Synthesis and Crystal Structure of Compound 1-Phenyl-2-(1H-1,2,4-triazolo-yl)-3-phenyl-propen-1-one and 1-Diphenyl-3-(1,2,4-triazolo-yl)-1H,4H-1,5-benzothiazepine

Abstract  

The crystal structures of the compounds 1-phenyl-2-(1H-1,2,4-triazolo-yl)-3-phenyl-propen-1-one (2), and 2,4-diphenyl-3-(1,2,4-triazolo-yl)-1H,4H-1,5-benzothiazepine (3) were obtained by single crystal X-ray diffraction. Compound 2 crystallizes in the triclinic system with space group P − 1, a = 8.5553(17) ?, b = 9.6229(19) ?, c = 9.924(2) ?, α = 106.16(3)°, β = 108.03(3)°, γ = 105.14(3)°, V = 690.1(2) ?³, Z = 2. The compound 3 crystallizes in the orthorhombic system with space group Pbca, a = 12.904(3) ?, b = 15.864(3) ?, c = 19.140(4) ?, α = 90°, β = 90°, γ = 90°, V = 3918.3(14) ?³, Z = 8. H-bonds and π–π stacking are the main non-bonding interactions in the molecular structure. Details of the synthesis, structures, and spectroscopic properties of the two compounds are discussed.     

The Synthesis and Structure of Two Novel <Emphasis Type="Italic">N</Emphasis>-(Benzothiazol-2-yl)benzamides

Abstract  Two novel benzothiazoles 2-chloro-N-(benzothiazol-2-yl)benzamide (1) and 2-chloro-N-(6-cyanobenzothiazol-2-yl)benzamide (2) were obtained in multistep synthesis. They were characterised by means of IR, ¹H- and ¹³C-NMR spectroscopy and also by single-crystal X-ray diffraction. The compound 1 crystallises with triclinic space group P , a = 9.5923(8) ?, b = 9.8583(8) ?, c = 13.8962(10) ?, α = 89.162(6)°, β = 77.741(7)°, γ = 80.064(7)°, V = 1264.5(2) ?³, Z = 4 and compound 2 crystallises as methanol solvate with monoclinic space group P 2₁/n, a = 7.5093(9) ?, b = 13.0211(14) ?, c = 16.032(2) ?, β = 92.717(10)°, V = 1565.9(3) ?³, Z = 4. Both crystal structures consist of discrete dimers connected into a three-dimensional network by intermolecular C–H···O and C–H···X (X = Cl or S) hydrogen bonds and by face-to-face π–π stacking interactions. Index Abstract  The synthesis and structure of two novel N-(benzothiazol-2-yl)benzamides. Irena Ćaleta, Dominik Cinčić, GraceKarminski-Zamola and Branko Kaitner. Hydrogen bonds and π–π interactions in N-(benzothiazol-2-yl)benzamides N-(benzothiazol-2-yl)benzamides.      

Synthesis,Crystal Structure and Thermal Properties of <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline and <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline

Abstract  

Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, ¹H-NMR, ¹³C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C₁₉H₁₈N₂O₂Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C₁₉H₁₈N₂OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions.     

Pentacarbonyl(trimethylamine)chromium and Pentacarbonyl(trimethylamine)Molybdenum

Abstract  

Pentacarbonyl(trimethylamine)chromium (1) and pentacarbonyl(trimethylamine)molybdenum (2) are isomorphous and crystallize in the space group P2₁/n, a = 6.8267(14) ?, b = 11.269(2) ?, c = 14.692(3) ?, β = 102.89(3)°, V = 1,101.8(4) ?³, Z = 4 for 1 and a = 6.949(5) ?, b = 11.362(5) ?, c = 14.927(5) ?, β = 102.639(5)°, V = 1,150.0(10) ?³, Z = 4 for 2; both compounds possess distorted octahedral molecular geometries that result from the steric influence of the coordinated amine ligand.     

