Peri Interactions in Naphthalene Diketones: A Preference for (Z,Z) Conformations

The crystal structures of 1,8-dibenzoylnaphthalene (9), 1,4,5,8-tetrabenzoylnaphthalene (10), and 1,8-diacetylnaphthalene (11) have been determined by X-ray diffraction. Diketone 9 crystallizes in triclinic space group P ^—1 with a = 7.924(2), b = 14.068(3), c = 7.876(1) Å, = 99.47(2), = 90.58(1), = 91.43(2)°. Tetraketone 10 crystallizes in monoclinic space group P2₁/c a = 7.374(4), b = 11.960(5), c = 15.524(5) Å, = 93.15(5)°. Diketone 11 crystallizes in orthorhombic space group Pbca a = 6.986(3), b = 15.946(4), c = 8.257(1) Å. Each of these naphthalene ketones adopt a (Z,Z) conformation, with torsion angles O—C—C¹—C^8a/O—C—C⁸—C^8a of 49.8°/44.5° (9), 52.1°/46.6° (10), and 44.8°/42.4° (11). The structures 9–11 are overcrowded with the distances between two neighboring carbonyl carbon atoms being significantly shorter than the sum of the van der Waals radii of two carbon atoms (342 pm): 293.4 pm (9), 281.6 pm (10), and 293.0 pm (11).     

Crystal and Molecular Structures of (Dibenzo-18-Crown-6)(Nitrato-O,O")-Tetrahydrofuranpotassium, [K(DB18C6)(THF)(NO3)]

The (dibenzo-18-crown-6)(nitrato-O,O")tetrahydrofuranpotassium complex [K(DB18C6)(THF)(NO₃)] (I) was synthesized and studied using X-ray diffraction analysis. The crystals are orthorhombic: a= 9.608 Å, b= 9.926 Å, c= 27.234 Å, Z= 4, space group P2₁2₁2₁. The structure was solved by the direct method and refined by the least-squares method in the anisotropic approximation to R= 0.099 over all 2620 measured independent reflections (CAD4 automated diffractometer, MoK radiation). Complex Iin the crystal exists as individual host–guest molecules, the K⁺cation (CN 9) being located in the DB18C6 macrocycle cavity and being coordinated to its six oxygen atoms and to two oxygen atoms of the nitrato ligand on one side of the macrocycle and to the THF oxygen atoms on the other side. The DB18C6 molecule in Ihas a butterfly conformation with approximate C _2V symmetry.     

Pinched-cone Calix[6]arene: New Synthesis of p- (1,1,3,3-tetramethylbutyl)calix[6]arene. Structure of its 1 : 3 Complex with Chloroform

A new method is described for the synthesis of p-(1,1,3,3-tetramethylbutyl)calix[6]arene isolated ina 30 % yield. For the first time the crystal structure isgiven. The crystals are monoclinic, space group C2/c,a = 24.144(5) Å, b = 14.093(3) Å,c = 26.972(5) Å, = 93.36(3)^circ, V = 9162(3) ų, Z = 4. The macrocycle with C2symmetry presents the pinched-cone conformation. It crystallizes with three chloroform molecules, two of them are positioned in the cones shaped by the phenol moieties; the third chloroform is located in the cavity near the hydroxyl groups; this solvent molecule is disordered around the 2 axis. The packing of the complex is described.     

Crystal Structures of 1,3-Calix[4]-bis-crown-6·3CH3CN and 1,3-Calix[4]-bis-(benzo-crown-6)·3 CH3CN

The crystal structures of a new solvate of the ditopic receptor 1,3-calix[4]-bis-crown-6, Bis-C6, and of 1,3-calix[4]-bis-(benzo-crown-6), Bis-benzoC6, are reported. Bis-C6.3 CH3CN (1) crystallizes in the monoclinic space group P21/n, a = 14.388(3), b = 26.947(8), c = 14.707(4) Å, = 113.19(3)°, V = 5241(5) Å3, Z = 4. Refinement led to a final conventional R value of 0.092 for 2723 reflections. The structure of (1) differs from the previously reported structure of Bis-C6.4 CH3CN by the conformation of one crown either chain. Two acetonitrile molecules are in the close neighbourhood of the crown ether cavities. Bis-benzoC6.3 CH3CN (2) crystallizes in the monoclinic space group P21/c, a = 10.391(4), b = 17.264(11), c = 30.426(9) Å, = 94.62(3)°, V = 5440(7) Å3, Z = 4. Refinement led to a final conventional R value of 0.106 for 2965 reflections. Two acetonitrile molecules are located near the crown ether cavities, as in (1). One of the crown ether conformations is the same as in the binuclear caesium complex of Bis-benzoC6, supporting the hypothesis of a preorganization of this ligand towards the complexation of this ion; the second crown ether chain is partially disordered.     

