Bis(2,2′:6′,2′′-ter­pyridine)copper(II) diperchlorate hemihydrate

Valdés-Martínez, J.; Toscano, R.A.; Salazar-Mendoza, D.

doi:10.1107/S160053680100900X

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Bis(2,2':6',2''-terpyridine)copper(II) diperchlorate hemihydrate

J. Valdés-Martínez, R. A. Toscano and D. Salazar-Mendoza

In the title compound, [Cu(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O, the 2,2':6',2''-terpyridine (terpy) ligand coordinates to the Cu^II ion as a terdentate chelating ligand, giving a complex cation with compressed octahedral geometry. The [Cu(terpy)₂]²⁺ cations have crystallographically imposed C₂ symmetry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680100900X/cf6064sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680100900X/cf6064Isup2.hkl Contains datablock I

CCDC reference: 170860

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.009 Å
Disorder in solvent or counterion
R factor = 0.063
wR factor = 0.191
Data-to-parameter ratio = 11.6

checkCIF results

No syntax errors found


 Alert Level B:



PLAT_112  Alert B ADDSYM Detects Additional (Pseudo) Symm. Elem.          C


 Alert Level C:



PLAT_302  Alert C Anion/Solvent Disorder .......................      31.00 Perc.

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C30 H24 Cl2 Cu1 N6 O9
          Atom count from _chemical_formula_moiety:C30 H23 Cl2 Cu1 N6 O8.5


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 1 Alert Level C = Please check

Comment top

Several studies have been carried out on the structures and magnetic properties of copper(II) complexes with 2,2':6',2''-terpyridine (terpy) (Allmann et al., 1978; Folgado et al., 1990). In one of these studies (Folgado et al., 1990), the crystal structures and/or magnetic properties of some [Cu(terpy)₂]²⁺ salts were determined. Although the X-ray and EPR study revealed that the high-temperature phase of [Cu(terpy)₂](PF₆)₂, (II), was compressed octahedral, at low temperature, the structure contains elongated CuN₆ octahedra with an orthorhombic component. The EPR powder data for [Cu(terpy)₂](ClO₄)₂, (I), show the same magnetic behavior as (II), but the crystal structure of the former was not determined. In this paper, we report the crystal structure of [Cu(terpy)₂]²⁺(ClO₄)₂. 0.5 H₂O, (I), at 273 K.

Compound (I) consists of octahedral [Cu(terpy)₂]²⁺, with Cu, N1', C4', H4', N11', C14' and H14' in sites with a twofold symmetry axis, two [ClO₄]^- anions in general positions, and a water molecule with half occupancy. The terpy ligand coordinates to the metal ion as a meriodonal terdentate ligand. As a consequence of the rigid structure of the terpy ligand the Cu—N distances with the central pyridine ring are significantly shorter giving a compressed octahedral geometry in agreement with the high-temperature structure expected by the previous EPR study.

Experimental top

1.0 mmol of [Cu(H₂O)₆](ClO₄)₂ was dissolved in distilled H₂O and added to a solution of 1.0 mmoles of 2,2':6',2''-terpyridine in 25 ml of DMSO. The mixture was stirred for 1 h and left to evaporate until blue crystals were obtained.

Computing details top

Data collection: XSCANS (Siemens, 1993); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

Figures top

Fig. 1. A view of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 40% probability level.

Bis(2,2:6,2-terpyridine)copper(II) diperchlorate monohydrated top

Crystal data top

[Cu(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O	D_x = 1.559 Mg m⁻³
M_r = 746.99	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4₁/a	Cell parameters from 30 reflections
a = 12.551 (2) Å	θ = 3.5–12.5°
c = 40.418 (5) Å	µ = 0.92 mm⁻¹
V = 6367.0 (16) Å³	T = 293 K
Z = 8	Prism, green
F(000) = 3048	0.6 × 0.5 × 0.4 mm

Data collection top

Siemens P4/PC diffractometer	1368 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.062
Graphite monochromator	θ_max = 25.0°, θ_min = 1.5°
ω/2θ scans	h = 0→14
Absorption correction: ψ scan (North et al., 1968)	k = 0→14
T_min = 0.637, T_max = 0.693	l = 0→48
3081 measured reflections	3 standard reflections every 97 reflections
2808 independent reflections	intensity decay: <3%

