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The title compound, diaqua-1[kappa]O,3[kappa]O-di-[mu]-hydroxido-1:2[kappa]2O:O,2:3[kappa]2O:O-di-[mu]-methacrylato-1:2[kappa]2O:O',2:3[kappa]2O:O'-bis­(1,10-phenanthroline)-1[kappa]2N,N';3[kappa]2N,N'-tricopper(II) dinitrate dihydrate, [Cu3(C4H5O2)2(OH)2(C12H8N2)2(H2O)2](NO3)2·2H2O, has the central Cu atom on an inversion centre. The three CuII atoms are in a linear arrangement linked by meth­acrylate and hydroxide groups. The coordination environments of the CuII ions are five-coordinated distorted square-pyramidal for the outer Cu atoms and four-coordinated square-planar for the central Cu atom. All nitrate ions, hydroxide groups and water mol­ecules are linked by hydrogen bonds, forming a linear structure. The complex exhibits ferromagnetic exchange coupling, which is helpful in elucidating magnetic inter­actions between copper ions and other metallic ions in heteronuclear complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108005349/sf3070sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108005349/sf3070Isup2.hkl
Contains datablock I

CCDC reference: 686419

Comment top

Molecular magnetic compounds have recently attracted attention and have been developed to a large extent (Miller & Drillon, 2001a,b, 2002; Bruda et al., 2006; Narasimha et al., 2006). In particular, ferromagnetic exchange coupling in the mixed bridged unit CuII–RO/RCO2–CuII leads to a quartet ground state for the trinuclear system (Haase & Gehring, 1985). Because various ligands show different abilities for mediating electronic effects between copper ions, these coordination compounds display rich magnetic behaviour over various temperature ranges (Rao et al., 2004; Setifi et al., 2006; Chen et al., 2006; Das et al., 2006; Tao et al., 2006). Efforts to obtain new compounds in which rare earth ions are coupled magnetically to transition metal ions and/or organic radicals are increasing rapidly (Mishra et al., 2005; Mori et al., 2005, 2006; Costes, Dahan & Wernsdorfer, 2006; Costes, Auchel et al., 2006; Murugesu et al., 2006; Yeung et al., 2006). However, it is difficult to clarify what contributes most to the magnetic interaction between rare earth and transition metal ions, because a change in magnetic properties depends on many factors.

In recent years, we have pursued a research project investigating the structures and properties of heteronuclear complexes of rare earth and transition metals bridged by carboxyl groups (Wu et al., 2002a,b, 2003, 2004; Zhu et al., 2005). The title complex, (I), was obtained during the preparation of a dysprosium–copper carboxyl compound. Its structure and magnetic properties are promising for the elucidation of the magnetic interaction between different 4f and 3d metallic ions in heteroneuclear complexes.

The molecular structure and intramolecular arrangement of (I) are shown in Fig. 1. The symmetric centre of the molecule is situated at atom Cu1. The coordination environments that surround the CuII ions can be divided into two types. Atom Cu2 is in a CuN2O3 environment formed by two N atoms of a bidentate phenanthroline ligand and three O atoms from a water molecule, an α-methylacrylate group and a hydroxyl group, composing a distorted square-pyramidal geometry. Atoms O1, O2, N1 and N2 are in the equatorial plane and atom O5 occupies the vertex of the square-pyramid. Atom Cu1 is coordinated by atoms O1, O1iii, O3 and O3iii, which constitute a square plane [symmetry code: (iii) 1 - x, -y, -z]. It is noted that atoms O5 and O5iii of the water molecules occupy the axial sites of an octahedral polyhedron if atom Cu1 is considered as six-coordinated (dashed lines in Fig. 1). The Cu1—O5 distance is 2.567 Å. Three CuII ions in the molecule are in a linear arrangement linked by α-methylacrylate and hydroxyl groups to give two mixed bridged Cu2–OH/RCOO–Cu1 units with a Cu2···Cu1 distance of 3.0275 Å. As Table 1 shows, the Cu—O bond lengths in the square planes are similar, with an average bond length of 1.9468 Å. The axial Cu—O distance is 2.287 (2) Å, which is obviously longer than those in the square planes. The two Cu—N distances are nearly the same, with an average value of 2.021 Å. All bond lengths are in agreement with those in other reports (Gehring et al., 1993; Setifi et al., 2006; Tao et al., 2006). Electronic delocalization in the OCO fragment is complete, with two almost equivalent CO bond lengths [1.265 (4) Å for C31—O2 and 1.262 (3) Å for C31—O3]. The phenanthroline ligand adopts a bidentate coordination mode and possesses local C2v symmetry.