Investigation of the local structure of nanosized CdS crystals stabilized with glutathione by the radial distribution function method

For stabilized nanoparticles of cadmium sulfide, a highly resolved radial distribution function was derived from the dispersion curve of synchrotron radiation ( = 0.08824 Å). The nanoparticle core has dimensions of 15 Å–20 Å and consists of Cd and S atoms in a 1:1 ratio. In the inner part of the nanoparticle, these atoms have a random tetrahedral coordination similar to that in crystalline CdS. Half of all core S atoms belong to the ligands and are coordinated by the surface Cd atoms. In contrast to the inner S atoms, these S atoms each binds two or three Cd atoms, forming a CdSCd bond angle of 100°, which is smaller than the tetrahedral angle. The Cd-S bond lengths are similar for both types of sulfur and vary within 2.52 Å–2.53 Å. The spatial arrangement of the Cd and S atoms beyond the first coordination sphere is significantly different from that of bulk CdS, which may be caused by perturbations induced by the surface S atoms.Original Russian Text Copyright © 2004 by V. I. Korsunskii, R. Neder, K. Hradil, J. Neuefeind, K. Barglik-Chory, and G. MüllerTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 452–461, May–June 2004.     

Ferrocene Compounds. XXVII. Synthesis and Structure of 2-(Ferrocenylmethyl)propane-1,3-diol

The title compound was obtained by reduction of diethyl (ferrocenylmethyl)malonate with lithium aluminium hydride in diethyl ether. The structure of this novel ferrocene derivative was assigned by means of elemental analysis, IR, [¹H]NMR, and [¹³C]NMR spectroscopy. The structure was also confirmed by a single crystal X-ray study. The compound crystallizes in monoclinic P2₁/a space group with unit cell dimensions: a = 9.7360(6), b = 27.040(5), c = 14.767(3) Å, = 103.835(6)°, V = 3774.8(11) ų, Z = 12. The asymmetric unit contains three crystallographically independent molecules. In the ferrocenyl moieties, the Fe–C bond distance values are in the range 2.006(5)—2.051(3) Å and C–C distances in the range 1.366(7)–1.425(4) Å. The cyclopentadienyl rings in each of the molecules are mutually twisted by about 13° from the eclipsed conformation. The hydroxyl groups are involved in the intermolecular O–H...O hydrogen bond formation with O-O distances in the range 2.686(3)–2.801(4) Å forming infinite two-dimensional network in a [0 0 1] plane. The crystal structure is additionally stabilized by C–H-O weak intermolecular hydrogen bonds.     

Crystal Structure of N,N'-Bis(dodecyl)diaza- 18-crown-6 Complexed Sodium Perchlorate

The crystal structure of a new complex of a diaza-crown ether having two side arms has been determined from X-ray diffraction data. The compound crystallizes in space group P1 with cell dimensions a = 9.982(1), b = 10.685(1), c = 20.376(2)Å, = 81.09(1), = 80.92(1), = 88.43(1)0, Z = 2. The structure has been solved by direct methods and refined to the final R value of 0.053 for 3458 observed reflections and 424 parameters. The diaza-18-crown-6 ligand adopts an approximate D3d conformation. The Na+ ion is held inside the molecular cavity of this macroring ligand and a ClO-4 oxygen coordinates with Na+. The average Na–-O (18-crown-6) and Na–-N bond lengths are 2.426(4) and 2.786(5)Å, respectively; the Na–-O (ClO-4) bond length is 2.472(4)Å. The mean cavity radius is 1.10 Å and the NN nonbonding distance is 4.605(6)Å.     

