Poly[[bis­(salicylato-κO)copper(II)]-di-μ-3-pyridylmethanol-κ²N:O;κ²O:N]: a redetermination at 100 K

The crystal structure of the polymeric title compound, [Cu(C₇H₅O₃)₂(C₆H₇NO)₂]_n, has been reported previously at room temperature by Hoang, Valach, Macášková & Melník [Acta Cryst. (1992) C48, 1933–1936]. The centrosymmetric coordination environment of Cu^II at 100 K displays elongation of the Cu—N bonds and contraction of the Cu—O bonds to the 3-pyridylmethanol ligands, compared with the room-temperature structure. The Cu—O bond lengths to the carboxyl­ate groups of the salicylate ligands are comparable at both temperatures.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C)= 0.003 Å
• R factor = 0.039
• wR factor = 0.088
• Data-to-parameter ratio = 16.9

checkCIF/PLATON results

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Computing details

Data collection: CrysAlis CCD (Oxford Diffraction, 2002); cell refinement: CrysAlis RED (Oxford Diffraction, 2002); data reduction: CrysAlis RED; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Poly[[bis(salicylato-κO)copper(II)]-di-µ-3-pyridylmethanol-κ²N:O;κ²O:N]

Crystal data

[Cu(C7H5O3)2(C6H7NO)2]	F(000) = 1148
Mr = 556.03	Dx = 1.471 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 6823 reflections
a = 12.823 (2) Å	θ = 3.6–28.0°
b = 9.914 (3) Å	µ = 0.92 mm^−1
c = 19.750 (4) Å	T = 100 K
V = 2510.8 (10) Å^3	Block, blue
Z = 4	0.50 × 0.40 × 0.20 mm

Data collection

Kuma KM-4 CCD area-detector diffractometer	2889 independent reflections
Radiation source: fine-focus sealed tube	2653 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
ω scans	θmax = 28.0°, θmin = 3.3°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2002)	h = −16→14
Tmin = 0.655, Tmax = 0.837	k = −10→12
15502 measured reflections	l = −25→25