A packing diagram for complex (I) is shown in Fig. 2. The copper complex cations are associated with their identical neighbours through stacking of the phenanthroline aromatic rings in an `offset' manner. There is no evidence, however, of strong ππ stacking interactions. The aryl rings of neighbouring phenanthroline ligands are approximately parallel, with a dihedral angle of 0.82° and an approximate perpendicular distance of 3.687 Å.

Hydrogen bonds play an important role in the stability of the crystal structure of (I). As Fig. 3 shows, there are also many intermolecular hydrogen bonds between O atoms of the water molecules and O atoms of the nitrate ions or hydroxyl groups. Atoms O1, O4, O5i, O6ii, N3ii and O8ii are interlinked by hydrogen bonds to form a six-ring cycle [symmetry codes: (i) -1 + x, y, z; (ii) -x, -y, -z]. Atoms O1ii, O4ii, O5iii, O6, N3 and O8 are also joined together by hydrogen bonds to form another six-ring cycle. Meanwhile, there are two cycles linked by hydrogen bonds between atoms O4 and O8, and O4ii and O8ii. These hydrogen bonds form a one-dimensional structure along the a axis, which is advantageous for decreasing the energy. The hydrogen-bond distances are in the range 2.731–2.968 Å, with an average of 2.873 Å, which is in good agreement with typical values for O—H···O interactions [Reference?].

Related literature top

For related literature, see: Bruda et al. (2006); Chen et al. (2006); Costes, Auchel, Dahan, Peyrou, Shova & Wernsdorfer (2006); Costes, Dahan & Wernsdorfer (2006); Das et al. (2006); Gehring et al. (1993); Haase & Gehring (1985); Miller & Drillon (2001a, 2001b, 2002); Mishra et al. (2005); Mori et al. (2005, 2006); Murugesu et al. (2006); Narasimha et al. (2006); Rao et al. (2004); Setifi et al. (2006); Tao et al. (2006); Wu et al. (2002a, 2002b, 2003, 2004); Yeung et al. (2006); Zhu et al. (2005).

Experimental top

An aqueous solution (1 ml) of Cu(NO3)2 (188 mg, 1 mmol) was added to a solution of Dy(C4H5O2)3(H2O)6 (81.7 mg, 0.16 mmol) in water (3 ml) with stirring. An ethanol solution (1 ml) of phenanthroline (15.1 mg, 0.076 mmol) was added to the mixture. The resulting solution was filtered and the filtrate was allowed to stand at room temperature. After two weeks, blue needle crystals of (I) suitable for X-ray crystallographic study were obtained.

Temperature-dependent magnetic susceptibilities were collected from the pure crystal sample in the 5–300 K range using a Quantum Design PPMS-9 magnetometer in an applied field of 20 kOe (1 Oe = 79.58 A m-1). An effective magnetic moment of 3.589 µB was observed at 300 K. With decreasing temperature, the µeff(T) functions increase and reach 3.859 µB at 18 K, and then decrease rapidly to 3.54 µB at 5 K. Such behaviour is characteristic of predominantly ferromagnetic exchange coupling in CuII3 systems (Haase & Gehring, 1985). The observed susceptibility data are well fitted to the Curie–Weiss law [χm = C/(T - θ)], with Weiss constant θ = 3.52 K. IR: ν(OH) 3650–2900, ν(CC) 1645, ν(COO)as 1541, ν(COO)s 1426, ν(NO3) 1384 cm-1.

Refinement top

The H atoms of the hydrocarbon groups were placed in calculated positions, with C—H = 0.96 Å for the methyl group or 0.93 Å for the terminal CH2 group, and they were included in the final cycles of refinement in a riding model, with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C). H atoms from water molecules were located in a difference Fourier map, and their coordinates and displacement parameters were fixed during structure refinement, using a riding model, with Uiso(H) = 1.2 Ueq(O).

