Bis(N,N-di­methyl­ethyl­enedi­amine-κ²N,N′)­bis­(perchlorato-κO)copper(II)

In the title compound, [Cu(ClO₄)₂(C₄H₁₂N₂)₂], the Cu atom is located at a center of symmetry. It adopts an elongated octahedral trans-[CuN₄O₂] coordination geometry, which is a typical feature of the pseudo-Jahn–Teller effect. The axial Cu—O bond length is 2.605 (4) Å, while the in-plane Cu—N bond lengths are 1.987 (2) and 2.098 (2) Å.

Key indicators

• Single-crystal X-ray study
• T = 297 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.031
• wR factor = 0.113
• Data-to-parameter ratio = 17.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....        Cl1
PLAT480_ALERT_4_B Long H...A H-Bond Reported H2     ..  O1       =       3.01 Ang.

Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced ..........          ?
PLAT156_ALERT_4_C Axial System Input Cell not Standard ...........          ?
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....         O1
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        Cu1
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2     ..  O4       =       2.62 Ang.
PLAT482_ALERT_4_C Small D-H..A Angle Rep for N1     ..  O1       =      99.00 Deg.

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: WinAFC Diffractmeter Control Software (Rigaku, 1999); cell refinement: WinAFC Diffractmeter Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 2001); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

(I)

Crystal data

[Cu(ClO4)2(C4H12N2)2]	Z = 1
Mr = 438.76	F(000) = 227.0
Triclinic, P1	Dx = 1.668 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.7107 Å
a = 7.978 (4) Å	Cell parameters from 17 reflections
b = 8.593 (4) Å	θ = 11.2–12.4°
c = 7.797 (8) Å	µ = 1.60 mm^−1
α = 111.01 (6)°	T = 297 K
β = 104.91 (6)°	Prismatic, blue
γ = 61.65 (3)°	0.30 × 0.30 × 0.20 mm
V = 436.7 (6) Å^3

Data collection

Rigaku AFC-7R diffractometer	Rint = 0.061
ω–2θ scans	θmax = 27.5°
Absorption correction: ψ scan (North et al., 1968)	h = −10→10
Tmin = 0.625, Tmax = 0.726	k = −11→10
2269 measured reflections	l = −4→10
2007 independent reflections	3 standard reflections every 150 reflections
1894 reflections with I > 2σ(I)	intensity decay: 2.5%

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + (0.0348P)^2 + 0.3309P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.031	(Δ/σ)max = 0.001
wR(F^2) = 0.113	Δρmax = 0.41 e Å^−3
S = 0.91	Δρmin = −0.48 e Å^−3
1894 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
107 parameters	Extinction coefficient: 0.0234
H-atom parameters not refined

Special details

Refinement. Refinement using reflections with F² > 0.0 σ(F²). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cu1	1.0000	0.0000	1.0000	0.0299 (2)
Cl1	0.69554 (8)	−0.03463 (9)	1.28417 (8)	0.0424 (2)
O1	0.7340 (4)	−0.0038 (4)	1.1324 (3)	0.0659 (6)
O2	0.6051 (5)	−0.1540 (5)	1.2124 (5)	0.095 (1)
O3	0.5763 (4)	0.1339 (4)	1.3993 (4)	0.0830 (8)
O4	0.8734 (4)	−0.1147 (5)	1.3878 (4)	0.097 (1)
N1	1.1934 (3)	−0.0955 (3)	1.1993 (3)	0.0373 (4)
N2	1.0633 (3)	−0.2773 (3)	0.8601 (3)	0.0371 (4)
C1	1.2861 (4)	−0.2994 (4)	1.1424 (4)	0.0486 (6)
C2	1.1470 (4)	−0.3695 (3)	1.0107 (4)	0.0442 (6)
C3	0.8964 (5)	−0.3159 (4)	0.7599 (4)	0.0555 (7)
C4	1.2046 (5)	−0.3542 (4)	0.7260 (4)	0.0546 (7)
H1	1.2883	−0.0499	1.2257	0.0442*
H2	1.1323	−0.0530	1.3075	0.0442*
H3	1.3973	−0.3415	1.0838	0.0566*
H4	1.3246	−0.3431	1.2493	0.0566*
H5	1.0477	−0.3452	1.0767	0.0522*
H6	1.2121	−0.4993	0.9596	0.0522*
H7	0.8030	−0.2693	0.8444	0.0656*
H8	0.8381	−0.2571	0.6639	0.0656*
H9	0.9347	−0.4446	0.7096	0.0656*
H10	1.2456	−0.4834	0.6779	0.0649*
H11	1.1498	−0.2984	0.6273	0.0649*
H12	1.3141	−0.3297	0.7870	0.0649*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0295 (2)	0.0287 (2)	0.0301 (2)	−0.0130 (2)	−0.0008 (1)	0.0085 (1)
Cl1	0.0358 (3)	0.0563 (4)	0.0394 (4)	−0.0226 (3)	0.0034 (3)	0.0142 (3)
O1	0.073 (1)	0.079 (2)	0.061 (1)	−0.035 (1)	0.020 (1)	0.023 (1)
O2	0.103 (2)	0.096 (2)	0.118 (3)	−0.072 (2)	0.017 (2)	0.020 (2)
O3	0.076 (2)	0.077 (2)	0.070 (2)	−0.009 (1)	0.030 (1)	0.011 (1)
O4	0.052 (1)	0.149 (3)	0.055 (1)	−0.011 (2)	−0.003 (1)	0.042 (2)
N1	0.0350 (10)	0.0375 (10)	0.0340 (9)	−0.0143 (8)	−0.0031 (8)	0.0102 (8)
N2	0.041 (1)	0.0328 (9)	0.0372 (10)	−0.0176 (8)	0.0011 (8)	0.0084 (8)
C1	0.047 (1)	0.037 (1)	0.051 (2)	−0.011 (1)	−0.005 (1)	0.018 (1)
C2	0.050 (1)	0.034 (1)	0.050 (1)	−0.017 (1)	0.001 (1)	0.016 (1)
C3	0.061 (2)	0.049 (1)	0.057 (2)	−0.035 (1)	−0.008 (1)	0.009 (1)
C4	0.066 (2)	0.045 (1)	0.050 (2)	−0.019 (1)	0.021 (1)	0.005 (1)

