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In the crystals of bis(pyridine-N)tetrakis(μ-trimethylsilylacetato-O:O′)dicopper(II), [Cu2(C5H11O2Si)4(C5H5N)2], (I), the dinuclear CuII complexes have cage structures with Cu...Cu distances of 2.632 (1) and 2.635 (1) Å. In the crystals of bis(2-­methylpyridine-N)tetrakis(μ-trimethylsilylacetato-O:O′)dicopper(II), [Cu2(C5H11O2Si)4(C6H7N)2], (II), bis­(3-methylpyridine-N)tetrakis(μ-trimethylsilylacetato-O:O′)dicopper(II), [Cu2(C5H11O2Si)4(C6H7N)2], (III), and bis(quinoline-N)­tetrakis(μ-­trimethylsilylacetato-O:O′)dicopper(II), [Cu2(C5H11O2Si)4(C9H7N)2], (IV), the centrosymmetric dinuclear CuII complexes have a cage structure with Cu...Cu distances of 2.664 (1), 2.638 (3) and 2.665 (1) Å, respectively. In the crystals of catena-poly­[tetrakis(μ-trimethylsilylacetato-O:O′)dicopper(II)], [Cu2(C5H11O2Si)4]n, (V), the dinuclear CuII units of a cage structure are linked by the cyclic Cu—O bonds at the apical positions to form a linear chain by use of a glide translation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270199012147/oa1095sup1.cif
Contains datablocks tmsa, I, II, III, IV, V

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012147/oa1095Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012147/oa1095IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012147/oa1095IIIsup4.hkl
Contains datablock III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012147/oa1095IVsup5.hkl
Contains datablock IV

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012147/oa1095Vsup6.hkl
Contains datablock V

CCDC references: 140916; 140917; 140918; 140919; 140920

Comment top

The −2 J values of copper(II) carboxylates, i.e. the singlet-triplet energy separation, greatly depend on the kind of atom directly bonded to the COO bridge (Kato & Muto, 1988). There is a correlation between the electron density at the central C atom of the COO bridge and the antiferromagnetic spin-exchange interaction (Yamanaka et al., 1991; Harada et al., 1997). Silanecarboxylatocopper complexes show very large −2 J values due to the σ-electron donating character of the Si atom; for [Cu2(PhMe2SiCOO)4(H2O)2], −2 J = 1000±150 cm−1 (Steward et al., 1986). In (I)-(IV), a Si atom is bonded to the α-carbon of the carboxylate ions. Their −2 J values were determined to be (I) 323, (II) 334, (III) 322, and (IV) 333 cm−1 (H = −2JS1·S2). These −2 J values are slightly smaller than those of trimethylacetatocopper complexes (−2 J ~356 cm−1; Goto et al., 1999). In conclusion, the electronic influence of the Si atom on the spin-exchange interaction is very small if the Si atom is not bonded directly to the carboxylate ion.

The complexes (I)-(V) have a centre of symmetry. The trimethylsilyl groups are arranged to have approximately fourfold rotational symmetry along the Cu···Cu axis. Displacement ellipsoids of the terminal methyl-C atoms are large, indicating librational and rotational disorder. In (I)-(IV), the geometry around the Cu atoms is a typical square-pyramidal coordination, and the O—Cu—O bond angle between the bridges opposite each other is in the narrow range 166.9 (1) to 168.7 (2)°.

On the other hand, the Cu atoms in (V) have a distorted trigonal bipyramidal coordination geometry with O—Cu—O bond angles of 178.0 (3)–178.5 (3)° and 158.0 (3)–159.0 (3)°. The Cu—O—Cu bond angle in the polymer chain of (V) is 101.3 (2)°. In the April 1999 release of the CSD (Cambridge Structural Database, 1999) the number of entries of the polymeric copper carboxylates was fourteen, and the Cu—O—Cu angles range from 98.2 to 109.3°.

Polymeric copper carboxylates are essentially antiferromagnetic, although the spin-spin interaction through the Cu—O—Cu bonds is ferromagnetic. The −2 J values are generally much less than those of dimeric complexes (Muto et al., 1985). This may be due to a trigonal bipyramidal deformation of the cage structure, in accord with the magneto-structure correlations established in the study on the dimeric copper(II) trichloroacetates (Uekusa et al., 1992).

Experimental top

Trimethylsilylacetic acid (132 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 was stirred for 1 h at room temperature, a green precipitate was collected and desolved in ethanol. When pyridine (40 mg, 0.50 mmol) was added to the solution, the colour changed from green to blue, and from the solution the green crystals of (I) were grown by slow evaporation. Crystals of (II), (III), and (IV) were prepared in a similar way using 2-methylpyridine, 3-methylpyridine, and quinoline as axial ligands. When these monodentate ligands were not introduced and the ethanol solution was kept in a desiccator, blue-green small crystals of polymer (V) were obtained together with pale green plate-like crystals of tetranuclear complex, [Cu2(Me3SiCH2COO)4(H2O)]2: monoclinic, P21/n, a = 12.697 (5), b = 12.085 (5), c = 22.609 (3) Å, β = 94.30 (2)°, V = 3459 (2) Å3, Z = 2.

Refinement top

During the data collection of (II), intensity decay of 10.1% was observed, and was corrected based on the standard reflections.

In (II), there is an orientational disorder of the 2-methylpyridine ligand. The site occupation factors of N1, C12 and C13 were assumed to be 100%, and the remaining four C atoms are either of two sets of positions, (C11, C14, C15, C16) or (C17, C18, C19, C20) with 50% probabilities. The max/min ratio of the atom displacement parameters are abnormally large for the methyl-C atoms of the trimethylsilyl groups, which may be due to the librational and rotational disorder. To avoid insufficient convergence in the refinement of (V), all the 12 terminal methyl-C atoms were refined isotropically.

The magnetic susceptibilities over the temperature range 80–300 K were determined by the Faraday method at Saga University. The procedure for determining the −2 J value from cryomagnetic data based on the Bleaney-Bowers equation is described elsewhere (Harada et al., 1997).

Computing details top

For all compounds, data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software. Data reduction: local programs for (I), (III); TEXSAN (Molecular Structure Corporation, 1998) for (II), (IV), (V). Program(s) used to solve structure: CRYSTAN-GM (Edwards et al., 1996) for (I), (III). Program(s) used to refine structure: CRYSTAN-GM for (I), (III); TEXSAN for (II), (IV), (V). Molecular graphics: CRYSTAN-GM for (I), (III). Software used to prepare material for publication: CRYSTAN-GM for (I), (III); TEXSAN for (II), (IV), (V).

Figures top
[Figure 1] Fig. 1. The molecular structures of (I): (a) and (b) show the two independent molecules. Displacement ellipsoids are plotted at the 50% probability level and H atoms are shown as spheres of arbitrary radius.
[Figure 2] Fig. 2. The molecular structure of (II) with displacement ellipsoids at the 50% probability level. The 2-methylpyridine ligand has an orientational disorder, and one of two possible orientations is shown. H atoms are shown as spheres of arbitrary radius.
[Figure 3] Fig. 3. The molecular structure of (III) with displacement ellipsoids at the 50% probability level. H atoms are shown as spheres of arbitrary radius.
[Figure 4] Fig. 4. The molecular structure of (IV) with displacement ellipsoids at the 50% probability level. H atoms are shown as spheres of arbitrary radius.
[Figure 5] Fig. 5. The linear chain structure of (V) with displacement ellipsoids at the 50% probability level. Methyl groups of the trimethylsilylacetato ligands and H atoms are omitted for clarity.
(I) tetrakis(µ-trimethylsilylacetato-O:O')di(pyridine-N)dicopper(II) top
Crystal data top
[Cu2(C5H11O2Si)4(C5H5N)2]Z = 2
Mr = 810.20F(000) = 852
Triclinic, P1Dx = 1.239 Mg m3
a = 11.392 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 18.508 (2) ÅCell parameters from 25 reflections
c = 10.851 (1) Åθ = 10–15°
α = 91.87 (1)°µ = 1.13 mm1
β = 102.79 (1)°T = 299 K
γ = 76.82 (1)°Prism, green
V = 2171.9 (5) Å30.4 × 0.3 × 0.3 mm
Data collection top
Rigaku AFC-5
diffractometer
Rint = 0.017
θ–2θ scansθmax = 27.5°
Absorption correction: integration
(Coppens et al., 1965)
h = 015
Tmin = 0.971, Tmax = 0.978k = 2424
10462 measured reflectionsl = 1414
9960 independent reflections3 standard reflections every 100 reflections
5122 reflections with |Fo| > 3σ(|Fo|) intensity decay: none
Refinement top
Refinement on FH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.068 w = 1/[σ2(F) + 0.000225F2]
wR(F2) = 0.053(Δ/σ)max = 0.002
S = 1.34Δρmax = 0.80 e Å3
5122 reflectionsΔρmin = 0.57 e Å3
415 parameters
Crystal data top
[Cu2(C5H11O2Si)4(C5H5N)2]γ = 76.82 (1)°
Mr = 810.20V = 2171.9 (5) Å3
Triclinic, P1Z = 2
a = 11.392 (1) ÅMo Kα radiation
b = 18.508 (2) ŵ = 1.13 mm1
c = 10.851 (1) ÅT = 299 K
α = 91.87 (1)°0.4 × 0.3 × 0.3 mm
β = 102.79 (1)°
Data collection top
Rigaku AFC-5
diffractometer
5122 reflections with |Fo| > 3σ(|Fo|)
Absorption correction: integration
(Coppens et al., 1965)
Rint = 0.017
Tmin = 0.971, Tmax = 0.9783 standard reflections every 100 reflections
10462 measured reflections intensity decay: none
9960 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.068415 parameters
wR(F2) = 0.053H-atom parameters constrained
S = 1.34Δρmax = 0.80 e Å3
5122 reflectionsΔρmin = 0.57 e Å3
Special details top

Refinement. The positions of all the H atoms were calculated geometrically, and a riding model was used in their refinement for (I) and (III) [C—H 0.96 Å, Uiso(H) = 0.2 Å2]. H atom parameters were not refined for (II), (IV), and (V) [Uiso(H)= 1.2 Ueq(parent atom)].

