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The title two compounds, [Cu2(C5H9O2)4(C4H8O2)]n, (I), and [Cu2(C6H11O2)4(C4H8O2)]n, (II), are isomorphous. The binuclear CuII units have a cage structure and are linked by the dioxane mol­ecules to form a zigzag chain along the c axis. The binuclear copper unit and the dioxane ligand each have a centre of symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100002304/qa0224sup1.cif
Contains datablocks cudiox, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100002304/qa0224Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100002304/qa0224IIsup3.hkl
Contains datablock II

CCDC references: 143321; 143322

Comment top

The magnetic -2 J values of the binuclear Cu unit of (I) and (II) were determined to be 387 and 363 cm-1, respectively (H = -2JS1·S2). The spin-exchange interaction through the dioxane bridge is negligible. The -2 J values of [Cu2(Me3CCOO)4L2] (L = pyridine and 2-methylpyridine) were reported to be 366 and 371 cm-1, respectively (Muto et al., 1986). Structures of dimeric copper(II)–3,3-dimethylbutyrate adducts have been reported recently, the -2 J values of [Cu2(Me3CCH2COO)4L2] (L = pyridine, 2-methylpyridine, 3-methylpyridine and 4-methylpyridine) being in the range 348–363 cm-1 (Goto et al., 2000).

Experimental top

A solution of 2,2-dimethylpropionic acid (613 mg, 6.0 mmol) in 0.25 M sodium hydroxide (50 ml) was neutralized with 0.25 M nitric acid. An aqueous solution of Cu(NO3)2.3H2O (725 mg, 3.0 mmol) was added. After the solution had been stirred for 15 min at room temperature, a green precipitate was collected and dissolved in dioxane. From the solution, blue crystals of (I) were grown by slow evaporation. 3,3-Dimethylbutyric acid (116 mg, 1.0 mmol) and CuCO3.Cu(OH)2.H2O (60 mg, 0.25 mmol) were suspended in a mixture of water and methanol (3:1, 20 ml). After the solution had been stirred for 1 h at room temperature, a green precipitate was collected and dissolved in dioxane. From the solution, blue crystals of (II) were grown by slow evaporation.

Refinement top

The positional parameters of all the H atoms were calculated geometrically and fixed with U(H) = 1.2 Ueq(parent atom). The max/min ratio of the atomic displacement parameters are abnormally large for the tert-butyl moieties in (I) and (II), which may be due to vibrational and rotational disorder.

Computing details top

For both compounds, data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[Cu2(C5H9O2)4(C4H8O2)]Z = 1
Mr = 619.70F(000) = 326
Triclinic, P1Dx = 1.278 Mg m3
a = 9.633 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.665 (1) ÅCell parameters from 25 reflections
c = 9.030 (2) Åθ = 10–15°
α = 112.28 (1)°µ = 1.36 mm1
β = 110.19 (2)°T = 297 K
γ = 83.72 (1)°Prism, blue
V = 805.4 (3) Å30.5 × 0.1 × 0.1 mm
Data collection top
Rigaku AFC-7R
diffractometer
2697 reflections with I > 2σ(I)
Radiation source: Rigaku rotating anodeRint = 0.091
Graphite monochromatorθmax = 30°, θmin = 2.5°
θ–2θ scansh = 014
Absorption correction: integration
(Coppens et al., 1965)
k = 1515
Tmin = 0.829, Tmax = 0.886l = 1313
4955 measured reflections3 standard reflections every 150 reflections
4697 independent reflections intensity decay: 3.9%
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.051H-atom parameters not refined
wR(F2) = 0.070 w = 1/[σ2(Fo) + 0.00250|Fo|2]
S = 1.08(Δ/σ)max = 0.008
2697 reflectionsΔρmax = 0.58 e Å3
163 parametersΔρmin = 0.65 e Å3
Crystal data top
[Cu2(C5H9O2)4(C4H8O2)]γ = 83.72 (1)°
Mr = 619.70V = 805.4 (3) Å3
Triclinic, P1Z = 1
a = 9.633 (2) ÅMo Kα radiation
b = 10.665 (1) ŵ = 1.36 mm1
c = 9.030 (2) ÅT = 297 K
α = 112.28 (1)°0.5 × 0.1 × 0.1 mm
β = 110.19 (2)°
Data collection top
Rigaku AFC-7R
diffractometer
2697 reflections with I > 2σ(I)
Absorption correction: integration
(Coppens et al., 1965)
Rint = 0.091
Tmin = 0.829, Tmax = 0.8863 standard reflections every 150 reflections
4955 measured reflections intensity decay: 3.9%
4697 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.070H-atom parameters not refined
S = 1.08Δρmax = 0.58 e Å3
2697 reflectionsΔρmin = 0.65 e Å3
163 parameters
Special details top