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.063	H-atom parameters not refined
wR(F²) = 0.191	w = 1/[σ²(F_o²) + (0.1064P)²] where P = (F_o² + 2F_c²)/3
S = 0.88	(Δ/σ)_max = 0.019
2808 reflections	Δρ_max = 0.36 e Å⁻³
243 parameters	Δρ_min = −0.43 e Å⁻³
18 restraints	Extinction correction: SHELXL
Primary atom site location: structure-invariant direct methods	Extinction coefficient: none

Crystal data top

[Cu(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O	Z = 8
M_r = 746.99	Mo Kα radiation
Tetragonal, I4₁/a	µ = 0.92 mm⁻¹
a = 12.551 (2) Å	T = 293 K
c = 40.418 (5) Å	0.6 × 0.5 × 0.4 mm
V = 6367.0 (16) Å³

Data collection top

Siemens P4/PC diffractometer	1368 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.062
T_min = 0.637, T_max = 0.693	3 standard reflections every 97 reflections
3081 measured reflections	intensity decay: <3%
2808 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.063	18 restraints
wR(F²) = 0.191	H-atom parameters not refined
S = 0.88	Δρ_max = 0.36 e Å⁻³
2808 reflections	Δρ_min = −0.43 e Å⁻³
243 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu	0.5000	0.2500	0.12793 (3)	0.0473 (4)
N1	0.4331 (4)	0.0944 (4)	0.11615 (12)	0.0527 (13)
C2	0.4293 (4)	0.0748 (4)	0.08399 (16)	0.0489 (14)
C3	0.3963 (5)	−0.0221 (6)	0.07150 (18)	0.0635 (18)
H3	0.3960	−0.0347	0.0481	0.076*
C4	0.3635 (6)	−0.0995 (6)	0.0938 (2)	0.076 (2)
H4	0.3389	−0.1674	0.0860	0.091*
C5	0.3664 (6)	−0.0794 (6)	0.1265 (2)	0.072 (2)
H5	0.3451	−0.1333	0.1420	0.086*
C6	0.4002 (5)	0.0180 (5)	0.13738 (17)	0.0593 (17)
H6	0.4006	0.0328	0.1607	0.071*
N1'	0.5000	0.2500	0.07860 (17)	0.0499 (17)
C2'	0.4650 (4)	0.1631 (5)	0.06249 (15)	0.0489 (15)
C3'	0.4618 (6)	0.1623 (6)	0.02858 (18)	0.071 (2)
H3'	0.4334	0.1018	0.0171	0.085*
C4'	0.5000	0.2500	0.0113 (2)	0.080 (3)
H4'	0.5000	0.2500	−0.0125	0.096*
N11	0.6585 (4)	0.1849 (4)	0.14048 (12)	0.0501 (12)
C12	0.6767 (5)	0.1818 (4)	0.17290 (15)	0.0483 (14)
C13	0.7747 (5)	0.1474 (5)	0.18539 (18)	0.0635 (18)
H13	0.7872	0.1463	0.2088	0.076*
C14	0.8521 (5)	0.1151 (6)	0.1636 (2)	0.073 (2)
H14	0.9194	0.0898	0.1717	0.088*
C15	0.8334 (6)	0.1184 (6)	0.1302 (2)	0.072 (2)
H15	0.8875	0.0975	0.1148	0.086*
C16	0.7354 (5)	0.1532 (5)	0.11942 (17)	0.0583 (17)
H16	0.7210	0.1550	0.0961	0.070*
N11'	0.5000	0.2500	0.17764 (15)	0.0445 (16)
C12'	0.5865 (5)	0.2169 (5)	0.19417 (15)	0.0492 (15)
C13'	0.5893 (5)	0.2164 (5)	0.22814 (16)	0.0628 (18)
H13'	0.6522	0.1943	0.2397	0.075*
C14'	0.5000	0.2500	0.2455 (2)	0.074 (3)