An X-ray Crystallographic Study of 1,4-Di[(<Emphasis Type="Italic">E</Emphasis>)-2-(<Emphasis Type="Italic">p</Emphasis>-tolyl)-1-diazenyl]piperazine

Abstract  

The crystal structure of methyl 1,4-di[(E)-2-(p-tolyl)-1-diazenyl]piperazine (4) has been determined by single crystal X-ray diffraction analysis. The bis-triazene (4) adopts a normal chair conformation in the piperazine ring, with puckering parameters : φ₂ = −29(5)°, Q_T = 0.534(2) ? and θ₂ = 177.0(2)°. The crystal structure of 4 is compared with the structure of the triazene (2a) and the closely related bis-triazenes (3 and 5a). The piperazine ring of 2a and 4 adopt a typical chair conformation, whereas the piperazine ring of 3 adopts an unusual pseudo-boat conformation. Crystal data: 4 C₁₈H₂₂N₆, triclinic, space group P[`1] P\overline{1} , a = 6.8925(2) ?, b = 7.8574(3) ?, c = 16.8856(8) ?, α = 103.103(2)°, β = 90.528(2)°, γ = 101.776(2)° and V = 870.44 (6) ?³, for Z = 2.     

Structure of a New Bioactive Agent Containing Combined Antibacterial and Antifungal Pharmacophore Sites: 4-{[(<Emphasis Type="Italic">E</Emphasis>)-(5-Bromo-2-hydroxyphenyl)methylidene]amino}-<Emphasis Type="Italic">N</Emphasis>-(5-methyl-1,2-oxazol-3-yl)benzenesulfonamide

Abstract  

The title compound (3), C₁₇H₁₄BrN₃O₄S, is a Schiff base compound of 5-bromosalicylaldehyde (1) and sulfamethoxazole (2). The structure of (3) was determined by spectral (IR, ¹H and ¹³C NMR), elemental analyses and X-ray diffraction data. Compound (3) crystallizes in the monoclinic space group C2/c, with a = 31.936(3), b = 6.2571(5), c = 16.903(1) ?, β = 94.867(8), V = 3365.5(5) ?³, Z = 8. In the molecule of compound (3), the molecule is bent at the S atom with a C–SO₂–NH–C torsion angle of −86.3(3)°. Pairs of molecules, related by inversion centres, form intermolecular N–H···N hydrogen bonds to produce a dimer. An intramolecular phenolic O–H···N hydrogen bond is also formed. Intermolecular hydrogen bonding and π–π stacking hold the molecules together. The average distance between stacked benzene ring planes is 3.625(2) ?.     

Synthesis and Structure of bis(β-Diketiminate) Chromium(II) Complexes

Abstract  

The new ligand 2,4-N,N′-bis(napthylamino)-pent-2-ene (L^napth) (1) has been synthesized and crystallizes in space group P2₁2₁2₁ with crystal cell parameters a = 8.196(3) ?, b = 9.119(3) ?, c = 25.746(10) ?, V = 1924.3(12) ?³ and Z = 4. The complexes bis[2,4-pentane-N,N′-bis(napthyl)ketiminato] chromium(II) (2), bis[2,4-pentane-N,N′-bis(isopropylphenyl)ketiminato] chromium(II) (3), and bis[2,4-pentane-N,N′-bis(tertbutylphenyl)ketiminato] chromium(II) (4) were synthesized and structurally characterized. Complex 2, the first complex reported with a bis(napthyl) β-diketiminate ligand, crystallizes in space group P − 1 with crystal cell parameters a = 12.0824(15) ?, b = 12.2462(16) ?, c = 14.8975(19) ?, α = 87.035(2)°, β = 80.615(2)°, γ = 62.756(2)°, V = 1932.9(4) ?³ and Z = 2. Complex 3 crystallizes in space group P2₁/n with crystal cell parameters a = 13.088(3) ?, b = 22.222(5) ?, c = 14.206(3) ?, β = 102.310(4)°, V = 4036.6(17) ?³ and Z = 4. Complex 4 crystallizes in space group P2₁/n with crystal cell parameters a = 20.831(6) ?, b = 11.575(4) ?, c = 21.373(7) ?, β = 107.241(5)°, V = 4922(3) ?³ and Z = 4. The degree of twist between the ligand planes is dependent on the steric bulk of the ligand.     

