Disordered crystal structure of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane <Emphasis Type="Italic">bis</Emphasis>(picrate) hydrate

For 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis(picrate) hydrate [H₂(Crypt-222)]²⁺·2Pic^?·1.19 H₂O (I), its disordered crystal structure has been determined by X-ray diffraction (XRD) analysis. The structure of I (space group \(P\bar 1\), a = 10.662 Å, b = 12.586 Å, c = 15.342 Å, α = 107.73°, β = 102.33°, γ = 90.49°, Z = 2) was solved by direct methods and refined by full-matrix least-squares in an anisotropic approximation to R = 0.111 for all 5000 independent reflections collected (CAD-4 automatic diffractometer, CAD-4, λMoK_α). The 2.2.2-cryptand dication is disordered and has two different conformations with probabilities of 66.7% and 33.7%. In addition to one independent water molecule, the cavity of the dication has a low-probability site of another water molecule, whose occupancy is 0.19. In the two independent picrate anions, some of their NO₂ groups are disordered over two orientations. The crystal structure of I has various interionic (intermolecular) and intracation hydrogen bonds.     

Crystal and molecular structure of 2-(<Emphasis Type="Italic">o</Emphasis>-hydroxyphenyl)-4,6-diphenylpyridine

Crystal and molecular structure of 2-(o-hydroxyphenyl)-4,6-diphenylpyridine C₂₃H₁₇NO (I) has been studied by single crystal XRD. The structure (monoclinic, space group P2₁/c, a = 8.757(2) Å, b = 20.682(4) Å, c = 9.743(2) Å, β = 108.14(2)°, Z = 4) was solved by the direct method and refined anisotropically in the full-matrix approximation to R = 0.076 using all 2660 measured independent reflections (automated diffractometer CAD-4, CuK_α). OH group of the molecule of I is disordered in the crystal over three positions with occupation factors 70%, 15% and 15%. The structure contains a very strong intramolecular hydrogen bond O-H?N disordered over three directions.     

Disordered crystal structure of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane dibromide dihydrate

The disordered crystal structure of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane dibromide dihydrate, [H₂(2.2.2-Crypt)]²⁺·2Br^?2H₂O (I) was studied by X-ray diffraction (XRD) analysis. The orthorhombic structure of I (space group Aba2, a = 21.036(3) Å, b = 14.453(2) Å, c = 8.525(1) Å, Z = 4) was solved by direct methods and refined by full-matrix least squares in anisotropic approximation to R = 0.045 over all 2695 independent (taking into account anomalous scattering) reflections collected (CAD-4 automatic diffractometer, λCuK_α).     

Synthesis and crystal structure of two derivatives of benzodiazepines

Two benzodiazepine derivatives, C₂₃H₂₂N₂O (I), 2-methyl-8-methoxy-2,4-diphenyl-2,3-dihydro-1H-1,5-benzodiazepine, and C₂₂H₁₇N₃O₂Br₂ (II), 2-methyl-7-nitro-2,4-bis(4′-bromophenyl)-2,3-dihydro-1H-1,5-benzodiazepine, were studied by single crystal X-ray diffraction method. Compound (I) crystallizes in the monoclinic system, space group P2₁/c, a = 13.1703(17) Å, b = 11.1990(14) Å, c = 12.9093(16) Å, β = 107.831(2)°, V = 1812.6(3) ų, Z = 4. Compound (II) crystallizes in the monoclinic system, space group P2₁/n, a = 11.7345(12) Å, b = 12.7477(13) Å, c = 13.5965(14) Å, β = 95.221(2)°, V = 2025.4(4) ų, Z = 4. The molecules of (I) and (II) have T-shape form with the diazepine ring at the junction point. The seven membered central benzodiazepine ring in both structures adopt a twist-boat conformation. The crystal packing is stabilized by C-H…π (in I) and C-H…O (in II) interactions.     

