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The crystal structure of catena-poly­[[[acetato(1,10-phenanthroline-κ2N,N′)copper(II)]-μ-dicyan­amido-κ2N1:N5] trihydrate], {[Cu(C2H3O2)(C2N3)(C12H8N2)]·3H2O}n, consists of a zigzag chain formed by the polymer [Cu(CH3COO)(dca)(phen)]n (phen is 1,10-phenanthroline and dca is dicyan­amide), with three water mol­ecules per repeat unit of the polymer. The CuII atom has a slightly distorted square-pyramidal coordination environment consisting of two N atoms of the phen ligand, two nitrile N atoms of different dca ligands, one of them axial, and one O atom of the acetate anion. The compound forms a one-dimensional chain using dca as an end-to-end bridging ligand. Non-covalent interactions, π–π stacking and hydrogen bonding mediate the bundling of the polymer chains into a three-dimensional structure, with the water mol­ecules playing an important role in the hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103023114/fa1028sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103023114/fa1028Isup2.hkl
Contains datablock I

CCDC reference: 226115

Comment top

The construction of supramolecular aggregates has received much attention due to their intriguing network topologies and potential functions as new classes of materials (Eddaoudi et al., 2002; Li et al., 1999). Hydrogen-bonding and ππ stacking interactions have been commonly used as supramolecular cement due to their directionality, specificity and biological relevance (Fyfe & Stoddart, 1999; Roesky & Andruh, 2003). Combinations of hydrogen-bonding patterns can generate a variety of supramolecular synthons, which have been summarized in a review by Fyfe & Stoddart (1999). It is known that ππ stacking interactions can influence the stereochemistry of organic reactions, binding affinities in host–guest chemistry and protein stability (Hunter, 1994; Jorgensen & Severance, 1990).

In a separate area, metal dicyanamide {dca, [N(CN)2]} coordination chemistry is a fast-growing research field because of the interesting possibilities for coordination and physical properties that these complexes possess (Miller & Manson, 2001). Dicyanamide is a versatile ligand for coordinating to metal ions in various modes, such as monodentate bonding through a nitrile N atom (Marshall et al., 2000), end-to-end bridging through the two nitrile N atoms (Manson Arif & Miller, 1999; Jensen et al., 1999) and tris-monodentate bridging of three metal atoms (Jensen et al., 2000; Kurmco & Kepert, 1998). The coordination properties thus allow for the preparation of compounds with a large variety of architectures, both mononuclear and dinuclear, as well as one-, two- and three-dimensional networks. Compounds formulated as [M(dca)2]n (M is Mn, Fe, Co, Ni, Cu, Zn, etc.), containing only dca ligands, have been synthesized (Jensen et al., 1999; Batten et al., 1998). Many ternary compounds have been synthesized by the introduction of monodentate or bidentate co-ligands such as pyridine, bipyridine, 1,10-phenanthroline and 2,2'-biimidazole, resulting in various interesting structures (Marshall et al., 2000; Manson Arif Incarvito et al., 1999; Potocnák et al., 1995). As an extension of this research, we have synthesized the title new one-dimensional compound, [Cu(1,10-phen)(dca)(CH3COO)]n·3H2O, (I), and we report here its synthesis and crystal structure, the network of which is sustained by ππ stacking and hydrogen-bonding interactions. \sch

The Cu atom in (I) is in a distorted square-pyramidal environment, with the equatorial positions occupied by two phen N atoms [Cu1—N1 2.0246 (16) and Cu1—N2 2.0195 (16) Å], one nitrile N atom of the bridging dca [Cu1—N5i 1.9958 (16) Å; symmetry code (i): 1/2 + x, y − 1/2, z] and one carboxyl O atom of the acetate anion [Cu1—O1 1.9333 (13) Å], which are coplanar with a mean deviation of 0.159 (2) Å. The apical position is occupied by a nitrile N atom of another bridging dca, with a Cu1—N3 distance of 2.1777 (18) Å, which is about 0.164 (2) Å longer than the mean Cu—N(eq) bond distance. The Cu atom is displaced by 0.246 (2) Å from the equatorial plane in the direction of the apical atom.