H14'	0.5000	0.2500	0.2692	0.089*
Cl1	0.74847 (18)	0.0418 (2)	0.03063 (6)	0.0864 (7)
O1	0.6623 (5)	0.0005 (6)	0.04936 (18)	0.131 (3)
O2	0.7261 (7)	0.0500 (11)	−0.0015 (2)	0.185 (4)
O3	0.832 (2)	0.048 (3)	0.0496 (4)	0.184 (11)	0.50
O4	0.7575 (15)	0.1563 (9)	0.0376 (3)	0.126 (6)	0.50
O3B	0.767 (2)	−0.053 (3)	0.0194 (8)	0.240 (10)	0.50
O4B	0.8400 (11)	−0.0177 (18)	0.0345 (6)	0.144 (8)	0.50
O5	0.7081 (13)	0.2616 (11)	−0.0373 (3)	0.142 (6)	0.50
H5A	0.7428	0.3186	−0.0338	0.080*	0.50
H5B	0.7443	0.2126	−0.0281	0.080*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu	0.0340 (6)	0.0339 (6)	0.0739 (7)	−0.0008 (5)	0.000	0.000
N1	0.035 (3)	0.053 (3)	0.070 (3)	0.003 (2)	−0.008 (2)	−0.008 (3)
C2	0.034 (3)	0.036 (3)	0.076 (4)	0.001 (3)	0.000 (3)	−0.006 (3)
C3	0.054 (4)	0.059 (5)	0.078 (4)	−0.009 (3)	−0.003 (3)	−0.016 (3)
C4	0.061 (5)	0.047 (4)	0.119 (7)	−0.015 (4)	0.004 (4)	−0.009 (4)
C5	0.057 (5)	0.047 (4)	0.111 (6)	−0.009 (3)	0.004 (4)	0.013 (4)
C6	0.042 (4)	0.055 (4)	0.082 (4)	0.002 (3)	0.007 (3)	0.002 (3)
N1'	0.039 (4)	0.040 (4)	0.072 (4)	−0.001 (3)	0.000	0.000
C2'	0.036 (3)	0.044 (4)	0.067 (4)	0.000 (3)	−0.005 (3)	−0.006 (3)
C3'	0.073 (5)	0.056 (5)	0.084 (5)	0.004 (4)	−0.012 (4)	−0.010 (4)
C4'	0.110 (10)	0.075 (8)	0.055 (5)	0.000 (7)	0.000	0.000
N11	0.043 (3)	0.033 (3)	0.075 (3)	−0.003 (2)	−0.005 (2)	0.001 (2)
C12	0.044 (4)	0.033 (3)	0.068 (4)	−0.003 (3)	−0.005 (3)	−0.002 (3)
C13	0.043 (4)	0.063 (5)	0.085 (5)	0.005 (3)	−0.012 (3)	0.002 (4)
C14	0.040 (4)	0.073 (5)	0.107 (6)	0.011 (4)	−0.010 (4)	0.000 (4)
C15	0.058 (5)	0.057 (5)	0.101 (6)	0.005 (4)	0.020 (4)	−0.006 (4)
C16	0.052 (4)	0.048 (4)	0.075 (4)	0.002 (3)	0.008 (3)	−0.006 (3)
N11'	0.038 (4)	0.039 (4)	0.057 (4)	0.000 (3)	0.000	0.000
C12'	0.045 (4)	0.038 (3)	0.065 (4)	−0.002 (3)	−0.002 (3)	0.001 (3)
C13'	0.054 (4)	0.062 (5)	0.073 (5)	−0.001 (3)	−0.011 (3)	0.006 (3)
C14'	0.081 (8)	0.088 (8)	0.055 (5)	−0.013 (7)	0.000	0.000
Cl1	0.0682 (14)	0.1097 (17)	0.0812 (14)	0.0108 (13)	0.0044 (11)	0.0031 (12)
O1	0.089 (5)	0.153 (7)	0.151 (6)	0.020 (5)	0.045 (4)	0.062 (5)
O2	0.156 (8)	0.304 (13)	0.095 (5)	−0.056 (8)	−0.026 (5)	0.035 (6)
O3	0.138 (17)	0.32 (3)	0.092 (10)	−0.063 (18)	−0.037 (11)	−0.019 (15)
O4	0.218 (17)	0.042 (6)	0.118 (10)	−0.039 (8)	0.065 (10)	−0.028 (6)
O3B	0.19 (2)	0.25 (2)	0.28 (2)	0.003 (19)	−0.096 (17)	−0.067 (19)
O4B	0.028 (7)	0.174 (18)	0.23 (2)	0.046 (9)	0.014 (10)	0.079 (15)
O5	0.189 (17)	0.087 (10)	0.152 (12)	−0.007 (10)	0.000 (12)	0.017 (9)