Crystal structures of pyridine-4-aldehyde thiosemicarbazone perchlorate and trifluoromethane sulfonate

The new salts of pyridine-4-aldehyde thiosemicarbazone: perchlorate (I) and trifluoromethane sulfonate (II) HN⁺C₅H₄-CH=N-NH-C(S)-NH₂·X^? (X = ClO₄, CF₃SO₃) were synthesized and studied by IR and NMR spectroscopy and X-ray diffraction analysis. The compounds were synthesized by a reaction of pyridine-4-aldehyde thiosemicarbazone with chloric or trifluoromethane sulfonic acid, respectively. Compound I crystallized in the triclinic crystal system, space group P-1, a = 6.8691(2) Å, b = 9.5406(4) Å, c = 9.6348(4) Å, α = 78.838(1)°, β = 77.618(1)°, γ = 69.661(1)°, Z = 2. Compound II crystallized in the monoclinic crystal system, space group P2₁/c, a = 7.3149(8) Å, b = 11.9830(16) Å, c = 15.143(2) Å, β= 96.949(4)°, Z = 4. The structures are formed by hydrogen-bonded ions. Moreover, the cations are linked in “dimmers” due to the weak N-H...S hydrogen bonds.     

The crystal and molecular structure of Ni(II) complex with 1-(2-carboxyphenyl)-3-isopropyl-5-(benzimidazole-2-yl)formazane

The binuclear Ni(II) 1-(2-carboxyphenyl)-3-isopropyl-5-(benzimidazole-2-yl)formazanate (Ni₂L₂ · 2H₂O) (I) was synthesized and its crystal and molecule structures were determined by X-ray diffraction. Crystals I are triclinic: space group P \(\bar 1\), a = 7.4811(11), b = 10.8821(15), c = 11.4168(13) Å, α = 105.690(11) Å, β = 90.537(11) Å, γ = 93.166(11) Å, V = 893.2(2) ų, ρ(calcd.) = 1.581 g/cm³, Z = 1.     

Crystal structure of EuCeCuS<Subscript>3</Subscript>

The crystal structure of EuCeCuS₃, a complex sulfide synthesized for the first time, has been solved using X-ray powder diffraction data. Crystals are rhombic, space group Pnma, Ba₂MnS₃ structural type, a = 8.1023(1) Å, b = 4.0386(1) Å, c = 15.9022(2) Å, V = 520.36(1) ų, Z = 4, ρ_calcd = 5.767 g/cm³. The Eu,CeS₇ polyhedron incorporates the Eu and Ce atoms, which are randomly disordered over two crystallographic sites. The bond lengths d_Eu,Ce–S range from 2.885 to 3.044 Å.     

Synthesis,thermal analysis,IR spectrum,and crystal structure of rubidium hexanitratothorate

Rubidium hexanitratothorate was synthesized, and its crystal structure was determined by X-ray diffraction analysis: space group P2₁/n; a = 8.347(1) Å, b = 6.890(1) Å, c = 13.069(1) Å, β = 91.88(1)°, Z = 2; 1812 independent reflections, R = 0.0165.     

Crystal structure of triethylammonium dicitratoborate monohydrate

Triethylammonium dicitratoborate monohydrate (C₂H₅)₃NH[(C₆H₆O₇)₂B]·H₂O (I) was synthesized for the first time. Its crystal structure was solved from single crystal X-ray diffraction data (a = 9.7821(2) Å, b = 23.2196(4) Å, c = 10.0705(2) Å; β = 90.97(1)°; Z = 4, space group P2₁/n, 5091 reflections with R _int = 0.0219; R1 = 0.0733). The structural units of crystal I (the large dicitrato borate anion with a spirane structure, the triethylammonium cation, and the crystal water molecule) form a layered packing with a system of seven O-H...O and N-H...O hydrogen bonds.     

Crystal structure of EuLaCuS<Subscript>3</Subscript>

The crystal structure of the EuLaCuS₃complex sulfide synthesized for the first time has been solved by X-ray powder diffraction. Crystals are orthorhombic, space group Pnma, Ba₂MnS₃-type structure, a = 8.1297(3) Å, b = 4.0625(1) Å, c = 15.9810(4) Å, V = 527.80(3) ų, Z = 4, and ρ_calc = 5.669 g/cm³. The La and Eu atoms are randomly disordered over two crystallographic positions with a coordination number of 7, and the Eu(La)-S bond lengths range from 2.892(6) to 3.078(6) Å. The CuS₄ tetrahedra with Cu-S interatomic distances of 2.358(5)–2.40(1) Å form chains running along the b axis.     

