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The title compound, [Cu2(C5H9O2)4(C5H5N)2], consists of centrosymmetric binuclear cage units with four dimethyl­propanoate bridges linking the two Cu centres [Cu...Cu = 2.6229 (9) Å]. The square-pyramidal Cu coordination is completed by a pyridine N atom at the apical site. A π–π stacking inter­action helps to consolidate the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806003217/hb6318sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806003217/hb6318Isup2.hkl
Contains datablock I

CCDC reference: 601177

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.045
  • wR factor = 0.103
  • Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density .... 4.16
Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.60 Ratio
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 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 2 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001; Atwood & Barbour, 2003); software used to prepare material for publication: X-SEED.

Tetrakis(µ2-2,2-dimethylpropanoato-κ2O,O')bis[(pyridine-κN)copper(II)] top
Crystal data top
[Cu2(C5H9O2)4(C5H5N)2]Z = 1
Mr = 689.77F(000) = 362
Triclinic, P1Dx = 1.341 Mg m3
a = 9.7378 (19) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.0428 (19) ÅCell parameters from 3879 reflections
c = 10.435 (2) Åθ = 2.2–28.3°
α = 61.520 (3)°µ = 1.29 mm1
β = 72.495 (3)°T = 273 K
γ = 84.200 (3)°Rectangular slab, blue-green
V = 854.3 (3) Å30.20 × 0.17 × 0.10 mm
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3317 independent reflections
Radiation source: fine-focus sealed tube2568 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.065
ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Blessing, 1995; Sheldrick, 2002)
h = 1212
Tmin = 0.782, Tmax = 0.882k = 1212
7897 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.0444P)2]
where P = (Fo2 + 2Fc2)/3
3317 reflections(Δ/σ)max < 0.001
197 parametersΔρmax = 1.31 e Å3
0 restraintsΔρmin = 0.32 e Å3
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
xyzUiso*/Ueq
Cu10.53805 (5)0.51037 (4)0.60540 (5)0.01396 (14)
O10.6364 (3)0.6977 (3)0.4285 (3)0.0266 (6)
O20.6970 (3)0.3896 (3)0.5557 (3)0.0247 (6)
O40.4223 (3)0.3191 (3)0.7536 (3)0.0252 (6)
O30.3628 (3)0.6231 (3)0.6283 (3)0.0258 (6)
C20.6375 (4)0.7465 (4)0.2922 (4)0.0177 (8)
C40.2828 (4)0.6514 (4)0.5440 (4)0.0168 (8)
N10.6276 (3)0.5346 (3)0.7588 (3)0.0156 (6)
C130.7283 (4)0.5532 (4)0.9731 (4)0.0226 (9)
H1310.76070.55841.04590.027*
C90.1052 (4)0.7394 (4)0.7166 (4)0.0269 (9)
H920.07960.63560.79230.040*
H930.02290.79960.72410.040*
H910.18210.77640.73290.040*
C110.7173 (4)0.4338 (4)0.8276 (4)0.0186 (8)
H1110.74560.35600.80230.022*
C150.5919 (4)0.6457 (4)0.7969 (4)0.0200 (8)
H1510.53210.71850.74880.024*
C120.7690 (4)0.4400 (4)0.9328 (4)0.0230 (8)