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.088	H-atom parameters constrained
S = 1.11	w = 1/[σ^2(Fo^2) + (0.0287P)^2 + 3.2095P] where P = (Fo^2 + 2Fc^2)/3
2889 reflections	(Δ/σ)max < 0.001
171 parameters	Δρmax = 0.55 e Å^−3
0 restraints	Δρmin = −0.46 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cu	0.5000	0.0000	0.5000	0.01371 (10)
N1	0.47632 (11)	0.19848 (16)	0.53736 (8)	0.0156 (3)
O1	0.44674 (10)	0.05961 (13)	0.41204 (6)	0.0175 (3)
O2	0.57951 (10)	0.19366 (14)	0.37546 (7)	0.0218 (3)
O3	0.27523 (11)	0.04857 (18)	0.34879 (8)	0.0324 (4)
H3O	0.3202	0.0241	0.3772	0.049*
O4	0.18495 (10)	0.40747 (14)	0.51719 (7)	0.0212 (3)
H4O	0.1670	0.3707	0.5537	0.032*
C1	0.48894 (14)	0.14920 (18)	0.37046 (9)	0.0159 (3)
C2	0.41954 (14)	0.19821 (18)	0.31420 (9)	0.0169 (4)
C3	0.31793 (15)	0.1450 (2)	0.30623 (10)	0.0211 (4)
C4	0.25545 (16)	0.1931 (2)	0.25288 (10)	0.0279 (4)
H4	0.1874	0.1575	0.2464	0.034*
C5	0.29349 (18)	0.2944 (2)	0.20895 (11)	0.0307 (5)
H5	0.2499	0.3263	0.1735	0.037*
C6	0.39342 (17)	0.3487 (2)	0.21621 (11)	0.0278 (4)
H6	0.4178	0.4173	0.1866	0.033*
C7	0.45618 (15)	0.2994 (2)	0.26805 (10)	0.0213 (4)
H7	0.5250	0.3336	0.2730	0.026*
C8	0.39096 (13)	0.27442 (18)	0.52158 (9)	0.0153 (3)
H8	0.3417	0.2374	0.4908	0.018*
C9	0.37049 (13)	0.40755 (18)	0.54852 (9)	0.0159 (3)
C10	0.44305 (14)	0.4660 (2)	0.59259 (10)	0.0196 (4)
H10	0.4323	0.5534	0.6111	0.023*
C11	0.53255 (15)	0.39003 (19)	0.60831 (10)	0.0205 (4)
H11	0.5843	0.4266	0.6374	0.025*
C12	0.54597 (14)	0.25659 (19)	0.58029 (10)	0.0189 (4)
H12	0.6065	0.2069	0.5925	0.023*
C13	0.27487 (14)	0.49186 (18)	0.52884 (11)	0.0194 (4)
H13A	0.2592	0.5569	0.5655	0.023*
H13B	0.2905	0.5438	0.4873	0.023*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu	0.01491 (16)	0.01290 (17)	0.01334 (16)	0.00249 (11)	−0.00103 (11)	−0.00028 (11)
N1	0.0143 (7)	0.0153 (7)	0.0173 (7)	0.0009 (6)	0.0002 (6)	−0.0012 (6)
O1	0.0178 (6)	0.0193 (7)	0.0154 (6)	−0.0003 (5)	−0.0019 (5)	0.0016 (5)
O2	0.0146 (6)	0.0237 (7)	0.0271 (7)	−0.0007 (5)	−0.0013 (5)	0.0002 (6)
O3	0.0195 (7)	0.0463 (10)	0.0313 (8)	−0.0070 (7)	−0.0031 (6)	0.0167 (7)
O4	0.0122 (6)	0.0252 (7)	0.0263 (7)	−0.0003 (5)	−0.0017 (5)	0.0020 (6)
C1	0.0183 (8)	0.0127 (8)	0.0165 (8)	0.0038 (6)	0.0010 (6)	−0.0031 (7)
C2	0.0170 (8)	0.0180 (9)	0.0156 (8)	0.0029 (7)	0.0012 (6)	−0.0006 (7)
C3	0.0187 (9)	0.0248 (10)	0.0198 (9)	0.0001 (8)	−0.0002 (7)	0.0041 (8)
C4	0.0219 (9)	0.0372 (12)	0.0248 (10)	−0.0019 (9)	−0.0066 (8)	0.0059 (9)
C5	0.0333 (11)	0.0367 (12)	0.0222 (10)	0.0055 (9)	−0.0067 (9)	0.0075 (9)
C6	0.0350 (11)	0.0261 (10)	0.0224 (10)	−0.0005 (9)	0.0018 (8)	0.0082 (8)
C7	0.0222 (9)	0.0213 (9)	0.0203 (9)	−0.0006 (8)	0.0028 (7)	0.0007 (7)
C8	0.0113 (7)	0.0171 (9)	0.0174 (8)	−0.0018 (6)	−0.0001 (6)	0.0005 (7)
C9	0.0118 (7)	0.0157 (8)	0.0201 (8)	−0.0007 (7)	0.0022 (6)	0.0001 (7)
C10	0.0177 (9)	0.0175 (9)	0.0236 (9)	0.0001 (7)	0.0002 (7)	−0.0036 (7)
C11	0.0155 (8)	0.0222 (9)	0.0239 (9)	−0.0015 (7)	−0.0040 (7)	−0.0045 (8)
C12	0.0135 (8)	0.0208 (9)	0.0225 (9)	0.0021 (7)	−0.0033 (7)	−0.0031 (7)
C13	0.0140 (8)	0.0171 (9)	0.0273 (10)	0.0005 (7)	−0.0025 (7)	−0.0021 (7)

Geometric parameters (Å, º)