Synthesis and crystal structures of cobalt(III) and zinc(II) complexes derived from 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol with urease inhibitory activity

A new mononuclear cobalt(III) complex, [CoL₂(N₃)]₂ · CH₃OH (I), and a new mononuclear zinc(II) complex, [ZnLCl(CH₃OH)] (II) (HL = 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol), were prepared and structurally characterized by elemental analyses, infrared spectroscopy, and single- crystal X-ray diffraction. The crystal of I is monoclinic: space group P2₁/c, a = 18.742(2) Å, b = 15.197(2) Å, c = 25.646(2) Å, β = 125.996(3)°, V = 5909.8(11) ų, Z = 4. The crystal of II is monoclinic: space group P2₁/c, a = 7.257(1) Å, b = 24.707(2) Å, c = 9.637(1) Å, β = 101.557(2)°, V = 1692.9(3) ų, Z = 4. The Co atom in I is in an octahedral coordination, and the Zn atom in II is in a trigonal-bipyramidal coordination. The urease inhibitory test shows that complex I has strong urease inhibitory activity, while complex II has no activity.     

Structural investigation of [Au(en)<Subscript>2</Subscript>]Cl(ReO<Subscript>4</Subscript>)<Subscript>2</Subscript> and [Au(en)<Subscript>2</Subscript>](ReO<Subscript>4</Subscript>)<Subscript>3</Subscript> complexes

Novel complex salts [Au(en)₂]Cl(ReO₄)₂ (I) and [Au(en)₂](ReO₄)₃ (II), en = ethylenediamine, are obtained. Their crystal structures are determined by single crystal X-ray diffraction. Complex I crystallizes in the triclinic crystal system: a = 6.2172(7) Å, b = 7.1644(8) Å, c = 8.8829(8) Å, α = 96.605(4)°, β = 110.000(4)°, γ = 97.802(4)°, P-1 space group, Z = 1, d _x = 3.905 g/cm³; complex II crystallizes in the monoclinic crystal system: a = 15.244(2) Å, b = 7.6809(8) Å, c = 9.3476(12) Å, β = 127.004(3)°, C2 space group, Z = 4, d _x = 4.057 g/cm³.     

Crystal structure of (ethoxycarbonylmethyl)triphenylphosphonium tetrafluoroborate

The crystal structure of (ethoxycarbonylmethyl)triphenylphosphonium tetrafluoroborate, Ph₃P⁺CH₂C(O)OEt · BF ₄ ^? (space group P2₁/n, a = 12.727 Å, b = 13.983 Å, c = 12.833 Å, β = 108.83°, Z = 4) is studied by single-crystal X-ray diffraction. The structure was solved by a direct method and refined by full-matrix least squares in the anisotropic approximation to R = 0.056 by 3200 independent reflections (CAD-4 automated diffractometer, λMoK _α). In the phosphonium cation the P atom has a distorted tetrahedral coordination and the P-C-C=O torsion angle is 14.3°. The tetrahedral anion is slightly disordered over two orientations with site occupancies for all atoms of 0.875 and 0.125. The crystal contains unusual interionic hydrogen bonds of the P⁺-C-H…F-B^? type.     

Crystal and molecular structure of (±)-2-[(1<Emphasis Type="Italic">S</Emphasis>,3<Emphasis Type="Italic">S</Emphasis>)-3-acetyl-2,2-dimethylcyclobutyl]-N-(<Emphasis Type="Italic">p</Emphasis>-tolyl)acetamide

The structure of (±)-2-[(1S,3S)-3-acetyl-2,2-dimethylcyclobutyl]-N-(p-tolyl)acetamide has been determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, space group P-1, a = 8.8700(18) Å, b = 10.331(2) Å, c = 10.363(2) Å, α = 71.11(3)°, β = 65.06(3)°, γ = 72.18(3)°, V = 798.6(3) ų, Z = 2, formula unit C₁₇H₂₃NO₂. The title compound has a fragment of 2,2-dimethylcyclo-butane and its conformation represents semi-chair. The intermolecular hydrogen bonds N-H...O and C-H...O are revealed.     

New polymorph of CaHPO<Subscript>4</Subscript> (monetite): synthesis and crystal structure

A novel form of anhydrous dicalcium phosphate CaHPO₄ (monetite) is synthesized hydrothermally and characterized by single crystal X-ray diffraction. It crystallizes in the orthorhombic space group Ccm2₁ with a = 6.242(1) Å, b = 6.994(2) Å, c = 7.003(3) Å, V = 305.73(16) ų and it has four independent unit formulas in the unit cell (Z = 4). A three-dimensional crystal structure can be described by {HPO₄}_n infinite zigzag chains linked by Ca–O bonds. The comparison to the crystal structures of other polymorphs is given.     