Refinement. Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.97163 (6)0.49209 (5)0.12465 (6)0.0428 (1)
O11.1625 (4)0.4033 (4)0.1703 (4)0.0621 (10)
O21.2094 (4)0.4159 (4)0.0478 (4)0.0631 (10)
O30.8783 (4)0.3185 (3)0.0383 (4)0.0648 (10)
O40.9248 (4)0.3317 (3)0.2561 (4)0.0623 (9)
O50.9105 (3)0.4752 (3)0.3303 (3)0.0568 (9)
C11.2413 (5)0.3810 (4)0.0786 (5)0.052 (1)
C21.3846 (6)0.3070 (7)0.1191 (8)0.078 (2)
C31.407 (1)0.270 (2)0.267 (2)0.290 (9)
C41.5108 (9)0.386 (1)0.139 (2)0.219 (7)
C51.372 (1)0.174 (1)0.028 (2)0.238 (6)
C60.8739 (5)0.2716 (4)0.1898 (5)0.053 (1)
C70.8008 (7)0.1305 (6)0.2994 (7)0.078 (2)
C80.898 (1)0.0314 (8)0.235 (2)0.195 (5)
C90.789 (1)0.0917 (8)0.4835 (9)0.144 (3)
C100.655 (1)0.131 (1)0.282 (2)0.261 (6)
C110.9621 (7)0.3684 (5)0.3917 (6)0.073 (2)
C121.1046 (6)0.4061 (6)0.5323 (6)0.074 (2)
H11.32340.21630.24640.3484*
H21.49510.21860.28590.3484*
H31.41610.35080.36560.3484*
H41.59980.33600.16180.2623*
H51.49420.40210.03680.2623*
H61.52050.47100.23190.2623*
H71.28840.12250.04450.2847*
H81.35750.19200.12870.2847*
H91.46020.12440.00390.2847*
H100.85410.05780.29820.2340*
H110.99300.03300.24650.2340*
H120.91000.05530.11700.2340*
H130.74680.00180.54770.1722*
H140.72670.15440.52860.1722*
H150.88560.09450.49070.1722*
H160.66620.15620.16490.3138*
H170.59410.19490.32570.3138*
H180.61020.04210.34520.3138*
H190.89000.34840.43170.0872*
H200.97520.28950.30090.0872*
H211.17750.42400.49190.0894*
H221.13570.33250.57190.0894*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0521 (3)0.0552 (3)0.0294 (2)0.0001 (2)0.0177 (2)0.0199 (2)
O10.064 (2)0.086 (2)0.053 (2)0.015 (2)0.028 (1)0.039 (2)
O20.063 (2)0.089 (2)0.058 (2)0.016 (2)0.031 (2)0.042 (2)
O30.087 (2)0.066 (2)0.045 (2)0.020 (2)0.026 (2)0.016 (1)
O40.084 (2)0.063 (2)0.044 (1)0.013 (2)0.026 (2)0.015 (1)
O50.070 (2)0.077 (2)0.036 (1)0.001 (2)0.025 (1)0.028 (1)
C10.051 (2)0.060 (3)0.049 (2)0.004 (2)0.017 (2)0.024 (2)
C20.064 (3)0.103 (4)0.084 (4)0.020 (3)0.032 (3)0.052 (3)
C30.20 (1)0.58 (3)0.31 (2)0.26 (2)0.17 (1)0.38 (2)
C40.057 (4)0.26 (1)0.38 (2)0.004 (6)0.016 (8)0.21 (2)
C50.19 (1)0.16 (1)0.25 (2)0.113 (9)0.04 (1)0.02 (1)
