The preparation, characterization and X-ray structural analysis of tetrakis[1-methyl-3-(2-propyl)-2(3H)-imidazolethione]zinc(II) tetrafluoroborate and tetrakis[1-methyl-3-(1-butyl)-2(3H)- imidazolethione]zinc(II) tetrafluoroborate

Two compounds, [Zn(mipit)₄][BF₄]₂ (1) and [Zn(mnbit)₄][BF₄]₂ (2) have been synthesized and characterized via standard solid and solution state methods including single crystal X-ray crystallography (mipit: 1-methyl-3-(2-propyl)-2(3H)-imidazolethione and mnbit: 1-methyl-3-(1-butyl)-2(3H)-imidazolethione). Compound 1 crystallizes in monoclinic space group P2₁/n with a = 11.804(2) ?, b = 16.710(3) ?, c = 25.763(5) ?, γ = 90.14(3)° and Z = 4, whereas compound 2 crystallizes in tetragonal space group $${\rm I}\bar{4}$$ with a = b = 11.6517(16) ?, c= 16.820(3) ?, and Z = 2. Both complexes are high melting, colorless water soluble 2:1 electrolyte solids that state have flattened tetrahedral ZnS₄ coordination geometry. The isopropyl analog is slightly more distorted than the n-butyl analog, and the degree of distortion is not directly related to the steric bulk of the ligand.     

Crystallographic investigations of benzothiazol-2-yl-hydrazine

The title compound crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 10.842(9), b = 5.750(7), c = 12.964(6) Å, = 110.13(6), V = 758.8(11) ų and Z = 4. The final reliability index is 0.060 for 1034 observed reflections. The five-membered heterocyclic thiazole ring is coplanar with its fused benzene ring. The crystal structure is stabilized by two intermolecular N=H s N hydrogen bonded interactions.     

Crystal structure,spectroscopic investigations,and density functional studies of (Z)-2-(1H-imidazol-1-yl)-1-(3-methyl-3-mesitylcyclobutyl)ethanone oxime

The title molecule, (Z)-2-(1H-imidazol-1-yl)-1-(3-methyl-3-mesitylcyclo-butyl)ethanone oxime (C₁₉ H₂₅ N₃ O), was prepared and characterized by¹H-Nuclear magnetic resonance (NMR), ¹³C-NMR, infrared spectroscopic methods, and X-ray single-crystal determination. The compound crystallizes in the orthorhombic space group P c c n with a = 31.4660(17) Å, b = 11.2140(7) Å, and c = 10.0710(8) Å. In addition to molecular geometry from X-ray determination, vibrational frequencies and gauge, including atomic orbital, ¹H- and ¹³C-NMR chemical shift values of the title compound in the ground state, were calculated using the density functional method with the 6-31G(d) basis set. The calculated results show that the optimized geometries can well reproduce the crystal structure. Besides, the theoretical vibrational frequencies and chemical shift values show good agreement with experimental values. The predicted nonlinear optical properties of the title compound are greater than those of urea. Density functional theory calculations of molecular electrostatic potentials, frontier molecular orbitals, and thermodynamic properties of the title compound were carried out at the B3LYP/6-31G(d) level of theory.     

Crystallographic and conformational analysis of 2-methyl-3-(2-nitro-phenyl)-4-phenyl-[1,2,4]oxadiazolidin-5-one

Molecular and crystal structure of 2-methyl-3-(2-nitro-phenyl)-4-phenyl-[1,2,4]oxadiazolidin-5-one, C₁₅H₁₃N₃O₄, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 10.0313(8) Å, b = 9.0372(5) Å, c = 15.5964(14) Å, β = 96.926(7)^∘, Z = 4, D_x = 1.42 g/cm³, μ (Mo-K_α) = 0.105 mm⁻¹, and space group is P 2₁/c. The structure was solved by direct methods and refined to a final R = 0.036 for 1894 reflections with I > 4σ (I). The crystal structure is stabilized by C–H⋅sO type inter-molecular, C–H⋅sN and C–H⋅sO type intra-molecular, π–π stacking and edge to face (C–H⋅s π-ring) interactions. To enlighten conformational flexibility of the title molecule, selected two torsion angles are varied from −180^∘ to +180^∘ in every 10^∘ separetely and then molecular energy profile is calculated and construed.     