Geometric parameters (Å, º) top

Cu—N1'	1.994 (7)	N11—C12	1.331 (7)
Cu—N11'	2.009 (6)	N11—C16	1.347 (8)
Cu—N1	2.178 (5)	C12—C13	1.398 (8)
Cu—N1ⁱ	2.178 (5)	C12—C12'	1.489 (8)
Cu—N11	2.210 (5)	C13—C14	1.373 (9)
Cu—N11ⁱ	2.210 (5)	C14—C15	1.367 (10)
N1—C2	1.324 (7)	C15—C16	1.376 (10)
N1—C6	1.351 (8)	N11'—C12'ⁱ	1.341 (6)
C2—C3	1.380 (8)	N11'—C12'	1.341 (6)
C2—C2'	1.478 (8)	C12'—C13'	1.373 (9)
C3—C4	1.388 (10)	C13'—C14'	1.387 (8)
C4—C5	1.346 (10)	C14'—C13'ⁱ	1.387 (8)
C5—C6	1.368 (10)	Cl1—O3B	1.29 (3)
N1'—C2'	1.344 (6)	Cl1—O3	1.30 (2)
N1'—C2'ⁱ	1.344 (6)	Cl1—O2	1.333 (8)
C2'—C3'	1.371 (9)	Cl1—O4B	1.378 (12)
C3'—C4'	1.389 (8)	Cl1—O1	1.418 (6)
C4'—C3'ⁱ	1.389 (8)	Cl1—O4	1.468 (10)

N1'—Cu—N11'	180.0	C3'—C2'—C2	125.0 (6)
N1'—Cu—N1	77.37 (14)	C2'—C3'—C4'	119.2 (7)
N11'—Cu—N1	102.63 (14)	C3'ⁱ—C4'—C3'	119.5 (9)
N1'—Cu—N1ⁱ	77.37 (14)	C12—N11—C16	119.4 (6)
N11'—Cu—N1ⁱ	102.63 (14)	C12—N11—Cu	113.0 (4)
N1—Cu—N1ⁱ	154.7 (3)	C16—N11—Cu	127.5 (4)
N1'—Cu—N11	103.26 (14)	N11—C12—C13	121.0 (6)
N11'—Cu—N11	76.74 (14)	N11—C12—C12'	115.5 (5)
N1—Cu—N11	93.78 (18)	C13—C12—C12'	123.5 (6)
N1ⁱ—Cu—N11	91.97 (18)	C14—C13—C12	118.8 (6)
N1'—Cu—N11ⁱ	103.26 (14)	C15—C14—C13	120.2 (7)
N11'—Cu—N11ⁱ	76.74 (14)	C14—C15—C16	118.5 (6)
N1—Cu—N11ⁱ	91.97 (18)	N11—C16—C15	122.2 (6)
N1ⁱ—Cu—N11ⁱ	93.78 (18)	C12'ⁱ—N11'—C12'	120.2 (7)
N11—Cu—N11ⁱ	153.5 (3)	C12'ⁱ—N11'—Cu	119.9 (3)
C2—N1—C6	118.7 (6)	C12'—N11'—Cu	119.9 (3)
C2—N1—Cu	113.3 (4)	N11'—C12'—C13'	121.3 (6)
C6—N1—Cu	127.9 (4)	N11'—C12'—C12	114.8 (5)
N1—C2—C3	122.3 (6)	C13'—C12'—C12	123.8 (6)
N1—C2—C2'	115.3 (5)	C12'—C13'—C14'	118.9 (7)
C3—C2—C2'	122.5 (6)	C13'—C14'—C13'ⁱ	119.3 (9)
C2—C3—C4	117.9 (7)	O3B—Cl1—O3	96.9 (16)
C5—C4—C3	119.9 (7)	O2—Cl1—O4B	109.1 (12)
C4—C5—C6	119.4 (7)	O3B—Cl1—O1	89.2 (16)
N1—C6—C5	121.7 (7)	O3—Cl1—O1	108.8 (11)
C2'—N1'—C2'ⁱ	122.1 (7)	O2—Cl1—O1	112.8 (5)
C2'—N1'—Cu	119.0 (4)	O4B—Cl1—O1	112.2 (8)
C2'ⁱ—N1'—Cu	119.0 (4)	O2—Cl1—O4	97.3 (8)
N1'—C2'—C3'	119.9 (6)	O4B—Cl1—O4	116.4 (12)
N1'—C2'—C2	115.0 (5)	O1—Cl1—O4	108.3 (6)

