogen bonds. Graphical Abstract: A two-dimensional Co(II) metal-organic framework constructed from the mixed ligands 6-methylpyridine-2,4-dicarboxylic acid N-oxide (MPDCO) and 1,4-bis(imidazol-1-ylmethyl)-benzene (bix) was synthesized and characterized.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

(1,10-Phenanthroline)bis(4-morpholinecarbodithioato-S,S')zinc(II), [Zn(mdtc)2(1,10-phen)] (1) and (2,2' -bipyridine)bis(4-morpholinecarbodithioato-S,S') zinc(II), [Zn(mdtc)2(bipy)] (2) adducts were prepared, and the crystal structure of 2 is reported. The Zn-S distances in 2 are longer than those in [Zn(dtc)2](dtc = dithiocarbamate) complexes. The acceptance of an additional neutral ligand by the tetrahedral dithiocarbamato complex of zinc to form an octahedral adduct causes an increase in the Zn-S bond lengths and a consequent lowering of the S-Zn-S bite angle. The cyclic voltammetric study on the complexes shows an increase of electron density on the central metal ion in the adducts compared to Zn(mdtc)2. The use of HMDE as a working electrode in the CV studies indicate the involvement of Hg in complex formation, which is otherwise absent with a platinum working electrode. The thioureide C-N distance of 1.330 (4) Å in compound 2 is in line with the νC-N observed at 1465 cm-1. [ABSTRACT FROM AUTHOR]

Two coordination polymers, [Cd2Cl2(1,3-BDC)(TTBT)(H2O)] (1) and [CdCl(1,4-HBDC)(TTBT)] (2) (1,3-BDC = 1,3-benzenedicarboxylate, 1,4-BDC = 1,4-benzenedicarboxylate, and TTBT = 10,11,12,13-tetrahydro-4,5,9,14-tetraaza-benzo[b]triphenylene), have been prepared under hydrothermal conditions and characterized by elemental analyses, IR spectra, thermal gravimetry (TG), fluorescence emission and single crystal X-ray diffraction analyses. The crystal structures were determined by X-ray diffraction and refined by full-matrix least-squares methods to R = 0.0621 and wR = 0.1543 using 4937 reflections with I > 2σ(I) for 1; and R = 0.0525 and wR = 0.1427 using 3386 reflections with I > 2σ(I) for 2. Compound 1 possesses a chiral chain structure. Adjacent chiral chains are further linked through π-π interactions between TTBT ligands to give a three-dimensional supramolecular architecture. Compound 2 displays a helical chain structure, with neighboring chains stacked by π-π interactions, generating an unusual three-dimensional supramolecular structure. [ABSTRACT FROM AUTHOR]

The copper(II) compound, (1), [Cu2(L)2(Cl)2] · 2(C3H7NO), C22H28Cl2Cu2N6O4 [where HL = 1H-benzimidazol-2-yl-methanol, C3H7NO = N,N'-dimethylformamide(DMF)], crystallizes in the triclinic space group [image omitted] with a = 8.363(2) Å, b = 8.866(2) Å, c = 9.327(3) Å, α = 91.415(5), β = 93.924(5), γ = 109.318(4)° and Z = 1; R1 for 2280 observed reflections [I > 2σ(I)] was 0.0356. The centrosymmetric molecule comprises a pair of copper(II) atoms connected by two 1H-benzimidazol-2-yl-methanol ligands in syn-syn bridging mode. Four-coordination of copper(II) is further completed by chloride. The CuII-CuII distance and Cu-OR-Cu bond angle in 1 are 3.043(1) Å and 104.3(1)°, respectively. [ABSTRACT FROM AUTHOR]

Two new erbium compounds, [Er2(BDC)3(DMF)2] (1) and [Er2(CQC)3(DMF)3(H2O)] · DMF · H2O (2), where BDC stands for 1,4-benzenedicarboxylate, CQC for 2-(4-carboxyquinolin-2-yl)quinoline-4-carboxylate, and DMF for N,N-dimethylformamide, have been synthesized through pre-heating and cooling-down crystallization. In 1 the Er(III) is seven-coordinate with oxygen atoms from six BDC and one DMF, forming a three-dimensional open-framework structure. Compound 2 possesses a 2D structure based on dinuclear Er(III) building units. The photoluminescence of 1 has also been investigated. [ABSTRACT FROM AUTHOR]