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.89306 (6)0.52455 (4)1.03174 (6)0.0543 (3)
Cu20.55785 (6)0.93449 (4)0.46790 (7)0.0641 (3)
Si30.7829 (2)0.4101 (1)0.5919 (2)0.0890 (9)
Si40.9800 (2)0.7410 (1)0.7950 (2)0.0776 (8)
Si50.8726 (2)1.0894 (1)0.7212 (2)0.100 (1)
Si60.4540 (2)0.8704 (1)0.8739 (2)0.097 (1)
O70.8604 (3)0.5976 (2)0.8942 (3)0.067 (2)
O81.0405 (3)0.5539 (2)0.8377 (3)0.068 (2)
O90.8426 (3)0.4498 (2)0.9086 (3)0.067 (2)
O101.0244 (3)0.4085 (2)0.8533 (3)0.070 (2)
O110.7055 (3)0.9757 (3)0.4954 (4)0.084 (2)
O120.6053 (4)1.0876 (2)0.5455 (4)0.085 (2)
O130.5953 (3)0.9096 (2)0.6486 (4)0.076 (2)
O140.4939 (4)1.0203 (2)0.7032 (4)0.077 (2)
N150.7091 (4)0.5554 (3)1.0750 (5)0.063 (2)
N160.6420 (4)0.8241 (3)0.4067 (5)0.070 (2)
C170.9366 (5)0.6000 (3)0.8266 (5)0.060 (3)
C180.9073 (5)0.6616 (3)0.7319 (5)0.068 (3)
C190.9492 (8)0.8083 (4)0.6621 (8)0.132 (5)
C200.9105 (8)0.7816 (4)0.9274 (8)0.154 (5)
C211.1496 (6)0.7071 (4)0.8566 (7)0.103 (4)
C220.9111 (5)0.4098 (3)0.8451 (5)0.057 (2)
C230.8540 (5)0.3606 (3)0.7481 (5)0.071 (3)
C240.701 (1)0.3489 (5)0.4854 (9)0.188 (6)
C250.6733 (7)0.4983 (5)0.6114 (7)0.125 (4)
C260.9057 (8)0.4331 (7)0.5272 (8)0.187 (7)
C270.6794 (6)0.5162 (4)1.1580 (6)0.086 (3)
C280.5609 (7)0.5275 (5)1.1775 (7)0.113 (4)
C290.4713 (6)0.5813 (5)1.1099 (9)0.113 (4)
C300.4995 (6)0.6234 (4)1.0254 (8)0.111 (4)
C310.6217 (6)0.6089 (4)1.0101 (7)0.083 (3)
C320.7013 (6)1.0416 (4)0.5279 (6)0.081 (3)
C330.8177 (5)1.0703 (4)0.5523 (6)0.100 (3)
C341.0263 (7)1.1124 (6)0.7358 (9)0.191 (6)
C350.7638 (8)1.1700 (5)0.7681 (9)0.188 (6)
C360.880 (1)1.0100 (6)0.8205 (9)0.193 (7)
C370.5532 (5)0.9545 (4)0.7286 (6)0.069 (3)
C380.5721 (6)0.9249 (3)0.8613 (6)0.079 (3)
C390.4908 (9)0.8355 (5)1.0390 (7)0.143 (5)
C400.2970 (7)0.9328 (5)0.8359 (8)0.148 (5)
C410.4633 (9)0.7920 (4)0.7629 (7)0.146 (5)
C420.6142 (7)0.7634 (4)0.4391 (7)0.109 (4)
C430.669 (1)0.6933 (4)0.4012 (9)0.139 (5)
C440.7518 (9)0.6885 (6)0.327 (1)0.137 (5)
C450.7792 (7)0.7502 (6)0.2917 (9)0.138 (5)
C460.7220 (6)0.8176 (4)0.3328 (7)0.103 (4)
H18A0.936770.642820.658240.20*
H18B0.819170.679520.708740.20*
H19A0.986880.848250.695280.20*
H19B0.861880.826150.630880.20*
H19C0.985080.784850.594480.20*
H20A0.948180.821580.960690.20*
H20B0.923980.744580.992190.20*
H20C0.823180.799780.896790.20*
H21A1.187270.747080.889860.20*
H21B1.186570.684380.789360.20*
H21C1.163170.670580.922260.20*
H23A0.916380.317940.737060.20*
H23B0.790680.344840.778260.20*
H24A0.665230.374650.405830.20*
H24B0.636730.338350.521930.20*
H24C0.756430.302950.473930.20*
H25A0.637870.524060.531810.20*
H25B0.715770.529260.668910.20*
H25C0.608570.487260.646010.20*
H26A0.870290.458950.447620.20*
H26B0.962990.388050.515020.20*
H26C0.948990.463850.584620.20*
H270.742870.477621.205280.20*
H280.542480.497801.238590.20*
H290.388070.589151.121070.20*
H300.436820.662410.978020.20*
H310.643430.638520.951450.20*
H33A0.881121.034140.524780.20*
H33B0.801921.115540.504180.20*
H34A1.053881.121870.823650.20*
H34B1.016381.155770.685050.20*
H34C1.084181.072370.708550.20*
H35A0.791431.179480.856150.20*
H35B0.683231.159380.754250.20*
H35C0.759231.212980.718650.20*
H36A0.908091.019540.908400.20*
H36B0.936290.967340.797100.20*
H36C0.799590.999940.806900.20*
H38A0.653180.892990.884800.20*
H38B0.565880.965490.918400.20*
H39A0.429850.807961.043720.20*
H39B0.487050.875761.097120.20*
H39C0.572250.803861.058520.20*
H40A0.236170.905310.840640.20*
H40B0.281570.953110.752040.20*
H40C0.292370.972710.894840.20*
H41A0.402400.764490.767600.20*
H41B0.544400.760190.785800.20*
H41C0.450200.810490.678100.20*
H420.554010.767990.490010.20*
H430.649640.648980.426660.20*
H440.791940.641320.299420.20*
H450.838110.747890.239690.20*
H460.737880.862700.305970.20*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0383 (4)0.0603 (5)0.0553 (5)0.0080 (3)0.0139 (3)0.0076 (4)
Cu20.0526 (5)0.0575 (5)0.0681 (5)0.0087 (4)0.0161 (4)0.0148 (4)
Si30.074 (1)0.122 (2)0.060 (1)0.028 (1)0.010 (1)0.017 (1)
Si40.075 (1)0.066 (1)0.085 (1)0.008 (1)0.007 (1)0.011 (1)
Si50.077 (1)0.105 (2)0.108 (2)0.046 (1)0.013 (1)0.031 (1)
Si60.121 (2)0.100 (2)0.068 (1)0.036 (1)0.025 (1)0.000 (1)
O70.049 (2)0.076 (3)0.072 (3)0.007 (2)0.012 (2)0.008 (2)
O80.063 (3)0.069 (3)0.062 (3)0.006 (2)0.021 (2)0.001 (2)
O90.053 (2)0.075 (3)0.064 (3)0.023 (2)0.021 (2)0.020 (2)
O100.053 (2)0.067 (3)0.071 (3)0.011 (2)0.017 (2)0.022 (2)
O110.051 (3)0.090 (3)0.094 (3)0.020 (2)0.021 (2)0.025 (3)
O120.060 (3)0.080 (3)0.104 (3)0.027 (2)0.021 (2)0.018 (3)
O130.071 (3)0.073 (3)0.072 (3)0.004 (2)0.021 (2)0.003 (2)
O140.084 (3)0.066 (3)0.065 (3)0.012 (2)0.013 (2)0.013 (2)
N150.043 (3)0.064 (3)0.069 (3)0.007 (3)0.021 (3)0.014 (3)
N160.059 (3)0.062 (4)0.072 (4)0.007 (3)0.012 (3)0.019 (3)
C170.057 (4)0.061 (4)0.053 (4)0.018 (3)0.000 (3)0.009 (3)
C180.070 (4)0.071 (4)0.059 (4)0.009 (3)0.003 (3)0.016 (3)
C190.166 (8)0.100 (6)0.142 (8)0.039 (6)0.018 (6)0.051 (6)
C200.157 (8)0.105 (7)0.155 (8)0.002 (6)0.049 (6)0.041 (6)
C210.074 (5)0.101 (6)0.141 (7)0.029 (4)0.001 (4)0.025 (5)
C220.056 (4)0.056 (4)0.051 (4)0.012 (3)0.009 (3)0.005 (3)
C230.066 (4)0.066 (4)0.067 (4)0.021 (3)0.007 (3)0.022 (3)
C240.23 (1)0.17 (1)0.13 (1)0.07 (1)0.06 (1)0.04 (1)
C250.111 (6)0.137 (7)0.110 (6)0.005 (5)0.007 (5)0.025 (5)
C260.123 (7)0.341 (15)0.100 (7)0.049 (8)0.050 (6)0.030 (8)
C270.066 (4)0.098 (5)0.085 (5)0.008 (4)0.039 (4)0.005 (4)
C280.083 (5)0.132 (7)0.118 (7)0.022 (5)0.059 (5)0.001 (5)
C290.056 (5)0.126 (7)0.140 (8)0.017 (5)0.049 (5)0.019 (6)
C300.054 (4)0.099 (6)0.160 (8)0.009 (4)0.032 (5)0.000 (5)
C310.053 (4)0.075 (5)0.114 (6)0.006 (4)0.018 (4)0.011 (4)
C320.058 (4)0.107 (6)0.067 (5)0.024 (4)0.017 (3)0.014 (4)
C330.064 (4)0.128 (6)0.102 (5)0.052 (4)0.032 (4)0.033 (5)
C340.083 (6)0.244 (11)0.205 (10)0.082 (7)0.030 (6)0.103 (9)
C350.128 (7)0.177 (9)0.207 (10)0.071 (7)0.073 (7)0.119 (8)
C360.27 (1)0.19 (1)0.15 (1)0.11 (1)0.07 (1)0.05 (1)
C370.051 (4)0.077 (5)0.071 (5)0.021 (4)0.005 (3)0.008 (4)
C380.085 (5)0.087 (5)0.055 (4)0.013 (4)0.006 (3)0.003 (4)
C390.211 (9)0.132 (7)0.079 (6)0.046 (7)0.040 (6)0.001 (5)
C400.099 (6)0.199 (10)0.140 (8)0.037 (6)0.039 (6)0.005 (7)
C410.23 (1)0.12 (1)0.10 (1)0.09 (1)0.06 (1)0.03 (1)
C420.133 (7)0.067 (5)0.111 (6)0.025 (5)0.038 (5)0.015 (5)
C430.18 (1)0.06 (1)0.15 (1)0.02 (1)0.03 (1)0.03 (1)
C440.106 (7)0.110 (8)0.129 (9)0.025 (6)0.011 (6)0.063 (7)
C450.085 (6)0.129 (8)0.146 (9)0.002 (6)0.032 (5)0.068 (8)
C460.077 (5)0.098 (6)0.108 (6)0.015 (4)0.033 (4)0.034 (5)
Geometric parameters (Å, º) top
Cu1—Cu1i2.632 (1)C18—H18B0.960
Cu1—O71.962 (4)C19—H19A0.960
Cu1—O8i1.961 (4)C19—H19B0.960
Cu1—O91.982 (4)C19—H19C0.961
Cu1—O10i1.972 (4)C20—H20A0.960
Cu1—N152.194 (5)C20—H20B0.960
Cu2—Cu2ii2.635 (1)C20—H20C0.960
Cu2—O111.961 (4)C21—H21A0.960
Cu2—O12ii1.965 (4)C21—H21B0.960
Cu2—O131.959 (4)C21—H21C0.961
Cu2—O14ii1.972 (4)C23—H23A0.959
Cu2—N162.198 (6)C23—H23B0.959
Si3—C231.876 (6)C24—H24A0.960
Si3—C241.848 (11)C24—H24B0.960
Si3—C251.854 (9)C24—H24C0.961
Si3—C261.832 (9)C25—H25A0.960
Si4—C181.885 (7)C25—H25B0.960
Si4—C191.856 (9)C25—H25C0.960
Si4—C201.848 (9)C26—H26A0.960
Si4—C211.864 (7)C26—H26B0.961
Si5—C331.850 (7)C26—H26C0.961
Si5—C341.867 (9)C27—H270.960
Si5—C351.846 (10)C28—H280.961
Si5—C361.824 (11)C29—H290.960
Si6—C381.886 (7)C30—H300.960
Si6—C391.850 (8)C31—H310.959
Si6—C401.862 (9)C33—H33A0.960
Si6—C411.854 (9)C33—H33B0.961
O7—C171.263 (7)C34—H34A0.960
O8—C171.276 (7)C34—H34B0.960
O9—C221.255 (7)C34—H34C0.959
O10—C221.268 (7)C35—H35A0.961
O11—C321.252 (10)C35—H35B0.961
O12—C321.271 (8)C35—H35C0.960
O13—C371.276 (8)C36—H36A0.960
O14—C371.258 (8)C36—H36B0.961
N15—C271.319 (8)C36—H36C0.959
N15—C311.324 (8)C38—H38A0.961
N16—C421.314 (10)C38—H38B0.958
N16—C461.325 (9)C39—H39A0.960
C17—C181.490 (8)C39—H39B0.960
C22—C231.505 (8)C39—H39C0.960
C27—C281.380 (10)C40—H40A0.959