C60.055 (2)0.057 (3)0.046 (2)0.003 (2)0.016 (2)0.018 (2)
C70.096 (4)0.064 (3)0.064 (3)0.021 (3)0.025 (3)0.008 (2)
C80.27 (1)0.067 (5)0.19 (1)0.015 (7)0.01 (1)0.054 (6)
C90.24 (1)0.093 (5)0.067 (4)0.055 (6)0.038 (6)0.009 (4)
C100.19 (1)0.25 (1)0.25 (1)0.165 (10)0.15 (1)0.13 (1)
C110.124 (5)0.063 (3)0.046 (2)0.007 (3)0.041 (3)0.022 (2)
C120.099 (4)0.093 (4)0.061 (3)0.038 (3)0.051 (3)0.047 (3)
Geometric parameters (Å, º) top
Cu1—Cu1i2.560 (1)C5—H70.961
Cu1—O11.959 (3)C5—H80.960
Cu1—O2i1.947 (3)C5—H90.960
Cu1—O31.946 (3)C6—C71.537 (6)
Cu1—O4i1.959 (3)C7—C81.49 (1)
Cu1—O52.205 (2)C7—C91.518 (9)
O1—C11.251 (5)C7—C101.46 (1)
O2—C11.261 (5)C8—H100.960
O3—C61.253 (5)C8—H110.960
O4—C61.253 (5)C8—H120.960
O5—C111.419 (6)C9—H130.960
O5—C12ii1.434 (6)C9—H140.960
C1—C21.515 (7)C9—H150.960
C2—C31.48 (1)C10—H160.959
C2—C41.47 (1)C10—H170.961
C2—C51.51 (1)C10—H180.960
C3—H10.960C11—C121.479 (8)
C3—H20.960C11—H190.960
C3—H30.959C11—H200.960
C4—H40.960C12—H210.960
C4—H50.960C12—H220.960
C4—H60.961
Cu1···Cu1i2.560 (1)O4···C12iii3.320 (6)
O2···C12iii3.534 (5)O4···C11iii3.487 (5)
Cu1i—Cu1—O185.3 (1)C2—C5—H8109.5
Cu1i—Cu1—O2i84.7 (1)C2—C5—H9109.5
Cu1i—Cu1—O384.5 (1)H7—C5—H8109.4
Cu1i—Cu1—O4i85.4 (1)H7—C5—H9109.4
Cu1i—Cu1—O5176.9 (1)H8—C5—H9109.5
O1—Cu1—O2i170.0 (1)O3—C6—O4124.5 (4)
O1—Cu1—O389.4 (2)O3—C6—C7116.7 (4)
O1—Cu1—O4i89.2 (1)O4—C6—C7118.8 (4)
O1—Cu1—O596.9 (1)C6—C7—C8107.2 (6)
O2i—Cu1—O390.2 (2)C6—C7—C9111.4 (5)
O2i—Cu1—O4i89.5 (2)C6—C7—C10108.3 (6)
O2i—Cu1—O593.1 (1)C8—C7—C9107.7 (7)
O3—Cu1—O4i169.9 (1)C8—C7—C10110.8 (10)
O3—Cu1—O593.4 (1)C9—C7—C10111.3 (8)
O4i—Cu1—O596.7 (1)C7—C8—H10109.4
Cu1—O1—C1122.3 (3)C7—C8—H11109.5
Cu1i—O2—C1123.4 (3)C7—C8—H12109.5
Cu1—O3—C6123.6 (3)H10—C8—H11109.5
Cu1i—O4—C6121.9 (3)H10—C8—H12109.5
Cu1—O5—C11121.6 (3)H11—C8—H12109.5
Cu1—O5—C12ii120.9 (3)C7—C9—H13109.5
C11—O5—C12ii108.7 (3)C7—C9—H14109.5
O1—C1—O2124.2 (4)C7—C9—H15109.5
O1—C1—C2118.9 (4)H13—C9—H14109.5
O2—C1—C2116.9 (4)H13—C9—H15109.5
C1—C2—C3111.2 (5)H14—C9—H15109.5
C1—C2—C4111.0 (6)C7—C10—H16109.5
C1—C2—C5107.9 (6)C7—C10—H17109.4
C3—C2—C4112.7 (10)C7—C10—H18109.5
C3—C2—C5105.6 (10)H16—C10—H17109.5