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: CrystalStructure (Rigaku/MSC & Rigaku, 2002); data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of the molecule of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. Unlabelled atoms are related to labelled atoms by the symmetry code ? [Please complete].
[Figure 2] Fig. 2. A packing diagram for complex (I), viewed along the b axis, showing the ππ interactions between the phenanthroline rings. Water molecules and nitrate ions have been omitted for clarity.
[Figure 3] Fig. 3. Intermolecular hydrogen bonds, along the a axis. C atoms of the phenanthroline ligands have been omitted for clarity. [Symmetry codes: (i) -1 + x, y, z; (ii) -x, -y, -z; (iii) 1 - x, -y, -z.]
diaqua-1κO,3κO-di-µ-methacrylato-1:2κ2O:O',2:3κ2O:O'-bis(1,10-phenanthroline)-1κ2N,N';3κ2N,N'-di-µ-hydroxido-1:2κ2O:O,2:3κ2O:O-tricopper(II) dinitrate dihydrate top
Crystal data top
[Cu3(C4H5O2)2(OH)2(C12H8N2)2(H2O)2](NO3)2·2H2OZ = 1
Mr = 951.29F(000) = 485
Triclinic, P1Dx = 1.712 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 7.3779 (5) ÅCell parameters from 6352 reflections
b = 11.1570 (9) Åθ = 3.0–27.4°
c = 12.5830 (9) ŵ = 1.80 mm1
α = 71.081 (2)°T = 293 K
β = 81.596 (2)°Needle, blue
γ = 70.529 (2)°0.35 × 0.08 × 0.02 mm
V = 922.94 (12) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4172 independent reflections
Radiation source: fine-focus sealed tube3356 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
Detector resolution: 10.0 pixels mm-1θmax = 27.4°, θmin = 3.0°
ω scansh = 89
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1414
Tmin = 0.572, Tmax = 0.965l = 1616
8975 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0675P)2 + 0.1148P]
where P = (Fo2 + 2Fc2)/3
4172 reflections(Δ/σ)max = 0.002
271 parametersΔρmax = 0.53 e Å3
0 restraintsΔρmin = 0.53 e Å3
Crystal data top
[Cu3(C4H5O2)2(OH)2(C12H8N2)2(H2O)2](NO3)2·2H2Oγ = 70.529 (2)°
Mr = 951.29V = 922.94 (12) Å3
Triclinic, P1Z = 1
a = 7.3779 (5) ÅMo Kα radiation
b = 11.1570 (9) ŵ = 1.80 mm1
c = 12.5830 (9) ÅT = 293 K
α = 71.081 (2)°0.35 × 0.08 × 0.02 mm
β = 81.596 (2)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4172 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
3356 reflections with I > 2σ(I)
Tmin = 0.572, Tmax = 0.965Rint = 0.029
8975 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.120H-atom parameters constrained
S = 1.13Δρmax = 0.53 e Å3
4172 reflectionsΔρmin = 0.53 e Å3
271 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.50000.00000.00000.02985 (14)
Cu20.57035 (5)0.03202 (3)0.23383 (3)0.03213 (13)
O10.3649 (3)0.01196 (19)0.12575 (16)0.0323 (4)
O20.6478 (4)0.2161 (2)0.14337 (19)0.0486 (6)