N1'—Cu—N1—C2	2.6 (4)	N1'—Cu—N11—C12	177.6 (3)
N11'—Cu—N1—C2	−177.4 (4)	N11'—Cu—N11—C12	−2.4 (3)
N1ⁱ—Cu—N1—C2	2.6 (4)	N1—Cu—N11—C12	−104.5 (4)
N11—Cu—N1—C2	−100.2 (4)	N1ⁱ—Cu—N11—C12	100.1 (4)
N11ⁱ—Cu—N1—C2	105.7 (4)	N1'—Cu—N11—C16	−0.1 (5)
N1'—Cu—N1—C6	180.0 (5)	N11'—Cu—N11—C16	179.9 (5)
N11'—Cu—N1—C6	0.0 (5)	N1—Cu—N11—C16	77.8 (5)
N1ⁱ—Cu—N1—C6	180.0 (5)	N1ⁱ—Cu—N11—C16	−77.5 (5)
N11—Cu—N1—C6	77.2 (5)	N11ⁱ—Cu—N11—C16	179.9 (5)
N11ⁱ—Cu—N1—C6	−76.9 (5)	C16—N11—C12—C13	0.8 (9)
C6—N1—C2—C3	−2.1 (9)	Cu—N11—C12—C13	−177.1 (5)
Cu—N1—C2—C3	175.6 (5)	C16—N11—C12—C12'	−179.2 (5)
C6—N1—C2—C2'	179.0 (5)	Cu—N11—C12—C12'	2.9 (6)
Cu—N1—C2—C2'	−3.3 (6)	N11—C12—C13—C14	−0.9 (10)
N1—C2—C3—C4	1.7 (10)	C12'—C12—C13—C14	179.0 (6)
C2'—C2—C3—C4	−179.5 (6)	C12—C13—C14—C15	1.0 (11)
C2—C3—C4—C5	−1.1 (11)	C13—C14—C15—C16	−0.9 (11)
C3—C4—C5—C6	1.0 (11)	C12—N11—C16—C15	−0.7 (9)
C2—N1—C6—C5	1.9 (9)	Cu—N11—C16—C15	176.9 (5)
Cu—N1—C6—C5	−175.4 (5)	C14—C15—C16—N11	0.8 (10)
C4—C5—C6—N1	−1.3 (10)	N1—Cu—N11'—C12'ⁱ	−87.6 (3)
N1—Cu—N1'—C2'	−1.3 (3)	N1ⁱ—Cu—N11'—C12'ⁱ	92.4 (3)
N1ⁱ—Cu—N1'—C2'	178.7 (3)	N11—Cu—N11'—C12'ⁱ	−178.6 (3)
N11—Cu—N1'—C2'	89.6 (3)	N11ⁱ—Cu—N11'—C12'ⁱ	1.4 (3)
N11ⁱ—Cu—N1'—C2'	−90.4 (3)	N1—Cu—N11'—C12'	92.4 (3)
N1—Cu—N1'—C2'ⁱ	178.7 (3)	N1ⁱ—Cu—N11'—C12'	−87.6 (3)
N1ⁱ—Cu—N1'—C2'ⁱ	−1.3 (3)	N11—Cu—N11'—C12'	1.4 (3)
N11—Cu—N1'—C2'ⁱ	−90.4 (3)	N11ⁱ—Cu—N11'—C12'	−178.6 (3)
N11ⁱ—Cu—N1'—C2'ⁱ	89.6 (3)	C12'ⁱ—N11'—C12'—C13'	−0.3 (4)
C2'ⁱ—N1'—C2'—C3'	−1.6 (4)	Cu—N11'—C12'—C13'	179.7 (4)
Cu—N1'—C2'—C3'	178.4 (4)	C12'ⁱ—N11'—C12'—C12	179.7 (6)
C2'ⁱ—N1'—C2'—C2	−180.0 (6)	Cu—N11'—C12'—C12	−0.3 (6)
Cu—N1'—C2'—C2	0.0 (6)	N11—C12—C12'—N11'	−1.9 (7)
N1—C2—C2'—N1'	2.3 (7)	C13—C12—C12'—N11'	178.1 (5)
C3—C2—C2'—N1'	−176.6 (5)	N11—C12—C12'—C13'	178.1 (5)
N1—C2—C2'—C3'	−176.0 (6)	C13—C12—C12'—C13'	−1.8 (10)
C3—C2—C2'—C3'	5.1 (10)	N11'—C12'—C13'—C14'	0.7 (9)
N1'—C2'—C3'—C4'	3.1 (9)	C12—C12'—C13'—C14'	−179.3 (5)
C2—C2'—C3'—C4'	−178.7 (5)	C12'—C13'—C14'—C13'ⁱ	−0.3 (4)
C2'—C3'—C4'—C3'ⁱ	−1.5 (4)