C4—C2—C5108.2 (9)H16—C10—H18109.6
C2—C3—H1109.4H17—C10—H18109.4
C2—C3—H2109.4O5—C11—C12111.2 (4)
C2—C3—H3109.5O5—C11—H19109.0
H1—C3—H2109.5O5—C11—H20109.0
H1—C3—H3109.5C12—C11—H19109.0
H2—C3—H3109.5C12—C11—H20109.0
C2—C4—H4109.5H19—C11—H20109.5
C2—C4—H5109.5O5ii—C12—C11110.6 (4)
C2—C4—H6109.4O5ii—C12—H21109.2
H4—C4—H5109.5O5ii—C12—H22109.2
H4—C4—H6109.5C11—C12—H21109.2
H5—C4—H6109.4C11—C12—H22109.2
C2—C5—H7109.5H21—C12—H22109.5
Symmetry codes: (i) x+2, y+1, z; (ii) x+2, y+1, z+1; (iii) x, y, z1.
(II) top
Crystal data top
[Cu2(C6H11O2)4(C4H8O2)]Z = 1
Mr = 675.81Dx = 1.267 Mg m3
Triclinic, P1Mo Kα radiation, λ = 0.71073 Å
a = 10.080 (1) ÅCell parameters from 25 reflections
b = 11.308 (2) Åθ = 10–15°
c = 8.952 (1) ŵ = 1.25 mm1
α = 113.30 (1)°T = 298 K
β = 108.92 (1)°Prism, blue
γ = 84.64 (1)°0.4 × 0.4 × 0.4 mm
V = 885.8 (2) Å3
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.01
θ–2θ scansθmax = 30°
Absorption correction: integration
(Coppens et al., 1965)
h = 1414
Tmin = 0.559, Tmax = 0.665k = 160
5397 measured reflectionsl = 1313
5156 independent reflections3 standard reflections every 150 reflections
3998 reflections with I > 2σ(I) intensity decay: 2.4%
Refinement top
Refinement on FH-atom parameters not refined
R[F2 > 2σ(F2)] = 0.041 w = 1/[σ2(Fo) + 0.00250|Fo|2]
wR(F2) = 0.075(Δ/σ)max = 0.048
S = 1.07Δρmax = 0.48 e Å3
5155 reflectionsΔρmin = 0.37 e Å3
181 parameters
Crystal data top
[Cu2(C6H11O2)4(C4H8O2)]γ = 84.64 (1)°
Mr = 675.81V = 885.8 (2) Å3
Triclinic, P1Z = 1
a = 10.080 (1) ÅMo Kα radiation
b = 11.308 (2) ŵ = 1.25 mm1
c = 8.952 (1) ÅT = 298 K
α = 113.30 (1)°0.4 × 0.4 × 0.4 mm
β = 108.92 (1)°
Data collection top
Rigaku AFC-7R
diffractometer
3998 reflections with I > 2σ(I)
Absorption correction: integration
(Coppens et al., 1965)
Rint = 0.01
Tmin = 0.559, Tmax = 0.6653 standard reflections every 150 reflections
5397 measured reflections intensity decay: 2.4%
5156 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041181 parameters
wR(F2) = 0.075H-atom parameters not refined
S = 1.07Δρmax = 0.48 e Å3
5155 reflectionsΔρmin = 0.37 e Å3
Special details top