C28—C291.350 (12)C40—H40B0.960
C29—C301.358 (12)C40—H40C0.961
C30—C311.403 (9)C41—H41A0.960
C32—C331.506 (9)C41—H41B0.960
C37—C381.511 (9)C41—H41C0.961
C42—C431.397 (12)C42—H420.959
C43—C441.359 (14)C43—H430.960
C44—C451.337 (14)C44—H440.959
C45—C461.379 (13)C45—H450.961
C18—H18A0.960C46—H460.960
O7—Cu1—O8i168.3 (2)H20A—C20—H20B110.0
O7—Cu1—O990.4 (2)H20A—C20—H20C110.2
O7—Cu1—O10i89.0 (2)H20B—C20—H20C108.9
O7—Cu1—N1596.5 (2)Si4—C21—H21A111.1
O8i—Cu1—O989.5 (2)Si4—C21—H21B109.2
O8i—Cu1—O10i88.8 (2)Si4—C21—H21C108.9
O8i—Cu1—N1595.1 (2)H21A—C21—H21B109.3
O9—Cu1—O10i168.7 (2)H21A—C21—H21C109.3
O9—Cu1—N1591.9 (2)H21B—C21—H21C108.9
O10i—Cu1—N1599.4 (2)Si3—C23—H23A109.4
O11—Cu2—O12ii168.3 (2)Si3—C23—H23B108.6
O11—Cu2—O1389.3 (2)C22—C23—H23A109.0
O11—Cu2—O14ii88.8 (2)C22—C23—H23B108.7
O11—Cu2—N1697.2 (2)H23A—C23—H23B109.1
O12ii—Cu2—O1388.4 (2)Si3—C24—H24A107.7
O12ii—Cu2—O14ii91.2 (2)Si3—C24—H24B109.0
O12ii—Cu2—N1694.5 (2)Si3—C24—H24C110.7
O13—Cu2—O14ii168.5 (2)H24A—C24—H24B110.2
O13—Cu2—N1696.5 (2)H24A—C24—H24C110.2
O14ii—Cu2—N1695.0 (2)H24B—C24—H24C109.0
C23—Si3—C24108.6 (4)Si3—C25—H25A111.0
C23—Si3—C25110.8 (4)Si3—C25—H25B109.5
C23—Si3—C26108.7 (4)Si3—C25—H25C108.7
C24—Si3—C25109.7 (5)H25A—C25—H25B109.4
C24—Si3—C26111.4 (5)H25A—C25—H25C109.3
C25—Si3—C26107.6 (5)H25B—C25—H25C109.0
C18—Si4—C19107.1 (4)Si3—C26—H26A109.5
C18—Si4—C20108.0 (4)Si3—C26—H26B108.9
C18—Si4—C21110.5 (3)Si3—C26—H26C110.4
C19—Si4—C20112.4 (4)H26A—C26—H26B109.5
C19—Si4—C21110.5 (4)H26A—C26—H26C109.5
C20—Si4—C21108.3 (4)H26B—C26—H26C109.0
C33—Si5—C34106.4 (4)N15—C27—H27118.2
C33—Si5—C35109.4 (4)C28—C27—H27119.0
C33—Si5—C36110.9 (4)C27—C28—H28120.6
C34—Si5—C35109.4 (5)C29—C28—H28120.5
C34—Si5—C36112.5 (5)C28—C29—H29120.0
C35—Si5—C36108.2 (5)C30—C29—H29120.4
C38—Si6—C39107.0 (4)C29—C30—H30120.3
C38—Si6—C40109.2 (4)C31—C30—H30121.2
C38—Si6—C41109.7 (4)N15—C31—H31118.6
C39—Si6—C40110.2 (4)C30—C31—H31119.6
C39—Si6—C41110.5 (4)Si5—C33—H33A109.0
C40—Si6—C41110.2 (4)Si5—C33—H33B108.6
Cu1—O7—C17123.2 (4)C32—C33—H33A108.7
Cu1i—O8—C17124.6 (4)C32—C33—H33B108.7
Cu1—O9—C22125.0 (4)H33A—C33—H33B109.1
Cu1i—O10—C22120.7 (4)Si5—C34—H34A105.6
Cu2—O11—C32121.1 (4)Si5—C34—H34B109.2
Cu2ii—O12—C32125.5 (5)Si5—C34—H34C111.7
Cu2—O13—C37122.2 (4)H34A—C34—H34B110.7
Cu2ii—O14—C37124.4 (4)H34A—C34—H34C110.7
Cu1—N15—C27120.5 (4)H34B—C34—H34C109.0
Cu1—N15—C31120.9 (4)Si5—C35—H35A109.6
C27—N15—C31118.3 (5)Si5—C35—H35B109.2
Cu2—N16—C42122.2 (5)Si5—C35—H35C110.1
Cu2—N16—C46119.9 (5)H35A—C35—H35B109.4
C42—N16—C46117.9 (6)H35A—C35—H35C109.5
O7—C17—O8123.6 (6)H35B—C35—H35C109.1
O7—C17—C18118.9 (5)Si5—C36—H36A111.5
O8—C17—C18117.4 (5)Si5—C36—H36B109.4
Si4—C18—C17112.2 (4)Si5—C36—H36C108.7
O9—C22—O10125.5 (5)H36A—C36—H36B109.1
O9—C22—C23117.6 (5)H36A—C36—H36C109.2
O10—C22—C23116.8 (5)H36B—C36—H36C108.9
Si3—C23—C22112.0 (4)Si6—C38—H38A108.8
N15—C27—C28122.8 (7)Si6—C38—H38B109.0
C27—C28—C29119.0 (8)C37—C38—H38A108.9
C28—C29—C30119.6 (7)C37—C38—H38B109.4
C29—C30—C31118.6 (7)H38A—C38—H38B109.0
N15—C31—C30121.8 (7)Si6—C39—H39A105.8
O11—C32—O12125.0 (6)Si6—C39—H39B111.0
O11—C32—C33119.4 (6)Si6—C39—H39C109.9
O12—C32—C33115.6 (7)H39A—C39—H39B110.6
Si5—C33—C32112.7 (5)H39A—C39—H39C110.6
O13—C37—O14124.6 (6)H39B—C39—H39C108.9
O13—C37—C38117.2 (6)Si6—C40—H40A109.7
O14—C37—C38118.2 (6)Si6—C40—H40B109.2
Si6—C38—C37111.7 (5)Si6—C40—H40C109.7
N16—C42—C43122.0 (8)H40A—C40—H40B109.6
C42—C43—C44118.5 (9)H40A—C40—H40C109.6
C43—C44—C45119.9 (9)H40B—C40—H40C109.0
C44—C45—C46118.6 (9)Si6—C41—H41A110.3
N16—C46—C45123.1 (7)Si6—C41—H41B108.4
Si4—C18—H18A109.1Si6—C41—H41C109.9
Si4—C18—H18B109.0H41A—C41—H41B109.7
C17—C18—H18A108.8H41A—C41—H41C109.6
C17—C18—H18B108.7H41B—C41—H41C109.0
H18A—C18—H18B109.0N16—C42—H42118.3
Si4—C19—H19A106.2C43—C42—H42119.7
Si4—C19—H19B110.6C42—C43—H43121.7
Si4—C19—H19C110.0C44—C43—H43119.8
H19A—C19—H19B110.6C43—C44—H44120.9
H19A—C19—H19C110.5C45—C44—H44119.2
H19B—C19—H19C109.0C44—C45—H45121.0
Si4—C20—H20A108.3C46—C45—H45120.3
Si4—C20—H20B110.2N16—C46—H46117.0
Si4—C20—H20C109.2C45—C46—H46119.9
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y+2, z+1.
(II) tetrakis(µ-trimethylsilylacetato-O:O')di(2-methylpyridine-N)dicopper(II) top
Crystal data top
[Cu2(C5H11O2Si)4(C6H7N)2]Z = 1
Mr = 838.26F(000) = 442
Triclinic, P1Dx = 1.199 Mg m3
a = 10.874 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.508 (2) ÅCell parameters from 25 reflections
c = 10.330 (2) Åθ = 10–15°
α = 104.26 (2)°µ = 1.06 mm1
β = 109.10 (2)°T = 298 K
γ = 74.91 (2)°Plate-like, green
V = 1160.9 (4) Å30.5 × 0.5 × 0.2 mm
Data collection top
Rigaku AFC7R
diffractometer
5169 reflections with I > 1.5σ(I)
Radiation source: Rigaku rotating anodeRint = 0.009
Graphite monochromatorθmax = 32.5°, θmin = 2.5°
θ–2θ scansh = 1616
Absorption correction: ψ-scan
(North et al., 1968)
k = 1717
Tmin = 0.567, Tmax = 0.809l = 150
8822 measured reflections3 standard reflections every 150 reflections
8412 independent reflections intensity decay: 10.1%
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.051H-atom parameters not refined
wR(F2) = 0.079 w = 1/[σ2(Fo) + 0.00181|Fo|2]
S = 1.39(Δ/σ)max = 0.03
5352 reflectionsΔρmax = 0.45 e Å3
253 parametersΔρmin = 0.32 e Å3
Crystal data top
[Cu2(C5H11O2Si)4(C6H7N)2]γ = 74.91 (2)°
Mr = 838.26V = 1160.9 (4) Å3
Triclinic, P1Z = 1
a = 10.874 (2) ÅMo Kα radiation
b = 11.508 (2) ŵ = 1.06 mm1
c = 10.330 (2) ÅT = 298 K
α = 104.26 (2)°0.5 × 0.5 × 0.2 mm
β = 109.10 (2)°
Data collection top
Rigaku AFC7R
diffractometer
5169 reflections with I > 1.5σ(I)
Absorption correction: ψ-scan
(North et al., 1968)
Rint = 0.009
Tmin = 0.567, Tmax = 0.8093 standard reflections every 150 reflections
8822 measured reflections intensity decay: 10.1%
8412 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.079H-atom parameters not refined
S = 1.39Δρmax = 0.45 e Å3
5352 reflectionsΔρmin = 0.32 e Å3
253 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.10007 (3)0.01009 (3)0.95868 (3)0.05532 (10)
Si10.2736 (1)0.3765 (1)1.1944 (2)0.1130 (5)
Si20.1577 (1)0.2429 (1)0.5267 (1)0.0919 (3)
O10.2106 (2)0.0936 (2)1.0981 (2)0.0778 (7)
O20.0416 (2)0.1116 (2)1.1633 (2)0.0725 (6)
O30.0549 (2)0.1365 (2)0.8262 (3)0.0806 (7)
O40.1172 (3)0.1517 (2)0.8893 (2)0.0824 (7)
N10.2633 (3)0.0253 (4)0.8793 (3)0.0884 (10)
C10.1631 (3)0.1307 (3)1.1711 (3)0.0637 (7)
C20.2580 (4)0.2098 (4)1.2728 (4)0.088 (1)
C30.320 (2)0.4042 (8)1.042 (1)0.319 (8)
C40.394 (1)0.4687 (8)1.317 (1)0.290 (6)
C50.1162 (9)0.4185 (7)1.150 (2)0.302 (6)
C60.0395 (4)0.1870 (3)0.8144 (3)0.0703 (8)
C70.0630 (5)0.2913 (3)0.6984 (4)0.092 (1)
C80.1841 (8)0.3815 (6)0.3964 (6)0.158 (2)
C90.3179 (8)0.1508 (9)0.5400 (8)0.186 (3)
C100.0712 (10)0.1400 (8)0.4901 (7)0.183 (3)
C110.348 (1)0.043 (2)0.831 (1)0.100 (4)0.50
C120.4753 (8)0.012 (1)0.8051 (9)0.165 (4)
C130.4568 (7)0.099 (1)0.8522 (8)0.150 (3)
C140.3740 (9)0.193 (2)0.898 (2)0.167 (6)0.50
C150.2696 (9)0.167 (1)0.925 (1)0.097 (4)0.50
C160.340 (2)0.170 (2)0.800 (2)0.168 (6)0.50
C170.3211 (10)0.111 (1)0.8913 (8)0.084 (3)0.50
C180.4311 (9)0.120 (1)0.769 (1)0.126 (4)0.50
C190.319 (1)0.098 (1)0.816 (2)0.096 (4)0.50
C200.271 (2)0.234 (1)0.958 (2)0.137 (5)0.50
H10.34380.18851.30070.1060*
H20.22620.19521.35300.1060*
H30.32420.48931.00120.3847*
H40.40310.38251.06160.3847*
H50.25300.35600.97730.3847*
H60.39820.55371.27700.3497*
H70.36800.45201.40110.3497*
H80.47980.44881.33810.3497*
H90.05270.37061.08330.3629*
H100.08750.40451.23080.3629*
H110.12390.50381.10770.3629*
H120.02130.34060.69100.1106*
H130.11240.33900.71910.1106*
H140.23650.35950.30820.1893*
H150.22960.42790.42500.1893*
H160.09980.43060.38820.1893*
H170.36630.12210.45410.2218*
H180.30560.08260.61450.2218*
H190.36800.20000.55820.2218*
H200.01510.18430.48230.2197*
H210.06130.07140.56470.2197*
H220.12200.11210.40450.2197*