The [N(CN)2] ligands form end-to-end bridges between the CuII atoms to give an infinite zigzag chain extended along the b axis, while the phen ligands chelated to the Cu atoms are located on the same side of the chain, as shown in Fig. 1. The –Cu-dca-Cu-dca- backbone chain in (I) is similar to those found in other dca-bridged Cu chain compounds (Wang et al., 2000; Wu et al., 2003; Luo et al., 2002). However, the Cu1···N4···Cu1 and N4···Cu1···N4 angles in (I) are both 113.46 (4)°, which is notably different from the corresponding values for the four-coordinate Cu compound (132.82 and 95.98°, respectively; Wu et al., 2003), as a result of the different coordination modes of Cu in the two cases. A similar result was found for the five-coordinate Cu analogues (Luo et al., 2002), in which the corresponding angles are 120.82 and 114.31°, respectively.

The intrachain Cu···Cu distance of 7.485 (1) Å and the shortest interchain Cu···Cu distance of 6.353 (1) Å in (I) are shorter than those found in the analogues mentioned above {7.708 and 6.452 Å, respectively, in [Cu(phen)(dca)2] (Wang et al., 2000), 8.007 and 6.703 Å, respectively, in [Cu(phen)(dca)] (Wu et al., 2003), and 7.710 and 6.546 Å, respectively, in [Cu(phen)(dca)2] (Luo et al., 2002)].

The dca ligands in (I) have approximate C2v symmetry, with average single C—N and triple N—C bond lengths of 1.296 (3) and 1.136 (3) Å, respectively, which are consistent with typical values for the N(CN)2 anion (Potocnák et al., 1996). The bond distances and angles in the phen ligands of (I) are in accord with those reported by Anderson (1973).

In the comparison with the Cu analogues mentioned above (Wang et al., 2000; Wu et al., 2003; Luo et al., 2002), it is noteworthy that adjacent chains in (I) are organized into pairs through face-to-face ππ stacking interactions between adjacent phen ligands to form a double chain, as shown in Fig. 2. The ππ stacking interactions in (I) can be classified as two types, firstly, ring R1 (atoms C4, C5, C6, C7, C11 and C12) to ring R1 of a neighbouring phen, denoted R1···R1, and secondly, ring R1 to ring R2 (atoms C7, C8, C9, C10, N2 and C11) of two adjacent phens, denoted R1···R2. The two rings involved in a ππ stacking interaction are nearly parallel, with a dihedral angle of 2.28 (9)° and a centroid-to-centroid distance of 3.6161 (16) Å. Two R1···R2 and one R1···R1 ππ stacking interactions alternately link two adjacent backbones to form a double chain propagated along the b axis. The water molecules are located between the double chains and form hydrogen bonds to each other and to the unbonded O atom of the acetate ligand, thus bridging the double-chain units to form a three-dimensional framework along the a and c directions, as shown in Fig. 3. The ππ stacking and hydrogen-bonding interactions lead to the stabilization of the crystal structure of (I).

Experimental top

An aqueous solution of Cu(CH3COO)2 (101 mg, 0.51 mmol) and an aqueous solution of Na(dca) (91 mg, 1.0 mmol, 4 ml) were mixed thoroughly and then an ethanol solution of 1,10-phen (100 mg, 0.51 mg, 10 ml) was added dropwise with stirring. The resulting mixture was filtered and the filtrate was left undisturbed at room temperature. A small quantity of transparent blue crystals of (I) was obtained after a few days.

Refinement top

The H atoms of the water molecules were located in difference Fourier syntheses and refined with O—H distances restrained to a target value of 0.96 Å, and with Uiso(H) = 1.2Ueq(O). The remaining H atoms were added according to theoretical models, assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms before the final cycle of least-squares refinement. All calculations were performed with the SHELXTL program package (Sheldrick, 1995).