The crystal structure of iron tris-acetylacetonate is re-determined. Crystal data at 293 K are: a = 15.4524(5) Å, b = 13.5876(4) Å, c = 16.5729(7) Å, Z = 8; at 150 K: a = 15.2541(4) Å, b = 13.4451(3) Å, c = 16.4256(5) Å, Z = 8. The structure is molecular and comprises isolated molecules. The coordination polyhderon of iron is an almost regular octahedron, Fe-O bond lengths are 1.977–2.003 Å (293 K) and 1.982–2.006 Å (150 K). In the crystalline state, the molecules are arranged in layers, and iron atoms are located on a plane yielding an almost regular trigonal net with the Fe...Fe separations of 7.558–8.103 Å (293 K) and 7.472–8.017 Å (150 K). The adjacent layer is positioned exactly over the first one with a Fe...Fe distance of 8.303 Å (293 K) and 8.236 Å (150 K). [ABSTRACT FROM AUTHOR]

Abstract: The crystal structure of [Cd(tsac)2(bzim)2]·CH3OH (tsac, anion of thiosaccharine; bzim, benzimidazole) has been determined by single crystal X-ray diffractometry. It crystallizes in the triclinic space group with Z =2. The Cd(II) cation is in a distorted tetrahedral environment coordinated to two thiosaccharinate anions [Cd–S bond lengths of 2.5117(6) and 2.5598(6)Å] and two benzimidazole molecules [Cd–N lengths of 2.235(2) and 2.256(2)Å]. The FTIR spectrum of the complex is also recorded and briefly discussed. Some comparisons with related complexes are made. [Copyright &y& Elsevier]

A representative of uranyl tungstates Cs2U2WO10 has been synthesized. A single crystal X-ray diffraction experiment has been performed for the compound prepared and its crystal structure has been solved. It is monoclinic, space group P21/ n, a = 8.4611(5) Å, b = 28.691(2) Å, c = 9.6499(6) Å; β = 107.073(1)°, R 1 = 0.086 for 4599 independent reflections with I > 2σ( I). The crystalline structure of the compound is formed by infinite negatively charged layers [U2WO10] interleaved with cesium cations which bond the layers. The compound has been studied with IR spectroscopy, and absorption bands of its spectrum have been assigned. [ABSTRACT FROM AUTHOR]

A representative of uranyl tungstates Cs2U2WO10 has been synthesized. A single crystal X-ray diffraction experiment has been performed for the compound prepared and its crystal structure has been solved. It is monoclinic, space group P21/ n, a = 8.4611(5) Å, b = 28.691(2) Å, c = 9.6499(6) Å; β = 107.073(1)°, R 1 = 0.086 for 4599 independent reflections with I > 2σ( I). The crystalline structure of the compound is formed by infinite negatively charged layers [U2WO10] interleaved with cesium cations which bond the layers. The compound has been studied with IR spectroscopy, and absorption bands of its spectrum have been assigned. [ABSTRACT FROM AUTHOR]

This paper presents a structural and vibrational study of a new compound, namely, monohydrate 1,5-pentanediammonium hydrogen sulfate (NH3(CH2)5NH3(HSO4)2·H2O). The X-ray crystal structure shows that this compound crystallizes in the monoclinic system, space group P21/c, with the lattice parameters a=9.2250(2) Å, b=7.7540(4) Å, c=20.8520(1) Å, β=116.23(3)°, V=1337.97(10) Å3, and Z=4. From the structural investigations, it is found that the studied compound is built by infinite anionic ribbons parallel to the “a” axis. These ribbons form tunnels in which organic cations are inserted. Infrared (IR) spectrum of the compound in the 300–4000 cm-1 spectral region is reported. A tentative assignment of the observed bands, supported by a molecular orbital semi-empirical calculation, is given. [Copyright &y& Elsevier]

