Tetrakis(μ-acetato-κ²O:O′)­bis­[(4-pyridone-κO)copper(II)]

In the title centrosymmetric dinuclear complex, [Cu₂(C₂H₃O₂)₄(C₅H₅NO)₂], the two Cu^II atoms are bridged by four atetate groups, the Cu...Cu separation being 2.6468 (7) Å. Each Cu^II atom exists in a square-pyramidal coordination environment defined by four carboxyl acetate O atoms and one 4-pyridone O atom. Intermolecular hydrogen bonds give rise to a two-dimensional layer structure.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.028
• wR factor = 0.079
• Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.97
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.03
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.17 Ratio

   0 ALERT level A = In general: serious problem
   0 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
   1 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
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Tetrakis(µ-acetato-κ²O:O')bis[(4-pyridone-κO)copper(II)]

Crystal data

[Cu2(C2H3O2)4(C5H5NO)2]	F(000) = 1128
Mr = 553.48	Dx = 1.691 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8497 reflections
a = 13.445 (3) Å	θ = 3.1–27.5°
b = 8.6747 (17) Å	µ = 2.01 mm^−1
c = 18.821 (4) Å	T = 293 K
β = 98.04 (3)°	Prism, blue
V = 2173.5 (8) Å^3	0.37 × 0.26 × 0.19 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer	2493 independent reflections
Radiation source: fine-focus sealed tube	2275 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
Detector resolution: 10 pixels mm^-1	θmax = 27.5°, θmin = 3.1°
ω scans	h = −17→17
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −11→9
Tmin = 0.522, Tmax = 0.701	l = −24→24
10015 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0504P)^2 + 1.7434P] where P = (Fo^2 + 2Fc^2)/3
2493 reflections	(Δ/σ)max = 0.001
150 parameters	Δρmax = 0.70 e Å^−3
1 restraint	Δρmin = −0.34 e Å^−3