Geometric parameters (Å, º)

Cu1—O1	2.605 (4)	N2—C4	1.485 (4)
Cu1—N1	1.987 (2)	C1—C2	1.501 (4)
Cu1—N2	2.098 (2)	C1—H3	0.955
Cl1—O1	1.433 (4)	C1—H4	0.955
Cl1—O2	1.404 (4)	C2—H5	0.955
Cl1—O3	1.416 (3)	C2—H6	0.954
Cl1—O4	1.421 (3)	C3—H7	0.964
N1—C1	1.482 (3)	C3—H8	0.950
N1—H1	0.955	C3—H9	0.948
N1—H2	0.951	C4—H10	0.948
N2—C2	1.487 (4)	C4—H11	0.952
N2—C3	1.480 (4)	C4—H12	0.961
O1—Cu1—N1	90.9 (1)	N1—C1—H3	109.4
O1—Cu1—N2	85.65 (9)	N1—C1—H4	109.3
N1—Cu1—N2	85.40 (8)	C2—C1—H3	109.9
O1—Cl1—O2	108.2 (2)	C2—C1—H4	110.4
O1—Cl1—O3	110.5 (2)	H3—C1—H4	108.6
O1—Cl1—O4	107.8 (2)	N2—C2—C1	110.2 (3)
O2—Cl1—O3	110.1 (2)	N2—C2—H5	109.9
O2—Cl1—O4	110.9 (2)	N2—C2—H6	109.8
O3—Cl1—O4	109.2 (2)	C1—C2—H5	109.0
Cu1—O1—Cl1	143.3 (1)	C1—C2—H6	109.2
Cu1—N1—C1	110.8 (1)	H5—C2—H6	108.7
Cu1—N1—H1	109.0	N2—C3—H7	109.4
Cu1—N1—H2	109.2	N2—C3—H8	110.6
C1—N1—H1	109.5	N2—C3—H9	110.4
C1—N1—H2	109.4	H7—C3—H8	108.3
H1—N1—H2	109.0	H7—C3—H9	108.4
Cu1—N2—C2	103.5 (1)	H8—C3—H9	109.7
Cu1—N2—C3	115.3 (1)	N2—C4—H10	110.3
Cu1—N2—C4	111.7 (2)	N2—C4—H11	110.4
C2—N2—C3	108.4 (3)	N2—C4—H12	109.5
C2—N2—C4	110.3 (2)	H10—C4—H11	109.4
C3—N2—C4	107.6 (2)	H10—C4—H12	108.7
N1—C1—C2	109.2 (2)	H11—C4—H12	108.4
Cu1—O1—Cl1—O2	−131.5 (3)	O1—Cu1—N2—C3	48.6 (2)
Cu1—O1—Cl1—O3	107.9 (3)	O1—Cu1—N2—C4	171.8 (2)
Cu1—O1—Cl1—O4	−11.4 (3)	N1—Cu1—N2—C2	21.6 (2)
Cu1—N1—C1—C2	−29.8 (3)	N1—Cu1—N2—C3	139.8 (2)
Cu1—N2—C2—C1	−44.0 (2)	N1—Cu1—N2—C4	−96.9 (2)
Cl1—O1—Cu1—N1	6.1 (3)	N1—C1—C2—N2	50.5 (3)
Cl1—O1—Cu1—N2	91.4 (3)	N2—Cu1—N1—C1	4.2 (2)
O1—Cu1—N1—C1	89.8 (2)	C1—C2—N2—C3	−166.9 (2)
O1—Cu1—N2—C2	−69.6 (2)	C1—C2—N2—C4	75.6 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H2···O1	0.95	3.01	3.300 (4)	99
N1—H2···O4	0.95	2.62	3.348 (5)	133
N1—H1···O2^i	0.96	2.26	3.057 (5)	140

Symmetry code: (i) x+1, y, z.