Symmetry code: (i) −x+1, −y+1/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O3Bⁱⁱ	0.85	1.74	2.55 (4)	158
O5—H5B···O2	0.85	2.32	3.032 (19)	142

Symmetry code: (ii) x, y+1/2, −z.

Experimental details

Crystal data
Chemical formula	[Cu(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O
M_r	746.99
Crystal system, space group	Tetragonal, I4₁/a
Temperature (K)	293
a, c (Å)	12.551 (2), 40.418 (5)
V (Å³)	6367.0 (16)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	0.92
Crystal size (mm)	0.6 × 0.5 × 0.4

Data collection
Diffractometer	Siemens P4/PC diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.637, 0.693
No. of measured, independent and observed [I > 2σ(I)] reflections	3081, 2808, 1368
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.063, 0.191, 0.88
No. of reflections	2808
No. of parameters	243
No. of restraints	18
H-atom treatment	H-atom parameters not refined
Δρ_max, Δρ_min (e Å⁻³)	0.36, −0.43

Computer programs: XSCANS (Siemens, 1993), XSCANS, SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), SHELXTL/PC (Sheldrick, 1990), SHELXL97.

Selected geometric parameters (Å, º) top

Cu—N1'	1.994 (7)	Cu—N1	2.178 (5)
Cu—N11'	2.009 (6)	Cu—N11	2.210 (5)

N1'—Cu—N11'	180.0	N1—Cu—N11	93.78 (18)
N1'—Cu—N1	77.37 (14)	N11—Cu—N11ⁱ	153.5 (3)
N11'—Cu—N1	102.63 (14)	N1—C2—C2'	115.3 (5)
N1—Cu—N1ⁱ	154.7 (3)	N1'—C2'—C2	115.0 (5)
N1'—Cu—N11	103.26 (14)	N11—C12—C12'	115.5 (5)
N11'—Cu—N11	76.74 (14)	N11'—C12'—C12	114.8 (5)

N1—C2—C2'—N1'	2.3 (7)	N11—C12—C12'—N11'	−1.9 (7)

Symmetry code: (i) −x+1, −y+1/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O3Bⁱⁱ	0.85	1.74	2.55 (4)	157.5
O5—H5B···O2	0.85	2.32	3.032 (19)	141.9

Symmetry code: (ii) x, y+1/2, −z.

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Bis(2,2':6',2''-ter­pyridine)copper(II) diperchlorate hemihydrate