Refinement. Refinement using reflections with F2 > -10.0 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
Cu10.47683 (3)0.00999 (3)0.12658 (3)0.04156 (9)
O10.5023 (2)0.1785 (2)0.2370 (2)0.0566 (5)
O20.5393 (3)0.1953 (2)0.0127 (3)0.0622 (6)
O30.2804 (2)0.0087 (2)0.0096 (3)0.0573 (6)
O40.3195 (2)0.0239 (2)0.2138 (3)0.0607 (6)
O50.4197 (2)0.0394 (2)0.3268 (2)0.0483 (5)
C10.5297 (3)0.2428 (2)0.1626 (3)0.0510 (6)
C20.5544 (3)0.3869 (3)0.2578 (4)0.0617 (8)
C30.7072 (4)0.4326 (3)0.3426 (6)0.078 (1)
C40.7652 (8)0.3744 (7)0.482 (1)0.197 (3)
C50.7172 (5)0.5773 (3)0.4375 (6)0.088 (1)
C60.7944 (7)0.3900 (6)0.232 (1)0.169 (3)
C70.2405 (3)0.0256 (3)0.1286 (3)0.0514 (6)
C80.0878 (3)0.0515 (3)0.1947 (4)0.0604 (8)
C90.0553 (3)0.1953 (3)0.1346 (5)0.0690 (10)
C100.1290 (6)0.2627 (6)0.203 (1)0.132 (3)
C110.1008 (5)0.2567 (5)0.0592 (7)0.115 (2)
C120.1034 (4)0.2051 (5)0.2042 (7)0.104 (2)
C130.3809 (3)0.0679 (3)0.4551 (3)0.0522 (7)
C140.5077 (3)0.1312 (2)0.6046 (3)0.0528 (7)
H10.51190.42680.17770.0741*
H20.50960.41420.34510.0741*
H30.70930.40090.55810.2361*
H40.76130.28210.42830.2361*
H50.86070.40460.54690.2361*
H60.81250.60430.50720.1052*
H70.68750.61790.35650.1052*
H80.65780.60180.50900.1052*
H90.79050.29750.18010.2036*
H100.76100.42370.14370.2036*
H110.88960.42040.29780.2036*
H120.05920.01550.31760.0725*
H130.03470.00990.15630.0725*
H140.22870.25640.15910.1587*
H150.09930.22300.32600.1587*
H160.10590.35190.16800.1587*
H170.20050.25150.10410.1379*
H180.07630.34560.09510.1379*
H190.05420.21230.10110.1379*
H200.12680.29410.16820.1251*
H210.13330.16580.32700.1251*
H220.14970.16150.16100.1251*
H230.33640.12930.40710.0627*
H240.31670.03840.49330.0627*
H250.47900.20000.69180.0634*
H260.56950.16530.56790.0634*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0514 (2)0.0463 (2)0.0293 (1)0.0001 (1)0.0148 (1)0.0148 (1)
O10.070 (1)0.0506 (10)0.0481 (9)0.0057 (9)0.0252 (9)0.0102 (8)
O20.092 (2)0.049 (1)0.0478 (10)0.0005 (10)0.0259 (10)0.0164 (8)
O30.054 (1)0.073 (1)0.053 (1)0.0003 (9)0.0155 (8)0.0324 (9)
O40.057 (1)0.085 (1)0.0453 (9)0.0089 (10)0.0175 (8)0.0303 (10)
O50.061 (1)0.0556 (10)0.0344 (7)0.0045 (8)0.0177 (7)0.0214 (7)
C10.053 (1)0.046 (1)0.049 (1)0.002 (1)0.017 (1)0.0119 (10)
C20.069 (2)0.045 (1)0.068 (2)0.005 (1)0.029 (1)0.012 (1)
C30.067 (2)0.048 (2)0.107 (3)0.005 (1)0.031 (2)0.014 (2)
C40.166 (6)0.114 (5)0.224 (8)0.041 (4)0.096 (6)0.091 (5)
C50.111 (3)0.051 (2)0.095 (3)0.018 (2)0.044 (2)0.008 (2)
C60.139 (5)0.107 (4)0.228 (8)0.045 (4)0.131 (6)0.040 (4)
C70.051 (1)0.056 (1)0.044 (1)0.002 (1)0.0104 (10)0.018 (1)
C80.046 (1)0.077 (2)0.056 (1)0.003 (1)0.009 (1)0.028 (1)
C90.048 (2)0.075 (2)0.085 (2)0.009 (1)0.019 (1)0.036 (2)
C100.099 (3)0.117 (4)0.242 (8)0.023 (3)0.070 (4)0.123 (5)