H230.54340.06450.76520.1989*0.50
H240.53340.12820.85690.1811*0.50
H250.38580.27530.91230.1965*0.50
H260.20740.22770.96640.1167*0.50
H270.25760.18060.73230.1993*0.50
H280.34700.19630.88300.1993*0.50
H290.41240.21630.76260.1993*0.50
H300.50730.15950.86230.1811*0.50
H310.55900.03180.78420.1989*0.50
H320.46960.19710.72040.1500*0.50
H330.27740.16490.80750.1148*0.50
H340.32440.28890.95830.1633*0.50
H350.27430.23321.05120.1633*0.50
H360.18060.26140.90610.1633*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0511 (2)0.0635 (2)0.0555 (2)0.0114 (1)0.0156 (1)0.0158 (1)
Si10.1011 (8)0.0738 (7)0.159 (1)0.0006 (6)0.0141 (8)0.0560 (8)
Si20.1253 (9)0.0816 (6)0.0593 (5)0.0268 (6)0.0206 (5)0.0058 (4)
O10.0556 (10)0.094 (2)0.089 (1)0.009 (1)0.0106 (10)0.042 (1)
O20.066 (1)0.085 (1)0.071 (1)0.0027 (10)0.0187 (9)0.035 (1)
O30.082 (1)0.075 (1)0.081 (1)0.014 (1)0.030 (1)0.004 (1)
O40.109 (2)0.080 (1)0.070 (1)0.044 (1)0.028 (1)0.002 (1)
N10.055 (1)0.144 (3)0.080 (2)0.024 (2)0.016 (1)0.044 (2)
C10.064 (1)0.061 (1)0.063 (1)0.009 (1)0.008 (1)0.020 (1)
C20.076 (2)0.092 (2)0.092 (2)0.011 (2)0.004 (2)0.048 (2)
C30.57 (2)0.107 (6)0.32 (1)0.007 (10)0.25 (2)0.009 (7)
C40.28 (1)0.159 (7)0.34 (1)0.023 (7)0.06 (1)0.162 (9)
C50.181 (8)0.098 (5)0.57 (3)0.042 (5)0.01 (1)0.055 (9)
C60.096 (2)0.054 (1)0.056 (1)0.018 (1)0.012 (1)0.009 (1)
C70.135 (3)0.060 (2)0.075 (2)0.026 (2)0.023 (2)0.001 (2)
C80.223 (7)0.126 (4)0.087 (3)0.057 (5)0.004 (4)0.022 (3)
C90.156 (6)0.219 (8)0.120 (5)0.008 (6)0.012 (4)0.001 (5)
C100.266 (9)0.210 (7)0.116 (4)0.113 (7)0.041 (5)0.047 (5)
C110.066 (5)0.16 (1)0.083 (6)0.007 (6)0.032 (4)0.037 (7)
C120.122 (5)0.28 (1)0.112 (5)0.054 (7)0.017 (4)0.070 (7)
C130.090 (4)0.249 (10)0.123 (5)0.031 (6)0.029 (3)0.054 (6)
C140.071 (5)0.26 (2)0.23 (1)0.068 (8)0.012 (7)0.16 (1)
C150.066 (5)0.14 (1)0.116 (8)0.030 (6)0.033 (4)0.048 (8)
C160.101 (8)0.19 (2)0.18 (1)0.03 (1)0.061 (8)0.01 (1)
C170.082 (5)0.121 (8)0.066 (4)0.034 (5)0.017 (4)0.034 (4)
C180.081 (5)0.18 (1)0.120 (7)0.003 (6)0.058 (5)0.015 (7)
C190.068 (6)0.108 (10)0.119 (8)0.009 (6)0.041 (5)0.020 (7)
C200.16 (1)0.094 (7)0.18 (1)0.061 (8)0.051 (9)0.032 (8)
Geometric parameters (Å, º) top
Cu1—Cu1i2.664 (1)C7—H120.960
Cu1—O11.977 (2)C7—H130.960
Cu1—O2i1.960 (2)C8—H140.958
Cu1—O31.953 (2)C8—H150.962
Cu1—O4i1.965 (2)C8—H160.961
Cu1—N12.244 (3)C9—H170.960
Si1—C21.876 (4)C9—H180.957
Si1—C31.74 (1)C9—H190.967
Si1—C41.816 (7)C10—H200.963
Si1—C51.783 (10)C10—H210.958
Si2—C71.873 (4)C10—H220.958
Si2—C81.835 (5)C11—C121.63 (1)
Si2—C91.816 (8)C11—C161.43 (2)
Si2—C101.861 (7)C12—C131.24 (1)
O1—C11.243 (4)C12—C181.37 (2)
O2—C11.261 (4)C12—H230.962
O3—C61.264 (4)C12—H310.961
O4—C61.254 (4)C13—C141.31 (2)
N1—C111.20 (1)C13—C171.62 (1)
N1—C151.60 (2)C13—H240.959
N1—C171.263 (10)C13—H300.960
N1—C191.47 (2)C14—C151.37 (1)
C1—C21.507 (4)C14—H250.962
C2—H10.960C15—H260.961
C2—H20.960C16—H270.958
C3—H30.961C16—H280.949
C3—H40.950C16—H290.961
C3—H50.967C17—C201.46 (2)
C4—H60.958C18—C191.40 (1)
C4—H70.961C18—H320.964
C4—H80.962C19—H330.962
C5—H90.965C20—H340.957
C5—H100.951C20—H350.960
C5—H110.964C20—H360.963
C6—C71.482 (4)
Cu1i—Cu1—O184.4 (1)Si2—C7—C6113.1 (2)
Cu1i—Cu1—O2i82.8 (1)Si2—C7—H12108.5 (3)
Cu1i—Cu1—O382.1 (1)Si2—C7—H13108.6 (3)
Cu1i—Cu1—O4i85.2 (1)C6—C7—H12108.5 (4)
Cu1i—Cu1—N1177.5 (1)C6—C7—H13108.5 (3)
O1—Cu1—O2i167.1 (1)H12—C7—H13109.5 (4)
O1—Cu1—O389.4 (1)Si2—C8—H14109.7 (5)
O1—Cu1—O4i87.5 (1)Si2—C8—H15109.5 (5)
O1—Cu1—N197.4 (1)Si2—C8—H16109.5 (5)
O2i—Cu1—O389.8 (1)H14—C8—H15109.4 (7)
O2i—Cu1—O4i90.5 (1)H14—C8—H16109.5 (7)
O2i—Cu1—N195.5 (1)H15—C8—H16109.2 (7)
O3—Cu1—O4i167.2 (1)Si2—C9—H17109.7 (7)
O3—Cu1—N196.1 (1)Si2—C9—H18109.9 (6)
O4i—Cu1—N196.7 (1)Si2—C9—H19109.4 (7)
C2—Si1—C3110.1 (3)H17—C9—H18109.7 (9)
C2—Si1—C4110.5 (4)H17—C9—H19108.9 (8)
C2—Si1—C5109.2 (3)H18—C9—H19109.2 (9)
C3—Si1—C4110.3 (7)Si2—C10—H20109.3 (6)
C3—Si1—C5107.4 (8)Si2—C10—H21109.5 (5)
C4—Si1—C5109.2 (6)Si2—C10—H22109.5 (6)
C7—Si2—C8107.7 (2)H20—C10—H21109.4 (8)
C7—Si2—C9108.6 (3)H20—C10—H22109.4 (7)
C7—Si2—C10109.6 (3)H21—C10—H22109.8 (9)
C8—Si2—C9108.9 (3)N1—C11—C12128 (1)
C8—Si2—C10116.1 (4)N1—C11—C16115 (1)
C9—Si2—C10105.6 (5)C12—C11—C16115 (1)
Cu1—O1—C1122.5 (2)C11—C12—C1398.4 (10)
Cu1i—O2—C1124.8 (2)C11—C12—H23130 (1)
Cu1—O3—C6125.9 (2)C13—C12—C18148.7 (10)
Cu1i—O4—C6121.8 (2)C13—C12—H23131 (1)
Cu1—N1—C11137.0 (8)C13—C12—H31105 (1)
Cu1—N1—C15103.5 (4)C18—C12—H31105 (1)
Cu1—N1—C17133.8 (6)C12—C13—C14144.9 (10)
Cu1—N1—C19108.0 (5)C12—C13—C1798.3 (9)
C11—N1—C15118.7 (8)C12—C13—H24107.6 (9)
C17—N1—C19117.7 (7)C12—C13—H30130.9 (9)
O1—C1—O2125.4 (3)C14—C13—H24107.6 (10)
O1—C1—C2117.3 (3)C17—C13—H30130.8 (10)
O2—C1—C2117.3 (3)C13—C14—C15116 (1)
Si1—C2—C1111.7 (2)C13—C14—H25121.7 (10)
Si1—C2—H1108.9 (3)C15—C14—H25121 (1)
Si1—C2—H2108.9 (3)N1—C15—C14112 (1)
C1—C2—H1108.9 (3)N1—C15—H26123.9 (8)
C1—C2—H2108.9 (3)C14—C15—H26123 (1)
H1—C2—H2109.4 (4)C11—C16—H27108 (1)
Si1—C3—H3109 (1)C11—C16—H28109 (1)
Si1—C3—H4109 (1)C11—C16—H29108 (1)
Si1—C3—H5108 (1)H27—C16—H28110 (2)
H3—C3—H4110 (1)H27—C16—H29109 (1)
H3—C3—H5108 (1)H28—C16—H29110 (1)
H4—C3—H5109 (1)N1—C17—C13126.8 (9)
Si1—C4—H6109.6 (8)N1—C17—C20119.4 (9)
Si1—C4—H7109.5 (8)C13—C17—C20113.6 (8)
Si1—C4—H8109.5 (8)C12—C18—C19106 (1)
H6—C4—H7109 (1)C12—C18—H32127 (1)
H6—C4—H8109 (1)C19—C18—H32126 (1)
H7—C4—H8109 (1)N1—C19—C18121 (1)
Si1—C5—H9109.2 (10)N1—C19—H33118 (1)
Si1—C5—H10109.9 (9)C18—C19—H33119 (1)
Si1—C5—H11109.2 (9)C17—C20—H34109 (1)
H9—C5—H10109 (1)C17—C20—H35109 (1)
H9—C5—H11108 (1)C17—C20—H36109 (1)
H10—C5—H11109 (1)H34—C20—H35109 (1)
O3—C6—O4124.8 (3)H34—C20—H36109 (1)
O3—C6—C7116.8 (3)H35—C20—H36109 (1)
O4—C6—C7118.2 (3)
Symmetry code: (i) x, y, z2.
(III) tetrakis(µ-trimethylsilylacetato-O:O')di(3-methylpyridine-N)dicopper(II) top
Crystal data top
[Cu2(C5H11O2Si)4(C6H7N)2]Z = 1
Mr = 838.26F(000) = 442
Triclinic, P1Dx = 1.220 Mg m3
a = 11.148 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.755 (1) ÅCell parameters from 25 reflections
c = 10.563 (3) Åθ = 10–15°
α = 110.91 (1)°µ = 1.08 mm1
β = 117.70 (2)°T = 297 K
γ = 84.23 (2)°Plate-like, light green
V = 1141.3 (5) Å30.4 × 0.3 × 0.1 mm
Data collection top
Rigaku AFC-5
diffractometer
Rint = 0.017
θ–2θ scansθmax = 27.5°
Absorption correction: integration
(Coppens et al., 1965)
h = 014
Tmin = 0.676, Tmax = 0.893k = 1515
5532 measured reflectionsl = 1414
5261 independent reflections3 standard reflections every 100 reflections
3377 reflections with |Fo| > 3σ(|Fo|) intensity decay: none
Refinement top
Refinement on FH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.064 w = 1/[σ2(F) + 0.000225F2]
wR(F2) = 0.054(Δ/σ)max = 0.001
S = 1.23Δρmax = 0.66 e Å3
3377 reflectionsΔρmin = 0.51 e Å3
217 parameters
Crystal data top
[Cu2(C5H11O2Si)4(C6H7N)2]γ = 84.23 (2)°
Mr = 838.26V = 1141.3 (5) Å3
Triclinic, P1Z = 1
a = 11.148 (3) ÅMo Kα radiation
b = 11.755 (1) ŵ = 1.08 mm1
c = 10.563 (3) ÅT = 297 K
α = 110.91 (1)°0.4 × 0.3 × 0.1 mm
β = 117.70 (2)°
Data collection top
Rigaku AFC-5
diffractometer
3377 reflections with |Fo| > 3σ(|Fo|)
Absorption correction: integration
(Coppens et al., 1965)
Rint = 0.017
Tmin = 0.676, Tmax = 0.8933 standard reflections every 100 reflections
5532 measured reflections intensity decay: none
5261 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.064217 parameters
wR(F2) = 0.054H-atom parameters constrained
S = 1.23Δρmax = 0.66 e Å3
3377 reflectionsΔρmin = 0.51 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.89600 (4)0.03538 (4)0.50817 (5)0.0465 (2)
Si21.1805 (1)0.2993 (1)1.0221 (1)0.0742 (7)
Si30.7665 (1)0.3346 (1)0.3148 (2)0.0769 (8)
O41.0200 (3)0.0260 (2)0.7293 (3)0.061 (1)
O51.1962 (2)0.0846 (2)0.7147 (3)0.062 (1)
O60.8398 (2)0.1315 (2)0.5199 (3)0.057 (1)
O71.0195 (2)0.1923 (2)0.5127 (3)0.062 (2)
N80.7301 (3)0.0919 (3)0.5323 (4)0.058 (2)