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 1995); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The chain structure of (I) with displacement ellipsoids at the 30% probability level; the H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The ππ stacking interactions (dotted lines) between two adjacent chains in (I), extending along the b direction.
[Figure 3] Fig. 3. The hydrogen bonding involving acetate O atoms and unligated water molecules in the hydrophilic region of the structure of (I). [Suffix A denotes atoms at the symmetry position (1/2 − x, 1/2 − y, 1 − z), B (1/2 − x, 3/2 − y, 1 − z), C (x, 1 − y, z − 1/2) and D (1/2 − x, y − 1/2, 1/2 − z)].
catena-poly[[[acetato(1,10-phenanthroline-κ2N,N')copper(II)]-µ- dicyanamido-κ2N1:N5] trihydrate] top
Crystal data top
[Cu(C2H3O2)(C2N3)(C12H8N2)]·3H2OF(000) = 1736
Mr = 422.89Dx = 1.543 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 26.717 (4) ÅCell parameters from 5119 reflections
b = 7.4853 (10) Åθ = 3.1–27.5°
c = 20.601 (3) ŵ = 1.24 mm1
β = 117.906 (9)°T = 293 K
V = 3640.8 (10) Å3Block, blue
Z = 80.45 × 0.30 × 0.25 mm
Data collection top
Rigaku Mercury CCD area-detector
diffractometer
3212 independent reflections
Radiation source: fine-focus sealed tube2583 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
ω scansθmax = 25.0°, θmin = 3.1°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)
h = 3128
Tmin = 0.590, Tmax = 0.734k = 88
11803 measured reflectionsl = 2424
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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0654P)2]
where P = (Fo2 + 2Fc2)/3
3212 reflections(Δ/σ)max = 0.001
262 parametersΔρmax = 0.66 e Å3
6 restraintsΔρmin = 0.40 e Å3
Crystal data top
[Cu(C2H3O2)(C2N3)(C12H8N2)]·3H2OV = 3640.8 (10) Å3
Mr = 422.89Z = 8
Monoclinic, C2/cMo Kα radiation
a = 26.717 (4) ŵ = 1.24 mm1
b = 7.4853 (10) ÅT = 293 K
c = 20.601 (3) Å0.45 × 0.30 × 0.25 mm
β = 117.906 (9)°
Data collection top
Rigaku Mercury CCD area-detector
diffractometer
3212 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)
2583 reflections with I > 2σ(I)
Tmin = 0.590, Tmax = 0.734Rint = 0.046
11803 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0556 restraints
wR(F2) = 0.138H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 0.66 e Å3
3212 reflectionsΔρmin = 0.40 e Å3
262 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.

Here are some useful distances and angles that do not fit into any of the other categories. See the text of the manuscript for more information.