C110.079 (3)0.116 (4)0.092 (3)0.032 (3)0.013 (2)0.001 (3)
C120.056 (2)0.134 (4)0.125 (4)0.025 (2)0.017 (2)0.066 (3)
C130.062 (1)0.061 (1)0.047 (1)0.017 (1)0.027 (1)0.028 (1)
C140.075 (2)0.046 (1)0.043 (1)0.007 (1)0.024 (1)0.0205 (10)
Geometric parameters (Å, º) top
Cu1—Cu1i2.553 (1)C6—H90.960
Cu1—O11.964 (2)C6—H100.959
Cu1—O2i1.959 (2)C6—H110.961
Cu1—O31.953 (2)C7—C81.505 (4)
Cu1—O4i1.961 (2)C8—C91.537 (5)
Cu1—O52.198 (2)C8—H120.960
O1—C11.260 (3)C8—H130.960
O2—C11.266 (3)C9—C101.511 (6)
O3—C71.257 (3)C9—C111.515 (6)
O4—C71.263 (3)C9—C121.528 (5)
O5—C131.430 (3)C10—H140.961
O5—C14ii1.435 (3)C10—H150.959
C1—C21.510 (4)C10—H160.961
C2—C31.515 (5)C11—H170.960
C2—H10.960C11—H180.961
C2—H20.960C11—H190.959
C3—C41.564 (8)C12—H200.960
C3—C51.512 (4)C12—H210.960
C3—C61.450 (7)C12—H220.961
C4—H30.961C13—C141.497 (4)
C4—H40.960C13—H230.960
C4—H50.960C13—H240.960
C5—H60.960C14—H250.960
C5—H70.960C14—H260.960
C5—H80.960
Cu1···Cu1i2.5526 (5)O4···C13iii3.440 (3)
O2···C14iii3.341 (3)O5···C12iv3.479 (5)
O4···C14iii3.421 (3)
Cu1i—Cu1—O186.3 (1)C3—C6—H10109.5
Cu1i—Cu1—O2i84.5 (1)C3—C6—H11109.4
Cu1i—Cu1—O384.8 (1)H9—C6—H10109.6
Cu1i—Cu1—O4i85.8 (1)H9—C6—H11109.4
Cu1i—Cu1—O5174.6 (1)H10—C6—H11109.5
O1—Cu1—O2i170.7 (1)O3—C7—O4124.6 (3)
O1—Cu1—O389.4 (1)O3—C7—C8117.2 (2)
O1—Cu1—O4i89.3 (1)O4—C7—C8118.2 (2)
O1—Cu1—O597.4 (1)C7—C8—C9114.1 (2)
O2i—Cu1—O390.8 (1)C7—C8—H12108.3
O2i—Cu1—O4i89.1 (1)C7—C8—H13108.3
O2i—Cu1—O591.9 (1)C9—C8—H12108.3
O3—Cu1—O4i170.5 (1)C9—C8—H13108.3
O3—Cu1—O591.2 (1)H12—C8—H13109.5
O4i—Cu1—O598.3 (1)C8—C9—C10110.0 (4)
Cu1—O1—C1121.1 (2)C8—C9—C11110.1 (3)
Cu1i—O2—C1123.4 (2)C8—C9—C12107.7 (3)
Cu1—O3—C7123.1 (2)C10—C9—C11110.4 (4)
Cu1i—O4—C7121.5 (2)C10—C9—C12109.8 (4)
Cu1—O5—C13119.7 (1)C11—C9—C12108.9 (3)
Cu1—O5—C14ii119.7 (1)C9—C10—H14109.4
C13—O5—C14ii111.1 (2)C9—C10—H15109.5
O1—C1—O2124.7 (2)C9—C10—H16109.4
O1—C1—C2118.4 (2)H14—C10—H15109.5
O2—C1—C2116.9 (2)H14—C10—H16109.4
C1—C2—C3115.0 (3)H15—C10—H16109.5
C1—C2—H1108.1C9—C11—H17109.5
C1—C2—H2108.1C9—C11—H18109.4
C3—C2—H1108.1C9—C11—H19109.5
C3—C2—H2108.1H17—C11—H18109.4
H1—C2—H2109.5H17—C11—H19109.6
C2—C3—C4105.1 (4)H18—C11—H19109.5
C2—C3—C5109.7 (3)C9—C12—H20109.5
C2—C3—C6115.7 (4)C9—C12—H21109.5
C4—C3—C5106.3 (4)C9—C12—H22109.4
C4—C3—C6107.5 (6)H20—C12—H21109.5
C5—C3—C6112.0 (4)H20—C12—H22109.4
C3—C4—H3109.5H21—C12—H22109.5
C3—C4—H4109.6O5—C13—C14110.6 (2)
C3—C4—H5109.6O5—C13—H23109.2
H3—C4—H4109.4O5—C13—H24109.2
H3—C4—H5109.3C14—C13—H23109.2
H4—C4—H5109.5C14—C13—H24109.2
C3—C5—H6109.5H23—C13—H24109.5
C3—C5—H7109.5O5ii—C14—C13110.2 (2)
C3—C5—H8109.5O5ii—C14—H25109.3
H6—C5—H7109.4O5ii—C14—H26109.3
H6—C5—H8109.5C13—C14—H25109.3
H7—C5—H8109.4C13—C14—H26109.3
C3—C6—H9109.4H25—C14—H26109.5
Symmetry codes: (i) x+1, y, z; (ii) x+1, y, z+1; (iii) x, y, z1; (iv) x, y, z.