Synthesis,Crystal Structure and Fluorescent Study of Bis(2-(2-hydroxyphenyl)benzimidazolate)zinc with Ethanol Solvate

Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)₂]·C₂H₅OH (1 · C₂H₅OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P2₁/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?³. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.      

Stereochemical Assignment of Substituted 2-Aminobicyclo[3.1.0]hexane and 2-Aminobicyclo[5.1.0]octane Derivatives via Single Crystal X-ray Diffraction

Abstract  

Crystals of benzyl (RS,RS,RS)-7-phenylbicyclo[5.1.0]octan-2-ylcarbamate 9 and (RS,RS,RS)-N-[3′-(4″-methylpiperazin-1″-yl)propyl]-N-{5-(4′′′-cyanophenyl)bicyclo[3.1.0]hexan-2-yl}amine dihydrochloride 10·2HCl were synthesised and single crystal X-ray diffraction was used to establish unambiguously the relative configurations within these structures. Compound 9 crystallizes in the orthorhombic space group P2 ₁ 2 ₁ 2 ₁ with cell parameters of a = 6.85340(10) ?, b = 9.8732(2) ?, c = 27.5407(6) ?, V = 1863.54(6) ?³ and Z = 4. In the crystal structure adjacent molecules are linked by N–H···O=C hydrogen bonds. Compound 10·2HCl crystallizes as the corresponding monohydrate in the monoclinic space group P2 ₁/n with cell parameters of a = 7.1540(17) ?, b = 39.763(12) ?, c = 8.163(3) ?, β = 91.062(7)°, V = 2321.7(11) ?³ and Z = 4. In the crystal structure adjacent molecules are linked by a series of hydrogen bonds between the ammonium groups, chloride ions and adventitious water molecules.     

Synthesis and Structure of (TMEDA)Cr(I)<Subscript>2</Subscript>(THF) and [(<Emphasis Type="Italic">N,N</Emphasis>-DMEDA)<Subscript>2</Subscript>CrI] I

Abstract  

The complexes (TMEDA)Cr(I)₂(THF) (1) and [(N,N-DMEDA)₂CrI] I (2) were synthesized and spectroscopically characterized (TMEDA = tetramethylethylenediamine, N,N-DMEDA = N,N dimethylethylenediamine). Complex 1 possesses square pyramidal geometry and crystallizes in spacegroup Pbca with crystal cell parameters a = 11.206(2) ?, b = 12.698(3) ?, c = 23.434(5) ?, V = 3,334.6(12) ?³ and Z = 4. Complex 2 also possesses square pyramidal geometry with a non-coordinated iodide counter anion and crystallizes in spacegroup P2₁/n with crystal cell parameters a = 9.4071(13) ?, b = 14.628(2) ?, c = 11.7516(16) ?, β = 98.904(2) ?°, V = 1,597.6(4) ?³ and Z = 4. Complex 2 has previously been incorrectly assigned as an octahedral complex based on spectroscopy.     

Synthesis,Structure, and Two Polymorphs of 4-((1,3-Dioxoisoindolin-2-yl)methyl)-1-methoxypyridinium tetrafluoroborate

Abstract  

4-((1,3-Dioxoisoindolin-2-yl)methyl)-1-methoxypyridinium tetrafluoroborate, C₁₅H₁₃BF₄N₂O₃, 1, was obtained by alkylation of the corresponding N-oxide and has been characterized by ¹H and ¹³C NMR, IR, UV spectroscopy and by X-ray crystallography. The crystal undergoes a reversible phase transition between 173 and 293 K. At room temperature, crystals are orthorhombic, space group Pna2₁ with a = 7.2487(3) ?, b = 17.8359 (8) ?, c = 12.4077(6) ?, V = 1604.16(12) ?³, and Z = 4. At 173 K, cations adopt four conformations in monoclinic space group Cc with a = 24.7076(29) ?, b = 14.4145(9) ?, c = 21.8765(25) ?, β = 126.249(17)°, V = 6283.3(7) ?³, and Z = 16. The compound is photostable in the crystal and does not undergo homolytic N–O bond cleavage as observed in solution.     