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

	x	y	z	Uiso*/Ueq
Cu1	0.02948 (2)	0.07656 (3)	0.56008 (1)	0.0280 (1)
O1	0.0710 (1)	0.1691 (2)	0.66408 (7)	0.0439 (4)
O2	−0.1152 (1)	0.0966 (2)	0.56375 (8)	0.0377 (3)
O3	−0.1653 (1)	−0.0282 (2)	0.46132 (8)	0.0436 (4)
O4	0.0271 (1)	0.2597 (2)	0.49761 (8)	0.0412 (3)
O5	−0.0229 (1)	0.1325 (2)	0.39628 (8)	0.0426 (3)
N1	0.3128 (2)	0.3834 (3)	0.7725 (1)	0.0539 (5)
C1	0.3119 (2)	0.3524 (3)	0.7025 (1)	0.0547 (6)
C2	0.2317 (2)	0.2826 (3)	0.6642 (1)	0.0458 (5)
C3	0.1463 (2)	0.2406 (2)	0.6967 (1)	0.0344 (4)
C4	0.1511 (2)	0.2798 (3)	0.7708 (1)	0.0481 (5)
C5	0.2337 (2)	0.3484 (3)	0.8059 (1)	0.0536 (6)
C6	0.0027 (1)	0.2531 (2)	0.4308 (1)	0.0332 (4)
C7	0.0076 (2)	0.4000 (3)	0.3884 (1)	0.0492 (6)
C8	−0.1815 (1)	0.0424 (2)	0.5168 (1)	0.0315 (4)
C9	−0.2897 (2)	0.0642 (3)	0.5271 (1)	0.0451 (5)
H1	0.3669	0.3792	0.6802	0.066*
H2	0.2324	0.2617	0.6158	0.055*
H4	0.0970	0.2579	0.7949	0.058*
H5	0.2360	0.3719	0.8543	0.064*
H7A	0.0733	0.4103	0.3745	0.074*
H7B	−0.0056	0.4865	0.4175	0.074*
H7C	−0.0418	0.3965	0.3463	0.074*
H9A	−0.2928	0.1118	0.5728	0.068*
H9B	−0.3226	−0.0342	0.5255	0.068*
H9C	−0.3226	0.1290	0.4896	0.068*
H10	0.366 (2)	0.423 (3)	0.801 (1)	0.065*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0256 (1)	0.0330 (2)	0.0233 (1)	0.00183 (8)	−0.00323 (9)	−0.00417 (8)
O1	0.0383 (8)	0.060 (1)	0.0313 (7)	−0.0051 (7)	−0.0024 (6)	−0.0165 (7)
O2	0.0282 (7)	0.0506 (9)	0.0335 (7)	0.0025 (6)	0.0013 (5)	−0.0071 (6)
O3	0.0291 (7)	0.060 (1)	0.0406 (8)	0.0045 (7)	−0.0012 (6)	−0.0148 (7)
O4	0.0491 (9)	0.0367 (8)	0.0370 (7)	−0.0044 (6)	0.0032 (6)	−0.0002 (6)
O5	0.0528 (9)	0.0364 (8)	0.0348 (7)	0.0011 (7)	−0.0074 (6)	0.0024 (6)
N1	0.045 (1)	0.057 (1)	0.0534 (1)	−0.0072 (9)	−0.0130 (9)	−0.015 (1)
C1	0.051 (1)	0.060 (2)	0.053 (1)	−0.012 (1)	0.009 (1)	−0.012 (1)
C2	0.053 (1)	0.052 (1)	0.032 (1)	−0.008 (1)	0.0037 (9)	−0.0069 (9)
C3	0.039 (1)	0.035 (1)	0.0260 (8)	0.0043 (8)	−0.0053 (7)	−0.0048 (7)
C4	0.052 (1)	0.062 (2)	0.028 (1)	−0.007 (1)	0.0013 (9)	−0.012 (1)
C5	0.062 (2)	0.066 (2)	0.029 (1)	−0.002 (1)	−0.0104 (9)	−0.013 (1)
C6	0.0277 (8)	0.034 (1)	0.038 (1)	0.0055 (7)	0.0029 (7)	0.0031 (8)
C7	0.055 (1)	0.043 (1)	0.052 (1)	0.001 (1)	0.011 (1)	0.012 (1)
C8	0.0267 (8)	0.0336 (9)	0.0331 (9)	0.0039 (7)	0.0010 (7)	0.0042 (8)
C9	0.028 (1)	0.054 (1)	0.053 (1)	0.0029 (9)	0.0072 (9)	−0.004 (1)

Geometric parameters (Å, º)

