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In the title compound, [Cu(ClO4)2(C3H10N2)2], the Cu atom is located at a center of symmetry. Despite asymmetric introduction of N-methyl groups into the ethyl­enedi­amine moieties, a second-order Jahn–Teller effect produces a typical semi-coordination trans-[CuN4(O2)] environment with long axial Cu—O bonds of 2.569 (2) Å. The Cu—N bond distances are 2.004 (2) and 2.057 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302213X/ob6313sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680302213X/ob6313Isup2.hkl
Contains datablock I

CCDC reference: 226645

Key indicators

  • Single-crystal X-ray study
  • T = 297 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.024
  • wR factor = 0.068
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cl1
Alert level C PLAT128_ALERT_4_C Non-standard setting of Space group P21/c .... P21/a PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O4 = 9.05 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O4
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: WinAFC Diffractometer Control Software (Rigaku, 1999); cell refinement: WinAFC Diffractometer 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); software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[Cu(ClO4)2(C3H10N2)2]F(000) = 422.0
Mr = 410.71Dx = 1.787 Mg m3
Monoclinic, P21/aMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2yabCell parameters from 25 reflections
a = 8.436 (3) Åθ = 10.1–15.0°
b = 11.857 (4) ŵ = 1.82 mm1
c = 8.352 (3) ÅT = 297 K
β = 113.96 (3)°Prismatic, blue
V = 763.4 (5) Å30.40 × 0.30 × 0.30 mm
Z = 2
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.008
ω–2θ scansθmax = 27.5°
Absorption correction: ψ scan
(North et al., 1968)
h = 104
Tmin = 0.524, Tmax = 0.579k = 015
2072 measured reflectionsl = 910
1749 independent reflections3 standard reflections every 150 reflections
1538 reflections with I > 2σ(I) intensity decay: 0.2%
Refinement top
Refinement on F2H-atom parameters not refined
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.0348P)2 + 0.3309P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.068(Δ/σ)max = 0.002
S = 1.08Δρmax = 0.33 e Å3
1538 reflectionsΔρmin = 0.29 e Å3
98 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Cu11.00000.00001.00000.0275 (1)
Cl10.73426 (6)0.07774 (4)1.21713 (7)0.0386 (1)
O10.8766 (3)0.1037 (2)1.3773 (3)0.0841 (7)
O20.7048 (4)0.0395 (2)1.2088 (4)0.0930 (8)
O30.5861 (2)0.1389 (2)1.2088 (3)0.0620 (5)
O40.7800 (2)0.1125 (2)1.0767 (2)0.0558 (4)
N11.1792 (2)0.1188 (1)1.1155 (2)0.0375 (4)
N21.1113 (2)0.0813 (1)1.2374 (2)0.0342 (3)
C11.2620 (3)0.0962 (2)1.3064 (3)0.0426 (5)
C21.2840 (3)0.0286 (2)1.3290 (3)0.0423 (5)