Crystal Structures of a Series of Bis{(2-Aminobenzoyl-)amino}alkanes

Abstract  The crystal structures of 1,2-bis-{(2-aminobenzoyl-)amino}ethane(1), 1,4-bis-{(2-aminobenzoyl-)amino}butane(2) and 2,2-dimethyl-1,3-bis-{(2-aminobenzoyl-)amino}-propane(3) have been determined by single crystal X-ray diffraction analysis. 1 and 2 are centrosymmetric molecules which lie on crystallographic centers of symmetry and adopt extended conformations. On the other hand, owing to the odd number of carbon atoms in the spacer unit, 3 does not show centrosymmetry, but crystallizes in a non-centrosymmetric space group and assumes a folded conformation. The crystal structures of 1, 2 and 3 are compared with the known structures of anthranilamide (7) and the N-alkyl anthranilamide derivative 8. Crystal data: 1 C₁₆H₁₈N₄O₂, monoclinic, space group P2₁/a, a = 9.5262(8) ?, b = 5.4200(5) ?, c = 15.3821(14) ?, β = 105.980(5)° and V = 763.52(12) ?³, for Z = 2. 2 C₁₈H₂₂N₄O₂, monoclinic, space group C2/c, a = 32.0710(17) ?, b = 5.4732(4) ?, c = 9.7326(5) ?, β = 102.570(4)° and V = 1667.42(17) ?³, for Z = 4. 3 C₁₉H₂₄N₄O₂, orthorhombic, space group Pca2₁, a = 16.7676(4) ?, b = 10.1847(2) ?, c = 10.5338(5) ?, and V = 1798.89(7) ?³, for Z = 4. Index Abstract  The crystal structures of 1,2-bis-{(2-aminobenzoyl-)amino}ethane(1), 1,4-bis-{(2-aminobenzoyl-)amino}butane(2) and 2,2-dimethyl-1,3-bis-{(2-aminobenzoyl-)amino}-propane(3) have been determined by single crystal X-ray diffraction analysis. 1 and 2 are centrosymmetric molecules which lie on crystallographic centers of symmetry and adopt extended conformations, whereas 3 does not show centrosymmetry, but crystallizes in a non-centrosymmetric space group and assumes a folded conformation.      

One-Dimensional Polymers Constructed with Paddle-Wheel Dinuclear Copper(II) Bridged by 4,4′-Bipyridine

Abstract  

The coordination compound {[Cu(NAP)₂](4,4′-bpy)_1/2}·DMF (1) was prepared by the reaction of α-naphthoic acid, 4,4′-bipyridine and Copper(II) acetate hydrate in basic solution, and was fully characterized by X-ray diffraction, element analysis, FTIR and TG analysis. Crystals of compound 1 belongs to the monoclinic crystal system, space group C2/c; a = 17.460(4) ?, b = 13.928(3) ?, c = 21.240(4) ?, β = 93.83(3), V = 5153.7 ?³, Z = 8. The structure analyses of 1 show a one-dimensional chain structure where the binuclear structural units [Cu₂(NAP)₄] are bridged by 4,4′-bipyridine molecules. Furthermore, the 1D chains are assembled to form 2D supramolecular sheet by intermolecular π···π stacking interactions between naphthalene rings.     

Crystal Structures of a Series of 1,1-Spiro-bis(1,2,3,4-tetrahydronaphthalene)-Based Derivatives

Abstract  

The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) ?, b = 7.5298(18) ?, c = 19.130(5) ?, β = 97.935(4)°, V = 1165.0(5) ?³, Z = 2, D = 1.210 Mg m⁻³. Compound 2 crystallized in the monoclinic P2₁/n space group with unit cell parameters a = 12.6940(9) ?, b = 7.7267(6) ?, c = 19.9754(15) ?, β = 97.220(1)°, V = 1943.7(3) ?³, Z = 4, D = 1.355 Mg m⁻³. Compound 3a crystallized in the monoclinic P2₁/c space group with unit cell parameters a = 16.8137(14) ?, b = 10.5577(9) ?, c = 31.344(3) ?, β = 103.618(1)°, V = 5407.5(8) ?³, Z = 8, D = 1.308 Mg m⁻³. Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 ?, b = 12.564 ?, c = 18.339 ?, β = 90.224(1)°, V = 3593.0 ?³, Z = 4, D = 1.236 Mg m⁻³.     