Cu1—Cu1^i	2.6468 (7)	N1—C5	1.344 (4)
Cu1—O2	1.964 (1)	N1—H10	0.90 (3)
Cu1—O3^i	1.9694 (15)	C1—H1	0.9300
Cu1—O4	1.974 (2)	C2—C3	1.421 (3)
Cu1—O5^i	1.998 (2)	C2—H2	0.9300
Cu1—O1	2.117 (1)	C3—C4	1.427 (3)
O1—C3	1.271 (2)	C4—H4	0.9300
C1—C2	1.354 (3)	C5—H5	0.9300
C4—C5	1.349 (3)	C6—C7	1.510 (3)
O2—C8	1.255 (2)	C7—H7A	0.9600
O3—C8	1.256 (2)	C7—H7B	0.9600
O3—Cu1^i	1.970 (2)	C7—H7C	0.9600
O4—C6	1.256 (2)	C8—C9	1.507 (3)
O5—C6	1.254 (3)	C9—H9A	0.9600
O5—Cu1^i	1.998 (2)	C9—H9B	0.9600
N1—C1	1.342 (3)	C9—H9C	0.9600
O2—Cu1—O3^i	167.81 (6)	C2—C3—C4	115.5 (2)
O2—Cu1—O4	90.92 (7)	C3—C2—H2	119.5
O2—Cu1—O5^i	88.01 (7)	C3—C4—H4	119.8
O2—Cu1—O1	93.90 (6)	C3—O1—Cu1	136.2 (1)
O3^i—Cu1—O1	97.93 (6)	C4—C5—H5	119.3
O3^i—Cu1—O5^i	89.21 (7)	C5—N1—H10	115 (2)
O3^i—Cu1—O4	89.30 (7)	C5—C4—C3	120.3 (2)
O4—Cu1—O5^i	167.82 (6)	C5—C4—H4	119.8
O4—Cu1—O1	103.04 (7)	C6—O4—Cu1	122.6 (1)
O5^i—Cu1—O1	89.14 (7)	C6—O5—Cu1^i	124.7 (1)
O1—Cu1—Cu1^i	171.49 (5)	C6—C7—H7A	109.5
O1—C3—C2	123.6 (2)	C6—C7—H7B	109.5
O1—C3—C4	120.8 (2)	C6—C7—H7C	109.5
O2—Cu1—Cu1^i	83.96 (5)	C8—O2—Cu1	123.5 (1)
O2—C8—O3	125.4 (2)	C8—O3—Cu1^i	123.2 (1)
O2—C8—C9	117.8 (2)	C8—C9—H9A	109.5
O3—C8—C9	116.8 (2)	C8—C9—H9B	109.5
O3^i—Cu1—Cu1^i	83.91 (5)	C8—C9—H9C	109.5
O4—Cu1—Cu1^i	85.25 (5)	N1—C1—C2	120.6 (2)
O4—C6—C7	117.7 (2)	N1—C1—H1	119.7
O5—C6—O4	124.9 (2)	N1—C5—C4	121.4 (2)
O5—C6—C7	117.4 (2)	N1—C5—H5	119.3
O5^i—Cu1—Cu1^i	82.57 (5)	H7A—C7—H7B	109.5
C1—N1—C5	121.0 (2)	H7A—C7—H7C	109.5
C1—N1—H10	124 (2)	H7B—C7—H7C	109.5
C1—C2—C3	121.1 (2)	H9A—C9—H9B	109.5
C1—C2—H2	119.5	H9A—C9—H9C	109.5
C2—C1—H1	119.7	H9B—C9—H9C	109.5
O2—Cu1—O1—C3	−153.3 (2)	Cu1—O1—C3—C2	1.4 (3)
O3^i—Cu1—O1—C3	29.7 (2)	Cu1—O1—C3—C4	−176.5 (2)
O4—Cu1—O1—C3	−61.5 (2)	C1—C2—C3—O1	−176.9 (2)
O5^i—Cu1—O1—C3	118.7 (2)	C1—C2—C3—C4	1.2 (4)
O3^i—Cu1—O2—C8	−6.3 (4)	O1—C3—C4—C5	176.5 (2)
O4—Cu1—O2—C8	84.7 (2)	C2—C3—C4—C5	−1.7 (4)
O5^i—Cu1—O2—C8	−83.2 (2)	C1—N1—C5—C4	0.6 (4)
O1—Cu1—O2—C8	−172.2 (2)	C3—C4—C5—N1	0.9 (4)
Cu1^i—Cu1—O2—C8	−0.4 (2)	Cu1^i—O5—C6—O4	−0.5 (3)
O2—Cu1—O4—C6	−83.8 (2)	Cu1^i—O5—C6—C7	177.4 (2)
O3^i—Cu1—O4—C6	84.0 (2)	Cu1—O4—C6—O5	0.2 (3)
O5^i—Cu1—O4—C6	1.1 (4)	Cu1—O4—C6—C7	−177.7 (2)
O1—Cu1—O4—C6	−178.0 (2)	Cu1—O2—C8—O3	−1.4 (3)
Cu1^i—Cu1—O4—C6	0.1 (2)	Cu1—O2—C8—C9	179.0 (1)
C5—N1—C1—C2	−1.1 (4)	Cu1^i—O3—C8—O2	3.2 (3)
N1—C1—C2—C3	0.2 (4)	Cu1^i—O3—C8—C9	−177.3 (2)

Symmetry code: (i) −x, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H10···O5^ii	0.90 (3)	2.22 (2)	2.981 (3)	142 (2)
N1—H10···O1^iii	0.90 (3)	2.36 (2)	3.080 (3)	137 (2)

Symmetry codes: (ii) x+1/2, −y+1/2, z+1/2; (iii) −x+1/2, y+1/2, −z+3/2.