Structural and spectral study of 7-chloro-3-hydroxy-1-methyl-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepin-2-one (temazepam)mercury(II) dichloride

The synthesis and crystal and molecular structure of the title compound is reported. It belongs to the monoclinic space groupP2₁/a witha=29.3990 (20),b=7.1150 (6),c=8.3140 (9) Å,=98.060 (9)° andZ=4. The structure was refined to a finalR of 3.52% (R _w %=3.82) for 2354 observed reflections. Vibrational spectra have been recorded and discussed.     

The preparation, characterization, and X-ray structural analysis of dichlorobis[1-methyl-3-(2-propyl) -2(3H)-imidazolethione]mercury(II)

A new compound of mercury(II) chloride complexed to 1-methyl-3-(2-propyl) -2(3H)-imidazolethione (mipit) has been prepared and characterized via standard methods and X-ray crystallography. The structural significance of this study is that it shows one of the few monomeric examples of a mercury(II) chloride thione complex reported to date. The compound crystallizes in space group P2₁/c with a = 17.143(6) Å, b = 17.047(6) Å, c = 14.759(5) Å, = 105.899(5)°, V = 4148(2) ų, Z = 8. The coordination sphere is distorted tetrahedral with Hg–S bonds and Hg–Cl bond distances falling within the normally expected ranges. Bond angles ranged from 108.11(4)° to 115.51(4)° with the widest angle being observed for the S–Hg–S linkage. Ligand bond distances and angles including the C=S distance are within the normally expected values observed for this compound.     

A Unique Example of a Co-crystal of [Co(AMTTO)2(H2O)2](NO3)2 and [Co(AMTTO)2(CH3CN)2](NO3)2 (AMTTO = 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione)

A co-crystal of cobalt(II) complexes, Co(AMTTO)₂(CH₃CN)₂]²⁺(NO₃)₂. [Co(AMTTO)₂(H₂O)₂]²⁺(NO₃)₂, compound (1) was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P2₁/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R₁?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)₂(CH₃CN)₂]²⁺ and [Co(AMTTO)₂(H₂O)₂]²⁺ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

     

Crystal and molecular structures of 1-(2-carboxypropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (1) (C17H21NO4) and 1-(2-carbamoyl propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C17H22N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol containing 2-methylalanine fragment are described in this paper. The space groups and unit-cell parameters are: compound1 (C₁₇H₂₁NO₄): monoclinic, space groupP2₁/n,a=5.787(1),b=18.703(4),c=23.526(5)Å,=96.49(2)°; compound2 (C₁₇H₂₂N₂O₃): triclinic, space groupP¯1,a=8.321(1),b=10.121(1),c=10.368(1)Å,=109.49(1)°,=90.49(1)°, =103.48(1)°. The structures were solved by direct methods and refined with full matrix least-squares techniques toR indices of 0.055 and 0.049, respectively. The molecules of compound1 exist in the crystal as dual ions. The molecules of compound2 are compact and their external chain is twisted in a characteristic way (similar to that found in peptides).     