H1210.83130.36810.97690.028*
C80.0300 (4)0.6992 (5)0.5297 (5)0.0415 (12)
H810.05810.71540.42670.062*
H830.05240.75660.54520.062*
H820.00620.59330.59850.062*
C30.1539 (4)0.7500 (4)0.5592 (4)0.0190 (8)
C10.7140 (4)0.9011 (4)0.1788 (4)0.0223 (8)
C140.6378 (4)0.6588 (4)0.9021 (4)0.0236 (9)
H1410.60850.73770.92550.028*
C100.2059 (5)0.9132 (4)0.4389 (5)0.0433 (12)
H1010.28320.94410.45990.065*
H1020.12770.97910.44130.065*
H1030.23950.91880.33990.065*
C50.7305 (5)0.9423 (4)0.0151 (4)0.0330 (10)
H510.78840.87000.00980.049*
H530.77641.04180.05100.049*
H520.63710.94120.00210.049*
C70.6161 (5)1.0191 (4)0.2159 (5)0.0385 (11)
H730.52251.01270.20580.058*
H710.65901.11950.14630.058*
H720.60680.99760.31830.058*
C60.8584 (4)0.9107 (5)0.2017 (5)0.0382 (11)
H620.84440.88980.30480.057*
H630.90241.01070.13310.057*
H610.91980.83760.18180.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0172 (2)0.0130 (2)0.0126 (2)0.00579 (16)0.00687 (18)0.00621 (17)
O10.0369 (17)0.0241 (14)0.0152 (14)0.0065 (12)0.0104 (12)0.0032 (11)
O20.0281 (15)0.0340 (15)0.0277 (15)0.0188 (12)0.0173 (13)0.0245 (13)
O40.0371 (17)0.0217 (14)0.0161 (14)0.0056 (12)0.0077 (13)0.0070 (11)
O30.0283 (16)0.0357 (15)0.0243 (15)0.0187 (13)0.0164 (13)0.0208 (13)
C20.017 (2)0.0164 (18)0.019 (2)0.0057 (15)0.0038 (16)0.0099 (16)
C40.016 (2)0.0131 (17)0.0156 (19)0.0042 (15)0.0040 (16)0.0035 (15)
N10.0153 (16)0.0174 (15)0.0117 (15)0.0008 (12)0.0025 (13)0.0056 (13)
C130.025 (2)0.029 (2)0.014 (2)0.0059 (17)0.0050 (17)0.0097 (17)
C90.026 (2)0.034 (2)0.025 (2)0.0125 (18)0.0095 (18)0.0177 (18)
C110.023 (2)0.0149 (18)0.0169 (19)0.0044 (15)0.0074 (16)0.0067 (15)
C150.026 (2)0.0144 (18)0.021 (2)0.0056 (16)0.0101 (17)0.0083 (16)
C120.025 (2)0.0227 (19)0.021 (2)0.0059 (16)0.0119 (17)0.0072 (16)
C80.024 (2)0.077 (3)0.046 (3)0.023 (2)0.020 (2)0.045 (3)
C30.019 (2)0.0232 (19)0.0144 (19)0.0108 (16)0.0049 (16)0.0100 (16)
C10.024 (2)0.0208 (19)0.0160 (19)0.0030 (16)0.0050 (17)0.0034 (16)
C140.029 (2)0.0199 (19)0.024 (2)0.0004 (17)0.0043 (18)0.0138 (17)
C100.049 (3)0.025 (2)0.028 (2)0.021 (2)0.002 (2)0.0019 (19)
C50.042 (3)0.029 (2)0.022 (2)0.0099 (19)0.008 (2)0.0057 (18)
C70.043 (3)0.023 (2)0.039 (3)0.0013 (19)0.006 (2)0.009 (2)
C60.033 (3)0.040 (3)0.029 (2)0.009 (2)0.010 (2)0.005 (2)
Geometric parameters (Å, º) top
Cu1—O11.963 (2)C15—H1510.9300
Cu1—O31.968 (2)C12—H1210.9300
Cu1—O21.968 (2)C8—C31.519 (5)
Cu1—O41.977 (2)C8—H810.9600
Cu1—N12.153 (3)C8—H830.9600
Cu1—Cu1i2.6229 (9)C8—H820.9600
O1—C21.262 (4)C3—C101.530 (5)
O2—C4i1.250 (4)C1—C51.513 (5)
O4—C2i1.243 (4)C1—C61.515 (5)
O3—C41.261 (4)C1—C71.565 (5)
C2—C11.523 (5)C14—H1410.9300
C4—C31.537 (4)C10—H1010.9600
N1—C151.336 (4)C10—H1020.9600
N1—C111.345 (4)C10—H1030.9600
C13—C121.375 (5)C5—H510.9600
C13—C141.381 (5)C5—H530.9600
C13—H1310.9300C5—H520.9600
C9—C31.519 (5)C7—H730.9600
C9—H920.9600C7—H710.9600