The Zolmitriptan-Pyridine (1:1) and Zolmitriptan-Propiophenone (3:2) Inclusion Complex

Abstract  

The crystal structures of zolmitriptan with pyridine (I) and propiophenone (II) solvates have been determined by single crystal X-ray diffraction studies. Compound (I) crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 8.5610(5) ?, b = 12.2709(7) ?, c = 19.6201(12) ?, V = 2061.1(2) ?³, and Z = 4, while compound (II) crystallizes in the monoclinic space group P2₁ with a = 15.085(1) ?, b = 19.656(12) ?, c = 21.0860(13) ?, β = 92.068(1)°, V = 6248(4) ?³ and Z = 4. The asymmetric unit of (I), C₁₆H₂₁N₃O₂·C₅H₅N, contains one zolmitriptan molecule and one pyridine solvate, while the asymmetric unit of (II), 3(C₁₆H₂₁N₃O₂)·2(C₉H₁₀O) comprises six zolmitriptan molecules and four propiophenone solvates. In both structures, the N–H···N hydrogen bonds, form an infinite helical chain and generate a C(11)-type motif in (I) and a D₂²(13)-type motif in (II). Both the complexes have layer structures, the layers being constructed from rings (cavity) of four zolmitriptan molecules, hydrogen bonded through N–H···N and N–H···O bonds, where the pyridine (I) and propiophenone (II) solvates are included in an R₄⁴(33) ring.     

Synthesis,Crystal Structure and IR Spectra of Complexes of Mn(II) by Indole-2-Carboxylic or Isoquinoline-1-Carboxylic Acids and 1,10-Phenanthroline

Abstract  

Two ternary complexes of manganese(II) indole-2-carboxylate (2-IC⁻) or isoquinolinecarboxylate (IQC⁻) with 1,10-phenanthroline (phen) in methanol or in dimethylacetamide (DMA) were synthesized and studied by X-ray diffraction and IR spectra. [Mn(C₉H₆NO₂)₂(C₁₂H₈N₂)₂]·CH₄O (1) crystallizes in the triclinic space group P-1 with cell parameters of a = 10.548(2) ?, b = 14.168(3) ?, c = 14.580(3) ?, α = 62.35(2)°, β = 69.16(2)°, γ = 78.61(2)°, V = 1802.4(6) ?³ and Z = 2; [Mn(C₁₀H₆NO₂)₂(C₁₂H₈N₂)].C₄H₉NO (2) crystallizes in the monoclinic space group P2₁/a with cell parameters of a = 15.304(5) ?, b = 12.871(5) ?, c = 17.421(5) ?, β = 114.39(1), V = 3125(2) ?³ and Z = 4. In 1, Mn is six-coordinate by two bidentate phen ligands and two 2-IC⁻ ligands and exhibits a very distorted octahedral geometry. This complex is solvated by methanol involved in hydrogen bonding. In 2, Mn atom is surrounded by one bidentate phen ligand and two bidentate IQC⁻ ligands. The complex exhibits a distorted octahedral geometry around the Mn^II atom. The crystal structure is completed by a disordered DMA solvate molecule. The IR spectra of both compounds are slightly different in the range 4000–2400 cm⁻¹ which may be attributed to hydrogen bond lack in 2.     

Structure and Antibacterial Activity of 3-(3,4-Dimethoxyphenyl)furan-2(5<Emphasis Type="Italic">H</Emphasis>)-ones

Abstract  

Crystalline hydrate of the title compound (5), C₁₉H₂₆N₂O₅·2(H₂O), was structurally characterized by single crystal X-ray diffraction. It crystallizes in monoclinic system space group P 21/c with a = 7.3987(7) ?, b = 17.8691(16) ?, c = 17.0022(13) ?, β = 112.944(3)°, V = 2070.0(3) ?³, Z = 4, R ₁ = 0.0592, wR ₂ = 0.1016, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with 3,4-dimethoxybenzene ring, making a dihedral angle of 0.860(69)°. Two kinds of centrosymmetric tetramers characterized by graph-set motifs of R ₇⁸(36) and R ₄⁶(32) are formed through O–H···O, O–H···N and C–H···O hydrogen bonding interactions, which generate a sheet of edge-fused rings parallel to the (011) plane. These sheets are further linked into a three dimensional network by C–H···π interactions. Nine 3-(3,4-dimethoxyphenyl)furan-2(5H)-ones were synthesized and fully characterized by elemental analysis, MS and ¹H NMR. All of them were evaluated for antimicrobial activities against three Gram-positive organisms and a Gram-negative organism, and compound 5 was the most active against Staphylococcus aureus ATCC 25923.     