C91.1389 (4)0.0758 (3)0.7875 (4)0.054 (2)
C101.2122 (4)0.1330 (4)0.9597 (4)0.067 (2)
C111.2646 (6)0.3610 (5)1.2363 (5)0.113 (3)
C121.2534 (6)0.3803 (5)0.9489 (6)0.117 (4)
C130.9930 (5)0.3121 (5)0.9406 (6)0.111 (3)
C140.9072 (4)0.2084 (3)0.5170 (4)0.052 (2)
C150.8504 (4)0.3295 (3)0.5129 (4)0.065 (2)
C160.6929 (6)0.4841 (5)0.3239 (7)0.135 (5)
C170.8923 (6)0.3155 (7)0.2437 (7)0.150 (6)
C180.6300 (5)0.2080 (6)0.1875 (6)0.120 (4)
C190.7183 (4)0.0375 (4)0.6602 (5)0.070 (3)
C200.6033 (5)0.0598 (5)0.6707 (6)0.086 (3)
C210.5015 (5)0.1402 (5)0.5471 (7)0.084 (4)
C220.5120 (4)0.1989 (4)0.4152 (7)0.084 (3)
C230.4011 (6)0.2842 (6)0.2733 (9)0.165 (5)
C240.6283 (4)0.1713 (4)0.4116 (5)0.074 (3)
H17A0.849630.316890.141670.20*
H17B0.932930.239590.244370.20*
H17C0.961830.381490.309970.20*
H16A0.650200.485520.221890.20*
H16B0.763800.548820.390890.20*
H16C0.627500.493520.361390.20*
H18A0.587230.209360.085520.20*
H18B0.564030.218460.224420.20*
H18C0.668030.130960.187820.20*
H190.791320.018760.746990.20*
H200.595160.019040.762630.20*
H210.421940.157170.552530.20*
H23A0.425690.316210.191960.20*
H23B0.322430.238380.246980.20*
H23C0.384630.347580.301980.20*
H240.636230.209940.319240.20*
H15A0.785020.343730.551020.20*
H15B0.923220.392830.577720.20*
H10A1.179600.091471.002650.20*
H10B1.308000.124970.995550.20*
H13A0.976270.396910.970900.20*
H13B0.955270.269710.978300.20*
H13C0.951170.276510.831200.20*
H11A1.247890.445791.266560.20*
H11B1.360490.351991.275860.20*
H11C1.227290.317691.273360.20*
H12A1.236660.465110.979170.20*
H12B1.212360.345010.839470.20*
H12C1.349460.372410.990070.20*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0337 (2)0.0498 (3)0.0536 (3)0.0002 (2)0.0204 (2)0.0158 (2)
Si20.0781 (8)0.0670 (9)0.0558 (8)0.0053 (7)0.0289 (7)0.0085 (6)
Si30.0752 (8)0.0875 (10)0.0921 (10)0.0196 (7)0.0424 (8)0.0521 (8)
O40.056 (2)0.070 (2)0.050 (2)0.003 (1)0.019 (1)0.020 (1)
O50.046 (1)0.076 (2)0.054 (2)0.004 (1)0.021 (1)0.013 (1)
O60.049 (1)0.055 (2)0.073 (2)0.009 (1)0.035 (1)0.024 (1)
O70.052 (2)0.051 (2)0.083 (2)0.001 (1)0.033 (1)0.023 (1)
N80.044 (2)0.060 (2)0.074 (2)0.005 (2)0.030 (2)0.026 (2)
C90.052 (2)0.047 (2)0.055 (3)0.010 (2)0.018 (2)0.019 (2)
C100.065 (3)0.071 (3)0.044 (2)0.002 (2)0.012 (2)0.014 (2)
C110.132 (4)0.098 (4)0.061 (3)0.005 (3)0.037 (3)0.000 (3)
C120.142 (5)0.085 (4)0.114 (4)0.016 (3)0.065 (4)0.026 (3)
C130.089 (4)0.117 (4)0.099 (4)0.030 (3)0.047 (3)0.019 (3)
C140.046 (2)0.056 (3)0.041 (2)0.007 (2)0.016 (2)0.010 (2)
C150.068 (3)0.049 (2)0.076 (3)0.015 (2)0.036 (2)0.024 (2)
C160.164 (6)0.112 (5)0.158 (6)0.053 (4)0.068 (5)0.090 (4)
C170.146 (6)0.224 (8)0.168 (6)0.035 (5)0.106 (5)0.119 (6)
C180.098 (4)0.141 (5)0.102 (4)0.001 (4)0.008 (3)0.055 (4)
C190.063 (3)0.089 (3)0.076 (3)0.009 (2)0.037 (2)0.041 (3)
C200.073 (3)0.126 (5)0.110 (4)0.024 (3)0.052 (3)0.077 (4)
C210.056 (3)0.103 (4)0.147 (5)0.025 (3)0.058 (3)0.082 (4)
C220.046 (2)0.062 (3)0.135 (5)0.005 (2)0.038 (3)0.031 (3)
C230.085 (4)0.111 (5)0.246 (8)0.026 (4)0.078 (5)0.017 (5)
C240.051 (2)0.059 (3)0.102 (4)0.003 (2)0.037 (2)0.020 (3)
Geometric parameters (Å, º) top
Cu1—Cu1i2.638 (3)C10—H10B0.960
Cu1—O41.971 (3)C11—H11A0.960
Cu1—O5i1.958 (3)C11—H11B0.960
Cu1—O61.976 (3)C11—H11C0.960
Cu1—O7i1.973 (3)C12—H12A0.960
Cu1—N82.176 (3)C12—H12B0.960
Si2—C101.881 (5)C12—H12C0.960
Si2—C111.875 (5)C13—H13A0.960
Si2—C121.853 (5)C13—H13B0.961
Si2—C131.868 (6)C13—H13C0.960
Si3—C151.875 (5)C15—H15A0.960
Si3—C161.853 (7)C15—H15B0.960
Si3—C171.839 (7)C16—H16A0.960
Si3—C181.861 (6)C16—H16B0.960
O4—C91.273 (5)C16—H16C0.960
O5—C91.240 (5)C17—H17A0.960
O6—C141.249 (4)C17—H17B0.960
O7—C141.267 (5)C17—H17C0.960
N8—C191.334 (6)C18—H18A0.960
N8—C241.343 (5)C18—H18B0.960
C9—C101.512 (6)C18—H18C0.960
C14—C151.505 (6)C19—H190.960
C19—C201.396 (6)C20—H200.960
C20—C211.357 (8)C21—H210.960
C21—C221.371 (9)C23—H23A0.960
C22—C231.495 (8)C23—H23B0.960
C22—C241.388 (6)C23—H23C0.960
C10—H10A0.960C24—H240.960
O4—Cu1—O5i168.2 (2)H11A—C11—H11B110.4
O4—Cu1—O690.0 (2)H11A—C11—H11C110.5
O4—Cu1—O7i90.3 (2)H11B—C11—H11C109.0
O4—Cu1—N894.5 (2)Si2—C12—H12A109.5
O5i—Cu1—O688.5 (2)Si2—C12—H12B109.7
O5i—Cu1—O7i88.8 (2)Si2—C12—H12C109.3
O5i—Cu1—N897.4 (2)H12A—C12—H12B109.7
O6—Cu1—O7i168.1 (1)H12A—C12—H12C109.6
O6—Cu1—N895.4 (2)H12B—C12—H12C109.0
O7i—Cu1—N896.4 (2)Si2—C13—H13A108.8
C10—Si2—C11107.7 (3)Si2—C13—H13B109.6
C10—Si2—C12108.9 (3)Si2—C13—H13C109.9
C10—Si2—C13108.5 (3)H13A—C13—H13B109.8
C11—Si2—C12110.8 (3)H13A—C13—H13C109.7
C11—Si2—C13111.1 (3)H13B—C13—H13C109.0
C12—Si2—C13109.7 (3)Si3—C15—H15A109.1
C15—Si3—C16107.7 (3)Si3—C15—H15B108.9
C15—Si3—C17109.7 (3)C14—C15—H15A108.9
C15—Si3—C18108.9 (3)C14—C15—H15B108.8
C16—Si3—C17111.0 (4)H15A—C15—H15B109.0
C16—Si3—C18110.3 (3)Si3—C16—H16A106.9
C17—Si3—C18109.2 (3)Si3—C16—H16B109.7
Cu1—O4—C9123.6 (3)Si3—C16—H16C110.5
Cu1i—O5—C9122.5 (3)H16A—C16—H16B110.4
Cu1—O6—C14122.4 (3)H16A—C16—H16C110.4
Cu1i—O7—C14123.9 (3)H16B—C16—H16C109.0
Cu1—N8—C19120.9 (3)Si3—C17—H17A110.1
Cu1—N8—C24120.1 (3)Si3—C17—H17B110.2
C19—N8—C24118.5 (4)Si3—C17—H17C108.4
O4—C9—O5125.5 (4)H17A—C17—H17B109.6
O4—C9—C10116.2 (4)H17A—C17—H17C109.6
O5—C9—C10118.2 (4)H17B—C17—H17C109.0
Si2—C10—C9110.2 (3)Si3—C18—H18A109.4
O6—C14—O7125.3 (4)Si3—C18—H18B109.1
O6—C14—C15118.6 (4)Si3—C18—H18C109.9
O7—C14—C15116.0 (4)H18A—C18—H18B109.7
Si3—C15—C14112.0 (3)H18A—C18—H18C109.7
N8—C19—C20121.9 (4)H18B—C18—H18C109.0
C19—C20—C21118.5 (5)N8—C19—H19118.7
C20—C21—C22120.8 (5)C20—C19—H19119.4
C21—C22—C23123.3 (5)C19—C20—H20121.2
C21—C22—C24117.8 (5)C21—C20—H20120.3
C23—C22—C24118.8 (5)C20—C21—H21119.7
N8—C24—C22122.5 (5)C22—C21—H21119.5
Si2—C10—H10A109.3C22—C23—H23A111.8
Si2—C10—H10B109.6C22—C23—H23B106.2
C9—C10—H10A109.2C22—C23—H23C105.6
C9—C10—H10B109.5H23A—C23—H23B111.9
H10A—C10—H10B109.0H23A—C23—H23C111.9
Si2—C11—H11A106.9H23B—C23—H23C109.0
Si2—C11—H11B109.8N8—C24—H24118.6
Si2—C11—H11C110.3C22—C24—H24118.9
Symmetry code: (i) x+2, y, z+1.
(IV) tetrakis(µ-trimethylsilylacetato-O:O')di(quinoline-N)dicopper(II) top
Crystal data top
[Cu2(C5H11O2Si)4(C9H7N)2]Z = 1
Mr = 910.32F(000) = 478
Triclinic, P1Dx = 1.260 Mg m3
a = 11.298 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.495 (3) ÅCell parameters from 25 reflections
c = 10.261 (3) Åθ = 10–15°
α = 104.03 (2)°µ = 1.03 mm1
β = 110.10 (2)°T = 298 K
γ = 76.99 (2)°Plate-like, dark green
V = 1199.4 (5) Å30.8 × 0.4 × 0.1 mm
Data collection top
Rigaku AFC7R
diffractometer
6024 reflections with I > 1.5σ(I)
Radiation source: Rigaku rotating anodeRint = 0.040
Graphite monochromatorθmax = 32.5°, θmin = 2.5°
θ–2θ scansh = 1717
Absorption correction: integration
(Coppens et al., 1965) numerical
k = 1717
Tmin = 0.659, Tmax = 0.902l = 160
9728 measured reflections3 standard reflections every 150 reflections
8692 independent reflections intensity decay: 2.2%
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.048H-atom parameters not refined
wR(F2) = 0.069 w = 1/[σ2(Fo) + 0.00181|Fo|2]
S = 1.18(Δ/σ)max = 0.004
6191 reflectionsΔρmax = 0.53 e Å3
244 parametersΔρmin = 0.26 e Å3
Crystal data top
[Cu2(C5H11O2Si)4(C9H7N)2]γ = 76.99 (2)°
Mr = 910.32V = 1199.4 (5) Å3
Triclinic, P1Z = 1
a = 11.298 (2) ÅMo Kα radiation
b = 11.495 (3) ŵ = 1.03 mm1
c = 10.261 (3) ÅT = 298 K
α = 104.03 (2)°0.8 × 0.4 × 0.1 mm
β = 110.10 (2)°
Data collection top
Rigaku AFC7R
diffractometer
6024 reflections with I > 1.5σ(I)
Absorption correction: integration
(Coppens et al., 1965) numerical
Rint = 0.040
Tmin = 0.659, Tmax = 0.9023 standard reflections every 150 reflections
9728 measured reflections intensity decay: 2.2%
8692 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0480 restraints
wR(F2) = 0.069H-atom parameters not refined
S = 1.18Δρmax = 0.53 e Å3
6191 reflectionsΔρmin = 0.26 e Å3
244 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 > 1.5σ(F2) is used.