Cu1 N4 4.3831 (19) 1_545 No Cu1 N4 4.5687 (19). No Cu1 Cu1 7.4853 (10) 1_565 No

N4 Cu1 N4 113.46 (4) 1_545. Yes Cu1 N4 Cu1 113.46 (4) 1_565. No

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
Cu10.094415 (9)0.60016 (3)0.417161 (11)0.03705 (7)
O10.17539 (5)0.57811 (17)0.45487 (7)0.0440 (4)
O20.18161 (5)0.37388 (19)0.53669 (7)0.0540 (5)
N10.10269 (6)0.7215 (2)0.50949 (7)0.0380 (5)
N20.01189 (6)0.62087 (19)0.39175 (8)0.0380 (5)
N30.08858 (7)0.8214 (2)0.34530 (9)0.0558 (6)
N40.08104 (10)1.1150 (2)0.29091 (10)0.0838 (7)
N50.07959 (7)1.39743 (19)0.34758 (8)0.0446 (5)
C10.14921 (8)0.7745 (3)0.56829 (10)0.0503 (7)
H1A0.18380.76360.56800.060*
C20.14862 (9)0.8448 (3)0.62978 (11)0.0580 (8)
H2A0.18240.88010.66970.070*
C30.09966 (9)0.8626 (3)0.63246 (10)0.0530 (7)
H3A0.09940.90880.67420.064*
C40.04875 (8)0.8109 (3)0.57162 (9)0.0436 (6)
C50.00594 (8)0.8281 (3)0.56632 (10)0.0520 (6)
H5A0.00940.87410.60600.062*
C60.05281 (8)0.7798 (3)0.50550 (11)0.0552 (7)
H6A0.08800.79270.50390.066*
C70.04962 (7)0.7088 (3)0.44303 (10)0.0438 (6)
C80.09636 (8)0.6608 (3)0.37601 (11)0.0561 (7)
H8A0.13290.67170.37000.067*
C90.08784 (9)0.5987 (3)0.32027 (12)0.0614 (9)
H9A0.11860.56920.27560.074*
C100.03341 (8)0.5792 (3)0.32985 (11)0.0508 (7)
H10A0.02840.53490.29110.061*
C110.00369 (7)0.6880 (2)0.44739 (9)0.0363 (6)
C120.05329 (7)0.7409 (2)0.51136 (9)0.0347 (5)
C130.20358 (8)0.4709 (3)0.50841 (10)0.0418 (6)
C140.26640 (8)0.4759 (3)0.53684 (11)0.0571 (7)
H14A0.28410.39180.57640.086*
H14B0.28020.59380.55440.086*
H14C0.27510.44510.49800.086*
C150.08496 (8)0.9620 (3)0.32277 (10)0.0451 (6)
C160.08087 (8)1.2602 (3)0.32402 (9)0.0438 (6)
O1W0.28697 (7)0.6126 (2)0.72872 (8)0.0761 (6)
H11B0.2649 (2)0.607 (3)0.7538 (3)0.091*
H11A0.2852 (6)0.7181 (9)0.7019 (5)0.091*
O2W0.25171 (6)0.2503 (2)0.67596 (8)0.0670 (6)
H21A0.2213 (5)0.262 (3)0.6273 (4)0.080*
H21B0.2606 (8)0.3734 (7)0.6878 (10)0.080*
O3W0.28985 (6)0.91490 (19)0.65445 (8)0.0659 (5)
H31B0.2923 (8)1.0345 (8)0.6715 (7)0.079*
H31A0.3069 (2)0.914 (3)0.6227 (3)0.079*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.04011 (11)0.03554 (13)0.03610 (10)0.00272 (10)0.01835 (8)0.00160 (9)
O10.0400 (6)0.0513 (8)0.0443 (6)0.0055 (6)0.0227 (5)0.0043 (6)
O20.0474 (7)0.0592 (9)0.0597 (7)0.0054 (7)0.0286 (5)0.0151 (7)
N10.0385 (7)0.0361 (9)0.0387 (7)0.0012 (7)0.0176 (5)0.0051 (7)
N20.0393 (7)0.0386 (9)0.0327 (7)0.0006 (7)0.0140 (6)0.0002 (6)
N30.0701 (10)0.0397 (10)0.0594 (9)0.0056 (9)0.0319 (7)0.0082 (8)
N40.1827 (16)0.0298 (10)0.0700 (9)0.0066 (10)0.0852 (8)0.0005 (7)
N50.0641 (9)0.0312 (9)0.0445 (7)0.0007 (7)0.0304 (6)0.0004 (6)
C10.0429 (10)0.0553 (13)0.0481 (10)0.0041 (10)0.0175 (8)0.0119 (10)
C20.0592 (12)0.0627 (14)0.0400 (10)0.0064 (11)0.0131 (9)0.0144 (10)
C30.0723 (12)0.0493 (13)0.0389 (9)0.0005 (11)0.0273 (8)0.0051 (9)
C40.0634 (10)0.0316 (10)0.0457 (8)0.0032 (9)0.0338 (7)0.0029 (8)
C50.0719 (10)0.0487 (12)0.0545 (9)0.0057 (10)0.0455 (7)0.0010 (9)
C60.0620 (10)0.0429 (13)0.0807 (11)0.0119 (10)0.0500 (8)0.0096 (10)
C70.0461 (9)0.0354 (11)0.0555 (9)0.0005 (9)0.0284 (7)0.0081 (9)
C80.0392 (10)0.0572 (14)0.0680 (12)0.0088 (10)0.0219 (8)0.0136 (11)
C90.0391 (11)0.0680 (16)0.0569 (13)0.0026 (11)0.0056 (10)0.0004 (11)