O30.6092 (3)0.1945 (2)0.03045 (18)0.0408 (5)
O40.1068 (3)0.1396 (3)0.0591 (2)0.0497 (6)
O50.7678 (3)0.0296 (2)0.1518 (2)0.0456 (5)
N30.1086 (4)0.3237 (3)0.2507 (2)0.0457 (6)
O60.2592 (4)0.3094 (3)0.2669 (3)0.0919 (11)
O70.0654 (5)0.4231 (3)0.3049 (3)0.0816 (10)
O80.0003 (4)0.2339 (3)0.1781 (2)0.0663 (8)
N10.5011 (3)0.1456 (2)0.3527 (2)0.0350 (5)
N20.7326 (3)0.0881 (3)0.3643 (2)0.0398 (6)
C10.3902 (5)0.2629 (3)0.3434 (3)0.0488 (8)
H10.33630.26950.27320.059*
C20.5825 (4)0.1392 (3)0.4559 (2)0.0386 (7)
C30.7076 (4)0.0115 (4)0.4616 (3)0.0417 (7)
C40.8479 (5)0.2074 (4)0.3662 (4)0.0569 (9)
H40.86660.27730.29990.068*
C50.3514 (6)0.3769 (4)0.4355 (4)0.0647 (11)
H50.27230.45750.42590.078*
C60.4281 (6)0.3709 (4)0.5388 (4)0.0710 (13)
H60.40160.44700.60030.085*
C70.5486 (5)0.2484 (4)0.5521 (3)0.0570 (10)
C80.6394 (7)0.2266 (6)0.6575 (3)0.0798 (16)
H80.61360.29700.72340.096*
C90.7585 (7)0.1086 (7)0.6625 (3)0.0774 (15)
H90.81730.09960.73140.093*
C100.7979 (5)0.0036 (5)0.5657 (3)0.0586 (11)
C110.9204 (6)0.1309 (6)0.5639 (4)0.0724 (14)
H110.98570.14620.62960.087*
C120.9435 (6)0.2309 (5)0.4672 (5)0.0748 (14)
H121.02240.31580.46650.090*
C310.6521 (4)0.2627 (3)0.0375 (2)0.0353 (6)
C320.7148 (5)0.4106 (3)0.0115 (3)0.0451 (7)
C330.7374 (7)0.4870 (4)0.0560 (4)0.0749 (13)
H33A0.77360.57910.02630.090*
H33B0.71690.44760.13240.090*
C340.7444 (7)0.4644 (4)0.1339 (3)0.0701 (12)
H34A0.72150.39230.16490.105*
H34B0.87420.52160.14670.105*
H34C0.65660.51420.16940.105*
H1010.25230.08430.14350.039*
H4010.08150.16540.01830.060*
H4020.21110.11530.07480.060*
H5010.89060.01760.12950.055*
H5020.77120.11970.18190.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0354 (3)0.0272 (2)0.0258 (2)0.00682 (19)0.00484 (18)0.00762 (18)
Cu20.0365 (2)0.0313 (2)0.0262 (2)0.00690 (15)0.00155 (13)0.00885 (14)
O10.0308 (9)0.0351 (10)0.0288 (10)0.0063 (8)0.0027 (7)0.0098 (8)
O20.0700 (16)0.0313 (11)0.0370 (12)0.0051 (10)0.0045 (11)0.0099 (9)
O30.0563 (13)0.0285 (10)0.0346 (11)0.0087 (9)0.0084 (9)0.0069 (9)
O40.0498 (13)0.0625 (15)0.0404 (12)0.0247 (11)0.0043 (10)0.0111 (11)
O50.0424 (12)0.0473 (13)0.0479 (13)0.0181 (10)0.0097 (10)0.0079 (11)
N30.0432 (15)0.0442 (15)0.0459 (16)0.0101 (12)0.0027 (12)0.0110 (13)
O60.0605 (18)0.075 (2)0.135 (3)0.0251 (15)0.0338 (19)0.008 (2)
O70.080 (2)0.0606 (18)0.088 (2)0.0295 (16)0.0158 (17)0.0135 (17)
O80.0517 (15)0.0621 (17)0.0552 (16)0.0008 (13)0.0044 (12)0.0042 (13)
N10.0345 (12)0.0355 (12)0.0321 (12)0.0116 (10)0.0040 (9)0.0042 (10)
N20.0337 (13)0.0510 (15)0.0418 (14)0.0125 (11)0.0018 (10)0.0249 (13)
C10.0439 (17)0.0383 (17)0.060 (2)0.0129 (14)0.0046 (15)0.0072 (16)
C20.0372 (15)0.0538 (18)0.0283 (14)0.0236 (14)0.0051 (11)0.0049 (13)