The molecular structure of [Cu(sulfadimet)2]·SO(CH3)2 (sulfadimet=sulfadimethoxine=4-p-aminobenzenesulfonamido-2,6-dimethoxypyrimidine) was determined by single crystal X-ray diffractometry. It crystallizes in the monoclinic space group P21/c with Z=4. The Cu(II) cation is in a distorted CuN5 square pyramidal coordination, involving four sulfadimethoxine molecules, one of them acting as a bidentate ligand. The infrared spectrum is briefly discussed on the basis of the structural peculiarities of the complex. [Copyright &y& Elsevier]

The NH∙∙∙Cl, CH∙∙∙Cl and π∙∙∙π interactions play an important role in the cooperative way of the 4-chloroethylcathinone (4-CEC) hydrochloride crystal architecture. [Display omitted] • Crystalline 4-chloroethylcathinone (4-CEC) hydrochloride was studied by DFT method. • The NH∙∙∙Cl, CH∙∙∙Cl and π∙∙∙π interactions are important in 4-CEC crystallization. • HS analysis approves the formation of the NH 2 +–Cl– salt fragment in the 4-CEC crystal. • All IR bands are assigned in the experimental spectrum of 4-CEC crystal sample. • The presence of NH 2 +Cl– fragment is a key condition for reproduction of IR spectrum. This paper represents a Hirshfeld surfaces analysis of crystalline 4-chloroethylcathinone (4-CEC) hydrochloride and a quantum chemical study of the IR spectrum of 4-CEC dimer, which models the crystalline structure of 4-CEC within the framework of density functional theory (DFT) with B3LYP functional and 6-31G(d,p) basis set. The Hirshfeld surfaces analysis of 4-CEC X-ray crystal structure reveals that NH∙∙∙Cl, CH∙∙∙Cl and π∙∙∙π interactions play a major role in the cooperative way of crystal architecture securing and approves the formation of the NH 2 +–Cl– salt fragment in the 4-CEC crystal. The same structural trends are supported by the Bader's QTAIM analysis of density gradients and critical points. The DFT calculated infrared spectrum of the investigated psychotropic substance contains absorption features, which correspond to the frequency and relative intensity of the experimental IR bands of the 4-CEC standard sample. All IR bands being assigned and interpreted in the experimental spectrum of the 4-CEC standard crystal sample represent an important aspect of analytical chemistry in the forensic problems. It is shown that the presence of the ionized form of the 4-CEC compound, which contains the NH 2 +Cl– fragment, is a key condition for the correct reproduction of the IR spectrum when calculating the dimer structure as a model of a crystalline sample. The unravel of the complicated nature of the IR bands associated with vibration of the NH 2 +Cl– fragment is an important achievement of the present study. [ABSTRACT FROM AUTHOR]

The crystal structure of synthetic monohydrocalcite was solved with Patterson and Fourier syntheses and refined for the subcell with á=6.0931 (9) Å, ć=7.5446 (18) Å, space group P321 or P321, Z=3 to R=0.039. Very weak superstructure reflections define a cell with $$a = a' \cdot \sqrt 3 $$ and c=ć, space group P3 or P3, Z=9. The superstructure result from ordering of the CO groups and was refined with rigid carbonate groups to R=0.086. The interpretation of the IR spectrum is in agreement with the results of the X-ray structure analysis. [ABSTRACT FROM AUTHOR]

Abstract: A novel Cu(II) coordination polymer, [Cu(ox)(DMSO)2] n (1) (ox-oxalate dianion, DMSO-dimethyl sulphoxide) has been prepared in the reaction of copper nitrate dihydrate and allantoin (5-ureidohydantoin) in DMSO/water solution. Compound (1) crystallizes in the monoclinic, space group P121/c1 with a =5.1785(7), b =13.6311(18), c =8.5386(12)Å, β =107.524(12)°, V =574,76(14)Å3, Z =4, D cal =1779mg/m3, R 1 =0.0449. The metal ion coordinates through four oxygen atoms belonging to two bidentate bridging oxalate ligands, and two oxygen atoms from two DMSO ligands forming an elongated octahedron. The crystal structure was confirmed by FT-IR and Uv–vis spectroscopic data. [Copyright &y& Elsevier]