Crystal structures of EuLnCuS<Subscript>3</Subscript> (Ln = Nd and Sm)

The compound sulfides EuLnCuS₃ (Ln = Nd and Sm) were obtained for the first time. Their crystal structures were determined from X-ray powder diffraction data. The crystals of both compounds are orthorhombic (space group Pnma). The compound EuNdCuS₃ is isostructural with BaLaCuS₃; the unit cell parameters are a = 11.0438(2) Å, b = 4.0660(1) Å, c = 11.4149(4) Å. The compound EuSmCuS₃ is isostructural with Eu₂CuS₃; the unit cell parameters are a = 10.4202(2) Å, b = 3.9701(1) Å, c = 12.8022(2) Å.     

<Emphasis Type="Italic">N,N</Emphasis>-diethylanilinium complex with borodicitric acid: Synthesis and crystal structure

N,N-Diethylanilinium dicitratoborate [C₆H₅NH(C₂H₅)₂][(C₆H₆O₇)₂B] (I) has been synthesized for the first time. Single crystals has been synthesized in an aqueous solution to study the crystal structure of complex I by single-crystal X-ray diffraction. Crystals are triclinic, space group Р1 a = 9.6183(2) Å, b = 10.3153(3) Å, c = 13.7364(4) Å, α = 69.0304(12)°, β = 77.0394(13)°, γ = 89.5518(10)°, V = 1236.25(6) ų, Z = 2, ρ_calcd = 1.454 g/cm³. Structural units in a crystal of complex I are large complex dicitratoborate anions with a spirane structure and N,N-diethylanilinium cations. The crystal packing is a three-dimensional framework implemented via a system of hydrogen bonds like О–Н…О, О–Н…О, ОI, and N–Н…О.     

High-symmetry polymorph of anhydrous disodium hydrogen phosphate

A new Na₂HPO₄ polymorph was prepared with space group Fddd, Z = 8, a = 5.8426(3) Å, b = 9.7908(5) Å, c = 12.2673(5) Å. The crystal structure includes PO₄ tetrahedra and Na atoms, each surrounded by six O atoms positioned in the corners of a heavily distorted octahedron. The proton is equiprobably disordered over the O atoms.     

Crystal structure of EuLnAgS<Subscript>3</Subscript> (Ln = Gd and Ho) compounds

The crystal structures of the first prepared EuLnAgS₃ (Ln = Gd and Ho) compounds, which have two polymorphs, were determined by X-ray powder diffraction. α-EuLnAgS₃ phases are isostructural to BaErAgS₃ (monoclinic crystal system, space group C2/m): a = 17.3168(10) Å, b = 3.9683(2) Å, c = 8.3174(4) Å, β = 103.94° (EuGdCuS₃); a = 17.1729(12) Å, b = 3.9367(3) Å, c = 8.2905(6) Å, β = 103.9° (EuHoCuS₃). β-EuLnAgS₃ phases belong to the AgBiS₂ structure type (cubic crystal system, space group Fm-3m): a = 5.739(2) Å (EuGdCuS₃) and a = 5.678 Å (EuHoCuS₃). In the α-EuLnAgS₃ crystal structure, LnS₆ octahedra and AgS₅ trigonal bipyramids share edges to form a three-dimensional (3D) structure with channels accommodating Eu²⁺ ions. A decrease in Ln³⁺ ionic radius gives rise to the crystal-chemical contraction of the 3D structure.     

Synthesis and crystal structures of two silver(I) complexes derived from 2-amino-6-methylpyridine with nicotinic acid and isonicotinic acid

The reaction of Ag₂O and 2-amino-6-methylpyridine (AMP) with nicotinic acid (HNA) and isonicotinic acid (HINA), respectively, afforded two silver(I) complexes, [Ag₂(NA)₂(AMP)₂] _n (I) and [Ag₂(INA)₂(AMP)₂] _n (II). Both complexes were characterized by elemental analyses and X-ray single-crystal diffraction. Complex I is a pyridine-3-carboxylate bridged polynuclear silver(I) complex, in which the Ag atom is in a tetrahedral geometry, while complex II is a pyridine-4-carboxylate bridged polynuclear silver(I) complex, in which the Ag atom is in a distorted T-shaped geometry. The crystal of I is monoclinic: space group P2₁/c, a = 8.079(2), b = 17.150(3), c = 8.912(2) Å, β = 98.106(2)°, V = 1222.5(5) ų, Z = 4. The crystal of II is monoclinic: space group P2₁/c, a = 7.225(1), b = 12.049(1), c = 15.053(2) Å, β = 102.050(1)°, V = 1281.6(3) ų, Z = 4.