C31.1224 (4)0.2051 (2)1.2403 (3)0.0538 (6)
H11.12560.19091.09500.0444*
H21.26470.11681.06880.0444*
H31.18950.12331.36120.0512*
H41.37130.13291.35730.0512*
H51.36120.05471.28070.0512*
H61.32970.04721.45090.0512*
H71.04430.06161.30200.0415*
H81.17020.23201.35720.0658*
H91.19450.22891.18290.0658*
H101.00970.23701.17960.0658*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0281 (2)0.0271 (2)0.0255 (2)0.0012 (1)0.0092 (1)0.0008 (1)
Cl10.0434 (3)0.0384 (3)0.0437 (3)0.0084 (2)0.0276 (2)0.0067 (2)
O10.058 (1)0.144 (2)0.048 (1)0.003 (1)0.0189 (9)0.002 (1)
O20.133 (2)0.0392 (10)0.140 (2)0.000 (1)0.089 (2)0.010 (1)
O30.0506 (9)0.066 (1)0.087 (1)0.0160 (8)0.0456 (10)0.0089 (10)
O40.072 (1)0.0622 (10)0.0532 (9)0.0143 (8)0.0455 (9)0.0130 (8)
N10.0347 (8)0.0325 (8)0.0421 (9)0.0037 (6)0.0124 (7)0.0026 (7)
N20.0339 (8)0.0401 (8)0.0303 (7)0.0030 (7)0.0147 (6)0.0050 (6)
C10.0321 (9)0.059 (1)0.035 (1)0.0077 (9)0.0113 (8)0.0137 (9)
C20.0305 (9)0.063 (1)0.0306 (9)0.0041 (9)0.0092 (8)0.0052 (9)
C30.067 (2)0.044 (1)0.050 (1)0.008 (1)0.023 (1)0.0152 (10)
Geometric parameters (Å, º) top
Cu1—O42.569 (2)N2—C31.470 (3)
Cu1—N12.004 (2)N2—H70.955
Cu1—N22.057 (2)C1—C21.493 (3)
Cl1—O11.422 (2)C1—H30.956
Cl1—O21.409 (2)C1—H40.950
Cl1—O31.421 (2)C2—H50.948
Cl1—O41.435 (2)C2—H60.956
N1—C11.482 (3)C3—H80.948
N1—H10.950C3—H90.957
N1—H20.950C3—H100.955
N2—C21.481 (3)
N1—Cu1—O4i90.28 (7)Cu1—N2—H7106.7
N1—Cu1—O489.72 (7)C2—N2—C3111.7 (2)
N2—Cu1—O4i84.49 (7)C2—N2—H7106.8
N2—Cu1—O495.51 (7)C3—N2—H7106.4
N1—Cu1—N1i180.0N1—C1—C2107.2 (2)
N1—Cu1—N284.58 (7)N1—C1—H3109.9
N1—Cu1—N2i95.42 (7)N1—C1—H4110.3
N2—Cu1—N2i180.0C2—C1—H3110.1
O1—Cl1—O2108.9 (2)C2—C1—H4110.4
O1—Cl1—O3109.0 (1)H3—C1—H4109.0
O1—Cl1—O4107.6 (1)N2—C2—C1107.9 (2)
O2—Cl1—O3111.5 (2)N2—C2—H5110.1
O2—Cl1—O4110.1 (2)N2—C2—H6109.9
O3—Cl1—O4109.6 (1)C1—C2—H5110.0
Cu1—N1—C1108.9 (1)C1—C2—H6109.8
Cu1—N1—H1109.6H5—C2—H6109.1
Cu1—N1—H2109.6N2—C3—H8110.5
C1—N1—H1109.8N2—C3—H9109.7
C1—N1—H2109.4N2—C3—H10110.1
H1—N1—H2109.5H8—C3—H9109.0
Cu1—N2—C2105.6 (1)H8—C3—H10109.2
Cu1—N2—C3119.0 (1)H9—C3—H10108.4
Cu1—N1—C1—C239.1 (2)N1—Cu1—N2i—C3i35.5 (2)
Cu1—N1i—C1i—C2i39.1 (2)N1—C1—C2—N256.2 (2)
Cu1—N2—C2—C144.5 (2)N2—Cu1—N1—C111.6 (1)
Cu1—N2i—C2i—C1i44.5 (2)N2—Cu1—N1i—C1i168.4 (1)
N1—Cu1—N2—C218.1 (1)C1—C2—N2—C3175.3 (2)
N1—Cu1—N2—C3144.5 (2)C1—C2—N2—C3175.3 (2)
N1—Cu1—N2i—C2i161.9 (1)
Symmetry code: (i) x+2, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O40.953.013.250 (3)96
N2—H7···O10.962.643.460 (3)144
N2—H7···O20.962.663.376 (4)132
N2—H7···O40.963.063.442 (2)106
N1—H2···O3ii0.952.493.206 (2)132
N1—H1···O3iii0.952.313.158 (2)148
N1—H1···O4iii0.952.703.347 (2)126
Symmetry codes: (ii) x+1, y, z; (iii) x+1/2, y1/2, z.
 

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