Molecular and crystal structure of 1∶1 guest-host bis(hexafluoroacetylacetonato)calcium complex with 18-crown-6

We have carried out an X-ray structural study of the title complex (a CAD-4F diffractometer, MoK, graphite monochromator, /2 scan mode, _max, direct methods, 1465 reflections, R=0.036). Crystals are monoclinic with a=17.971(13), b=13.475(3), c=13.379(8) , =106.67(5)°, Z=4CaO₁₀C₂₂H₂₆F₁₂, space group C2/c, d _calc =1.537 g/cm³. The complex (C₂ symmetry) has a molecular structure and belongs to the guest-host type. The Ca atom is located in the center of the 18-crown-6 cavity; bidentate hexafluoroacetylacetonate guest ligands occupy the trans-positions relative to the plane of a maxidentate macrocycle. The Ca–O distances in a ten-vertex Ca polyhedron are 2.474–2.666 . The macrocycle conformation is characterized by six gauche C–C bonds and two gauche and ten trans C–O bonds. The dihedral COCC angle differs significantly (by 38.1°) from the angle of 60°, which is common to a gauche conformation. The six-membered cycle formed by oxygen atoms has a twist form with the annular O–O distances of 5.132–5.329 . Structural features explaining an easy sublimation of the compound are discussed.X-ray structural analysis and the interpretation of results.Synthesis of single crystals.Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated fromZhurnal Strukturnoi Khimii, Vol. 34, No. 6, pp. 56–65, November–December 1993.Translated by T. Yudanova     

X-ray structural investigation of gossypol and its derivatives XXIX. Molecular and crystal structure of a complex of gossypolic acid lactone with acetic acid

The lactone of gossypolic acid, obtained by the demethylation of the tetramethyl ether of gossypolic acid, forms with acetic acid a stable complex having the 14 composition. The crystallographic parameters of single crystals are as follows:a=20.251(2) Å, b=12.028(3) Å, c=15.934(4) Å, V=3881.2(2.3) ų,Z=4, D _calc=1.32 g/cm³, sp. gr. Pbcn. The molecule is characterized by considerable strain because of the formation of the five-membered lactone ring the atoms of which are coplanar with the atoms of the naphthyl fragment. Unlike the clathrates of racemic gossypol and dianilinegossypol, the gossypolic acid lactone — acetic acid comples does not belong to the type of clathrate inclusion compounds.A. S. Sadykov Institute of Bioorganic Chemistry, Academy of Sciences of the Republic of Uzbekistan, Tashkent, Ul. Akad. Kh. Abdullaeva, 83. Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 458–463, July–August, 1999.     

Synthesis,crystal structure and magnetic properties of a two-dimensional mixed-valence assembly [Fe(salen)]2[Fe(CN)5NO]

A cyanide-bridged Fe^III–Fe^II mixed-valence assembly, [Fe^III(salen)]₂[Fe^II(CN)₅NO] [salen = N,N-ethylenebis(salicylideneiminato)dianion], prepared by slow diffusion of an aqueous solution of Na₂[Fe(CN)₅NO] · 2H₂O and a MeOH solution of [Fe(salen)NO₃] in an H tube, has been characterized by X-ray structure analysis, i.r. spectra and magnetic measurements. The product assumes a two-dimensional network structure consisting of pillow-like octanuclear [—Fe^II—CN—Fe^III—NC—]₄ units with dimensions: Fe^II—C = 1.942(7) Å, C—N = 1.139(9) Å, Fe^III—N = 2.173(6) Å, Fe^II—C—N = 178.0(6)°, Fe^III—N—C = 163.4(6)°. The Fe^II—N—O bond angle is linear (180.0°). The variable temperature magnetic susceptibility, measured in the 4.8–300 K range, indicates the presence of a weak intralayer antiferromagnetic interaction and gives an Fe^III–Fe^III exchange integral of –0.033 cm^–1.     

Synthesis of R-(-)-2-ethyl-N-benzyl (benzo-monoaza-15-crown-5) and the Crystal Structure of Its Sodium Perchlorate Complex

A new complex of a chiral monoaza-crown ether, [R-(-)-2-ethyl-N-benzyl-4,7,10,13-tetraoxa-8,9-benzo-1-azacyclopentadec-8-ene...NaClO₄], has been prepared and studied by x-ray diffraction. The compound crystallizes in space group P2₁ with cell dimensions a = 8.721(1), b = 16.318(2), c = 8.905(1) Å, = 100.80(1)°. The sodium cation is heptacoordinated and located significantly out of the best plane of the macrocycle ring. The donor atoms of the macrocycle are in the half-chair arrangement.     