The positions of all the H atoms were calculated geometrically, and a riding model was used in their refinement for (I) and (III) [C—H 0.96 Å, Uiso(H) = 0.2 Å2]. H atom parameters were not refined for (II), (IV), and (V) [Uiso(H)= 1.2 Ueq(parent atom)].

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.09339 (2)0.51565 (3)0.45752 (3)0.03655 (7)
Si10.2776 (1)0.12685 (8)0.6814 (1)0.0748 (3)
Si20.1308 (1)0.75034 (10)0.98828 (9)0.0695 (3)
O10.2044 (2)0.4123 (2)0.5940 (2)0.0529 (5)
O20.0466 (2)0.3836 (2)0.6612 (2)0.0554 (5)
O30.1126 (2)0.6567 (2)0.6133 (2)0.0561 (6)
O40.0456 (2)0.6306 (2)0.6796 (2)0.0564 (5)
N10.2502 (2)0.5550 (2)0.3903 (2)0.0462 (5)
C10.1617 (2)0.3695 (2)0.6678 (2)0.0426 (5)
C20.2556 (3)0.2907 (3)0.7664 (3)0.0556 (7)
C30.1304 (9)0.0698 (6)0.634 (1)0.238 (5)
C40.397 (1)0.0418 (7)0.809 (1)0.314 (5)
C50.3127 (10)0.1084 (5)0.5167 (8)0.179 (3)
C60.0417 (2)0.6865 (2)0.6912 (3)0.0451 (6)
C70.0633 (3)0.7939 (3)0.8083 (3)0.0630 (8)
C80.2585 (7)0.6221 (5)0.9873 (5)0.141 (2)
C90.0030 (8)0.702 (1)1.0292 (8)0.273 (5)
C100.1905 (8)0.8831 (6)1.1173 (6)0.198 (3)
C110.2761 (3)0.6658 (3)0.4399 (3)0.0576 (8)
C120.3834 (3)0.7056 (3)0.4351 (4)0.0650 (9)
C130.4672 (3)0.6256 (3)0.3774 (3)0.0627 (9)
C140.4431 (2)0.5072 (3)0.3190 (3)0.0517 (7)
C150.5241 (3)0.4197 (4)0.2524 (4)0.071 (1)
C160.4962 (4)0.3077 (4)0.1952 (5)0.084 (1)
C170.3864 (4)0.2737 (3)0.2020 (5)0.082 (1)
C180.3071 (3)0.3549 (3)0.2686 (4)0.0613 (8)
C190.3326 (2)0.4736 (2)0.3270 (3)0.0460 (6)
H10.22580.29760.84540.0667*
H20.33650.31880.79890.0667*
H30.10640.07680.71660.2851*
H40.06480.11600.56920.2851*
H50.14070.01390.58890.2851*
H60.37110.05250.89110.3772*
H70.40800.04270.76780.3772*
H80.47750.07110.83570.3772*
H90.32130.02400.47440.2143*
H100.24440.15340.45350.2143*
H110.39090.13810.53520.2143*
H120.01670.84650.80290.0756*
H130.12200.83630.79630.0756*
H140.22610.55520.91720.1696*
H150.32570.64460.96590.1696*
H160.29130.59881.07840.1696*
H170.06580.76871.02990.3278*
H180.02770.63490.95880.3278*
H190.03670.67871.12020.3278*
H200.22480.86291.21000.2380*
H210.25600.90571.09320.2380*
H220.12160.94971.11590.2380*
H230.21810.72370.48240.0692*
H240.39670.78830.47220.0780*
H250.54280.65000.37660.0753*
H260.59990.44100.24810.0850*
H270.55160.24980.14900.1008*
H280.36720.19330.15990.0985*
H290.23380.33050.27530.0736*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0316 (1)0.0420 (2)0.0384 (1)0.00332 (9)0.01314 (10)0.0092 (1)
Si10.0872 (7)0.0467 (5)0.0874 (7)0.0051 (4)0.0227 (5)0.0244 (4)
Si20.0777 (6)0.0803 (6)0.0411 (4)0.0118 (5)0.0188 (4)0.0073 (4)
O10.0382 (8)0.061 (1)0.064 (1)0.0004 (7)0.0141 (8)0.0284 (9)
O20.0421 (8)0.072 (1)0.060 (1)0.0034 (8)0.0173 (8)0.0333 (10)
O30.065 (1)0.054 (1)0.059 (1)0.0202 (9)0.0312 (9)0.0010 (9)
O40.0519 (10)0.062 (1)0.057 (1)0.0136 (8)0.0262 (9)0.0053 (9)
N10.0392 (9)0.051 (1)0.054 (1)0.0035 (8)0.0203 (8)0.0140 (9)
C10.042 (1)0.040 (1)0.042 (1)0.0006 (8)0.0098 (9)0.0084 (9)
C20.051 (1)0.060 (2)0.050 (1)0.004 (1)0.008 (1)0.023 (1)
C30.220 (9)0.102 (5)0.42 (2)0.090 (5)0.155 (10)0.048 (7)
C40.43 (2)0.133 (6)0.214 (9)0.158 (8)0.01 (1)0.063 (6)
C50.32 (1)0.081 (3)0.158 (6)0.022 (5)0.140 (7)0.024 (4)
C60.050 (1)0.041 (1)0.040 (1)0.0038 (9)0.0113 (9)0.0069 (9)
C70.083 (2)0.047 (1)0.052 (1)0.013 (1)0.018 (1)0.005 (1)
C80.191 (6)0.129 (4)0.071 (3)0.059 (4)0.042 (3)0.031 (3)
C90.142 (6)0.63 (2)0.117 (5)0.104 (9)0.029 (4)0.168 (9)
C100.29 (1)0.108 (4)0.086 (4)0.023 (5)0.043 (5)0.028 (3)
C110.058 (1)0.054 (1)0.072 (2)0.008 (1)0.031 (1)0.014 (1)
C120.067 (2)0.059 (2)0.083 (2)0.021 (1)0.029 (2)0.016 (2)
C130.049 (1)0.083 (2)0.071 (2)0.018 (1)0.021 (1)0.026 (2)
C140.039 (1)0.070 (2)0.052 (1)0.003 (1)0.0156 (10)0.023 (1)
C150.052 (1)0.090 (2)0.083 (2)0.001 (1)0.038 (2)0.022 (2)
C160.065 (2)0.089 (3)0.102 (3)0.005 (2)0.049 (2)0.004 (2)
C170.077 (2)0.066 (2)0.108 (3)0.004 (2)0.050 (2)0.004 (2)
C180.048 (1)0.064 (2)0.074 (2)0.008 (1)0.027 (1)0.004 (1)
C190.038 (1)0.057 (1)0.044 (1)0.0018 (9)0.0126 (9)0.015 (1)
Geometric parameters (Å, º) top
Cu1—Cu1i2.665 (1)C5—H100.960
Cu1—O11.969 (2)C5—H110.960
Cu1—O2i1.965 (2)C6—C71.497 (4)
Cu1—O31.973 (2)C7—H120.960
Cu1—O4i1.959 (2)C7—H130.960
Cu1—N12.274 (2)C8—H140.960
Si1—C21.874 (3)C8—H150.960
Si1—C31.792 (8)C8—H160.960
Si1—C41.820 (7)C9—H170.960
Si1—C51.818 (7)C9—H180.959
Si2—C71.885 (3)C9—H190.960
Si2—C81.816 (5)C10—H200.960
Si2—C91.858 (7)C10—H210.960
Si2—C101.846 (5)C10—H220.960
O1—C11.259 (3)C11—C121.408 (4)
O2—C11.254 (3)C11—H230.960
O3—C61.258 (3)C12—C131.349 (4)
O4—C61.251 (3)C12—H240.960
N1—C111.311 (4)C13—C141.395 (4)
N1—C191.376 (3)C13—H250.960
C1—C21.498 (3)C14—C151.414 (4)
C2—H10.960C14—C191.420 (3)
C2—H20.960C15—C161.339 (6)
C3—H30.960C15—H260.960
C3—H40.961C16—C171.410 (5)
C3—H50.960C16—H270.960
C4—H60.958C17—C181.370 (4)
C4—H70.959C17—H280.960
C4—H80.964C18—C191.402 (4)
C5—H90.960C18—H290.960
Cu1i—Cu1—O184.8 (1)H9—C5—H10109.5 (8)
Cu1i—Cu1—O2i82.6 (1)H9—C5—H11109.4 (8)
Cu1i—Cu1—O385.1 (1)H10—C5—H11109.5 (7)
Cu1i—Cu1—O4i81.9 (1)O3—C6—O4124.3 (2)
Cu1i—Cu1—N1176.4 (1)O3—C6—C7118.8 (2)
O1—Cu1—O2i167.3 (1)O4—C6—C7116.9 (2)
O1—Cu1—O388.5 (1)Si2—C7—C6112.8 (2)
O1—Cu1—O4i89.2 (1)Si2—C7—H12108.6 (2)
O1—Cu1—N196.9 (1)Si2—C7—H13108.6 (2)
O2i—Cu1—O389.2 (1)C6—C7—H12108.6 (3)
O2i—Cu1—O4i90.2 (1)C6—C7—H13108.6 (3)
O2i—Cu1—N195.7 (1)H12—C7—H13109.5 (3)
O3—Cu1—O4i166.9 (1)Si2—C8—H14109.5 (5)
O3—Cu1—N191.8 (1)Si2—C8—H15109.5 (5)
O4i—Cu1—N1101.3 (1)Si2—C8—H16109.5 (4)
C2—Si1—C3109.1 (3)H14—C8—H15109.5 (5)
C2—Si1—C4108.6 (3)H14—C8—H16109.5 (6)
C2—Si1—C5111.3 (2)H15—C8—H16109.5 (7)
C3—Si1—C4108.2 (5)Si2—C9—H17109.4 (9)
C3—Si1—C5105.3 (5)Si2—C9—H18109.5 (6)
C4—Si1—C5114.0 (5)Si2—C9—H19109.4 (6)
C7—Si2—C8109.6 (2)H17—C9—H18109.5 (7)
C7—Si2—C9108.7 (2)H17—C9—H19109.4 (9)
C7—Si2—C10108.2 (3)H18—C9—H19109 (1)
C8—Si2—C9107.9 (5)Si2—C10—H20109.5 (5)
C8—Si2—C10110.9 (3)Si2—C10—H21109.5 (5)
C9—Si2—C10111.5 (5)Si2—C10—H22109.4 (5)
Cu1—O1—C1122.2 (1)H20—C10—H21109.5 (7)
Cu1i—O2—C1125.1 (2)H20—C10—H22109.4 (8)
Cu1—O3—C6122.0 (2)H21—C10—H22109.5 (7)
Cu1i—O4—C6126.7 (2)N1—C11—C12124.4 (3)
Cu1—N1—C11113.7 (2)N1—C11—H23117.8 (3)
Cu1—N1—C19128.0 (2)C12—C11—H23117.8 (3)
C11—N1—C19117.2 (2)C11—C12—C13119.0 (3)
O1—C1—O2125.3 (2)C11—C12—H24120.5 (3)
O1—C1—C2117.1 (2)C13—C12—H24120.5 (3)
O2—C1—C2117.6 (2)C12—C13—C14119.4 (3)
Si1—C2—C1112.8 (2)C12—C13—H25120.3 (3)
Si1—C2—H1108.6 (2)C14—C13—H25120.3 (3)
Si1—C2—H2108.6 (2)C13—C14—C15122.7 (3)
C1—C2—H1108.6 (2)C13—C14—C19118.5 (2)
C1—C2—H2108.6 (2)C15—C14—C19118.9 (3)
H1—C2—H2109.5 (3)C14—C15—C16120.8 (3)
Si1—C3—H3109.5 (8)C14—C15—H26119.6 (4)
Si1—C3—H4109.4 (6)C16—C15—H26119.6 (3)
Si1—C3—H5109.5 (7)C15—C16—C17120.7 (3)
H3—C3—H4109.4 (9)C15—C16—H27119.7 (4)
H3—C3—H5109.5 (9)C17—C16—H27119.7 (4)
H4—C3—H5109 (1)C16—C17—C18120.3 (3)
Si1—C4—H6109.6 (7)C16—C17—H28119.8 (3)
Si1—C4—H7109.6 (8)C18—C17—H28119.8 (4)
Si1—C4—H8109.3 (7)C17—C18—C19120.2 (3)
H6—C4—H7109 (1)C17—C18—H29119.9 (3)
H6—C4—H8109 (1)C19—C18—H29119.9 (3)
H7—C4—H8109.2 (10)N1—C19—C14121.5 (2)
Si1—C5—H9109.5 (6)N1—C19—C18119.4 (2)
Si1—C5—H10109.5 (6)C14—C19—C18119.1 (2)
Si1—C5—H11109.5 (6)
Symmetry code: (i) x, y+1, z+1.
(V) catena-poly[tetrakis(µ-trimethylsilylacetato-O:O')dicopper(II)] top
Crystal data top
[Cu2(C5H11O2Si)4]F(000) = 1368
Mr = 652.00Dx = 1.312 Mg m3
Monoclinic, P21/aMo Kα radiation, λ = 0.71073 Å
a = 10.288 (6) ÅCell parameters from 25 reflections
b = 24.692 (5) Åθ = 10–15°
c = 13.116 (5) ŵ = 1.47 mm1
β = 97.71 (4)°T = 298 K
V = 3302 (2) Å3Plate-like, blue-green
Z = 40.3 × 0.1 × 0.05 mm
Data collection top
Rigaku AFC7R
diffractometer
3260 reflections with I > 1.5σ(I)
Radiation source: Rigaku rotating anodeRint = 0.042
Graphite monochromatorθmax = 27.5°, θmin = 2.5°
ω scansh = 130
Absorption correction: Ψ-scan
(North et al., 1968)
k = 032
Tmin = 0.852, Tmax = 0.929l = 1717
7986 measured reflections3 standard reflections every 150 reflections
7574 independent reflections intensity decay: 1.4%
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.068H-atom parameters not refined
wR(F2) = 0.100 w = 1/[σ2(Fo) + 0.00212|Fo|2]
S = 1.48(Δ/σ)max = 0.003
3309 reflectionsΔρmax = 0.78 e Å3
247 parametersΔρmin = 0.60 e Å3
Crystal data top
[Cu2(C5H11O2Si)4]V = 3302 (2) Å3
Mr = 652.00Z = 4
Monoclinic, P21/aMo Kα radiation
a = 10.288 (6) ŵ = 1.47 mm1
b = 24.692 (5) ÅT = 298 K
c = 13.116 (5) Å0.3 × 0.1 × 0.05 mm
β = 97.71 (4)°
Data collection top
Rigaku AFC7R
diffractometer
3260 reflections with I > 1.5σ(I)
Absorption correction: Ψ-scan
(North et al., 1968)
Rint = 0.042
Tmin = 0.852, Tmax = 0.9293 standard reflections every 150 reflections
7986 measured reflections intensity decay: 1.4%
7574 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0680 restraints
wR(F2) = 0.100H-atom parameters not refined
S = 1.48Δρmax = 0.78 e Å3
3309 reflectionsΔρmin = 0.60 e Å3
247 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 > 1.5σ(F2) is used.