X-Ray diffraction and IR-spectroscopic studies of UO2(n-C3H7COO)2(H2O)2 and Mg(H2O)6[UO2(n-C3H7COO)3]2

Single crystals of UO₂(n-C₃H₇COO)₂(H₂O)₂ (I) and Mg(H₂O)₆[UO₂(n-C₃H₇COO)₃]₂ (II) are synthesized. Their IR-spectroscopic and X-ray diffraction studies are performed. Crystals I are monoclinic, a = 9.8124(7) Å, b = 19.2394(14) Å, c = 12.9251(11) Å, β = 122.423(1)°, space group P2₁/c, Z = 6, and R = 0.0268. Crystals II are cubic, a = 15.6935(6) Å, space group $Pa\bar 3$ , Z = 4, and R = 0.0173. The main structural units of I and II are [UO₂(C₃H₇COO)₂(H₂O)₂] molecules and [UO₂(C₃H₇COO)₃]^? anionic complexes, respectively, which belong to AB ₂ ⁰¹ M ₂ ¹ (I) and AB ₃ ⁰¹ (II) crystal chemical groups of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₇COO^?, and M ¹ = H₂O). A crystal chemical analysis of UO₂ L ₂ · nH₂O compounds, where L is a carboxylate ion, is performed.     

Crystal Structure of 4-Amino-3-(thiophen-2-ylmethyl)-1H-1,2,4-triazole-5(4H)one Monohydrate

The molecular structure of the 4-amino-3-(thiophen-2-ylmethyl)-1H-1,2,4-triazole-5(4H)one monohydrate was determined by X-ray diffraction. The compound crystallizes in the monoclinic sp. gr. C2/c with Z = 4 in the unit cell. The title compound is not planar. The dihedral angle between the thiophene and 1,2,4-triazole rings is 73.4(5)°. In the crystal structure, the molecules are connected by intermolecular N–H···O, N–H···N, O–H···O, and C–H···N type hydrogen bonds. The N–H···N and C–H···N hydrogen bonds link the molecules into infinite chains along the c axis.     

Crystal and molecular structures of 1-(2-methyloxycarbonylo-propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol hydrochloride (1) (C18H24NO4Cl) and 1-(2-methylcarbamoylpropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C18H24N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol, are reported in this paper. The space groups and unit-cell parameters are: compound1 (C₁₈H₂₄NO₄Cl), monoclinic,P2₁,a=7.215(1),b=8.591(1),c=15.017(1)Å,=95.64(1)°; compound2 (C₁₈H₂₄N₂O₃), monoclinic,P2₁/c,a=10.218(3),b=21.616(5),c=8.124(2)Å,=101.28(2)°. The structures were solved with direct methods and refined by full-matrix least-squares techniques toR indices of 0.036 and 0.066, respectively. The molecule of compound1 has an extended external chain, and thus its structure is linear, whereas the molecule of compound2 is compact, and its external chain is twisted in a characteristic way, as is the case of peptides.     

Crystal and molecular structures of 1-(2-iso butylylcarbamoyl propan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol hydrochloride (1) (C21H31N2O3Cl) and 1-(2-isobutyloxycarbonylo propan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol hydrochloride (2) (C21H30NO4Cl)

This paper shows the crystal structures of two new-adrenergic antagonists, derivatives of propranolol, which were determined with three-dimensional x-ray diffraction data. The space groups and unit-cell parameters are: compound1 (C₂₁H₃₁N₂O₃Cl) monoclinic space groupP2₁/c,a=20.523(4),b=6.909(2),c=15.950(2) Å,=105.03(1)°; compound2 (C₂₁H₃₁NO₄Cl) monoclinic space groupP2₁/c,a=6.364(2),b=36.043(8),c=10.149(1) Å,=104.48(2)°. The structures were solved with direct methods, and refined with full-matrix least-squares techniques toR indices of 0.059 and 0.067, respectively. The-CH(OH)-CH₂-NH-sections of the side chains show the conformation approximate togauche.     

Crystal and molecular structure of bis(8-phenylmenthyl) 2-(2-methyl-5-oxo-3-cyclohexen-1-yl)propandioate, C42H54O5· CH3CN

The X-ray crystal structure of the title compound, as crystallized from acetonitrile-water was determined. The relative stereochemistry of the cyclohexenone ring with respect to the 8-phenylmenthyl esters was determined. The title compound crystallizes in the noncentrosymmetric space group P2₁, with a=8.9850(10) ?, b=15.575(3) ?, c=14.478(2) ?, β=94.61(2)°, and D _calc=1.118 g cm⁻³ for Z=2.     