Crystal Structure of the Diaqua(1,10-Diaza-18-Crown-6) (Tetrafluorosuccinato-O)barium Complex

The diaqua(1,10-diaza-18-crown-6)(tetrafluorosuccinato-O)barium complex [Ba(DA18C6)(C₄F₄O₄)(H₂O)₂] (I) is synthesized and studied using X-ray diffraction analysis: space group P2₁/n, a = 16.342 Å, b = 8.989 Å, c = 17.087 Å, = 107.09°, Z = 4. The structure was solved by the direct method and refined by the full-matrix least squares method in anisotropic approximation to R = 0.075 for all 3515 unique reflections (CAD4 automated diffractometer, MoK ). Complex I exists in the crystal as individual host–guest molecules of the aforementioned composition. The Ba²⁺ cation (coordination number 9) is located in the void of the DA18C6 macrocycle and is coordinated by its six O and N heteroatoms. It is also coordinated by the O atom of the tetrafluorosuccinate ligand and the O atom of the water molecule on one side of the macrocycle and by the O atom of the second water molecule on the other macrocycle side. The DA18C6 ligand has a crown conformation with approximate D _3d symmetry. The complex molecules in the crystal are combined into infinite two-dimensional layers by intermolecular hydrogen bonds.     

Crystal structure of a dimeric nickel(II) complex with 3-imidazoline nitroxide radical

The crystal structure of an unusual dimeric Ni(II) complex with 3-imidazoline nitroxide LH=C₉H₁₄N₂O₂ of the formula Ni₂(LH)₄ has been determined. The structure is molecular, space group P2₁/c, with a=12.150(3) Å, b=11.229(3) Å, c=15.780(4) Å, =101.59(3)^o, and d _calc =1.54 g/cm³, for Z=2; V=2109(1) ų, R=0.059. In the centrosymmetric dimer, the Ni...Ni distance is 3.254(2) Å; the coordination polyhedron of Ni is a square pyramid (the coordination number is 5) formed by the donor O and N atoms of LH ligands acting as the bidentate-cyclic and bidentate bridged-cyclic structures. The Ni–O and Ni–N distances are 1.989(7) and 2.032(8) Å, respectively (for the atoms forming the pyramid base), and 2.000(8) Å to the apical N atom. The Ni atom is displaced from the base to the apex of the pyramid by 0.35 Å. The interatomic distances and the bond angles in the ligands agree with those for the previously studied M(LR)₂ complexes. The distances between the Ni(II) ions and the O O atoms inside the Ni(LH)₂ fragments are 5.39(1) and 5.45(1) Å, the intermolecular Ni...O distances exceed 6 Å, and the O...O distances are as long as 4.73(1) Å.Institute of Inorgamic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated fromZhurnal Stukturnoi Khimii, Vol. 34, No. 3, pp. 80–85, May–June 1993.Translated by T. Yudanova     

Synthesis and Structure of New Cobalt–Carbonyl Complexes Containing Tellurium Atoms

Co₂(CO)₈ and Te₂O react to form the well known Co₄(CO)₁₀Te₂, Co₄(CO)₁₁Te₂ complexes and the two new cluster complexes CCo₆(CO)₁₂Te₂(1), and CCo₆(CO)₁₀Te₂(Te₃) (2). The structures of 1 and 2 were determined by X-ray analysis, together with the triphenylphosphine derivative of 1, CCo₆(CO)₁₁(PPh₃)Te₂(3), which was analyzed to clarify the disordered structure of the parent compound. Complex 1 is formed by a prismatic cluster of cobalt atoms with a carbon embedded in the cage; two tellurium atoms cap the triangular faces of the prism and each cobalt atom links two terminal carbonyl groups. The complex 2 has a similar prismatic cage CCo₆; two ₄-Te atoms cap two rectangular faces of the prism, while other two Te atoms bridge two edges of the triangular faces and are linked each other through a third Te atom. Electron counting gives for complex 2 92 electrons: the presence of two long Co–Co distances suggests that the two excess electrons are located on Co–Co antibonding orbitals. Crystal data for 1, space group C2/c, a = 12.845(2) Å, b = 13.449(2) Å, c = 13.246(2) Å, = 91.95(2)°, Z = 4, R = 0.097 for 2555 reflections; for 2, space group Pnna, a = 17.219(5) Å, b= 14.969(6) Å, c = 9.178(4) Å, Z = 4,R = 0.037 for 3103 reflections; for 3, space group P2₁/c, a = 9.288(2) Å, b = 14.920(6) Å, c = 26.300(9) Å, = 99.99(2)°, Z = 4, R = 0.037 for 4300 reflections. The vibrational analysis of the complex 1 was performed and most of the (CO), (₆C–Co), (Co–Co) and (Co–Co) modes were assigned. The (Co–Te) modes were interpreted on the basis of the intermolecular coupling, due to the close contact between neighboring clusters in one distinct direction in the crystal.     