C30.0344 (15)0.067 (2)0.0357 (16)0.0253 (14)0.0029 (12)0.0221 (15)
C40.0449 (19)0.060 (2)0.071 (3)0.0074 (16)0.0002 (17)0.036 (2)
C50.056 (2)0.0388 (19)0.086 (3)0.0116 (16)0.013 (2)0.0006 (19)
C60.063 (2)0.064 (3)0.068 (3)0.031 (2)0.027 (2)0.027 (2)
C70.053 (2)0.078 (3)0.0394 (18)0.0393 (19)0.0147 (15)0.0094 (17)
C80.082 (3)0.135 (5)0.0292 (19)0.072 (3)0.0093 (19)0.009 (2)
C90.071 (3)0.152 (5)0.034 (2)0.068 (3)0.0116 (18)0.032 (3)
C100.049 (2)0.113 (3)0.0416 (19)0.050 (2)0.0131 (15)0.039 (2)
C110.051 (2)0.122 (4)0.078 (3)0.041 (3)0.028 (2)0.074 (3)
C120.048 (2)0.095 (4)0.106 (4)0.017 (2)0.014 (2)0.074 (3)
C310.0396 (15)0.0266 (13)0.0387 (16)0.0095 (11)0.0045 (12)0.0077 (12)
C320.0504 (18)0.0294 (15)0.0510 (19)0.0092 (13)0.0002 (14)0.0100 (14)
C330.108 (4)0.0334 (19)0.077 (3)0.011 (2)0.007 (3)0.0188 (19)
C340.099 (3)0.0317 (18)0.058 (2)0.0074 (19)0.005 (2)0.0023 (17)
Geometric parameters (Å, º) top
Cu1—O1i1.9369 (19)C2—C71.393 (5)
Cu1—O11.9369 (19)C2—C31.433 (5)
Cu1—O31.973 (2)C3—C101.415 (4)
Cu1—O3i1.973 (2)C4—C121.418 (6)
Cu1—Cu2i3.0275 (4)C4—H40.9300
Cu1—Cu23.0275 (4)C5—C61.352 (6)
Cu2—O11.9295 (19)C5—H50.9300
Cu2—O21.932 (2)C6—C71.408 (6)
Cu2—N12.012 (2)C6—H60.9300
Cu2—N22.028 (2)C7—C81.452 (6)
Cu2—O52.286 (2)C8—C91.333 (7)
O1—H1010.939C8—H80.9300
O2—C311.265 (4)C9—C101.417 (7)
O3—C311.262 (3)C9—H90.9300
O4—H4010.931C10—C111.401 (7)
O4—H4020.874C11—C121.344 (7)
O5—H5010.915C11—H110.9300
O5—H5020.960C12—H120.9300
N3—O71.216 (4)C31—C321.494 (4)
N3—O61.228 (4)C32—C331.344 (5)
N3—O81.252 (4)C32—C341.480 (5)
N1—C11.324 (4)C33—H33A0.9300
N1—C21.363 (4)C33—H33B0.9300
N2—C41.325 (4)C34—H34A0.9600
N2—C31.347 (4)C34—H34B0.9600
C1—C51.392 (5)C34—H34C0.9600
C1—H10.9300
O1i—Cu1—O1180.00 (11)C5—C1—H1118.9
O1i—Cu1—O389.19 (8)N1—C2—C7123.2 (3)
O1—Cu1—O390.81 (8)N1—C2—C3116.2 (3)
O1i—Cu1—O3i90.81 (8)C7—C2—C3120.6 (3)
O1—Cu1—O3i89.19 (8)N2—C3—C10123.8 (3)
O3—Cu1—O3i180.00 (15)N2—C3—C2116.5 (3)
O1i—Cu1—Cu2i38.37 (5)C10—C3—C2119.7 (3)
O1—Cu1—Cu2i141.63 (5)N2—C4—C12121.5 (4)
O3—Cu1—Cu2i102.61 (6)N2—C4—H4119.2
O3i—Cu1—Cu2i77.39 (6)C12—C4—H4119.2
O1i—Cu1—Cu2141.63 (5)C6—C5—C1120.4 (4)
O1—Cu1—Cu238.37 (5)C6—C5—H5119.8
O3—Cu1—Cu277.39 (6)C1—C5—H5119.8
O3i—Cu1—Cu2102.61 (6)C5—C6—C7119.2 (3)
Cu2i—Cu1—Cu2180.000 (17)C5—C6—H6120.4
O1—Cu2—O290.89 (9)C7—C6—H6120.4
O1—Cu2—N197.49 (9)C2—C7—C6117.0 (4)
O2—Cu2—N1169.20 (10)C2—C7—C8117.5 (4)
O1—Cu2—N2164.93 (9)C6—C7—C8125.4 (4)
O2—Cu2—N288.74 (10)C9—C8—C7121.9 (4)
N1—Cu2—N281.41 (11)C9—C8—H8119.1
O1—Cu2—O590.64 (8)C7—C8—H8119.1
O2—Cu2—O594.88 (10)C8—C9—C10121.7 (4)
N1—Cu2—O591.82 (9)C8—C9—H9119.2
N2—Cu2—O5104.40 (9)C10—C9—H9119.2
O1—Cu2—Cu138.55 (6)C11—C10—C9125.2 (4)