C100.0475 (10)0.0555 (14)0.0430 (10)0.0038 (10)0.0158 (8)0.0024 (9)
C110.0408 (8)0.0286 (10)0.0409 (8)0.0013 (8)0.0202 (6)0.0024 (8)
C120.0426 (8)0.0258 (10)0.0389 (8)0.0005 (8)0.0218 (6)0.0002 (7)
C130.0404 (9)0.0416 (11)0.0439 (9)0.0028 (9)0.0202 (7)0.0025 (9)
C140.0452 (10)0.0664 (14)0.0613 (11)0.0014 (11)0.0262 (8)0.0085 (11)
C150.0589 (10)0.0376 (11)0.0411 (9)0.0024 (10)0.0252 (7)0.0012 (9)
C160.0612 (10)0.0369 (11)0.0391 (8)0.0030 (9)0.0283 (7)0.0114 (8)
O1W0.1076 (11)0.0615 (11)0.0689 (8)0.0034 (9)0.0494 (7)0.0118 (8)
O2W0.0829 (9)0.0570 (10)0.0583 (7)0.0025 (8)0.0309 (6)0.0038 (7)
O3W0.0795 (8)0.0683 (11)0.0690 (7)0.0134 (8)0.0509 (6)0.0139 (7)
Geometric parameters (Å, º) top
Cu1—O11.9333 (13)C5—C61.342 (2)
Cu1—N5i1.9958 (16)C5—H5A0.9300
Cu1—N22.0195 (16)C6—C71.431 (3)
Cu1—N12.0246 (16)C6—H6A0.9300
Cu1—N32.1777 (18)C7—C111.393 (3)
O1—C131.285 (2)C7—C81.407 (2)
O2—C131.237 (3)C8—C91.353 (4)
N1—C11.326 (2)C8—H8A0.9300
N1—C121.346 (3)C9—C101.381 (3)
N2—C101.320 (2)C9—H9A0.9300
N2—C111.360 (3)C10—H10A0.9300
N3—C151.136 (3)C11—C121.419 (2)
N4—C161.285 (3)C13—C141.497 (3)
N4—C151.300 (3)C14—H14A0.9600
N5—C161.143 (2)C14—H14B0.9600
C1—C21.379 (3)C14—H14C0.9600
C1—H1A0.9300O1W—H11B0.950 (7)
C2—C31.342 (3)O1W—H11A0.952 (7)
C2—H2A0.9300O2W—H21A0.954 (6)
C3—C41.406 (2)O2W—H21B0.955 (6)
C3—H3A0.9300O3W—H31B0.953 (7)
C4—C121.404 (3)O3W—H31A0.957 (7)
C4—C51.419 (3)
O1—Cu1—N5i91.85 (6)C5—C6—C7121.2 (2)
O1—Cu1—N2172.41 (6)C5—C6—H6A119.4
N5i—Cu1—N292.67 (7)C7—C6—H6A119.4
O1—Cu1—N192.93 (6)C11—C7—C8116.4 (2)
N5i—Cu1—N1156.03 (7)C11—C7—C6118.22 (15)
N2—Cu1—N180.51 (6)C8—C7—C6125.3 (2)
O1—Cu1—N392.79 (6)C9—C8—C7119.7 (2)
N5i—Cu1—N399.38 (7)C9—C8—H8A120.1
N2—Cu1—N392.48 (7)C7—C8—H8A120.1
N1—Cu1—N3103.83 (7)C8—C9—C10119.95 (18)
C13—O1—Cu1119.64 (14)C8—C9—H9A120.0
C1—N1—C12116.99 (17)C10—C9—H9A120.0
C1—N1—Cu1129.47 (15)N2—C10—C9122.8 (2)
C12—N1—Cu1113.43 (10)N2—C10—H10A118.6
C10—N2—C11117.70 (18)C9—C10—H10A118.6
C10—N2—Cu1128.92 (16)N2—C11—C7123.38 (14)
C11—N2—Cu1113.38 (10)N2—C11—C12115.92 (17)
C15—N3—Cu1161.39 (18)C7—C11—C12120.69 (18)
C16—N4—C15119.8 (2)N1—C12—C4123.85 (14)
C16—N5—Cu1ii162.30 (13)N1—C12—C11116.43 (17)
N1—C1—C2123.0 (2)C4—C12—C11119.72 (18)
N1—C1—H1A118.5O2—C13—O1123.65 (17)
C2—C1—H1A118.5O2—C13—C14121.49 (17)
C3—C2—C1120.42 (18)O1—C13—C14114.82 (19)
C3—C2—H2A119.8C13—C14—H14A109.5
C1—C2—H2A119.8C13—C14—H14B109.5
C2—C3—C4119.4 (2)H14A—C14—H14B109.5
C2—C3—H3A120.3C13—C14—H14C109.5
C4—C3—H3A120.3H14A—C14—H14C109.5
C12—C4—C3116.3 (2)H14B—C14—H14C109.5
C12—C4—C5118.55 (15)N3—C15—N4173.8 (2)
C3—C4—C5125.1 (2)N5—C16—N4173.7 (2)
C6—C5—C4121.6 (2)H11B—O1W—H11A118.5 (15)
C6—C5—H5A119.2H21A—O2W—H21B99.7 (15)
C4—C5—H5A119.2H31B—O3W—H31A106.5 (17)
Symmetry codes: (i) x, y1, z; (ii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H31A···O1iii0.96 (1)1.87 (1)2.810 (2)168 (1)
O3W—H31B···O2Wii0.95 (1)1.97 (1)2.821 (2)147 (2)
O2W—H21A···O20.95 (1)1.86 (1)2.7506 (18)154 (2)
O2W—H21B···O1W0.96 (1)1.96 (1)2.910 (2)171 (2)
O1W—H11B···O2Wiv0.95 (1)2.01 (1)2.808 (3)140 (2)
O1W—H11A···O3W0.95 (1)1.80 (1)2.752 (2)174 (2)
Symmetry codes: (ii) x, y+1, z; (iii) x+1/2, y+3/2, z+1; (iv) x+1/2, y+1/2, z+3/2.