Cu—O1	1.9579 (13)	C4—C5	1.414 (3)
Cu—O1^i	1.9579 (13)	C4—H4	0.950
Cu—N1^i	2.1233 (16)	C5—C6	1.397 (3)
Cu—N1	2.1233 (16)	C5—H5	0.950
Cu—O4^ii	2.5654 (13)	C6—C7	1.391 (3)
Cu—O4^iii	2.5654 (14)	C6—H6	0.950
N1—C12	1.360 (2)	C7—H7	0.950
N1—C8	1.365 (2)	C8—C9	1.447 (3)
O1—C1	1.325 (2)	C8—H8	0.950
O2—C1	1.246 (2)	C9—C10	1.400 (3)
O3—C3	1.386 (2)	C9—C13	1.534 (2)
O3—H3O	0.840	C10—C11	1.408 (3)
O4—C13	1.443 (2)	C10—H10	0.950
O4—H4O	0.840	C11—C12	1.444 (3)
C1—C2	1.504 (2)	C11—H11	0.950
C2—C3	1.415 (3)	C12—H12	0.950
C2—C7	1.435 (3)	C13—H13A	0.990
C3—C4	1.407 (3)	C13—H13B	0.990
O1—Cu—O1^i	180.00 (3)	C5—C4—H4	119.9
O1—Cu—N1^i	91.22 (6)	C6—C5—C4	121.81 (19)
O1^i—Cu—N1^i	88.78 (6)	C6—C5—H5	119.1
O1—Cu—N1	88.78 (6)	C4—C5—H5	119.1
O1^i—Cu—N1	91.22 (6)	C7—C6—C5	118.08 (19)
N1^i—Cu—N1	180.00 (8)	C7—C6—H6	121.0
O1—Cu—O4^ii	84.43 (5)	C5—C6—H6	121.0
O1^i—Cu—O4^ii	95.57 (5)	C6—C7—C2	121.59 (18)
N1^i—Cu—O4^ii	81.19 (5)	C6—C7—H7	119.2
N1—Cu—O4^ii	98.81 (5)	C2—C7—H7	119.2
O1—Cu—O4^iii	95.57 (5)	N1—C8—C9	124.38 (16)
O1^i—Cu—O4^iii	84.43 (5)	N1—C8—H8	117.8
N1^i—Cu—O4^iii	98.81 (5)	C9—C8—H8	117.8
N1—Cu—O4^iii	81.19 (5)	C10—C9—C8	119.07 (16)
O4^ii—Cu—O4^iii	180.0	C10—C9—C13	117.59 (16)
C12—N1—C8	115.82 (16)	C8—C9—C13	123.28 (16)
C12—N1—Cu	121.03 (12)	C9—C10—C11	117.20 (17)
C8—N1—Cu	123.14 (12)	C9—C10—H10	121.4
C1—O1—Cu	127.57 (11)	C11—C10—H10	121.4
C3—O3—H3O	109.5	C10—C11—C12	120.21 (17)
C13—O4—H4O	109.5	C10—C11—H11	119.9
O2—C1—O1	124.65 (17)	C12—C11—H11	119.9
O2—C1—C2	119.72 (17)	N1—C12—C11	123.29 (16)
O1—C1—C2	115.64 (15)	N1—C12—H12	118.4
C3—C2—C7	119.45 (17)	C11—C12—H12	118.4
C3—C2—C1	120.45 (16)	O4—C13—C9	111.30 (14)
C7—C2—C1	120.10 (16)	O4—C13—H13A	109.4
O3—C3—C4	117.60 (17)	C9—C13—H13A	109.4
O3—C3—C2	123.62 (17)	O4—C13—H13B	109.4
C4—C3—C2	118.77 (18)	C9—C13—H13B	109.4
C3—C4—C5	120.27 (19)	H13A—C13—H13B	108.0
C3—C4—H4	119.9
O1—Cu—N1—C12	−140.97 (14)	C1—C2—C3—C4	−179.82 (18)
O1^i—Cu—N1—C12	39.03 (14)	O3—C3—C4—C5	178.2 (2)
O4^ii—Cu—N1—C12	134.85 (14)	C2—C3—C4—C5	−1.0 (3)
O4^iii—Cu—N1—C12	−45.15 (14)	C3—C4—C5—C6	0.7 (4)
O1—Cu—N1—C8	40.43 (14)	C4—C5—C6—C7	0.6 (3)
O1^i—Cu—N1—C8	−139.57 (14)	C5—C6—C7—C2	−1.6 (3)
O4^ii—Cu—N1—C8	−43.74 (14)	C3—C2—C7—C6	1.2 (3)
O4^iii—Cu—N1—C8	136.26 (14)	C1—C2—C7—C6	−178.86 (18)
N1^i—Cu—O1—C1	−114.96 (15)	C12—N1—C8—C9	−1.4 (3)
N1—Cu—O1—C1	65.04 (15)	Cu—N1—C8—C9	177.22 (13)
O4^ii—Cu—O1—C1	164.02 (15)	N1—C8—C9—C10	1.6 (3)
O4^iii—Cu—O1—C1	−15.98 (15)	N1—C8—C9—C13	178.78 (17)
Cu—O1—C1—O2	13.0 (3)	C8—C9—C10—C11	−0.2 (3)
Cu—O1—C1—C2	−166.71 (11)	C13—C9—C10—C11	−177.60 (17)
O2—C1—C2—C3	177.57 (17)	C9—C10—C11—C12	−1.0 (3)
O1—C1—C2—C3	−2.7 (2)	C8—N1—C12—C11	0.1 (3)
O2—C1—C2—C7	−2.3 (3)	Cu—N1—C12—C11	−178.64 (14)
O1—C1—C2—C7	177.41 (16)	C10—C11—C12—N1	1.2 (3)
C7—C2—C3—O3	−179.03 (18)	C10—C9—C13—O4	−148.25 (17)
C1—C2—C3—O3	1.1 (3)	C8—C9—C13—O4	34.5 (2)
C7—C2—C3—C4	0.1 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3O···O1	0.84	1.80	2.532 (2)	145
O4—H4O···O2^iv	0.84	1.90	2.707 (2)	160

Symmetry code: (iv) x−1/2, −y+1/2, −z+1.