Experimental details

(I)(II)
Crystal data
Chemical formula[Cu2(C5H9O2)4(C4H8O2)][Cu2(C6H11O2)4(C4H8O2)]
Mr619.70675.81
Crystal system, space groupTriclinic, P1Triclinic, P1
Temperature (K)297298
a, b, c (Å)9.633 (2), 10.665 (1), 9.030 (2)10.080 (1), 11.308 (2), 8.952 (1)
α, β, γ (°)112.28 (1), 110.19 (2), 83.72 (1)113.30 (1), 108.92 (1), 84.64 (1)
V3)805.4 (3)885.8 (2)
Z11
Radiation typeMo KαMo Kα
µ (mm1)1.361.25
Crystal size (mm)0.5 × 0.1 × 0.10.4 × 0.4 × 0.4
Data collection
DiffractometerRigaku AFC-7R
diffractometer
Rigaku AFC-7R
diffractometer
Absorption correctionIntegration
(Coppens et al., 1965)
Integration
(Coppens et al., 1965)
Tmin, Tmax0.829, 0.8860.559, 0.665
No. of measured, independent and
observed [I > 2σ(I)] reflections
4955, 4697, 2697 5397, 5156, 3998
Rint0.0910.01
(sin θ/λ)max1)0.7030.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.070, 1.08 0.041, 0.075, 1.07
No. of reflections26975155
No. of parameters163181
No. of restraints0?
H-atom treatmentH-atom parameters not refinedH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.58, 0.650.48, 0.37

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), TEXSAN.

Selected geometric parameters (Å, º) for (I) top
Cu1—Cu1i2.560 (1)Cu1—O52.205 (2)
Cu1—O11.959 (3)O1—C11.251 (5)
Cu1—O2i1.947 (3)O2—C11.261 (5)
Cu1—O31.946 (3)O3—C61.253 (5)
Cu1—O4i1.959 (3)O4—C61.253 (5)
O1—Cu1—O2i170.0 (1)O1—C1—O2124.2 (4)
O3—Cu1—O4i169.9 (1)O3—C6—O4124.5 (4)
Symmetry code: (i) x+2, y+1, z.
Selected geometric parameters (Å, º) for (II) top
Cu1—Cu1i2.553 (1)Cu1—O52.198 (2)
Cu1—O11.964 (2)O1—C11.260 (3)
Cu1—O2i1.959 (2)O2—C11.266 (3)
Cu1—O31.953 (2)O3—C71.257 (3)
Cu1—O4i1.961 (2)O4—C71.263 (3)
O1—Cu1—O2i170.7 (1)O1—C1—O2124.7 (2)
O3—Cu1—O4i170.5 (1)O3—C7—O4124.6 (3)
Symmetry code: (i) x+1, y, z.
 

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