Structural and spectroscopic characteristics of α-cyano-substituted α-phosphoryl(thiophosphoryl)acetonates in neutral chelate-bridged complexes. Crystal structure of [Cu[(PrO)2P(O)C(CN)C(Me)O]2]

A comparative study of the three-dimensional and electronic structures of the chelate salts (ML _n ) of enol forms of -cyano-substituted -phosphoryl- and -(thiophosphoryl)acetones (RO)₂P(X)C(CN)C=CMe(OH) (X = O or S; R = Pr or Et) with the Cu^I, Cu^II, and Co^II cations was carried out. In all complexes under consideration, the geometry of the central moiety of the O—C(Me)—C(CN)—P chelate-bridging ligand remains unchanged. The substantial electron delocalization involving the cyano group is observed in the O—C—C(CN)—P(X) ligand framework. The structure of the bis-chelate Cu[(PrO)₂P(O)C(CN)C(O)Me]₂ complex was established by X-ray diffraction analysis at 180 K and vibrational (IR and Raman) spectroscopy. The study in the temperature range from 290 to 140 K revealed the phase transition at 200 K accompanied by a change in the coordination polyhedron about the copper cation from a symmetrical octahedron (4+2 coordination) to a strongly unsymmetrically distorted octahedron (4+1+1 coordination). In both crystal modifications, four oxygen atoms form the base of the octahedron, and the axial positions are occupied by the nitrogen atoms.     

Crown Ether-Dinitrile Interaction: An X-ray Study

Formation of the host-guest compounds between isomers of dicyclohexano-18-crown-6 as hosts (DC18C6) and various dinitriles as guests has been observed. The structures of two representative compounds (cis-anti-cis-DC18C6...2(NCCH2CH2CN) ( I) and (cis-syn-cis-DC18C6...(NCCH2CH2CH2CN) ( II) were obtained using X-ray diffractometry. Crystal data: ( I) P=¯1, a = 8.586(3), b = 9.324(3), c = 10.714(4) Å = 72.47(3)°, = 73.57(3)°, = 72.37(3), R1 = 0.034, GooF 1.08, Z = 1; ( II) Pbca, a = 12.881(5), b = 17.887(8), c = 23.042(13) Å, R1 = 0.049, GooF 1.02, Z = 8. Both structures show weak C–-H...O interactions between -methylene protons of dinitrile guest molecules and oxygen atoms of the macrocyclic host ring.     

A Chiral Coordination Polymer of Silver(I) with Saccharinate and Pyridine: Synthesis,Spectral, Thermal,and Structural Characterization of [Ag(sac)(py)]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript>

The first silver(I) complex of saccharinate (sac) with pyridine (py), [Ag(sac)(py)]_n has been synthesized and characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffractometry. The complex crystallizes in chiral, trigonal space group P3₁21 (No. 152) with unit cell parameters of a = 11.2605(2) Å, c = 17.3300(4) Å, V = 1903.02(6) ų and Z = 6. [Ag(sac)(py)]_n contains monomeric [Ag(sac)(py)] units linked into infinite helices by way of Ag⋅sAg interactions [d(Ag⋅sAg) = 2.909(2) and 2.985(1) Å]. The distorted square-planar environment of Ag is completed by an N-bonded sac [Ag—N = 2.084(2) Å] and a py molecule [Ag—N = 2.116(2) Å]. The N_sac—Ag—N_py angle is 173.85(10)^∘. The one-dimensional chains are crosslinked by C—H⋅sO interactions involving the carbonyl and sulfonyl O atoms of sac and aromatic-ring hydrogen atoms of both sac and py. The thermal stability of the title complex was investigated using thermogravimetry and differential thermal analysis in a static atmosphere of air. The first decomposition stage between 90 and 160^∘C corresponds to removal of the py molecule in a single stage, while the degradation of the sac moiety occurs at two stages in the temperature range 370–515^∘C, giving an end product of metallic Ag.     