Crystal and molecular structure of di(1-pyrazolyl)methane,CH2(C3N2H3)2

The title compound consists of two planar pyrazolyl fragments oriented at 73.0° to each other and linked to a common carbon atom. All hydrogen atoms were located unambiguously and their positions were refined.     

Synthesis and crystal structures of two potential gem-di(pyrazolyl)cycloalkane ligands, 1,1-di(pyrazol-1-yl)cyclohexane [C6H10(C3N2H3)2] and 1,1-di(pyrazol-1-yl)cyclopentane [C5H8(C3N2H3)2]

The species 1,1-di(pyrazol-1-yl)cyclohexane, C₁₂H₁₆N₄, crystallizes in the monoclinic space group P2₁/c with a = 8.340(2), b = 14.281(5), c = 10.153(3) Å, = 106.86(2)°, and Z = 4. The cyclohexane moiety has the chair conformation. The congener, 1,1-di(pyrazol-1-yl)cyclopentane, C₁₁H₁₄N₄, while not isomorphous, also crystallizes in space group P2₁/c with a = 14.350(2), b = 6.776(1), c = 11.043(2) Å, = 100.68(1)°, and Z = 4. The cyclopentane ring has a conformation in which four carbon atoms are essentially coplanar, while the fifth (that with the two pyrazolyl substituents) lies 0.63 Å from this plane, resulting in a bend of 41.3° across the C(2)···C(5) vector. The hydrogen atoms in each structure were located directly and their coordinates refined.     

Crystal and molecular structure of 1-(2-isopropylcarbamoylpropan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol (C20H28N2O3)

The crystal structure of the title compound has been determined with three-dimensional MoK X-ray diffraction data. The space group and unit-cell parameters are:P2₁/c,a=8.610(3) Å,b=13.516(5) Å,c=16.818(5) Å,=94.95(3)° andV=1950.0(7) ų. The structure was solved by direct methods, and refined by full-matrix least-squares techniques toR=0.0608 andR _w=0.0648. The compound is a derivative of the popular-adrenolytic propranolol, and in the propanol part of the side chain shows the typicalgauche conformation.     

Crystal and molecular structure of (2–3-η-2-Butyne-1,4-diol)-bis-(triphenylphosphan)-nickel(O) Ni{[(C6H5)3P]2 (C4H6O2)}

The crystal and molecular structure of (2–3-η-2-Butyne-1,4-diol)-bis-(triphenylphosphan)-nickel(O) has been determined by X-ray structure analysis. It crystallizes in the tetragonal space group 14 with the cell parameters a = b = 22.277(3), and c = 15.118 (4) Å. The structure was solved by the heavy atom method and refined to R = 0.0716. The coordination geometry about the nickel atom is trigonal-planar. Each molecule is hydrogen bonded to two neighbours. The result is an eight-membered oxygen ring.     

Determination of the crystal and molecular structure of 1,4-bis(p-chlorobenzoyl)-5-methylene-7-methyl-2,3,4,5-tetrahydro-1H-1,4-diazepine

The crystal and molecular structure of 1,4-bis(p-chlorobenzoyl)-5-methylene-7-methyl-2,3,4,5-tetrahydro-1H-1,4-diazepine has been determined by X-ray methods. The crystals are triclinic,P¯1,a = 10.605,b = 13.054,c = 7.351 Å, = 94.24, = 101.53, = 101.55 °,Z = 2. The structure was solved by direct methods, and refined by full-matrix least squares toR = 5.6% on 3495 observed reflections. The structure is of the enamide form with diacylation on nitrogen. There are no abnormal bond lengths or intermolecular contacts.