The positions of all the H atoms were calculated geometrically, and a riding model was used in their refinement for (I) and (III) [C—H 0.96 Å, Uiso(H) = 0.2 Å2]. H atom parameters were not refined for (II), (IV), and (V) [Uiso(H)= 1.2 Ueq(parent atom)].

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.17891 (9)0.28330 (5)0.74109 (8)0.0320 (3)
Cu20.43030 (9)0.28346 (5)0.80830 (8)0.0329 (3)
Si10.2659 (3)0.3594 (2)1.1210 (2)0.066 (1)
Si20.2816 (4)0.4689 (1)0.6079 (3)0.072 (1)
Si30.3737 (6)0.1901 (2)0.4418 (3)0.103 (2)
Si40.2556 (3)0.0964 (1)0.9330 (3)0.068 (1)
O10.1835 (6)0.3393 (3)0.8505 (5)0.043 (2)
O20.3986 (6)0.3364 (3)0.9063 (5)0.050 (2)
O30.2122 (7)0.3367 (3)0.6419 (5)0.054 (2)
O40.4233 (7)0.3408 (3)0.7034 (6)0.050 (2)
O50.2431 (6)0.2259 (3)0.6528 (5)0.043 (2)
O60.4564 (6)0.2286 (2)0.7076 (5)0.037 (2)
O70.1497 (6)0.2284 (2)0.8425 (5)0.037 (2)
O80.3636 (6)0.2263 (3)0.8965 (5)0.043 (2)
C10.2827 (10)0.3540 (4)0.9102 (8)0.042 (3)
C20.266 (1)0.3932 (4)0.9934 (8)0.054 (3)
C30.232 (2)0.4130 (7)1.212 (1)0.099 (5)*
C40.424 (2)0.3275 (8)1.158 (2)0.138 (7)*
C50.136 (1)0.3077 (6)1.112 (1)0.090 (4)*
C60.326 (1)0.3558 (4)0.6429 (8)0.046 (3)
C70.340 (1)0.4014 (5)0.5690 (9)0.068 (4)
C80.276 (2)0.5136 (9)0.496 (2)0.152 (8)*
C90.117 (2)0.4643 (9)0.645 (2)0.152 (8)*
C100.390 (2)0.4941 (9)0.721 (2)0.155 (8)*
C110.3566 (8)0.2095 (4)0.6507 (7)0.039 (3)
C120.378 (1)0.1657 (4)0.5734 (8)0.056 (3)
C130.391 (3)0.264 (1)0.438 (2)0.189 (10)*
C140.215 (4)0.172 (2)0.375 (3)0.31 (1)*
C150.482 (4)0.150 (2)0.376 (3)0.29 (1)*
C160.2493 (9)0.2106 (4)0.9012 (7)0.037 (2)
C170.2285 (9)0.1681 (4)0.9774 (8)0.049 (3)
C180.255 (3)0.095 (1)0.791 (2)0.24 (1)*
C190.125 (2)0.0540 (9)0.962 (2)0.156 (8)*
C200.389 (4)0.067 (1)1.022 (3)0.26 (1)*
H10.18470.41200.97590.0648*
H20.33730.41880.99870.0648*
H30.29880.44021.21510.1191*
H40.14800.42911.18840.1191*
H50.23030.39761.27870.1191*
H60.42470.31011.22320.1654*
H70.43870.30111.10680.1654*
H80.49150.35451.16240.1654*
H90.05240.32461.09210.1078*
H100.15130.28111.06170.1078*
H110.13640.29051.17770.1078*
H120.29170.39200.50380.0818*
H130.43170.40460.56180.0818*
H140.36180.51630.47600.1819*
H150.21590.49910.44070.1819*
H160.24680.54890.51420.1819*
H170.08910.49950.66480.1829*
H180.05680.45130.58770.1829*
H190.11740.43970.70170.1829*
H200.38820.46950.77750.1861*
H210.47830.49680.70480.1861*
H220.36080.52920.73970.1861*
H230.31010.13890.57430.0673*
H240.46180.14930.59420.0673*
H250.47510.27480.47250.2272*
H260.38240.27630.36740.2272*
H270.32320.28100.47110.2272*
H280.14800.19140.40420.3762*
H290.21090.18050.30370.3762*
H300.20120.13360.38280.3762*
H310.46190.11200.38300.3533*
H320.47050.15910.30400.3533*
H330.57120.15630.40480.3533*
H340.13990.17100.99240.0593*
H350.28810.17471.03900.0593*
H360.17250.10750.75750.2836*
H370.32450.11700.77290.2836*
H380.26850.05800.76980.2836*
H390.11470.05791.03290.1872*
H400.04540.06430.91960.1872*
H410.14530.01700.94780.1872*
H420.36850.07031.09100.3126*
H430.39950.02981.00540.3126*
H440.46870.08651.01620.3126*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0254 (6)0.0347 (6)0.0360 (6)0.0009 (5)0.0040 (4)0.0048 (5)
Cu20.0251 (6)0.0326 (6)0.0410 (6)0.0001 (5)0.0041 (4)0.0036 (6)
Si10.061 (2)0.091 (3)0.046 (2)0.006 (2)0.010 (2)0.014 (2)
Si20.074 (2)0.048 (2)0.093 (3)0.001 (2)0.004 (2)0.023 (2)
Si30.142 (4)0.112 (4)0.051 (2)0.032 (3)0.005 (2)0.017 (2)
Si40.051 (2)0.038 (2)0.118 (3)0.005 (1)0.023 (2)0.023 (2)
O10.039 (4)0.045 (4)0.045 (4)0.003 (3)0.005 (3)0.010 (3)
O20.040 (4)0.050 (4)0.060 (5)0.002 (3)0.010 (3)0.016 (3)
O30.049 (4)0.060 (5)0.053 (4)0.004 (4)0.007 (3)0.019 (4)
O40.043 (4)0.039 (4)0.071 (5)0.002 (3)0.015 (4)0.010 (4)
O50.032 (3)0.048 (4)0.047 (4)0.001 (3)0.000 (3)0.010 (3)
O60.028 (3)0.040 (4)0.045 (4)0.002 (3)0.004 (3)0.009 (3)
O70.029 (3)0.042 (4)0.039 (4)0.002 (3)0.001 (3)0.007 (3)
O80.031 (3)0.045 (4)0.052 (4)0.007 (3)0.006 (3)0.006 (3)
C10.044 (6)0.031 (5)0.051 (6)0.000 (4)0.008 (5)0.003 (4)
C20.060 (7)0.039 (6)0.065 (7)0.001 (5)0.018 (5)0.017 (5)
C60.055 (7)0.036 (6)0.051 (6)0.002 (5)0.019 (5)0.004 (5)
C70.070 (8)0.066 (8)0.070 (8)0.001 (7)0.017 (6)0.022 (7)
C110.032 (5)0.039 (6)0.045 (5)0.003 (4)0.005 (4)0.001 (4)
C120.060 (7)0.054 (7)0.055 (7)0.003 (6)0.008 (5)0.022 (6)
C160.034 (5)0.035 (5)0.041 (5)0.003 (4)0.000 (4)0.001 (4)
C170.034 (5)0.055 (6)0.062 (7)0.002 (5)0.014 (5)0.019 (5)
Geometric parameters (Å, º) top
Cu1—Cu22.618 (2)C4—H70.960
Cu1—O11.988 (6)C4—H80.960
Cu1—O31.916 (7)C5—H90.960
Cu1—O51.997 (6)C5—H100.960
Cu1—O6i2.291 (6)C5—H110.960
Cu1—O71.950 (6)C6—C71.50 (1)
Cu2—O21.892 (6)C7—H120.960
Cu2—O41.970 (7)C7—H130.960
Cu2—O61.935 (6)C8—H140.960
Cu2—O7ii2.261 (6)C8—H150.960
Cu2—O82.003 (6)C8—H160.960
Si1—C21.87 (1)C9—H170.960
Si1—C31.85 (2)C9—H180.960
Si1—C41.81 (2)C9—H190.960
Si1—C51.84 (2)C10—H200.960
Si2—C71.87 (1)C10—H210.960
Si2—C81.83 (2)C10—H220.960
Si2—C91.83 (2)C11—C121.52 (1)
Si2—C101.84 (2)C12—H230.960
Si3—C121.82 (1)C12—H240.960
Si3—C131.85 (3)C13—H250.960
Si3—C141.80 (4)C13—H260.960