Crystalline complexes of N,N'-ditritylurea (DTU) and N-tritylurea (NTU) hosts with molecular guests

This paper reports crystalline complexes of the new hosts N,N'-ditritylurea (DTU) and N-tritylurea (NTU) with various uncharged molecular guests. The crystal structures of the following complexes were elucidated by single crystal X-ray diffraction analysis at 115^oK: (I) 1:1 DTU-propanamide — space group C2/c, a=15.839Å, b=9.088Å, c=24.584Å, =111.05^o, Z=4; (II) 1:1 DTU-ethyl N-acetylglycinate — space group P1, a=9.010Å, b=10.800Å, c=19.810 Å, =105.29^o =94.33^o, =93.03^o, Z=2; (III) 2:1 NTU-N, N-dimethylformamide — space group Cc, a=29.614Å, b=8.906Å, c=16.127Å, =121.04^o, Z=4. The three crystal structures are stabilized mainly by a cooperative effect of hydrogen bonding between amide fragments displaced along the shortest axis of each crystal. This interaction occurs between host and guest in complexes I and II, and between host and host in complex III. The latter also represents a cage-type clathrate in which the guest molecules are accommodated in voids between the hydrophobic fragments of four neighboring NTU hosts. On the other hand, complexes of DTU are characterized by a more specific interaction between the two components, each guest molecule being inserted between two adjacent hosts (related by translation) and strongly bound to them via hydrogen bridges. These results illustrate a useful concept in the design of molecular species which can be potential hosts upon crystallization with neutral molecular guests. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82022 (7 pages).     

Crystal and Molecular Structure of Bis(O,O"-diisopropyldithiophosphato-S,S")(dimethylglyoximato-N,N")rhodium(III)

The crystal and molecular structure of bis(O,O"-diisopropyldithiophosphato-S,S")(dimethylglyoximato-N,N")rhodium(III) (I) was studied using X-ray diffraction analysis: space group P2₁/c, a = 13.644 Å, b = 10.350 Å, c = 20.906 Å, = 109.02°, Z = 4. The structure was solved by the direct method and anisotropically refined by the full-matrix least-squares method to R = 0.029 using 5447 independent reflections (CAD-4 autodiffractometer, MoK ). Compound I is a mononuclear tris-chelate complex whose three ligands are singly charge anions. The individual molecule of the complex has a noncrystallographic two-fold axis; its Rh atom is coordinated by four S atoms and two N atoms, forming a distorted octahedron. The average coordination bond lengths are Rh–S 2.402 and Rh–N 2.023 Å. The molecules in structureI are joined into infinite chains via weak intramolecular C–H···S hydrogen bonds and intermolecular N–O–H···O–N hydrogen bonds.     

Diaqua[N,N-di(2-carboxyethyl)-o-anisidinato]copper(II) Dihydrate [Cu(o-Andp)(H2O)2] · 2H2O: Synthesis and Crystal Structure

Crystals of [Cu(o-Andp)(H₂O)₂] · 2H₂O (where o-Andp^2–is -anisidine-N,N-di-3-propionate) were synthesized and studied using X-ray diffraction analysis. The crystals are triclinic: a= 12.063(1) Å, b= 12.483(3) Å, c= 13.586(2) Å, = 91.29(1)°, = 111.67(1)°, = 104.00(1)°, V= 1830.5(5) ų, space group P , Z= 2, and R= 0.0528 for 5965 reflections with I2(I). The two crystallographically independent complexes are isostructural. The tetragonal–bipyramidal coordination of copper(III) involves three O atoms, the N atom of the tetradentate ligand o-Andp^2–, and two O atoms from water. The aminodipropionate group of the ligand (average Cu–O 1.939 Å and Cu–N 2.051 Å) and one of the coordinated water molecules (Cu–O(w) 1.991 Å) lie in the equatorial plane. The second water molecule (Cu–O(w) 2.32 Å) and the methoxy O atom of o-Andp^2–(Cu–O 2.37 Å) are in the apical positions of the bipyramid.