C9—H930.9600C7—H720.9600
C9—H910.9600C6—H620.9600
C11—C121.366 (5)C6—H630.9600
C11—H1110.9300C6—H610.9600
C15—C141.367 (5)
O1—Cu1—O388.90 (11)C3—C8—H81109.5
O1—Cu1—O291.07 (11)C3—C8—H83109.5
O3—Cu1—O2168.32 (9)H81—C8—H83109.5
O1—Cu1—O4168.25 (10)C3—C8—H82109.5
O3—Cu1—O489.10 (11)H81—C8—H82109.5
O2—Cu1—O488.56 (11)H83—C8—H82109.5
O1—Cu1—N193.71 (10)C9—C3—C8109.7 (3)
O3—Cu1—N198.69 (10)C9—C3—C10109.7 (3)
O2—Cu1—N192.97 (10)C8—C3—C10110.5 (3)
O4—Cu1—N198.04 (10)C9—C3—C4111.1 (3)
O1—Cu1—Cu1i81.23 (7)C8—C3—C4109.5 (3)
O3—Cu1—Cu1i86.46 (7)C10—C3—C4106.3 (3)
O2—Cu1—Cu1i81.99 (7)C5—C1—C6111.1 (3)
O4—Cu1—Cu1i87.09 (7)C5—C1—C2113.0 (3)
N1—Cu1—Cu1i172.75 (8)C6—C1—C2110.8 (3)
C2—O1—Cu1126.8 (2)C5—C1—C7107.8 (3)
C4i—O2—Cu1125.9 (2)C6—C1—C7107.8 (3)
C2i—O4—Cu1119.6 (2)C2—C1—C7106.0 (3)
C4—O3—Cu1120.4 (2)C15—C14—C13119.0 (3)
O4i—C2—O1125.2 (3)C15—C14—H141120.5
O4i—C2—C1118.9 (3)C13—C14—H141120.5
O1—C2—C1115.9 (3)C3—C10—H101109.5
O2i—C4—O3125.1 (3)C3—C10—H102109.5
O2i—C4—C3116.9 (3)H101—C10—H102109.5
O3—C4—C3117.9 (3)C3—C10—H103109.5
C15—N1—C11116.3 (3)H101—C10—H103109.5
C15—N1—Cu1122.1 (2)H102—C10—H103109.5
C11—N1—Cu1121.6 (2)C1—C5—H51109.5
C12—C13—C14117.9 (3)C1—C5—H53109.5
C12—C13—H131121.1H51—C5—H53109.5
C14—C13—H131121.1C1—C5—H52109.5
C3—C9—H92109.5H51—C5—H52109.5
C3—C9—H93109.5H53—C5—H52109.5
H92—C9—H93109.5C1—C7—H73109.5
C3—C9—H91109.5C1—C7—H71109.5
H92—C9—H91109.5H73—C7—H71109.5
H93—C9—H91109.5C1—C7—H72109.5
N1—C11—C12123.2 (3)H73—C7—H72109.5
N1—C11—H111118.4H71—C7—H72109.5
C12—C11—H111118.4C1—C6—H62109.5
N1—C15—C14124.0 (3)C1—C6—H63109.5
N1—C15—H151118.0H62—C6—H63109.5
C14—C15—H151118.0C1—C6—H61109.5
C11—C12—C13119.7 (3)H62—C6—H61109.5
C11—C12—H121120.2H63—C6—H61109.5
C13—C12—H121120.2
O3—Cu1—O1—C287.0 (3)O1—Cu1—N1—C11115.9 (3)
O2—Cu1—O1—C281.3 (3)O3—Cu1—N1—C11154.7 (3)
O4—Cu1—O1—C26.8 (7)O2—Cu1—N1—C1124.6 (3)
N1—Cu1—O1—C2174.4 (3)O4—Cu1—N1—C1164.4 (3)
O1—Cu1—O2—C4i79.0 (3)C15—N1—C11—C121.0 (5)
O3—Cu1—O2—C4i10.8 (7)Cu1—N1—C11—C12175.7 (3)
O4—Cu1—O2—C4i89.3 (3)C11—N1—C15—C141.7 (5)
N1—Cu1—O2—C4i172.8 (3)Cu1—N1—C15—C14175.0 (3)
O1—Cu1—O4—C2i8.9 (7)N1—C11—C12—C130.4 (6)
O3—Cu1—O4—C2i89.1 (3)C14—C13—C12—C111.2 (5)
O2—Cu1—O4—C2i79.4 (3)O2i—C4—C3—C9157.2 (3)
N1—Cu1—O4—C2i172.2 (2)O3—C4—C3—C925.5 (4)
O1—Cu1—O3—C479.0 (3)O2i—C4—C3—C835.9 (4)
O2—Cu1—O3—C411.0 (7)O3—C4—C3—C8146.8 (3)
O4—Cu1—O3—C489.4 (3)O2i—C4—C3—C1083.5 (4)
N1—Cu1—O3—C4172.6 (3)O3—C4—C3—C1093.9 (4)
Cu1—O1—C2—O4i1.6 (5)O4i—C2—C1—C510.9 (5)
Cu1—O1—C2—C1175.9 (2)O1—C2—C1—C5171.5 (3)
Cu1—O3—C4—O2i1.6 (5)O4i—C2—C1—C6136.2 (3)
Cu1—O3—C4—C3175.5 (2)O1—C2—C1—C646.1 (4)
O1—Cu1—N1—C1567.6 (3)O4i—C2—C1—C7107.1 (4)
O3—Cu1—N1—C1521.9 (3)O1—C2—C1—C770.6 (4)
O2—Cu1—N1—C15158.8 (3)N1—C15—C14—C130.9 (6)
O4—Cu1—N1—C15112.2 (3)C12—C13—C14—C150.6 (5)
Symmetry code: (i) x+1, y+1, z+1.
 

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