Experimental details

Crystal data
Chemical formula[Cu(C2H3O2)(C2N3)(C12H8N2)]·3H2O
Mr422.89
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)26.717 (4), 7.4853 (10), 20.601 (3)
β (°) 117.906 (9)
V3)3640.8 (10)
Z8
Radiation typeMo Kα
µ (mm1)1.24
Crystal size (mm)0.45 × 0.30 × 0.25
Data collection
DiffractometerRigaku Mercury CCD area-detector
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2002)
Tmin, Tmax0.590, 0.734
No. of measured, independent and
observed [I > 2σ(I)] reflections
11803, 3212, 2583
Rint0.046
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.055, 0.138, 1.07
No. of reflections3212
No. of parameters262
No. of restraints6
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.66, 0.40

Computer programs: CrystalClear (Rigaku, 2002), CrystalClear, SHELXTL (Sheldrick, 1995), SHELXTL.

Selected geometric parameters (Å, º) top
Cu1—O11.9333 (13)N3—C151.136 (3)
Cu1—N5i1.9958 (16)N4—C161.285 (3)
Cu1—N22.0195 (16)N4—C151.300 (3)
Cu1—N12.0246 (16)N5—C161.143 (2)
Cu1—N32.1777 (18)
O1—Cu1—N5i91.85 (6)N2—Cu1—N180.51 (6)
O1—Cu1—N2172.41 (6)O1—Cu1—N392.79 (6)
N5i—Cu1—N292.67 (7)N5i—Cu1—N399.38 (7)
O1—Cu1—N192.93 (6)N2—Cu1—N392.48 (7)
N5i—Cu1—N1156.03 (7)N1—Cu1—N3103.83 (7)
Symmetry code: (i) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H31A···O1ii0.957 (7)1.867 (7)2.810 (2)167.8 (6)
O3W—H31B···O2Wiii0.953 (7)1.971 (12)2.821 (2)147.4 (15)
O2W—H21A···O20.954 (6)1.859 (10)2.7506 (18)154.4 (16)
O2W—H21B···O1W0.955 (6)1.964 (8)2.910 (2)170.6 (15)
O1W—H11B···O2Wiv0.950 (7)2.010 (13)2.808 (3)140.4 (16)
O1W—H11A···O3W0.952 (7)1.804 (8)2.752 (2)173.8 (15)
Symmetry codes: (ii) x+1/2, y+3/2, z+1; (iii) x, y+1, z; (iv) x+1/2, y+1/2, z+3/2.
 

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