Abstract: As a result of Np(V) glycolate reaction with 2,2′-bipyridyl, the novel coordination polymer [NpO2(C2O3H3)(Bipy)]·2.5H2O was formed. The structure consists of infinite chains of [NpO2(C2O3H3)(Bipy)] and water molecules. The crystal structure is confirmed by IR and UV–vis spectroscopic data. This complex is the first example of An glycolate with neutral molecular ligand. [Copyright &y& Elsevier]

Abstract: The reaction of Np(V) methanesulfonate solution with imidazole led to the in situ formation of oxalic acid and the reduction of Np(V) to Np(IV). As a result, the novel organically templated organic polymer, (ImidazoleH)[Np(C2O4)(CH3SO3)3(H2O)2], was formed. The structure consists of infinite chains of [Np(C2O4)(CH3SO3)3(H2O)2]− and imidazolium cations. The crystal structure is confirmed by IR and UV–vis spectroscopic data. This complex is the first example of structurally characterized 1:1 An(IV) oxalate. [Copyright &y& Elsevier]

Initially, the quaternary nitride iodide LiLa 4 N 2 I 7 was synthesized at 600 °C by a partial metathesis reaction of lithium nitride (Li 3 N) and lanthanum triiodide (LaI 3) within 7 days. Single-phase samples were obtained through annealing of the corresponding binary compounds (LiI, LaN and LaI 3) for 20 days overall (4 days at 600 °C prior to 16 days at 500 °C). The title compound crystallizes in the orthorhombic space group Pnma with four formula units per unit cell (a = 1374.17(9), b = 1213.45(8), c = 1079.91(7) pm at 100 K). The dominating structural features are trans -edge shared [NLa 4 ]9+ tetrahedra building up { [ NLa 4 / 2 e ] 3 + } ∞ 1 chains running along [010]. The linkage of these chains via iodide anions leads to a three-dimensional framework, which embeds isolated trigonal bipyramids [LiI 4+1 ]4– with one long besides four short Li+–I– contacts. Infrared spectra of crystalline samples show four main bands between 300 and 600 cm−1, which can probably be assigned as vibrational modes of the condensed [NLa 4 ]9+ tetrahedra. 7Li-MAS NMR spectroscopy reveals a different coordination sphere of Li+ in rocksalt-type LiI than in LiLa 4 N 2 I 7 , but no significant lithium-cation mobility. Image 1 • Single-phase material obtained by metathesis reaction. • Li-MAS NMR spectroscopy for derivation of Li-ion conduction. • Temperature-depending crystal structure analysis. [ABSTRACT FROM AUTHOR]

Crystals of Hg2[N(CN)2]2 were grown by a slow diffusion-reaction between aqueous Hg2(NO3)2·2H2O and Na[N(CN)2]. Hg2[N(CN)2]2 adopts the triclinic space group P 1 ¯ (no. 2) with a = 3.7089(5), b = 6.4098(6), c = 8.150(6) Å, α = 81.575(6)°, β = 80.379(7)°, γ = 80.195(7)°, and Z = 1. Crystals of Tl[N(CN)2] were obtained from the reaction of TlBr with Ag[N(CN)2] in water. Single-crystal structure analyses evidence that Tl[N(CN)2] is isotypic to α-K[N(CN)2] and adopts the orthorhombic space group Pbcm (no. 57) with a = 8.5770(17), b = 6.4756(13), c = 7.2306(14) Å, and Z = 4. Regarding volume chemistry, the dicyanamide anion occupies ca. 44 cm3·mol−1, and so it corresponds to a large pseudohalide. The IR spectra of both compounds exhibit vibrational modes that are characteristic of the dicyanamide anion. [ABSTRACT FROM AUTHOR]