O2—Cu2—Cu179.42 (6)C11—C10—C3116.3 (4)
N1—Cu2—Cu1111.36 (7)C9—C10—C3118.5 (4)
N2—Cu2—Cu1155.17 (7)C12—C11—C10120.0 (3)
O5—Cu2—Cu155.67 (6)C12—C11—H11120.0
Cu2—O1—Cu1103.08 (9)C10—C11—H11120.0
Cu2—O1—H101124.01C11—C12—C4120.2 (4)
Cu1—O1—H101115.55C11—C12—H12119.9
C31—O2—Cu2128.47 (19)C4—C12—H12119.9
C31—O3—Cu1129.10 (19)O3—C31—O2125.3 (3)
H401—O4—H402110.6O3—C31—C32117.1 (3)
Cu2—O5—H501127.89O2—C31—C32117.5 (3)
Cu2—O5—H502117.26C33—C32—C34123.7 (3)
H501—O5—H502103.5C33—C32—C31119.1 (3)
O7—N3—O6120.5 (3)C34—C32—C31117.1 (3)
O7—N3—O8120.6 (3)C32—C33—H33A120.0
O6—N3—O8119.0 (3)C32—C33—H33B120.0
C1—N1—C2117.8 (3)H33A—C33—H33B120.0
C1—N1—Cu2129.2 (2)C32—C34—H34A109.5
C2—N1—Cu2112.9 (2)C32—C34—H34B109.5
C4—N2—C3118.1 (3)H34A—C34—H34B109.5
C4—N2—Cu2128.9 (3)C32—C34—H34C109.5
C3—N2—Cu2112.9 (2)H34A—C34—H34C109.5
N1—C1—C5122.2 (4)H34B—C34—H34C109.5
N1—C1—H1118.9
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H101···O8ii0.942.032.970 (4)177
O4—H401···O80.931.992.910 (3)171
O4—H402···O10.872.002.819 (4)156
O5—H501···O4iii0.921.842.731 (4)166
O5—H502···O6i0.961.992.936 (4)168
Symmetry codes: (i) x+1, y, z; (ii) x, y, z; (iii) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Cu3(C4H5O2)2(OH)2(C12H8N2)2(H2O)2](NO3)2·2H2O
Mr951.29
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.3779 (5), 11.1570 (9), 12.5830 (9)
α, β, γ (°)71.081 (2), 81.596 (2), 70.529 (2)
V3)922.94 (12)
Z1
Radiation typeMo Kα
µ (mm1)1.80
Crystal size (mm)0.35 × 0.08 × 0.02
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.572, 0.965
No. of measured, independent and
observed [I > 2σ(I)] reflections
8975, 4172, 3356
Rint0.029
(sin θ/λ)max1)0.648
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.120, 1.13
No. of reflections4172
No. of parameters271
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.53, 0.53

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC & Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Cu1—O11.9369 (19)Cu2—N12.012 (2)
Cu1—O31.973 (2)Cu2—N22.028 (2)
Cu1—Cu23.0275 (4)Cu2—O52.286 (2)
Cu2—O11.9295 (19)O2—C311.265 (4)
Cu2—O21.932 (2)O3—C311.262 (3)
O1i—Cu1—O389.19 (8)O2—Cu2—N288.74 (10)
O1—Cu1—O390.81 (8)N1—Cu2—N281.41 (11)
O1—Cu2—O290.89 (9)O1—Cu2—O590.64 (8)
O1—Cu2—N197.49 (9)O2—Cu2—O594.88 (10)
O2—Cu2—N1169.20 (10)N1—Cu2—O591.82 (9)
O1—Cu2—N2164.93 (9)N2—Cu2—O5104.40 (9)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H101···O8ii0.942.032.970 (4)177
O4—H401···O80.931.992.910 (3)171
O4—H402···O10.872.002.819 (4)156
O5—H501···O4iii0.921.842.731 (4)166
O5—H502···O6i0.961.992.936 (4)168
Symmetry codes: (i) x+1, y, z; (ii) x, y, z; (iii) x+1, y, z.
 

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