Crystal Structure Studies of Two Regioisomers of Bromo-4-Aryloxymethylcoumarins

Abstract  

The 4-(2-bromo-4-methyl-phenoxymethyl)-6-methylcoumarin (1) have been synthesized from bromination of corresponding 4-aryloxymethyl coumarin, which is a regioisomer of 4-(2-bromo-4-methyl-phenoxymethyl)-7-methylcoumarin (2) (CCDC-695895). The compound 1 crystallizes with triclinic space group P-1, a = 8.0943(3) ?, b = 9.3502(3) ?, c = 10.1476(4) ?, α = 90.234(2)°, β = 94.065(2)°, γ = 95.106(2)°, Z = 2 and compound 2 crystallizes with monoclinic space group P2₁/n, a = 8.465(5) ?, b = 13.649(5) ?, c = 13.304(5) ?, α = 90.000(5)°, β = 90.740(5)°, γ = 90.000(5)°, Z = 4. Both the compounds are planar with variation in their intermolecular hydrogen bonds between C–H···O and C–H···π.     

Dihydrogen Phosphate and Hydrogen Sulphate of 1,4-Dimethyl-1,4-diazabicyclo[2.2.2]octane-1,4-diium: Crystal Structures, Hydrogen Bonding and Infrared Spectra

Abstract  

The crystal structures of the title compounds consist of 1,4-dimethyl-1,4-diazabicyclo[2.2.2]octane-1,4-diium cation [C₈H₁₈N₂]²⁺ and [H₂PO₄]⁻ or [HSO₄]⁻ anions. Both crystal structures are monoclinic, the structure of the dihydrogen phosphate (I) is non-centrosymmetric (P2₁) with a = 6.4090(2) ?, b = 13.6920(5) ?, c = 7.6140(3) ?, β = 94.620(2)°, V = 665.97(4) ?³, Z = 2; whereas the unit cell of the hydrogen sulphate (II) is centrosymmetric (P2₁/c) with a = 13.8460(2) ?, b = 12.6610(2) ?, c = 8.0360(2) ?, β = 99.5800(12)°, V = 1389.10(5) ?³, Z = 4. Both the structures are formed by the different bonding patterns of the anions interlinked by strong and moderate O–H···O hydrogen bonds. While the structure of (I) consists of a two-dimensional network of the hydrogen bonded dihydrogen phosphates, the infinite chains of the hydrogen bonded hydrogen sulphates are the basic building unit of the structure (II). In addition to the dominant electrostatic interaction the divalent cations stabilize themselves in the structures by forming several C–H···O hydrogen bonds to the oxygen atoms of the anions. The IR spectra of both the compounds are strongly affected by the hydrogen bonds whose influence on OH stretching vibrations is analysed by means of the DFT calculations in the solid state.     

Synthesis and Structure of Chromium(II) Complexes Supported by Both a β-Diketiminate and an Amidinate Ligand

Abstract  

The complexes (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ₂-diisopropylacetamidinato) chromium(II) (1) and (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ₂-dicyclohexylacetamidinato) chromium(II) (2) have been synthesized and structurally characterized. Complex 1 crystallizes in space group Pbcn with crystal cell parameters a = 10.7183(13) ?, b = 16.4093(19) ?, c = 20.687(2) ?, V = 3,638.3(7) ?³ and Z = 4. Complex 2 crystallizes in triclinic space group P-1 with crystal cell parameters a = 10.750(3) ?, b = 12.174(3) ?, c = 16.308(4) ?, α = 75.903(4)°, β = 82.137(4)°, γ = 85.511(4), V = 2,048.4(8) ?³ and Z = 2. The complexes adopt a spiro distorted square planar geometry and have similar structural parameters.