Si3—C151.80 (4)C13—H270.960
Si4—C171.90 (1)C14—H280.958
Si4—C181.86 (3)C14—H290.961
Si4—C191.78 (2)C14—H300.961
Si4—C201.82 (4)C15—H310.960
O1—C11.25 (1)C15—H320.961
O2—C11.28 (1)C15—H330.959
O3—C61.26 (1)C16—C171.48 (1)
O4—C61.25 (1)C17—H340.960
O5—C111.24 (1)C17—H350.960
O6—C111.28 (1)C18—H360.960
O7—C161.27 (1)C18—H370.960
O8—C161.25 (1)C18—H380.960
C1—C21.49 (1)C19—H390.960
C2—H10.960C19—H400.960
C2—H20.960C19—H410.960
C3—H30.960C20—H420.959
C3—H40.960C20—H430.960
C3—H50.960C20—H440.961
C4—H60.960
Cu2—Cu1—O180.2 (2)H9—C5—H10109 (1)
Cu2—Cu1—O388.2 (2)H9—C5—H11109 (1)
Cu2—Cu1—O578.9 (2)H10—C5—H11109 (1)
Cu2—Cu1—O790.4 (2)O3—C6—O4124.1 (9)
O1—Cu1—O391.2 (3)O3—C6—C7116.4 (10)
O1—Cu1—O5159.0 (3)O4—C6—C7119.4 (9)
O1—Cu1—O789.0 (3)Si2—C7—C6115.3 (8)
O3—Cu1—O589.5 (3)Si2—C7—H12108.0 (9)
O3—Cu1—O7178.5 (3)Si2—C7—H13108.0 (9)
O5—Cu1—O789.8 (3)C6—C7—H12107 (1)
Cu1—Cu2—O288.7 (2)C6—C7—H13107 (1)
Cu1—Cu2—O479.9 (2)H12—C7—H13109 (1)
Cu1—Cu2—O689.5 (2)Si2—C8—H14109 (1)
Cu1—Cu2—O7ii169.0 (2)Si2—C8—H15109 (1)
Cu1—Cu2—O878.1 (2)Si2—C8—H16109 (1)
O2—Cu2—O489.1 (3)H14—C8—H15109 (2)
O2—Cu2—O6178.0 (3)H14—C8—H16109 (2)
O2—Cu2—O7ii102.3 (2)H15—C8—H16109 (2)
O2—Cu2—O889.5 (3)Si2—C9—H17109 (1)
O4—Cu2—O691.2 (3)Si2—C9—H18109 (1)
O4—Cu2—O7ii100.0 (3)Si2—C9—H19109 (1)
O4—Cu2—O8158.0 (3)H17—C9—H18109 (2)
O6—Cu2—O7ii79.5 (2)H17—C9—H19109 (2)
O6—Cu2—O889.5 (3)H18—C9—H19109 (2)
O7ii—Cu2—O8101.8 (2)Si2—C10—H20109 (1)
C2—Si1—C3106.2 (6)Si2—C10—H21109 (1)
C2—Si1—C4108.8 (7)Si2—C10—H22109 (1)
C2—Si1—C5109.9 (6)H20—C10—H21109 (2)
C3—Si1—C4112.5 (8)H20—C10—H22109 (2)
C3—Si1—C5109.8 (7)H21—C10—H22109 (2)
C4—Si1—C5109.5 (8)O5—C11—O6123.5 (9)
C7—Si2—C8107.3 (8)O5—C11—C12117.9 (8)
C7—Si2—C9111.3 (8)O6—C11—C12118.6 (8)
C7—Si2—C10109.8 (8)Si3—C12—C11114.1 (8)
C8—Si2—C9108 (1)Si3—C12—H23108.3 (8)
C8—Si2—C10113 (1)Si3—C12—H24108.3 (8)
C9—Si2—C10106.9 (10)C11—C12—H23108.3 (9)
C12—Si3—C13111.5 (9)C11—C12—H24108.3 (9)
C12—Si3—C14106 (1)H23—C12—H24109 (1)
C12—Si3—C15109 (1)Si3—C13—H25109 (2)
C13—Si3—C14108 (1)Si3—C13—H26109 (2)
C13—Si3—C15118 (1)Si3—C13—H27109 (2)
C14—Si3—C15101 (1)H25—C13—H26109 (2)
C17—Si4—C18110 (1)H25—C13—H27109 (2)
C17—Si4—C19109.7 (8)H26—C13—H27109 (2)
C17—Si4—C20107 (1)Si3—C14—H28109 (3)
C18—Si4—C19107 (1)Si3—C14—H29109 (3)
C18—Si4—C20122 (1)Si3—C14—H30109 (3)
C19—Si4—C2099 (1)H28—C14—H29109 (4)
Cu1—O1—C1126.2 (6)H28—C14—H30109 (4)
Cu2—O2—C1120.6 (6)H29—C14—H30109 (4)
Cu1—O3—C6120.1 (7)Si3—C15—H31109 (3)
Cu2—O4—C6127.5 (6)Si3—C15—H32109 (3)
Cu1—O5—C11129.1 (6)Si3—C15—H33109 (3)
Cu1—O6i—Cu2i100.7 (2)H31—C15—H32109 (3)
Cu2—O6—C11118.9 (6)H31—C15—H33109 (3)
Cu1—O7—Cu2i101.3 (2)H32—C15—H33109 (3)
Cu1—O7—C16117.8 (5)O7—C16—O8123.4 (8)
Cu2i—O7—C16140.9 (6)O7—C16—C17118.3 (8)
Cu2—O8—C16130.2 (6)O8—C16—C17118.4 (8)
O1—C1—O2124.2 (9)Si4—C17—C16114.4 (7)
O1—C1—C2119.0 (9)Si4—C17—H34108.2 (8)
O2—C1—C2116.8 (9)Si4—C17—H35108.2 (7)
Si1—C2—C1112.3 (7)C16—C17—H34108.2 (9)
Si1—C2—H1108.8 (8)C16—C17—H35108.2 (9)
Si1—C2—H2108.8 (9)H34—C17—H35109 (1)
C1—C2—H1108.8 (9)Si4—C18—H36109 (2)
C1—C2—H2108.8 (9)Si4—C18—H37109 (2)
H1—C2—H2109 (1)Si4—C18—H38109 (2)
Si1—C3—H3109 (1)H36—C18—H37109 (3)
Si1—C3—H4109 (1)H36—C18—H38109 (3)
Si1—C3—H5109 (1)H37—C18—H38109 (3)
H3—C3—H4109 (1)Si4—C19—H39109 (1)
H3—C3—H5109 (1)Si4—C19—H40109 (1)
H4—C3—H5109 (1)Si4—C19—H41109 (1)
Si1—C4—H6109 (1)H39—C19—H40109 (2)
Si1—C4—H7109 (1)H39—C19—H41109 (2)
Si1—C4—H8109 (1)H40—C19—H41109 (2)
H6—C4—H7109 (1)Si4—C20—H42109 (2)
H6—C4—H8109 (2)Si4—C20—H43109 (2)
H7—C4—H8109 (1)Si4—C20—H44109 (2)
Si1—C5—H9109 (1)H42—C20—H43109 (3)
Si1—C5—H10109 (1)H42—C20—H44109 (3)
Si1—C5—H11109 (1)H43—C20—H44109 (3)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x+1/2, y+1/2, z.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formula[Cu2(C5H11O2Si)4(C5H5N)2][Cu2(C5H11O2Si)4(C6H7N)2][Cu2(C5H11O2Si)4(C6H7N)2][Cu2(C5H11O2Si)4(C9H7N)2]
Mr810.20838.26838.26910.32
Crystal system, space groupTriclinic, P1Triclinic, P1Triclinic, P1Triclinic, P1
Temperature (K)299298297298
a, b, c (Å)11.392 (1), 18.508 (2), 10.851 (1)10.874 (2), 11.508 (2), 10.330 (2)11.148 (3), 11.755 (1), 10.563 (3)11.298 (2), 11.495 (3), 10.261 (3)
α, β, γ (°)91.87 (1), 102.79 (1), 76.82 (1)104.26 (2), 109.10 (2), 74.91 (2)110.91 (1), 117.70 (2), 84.23 (2)104.03 (2), 110.10 (2), 76.99 (2)
V3)2171.9 (5)1160.9 (4)1141.3 (5)1199.4 (5)
Z2111
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.131.061.081.03
Crystal size (mm)0.4 × 0.3 × 0.30.5 × 0.5 × 0.20.4 × 0.3 × 0.10.8 × 0.4 × 0.1
Data collection
DiffractometerRigaku AFC-5
diffractometer
Rigaku AFC7R
diffractometer
Rigaku AFC-5
diffractometer
Rigaku AFC7R
diffractometer
Absorption correctionIntegration
(Coppens et al., 1965)
ψ-scan
(North et al., 1968)
Integration
(Coppens et al., 1965)
Integration
(Coppens et al., 1965) numerical
Tmin, Tmax0.971, 0.9780.567, 0.8090.676, 0.8930.659, 0.902
No. of measured, independent and
observed reflections
10462, 9960, 5122 [|Fo| > 3σ(|Fo|)]8822, 8412, 5169 [I > 1.5σ(I)]5532, 5261, 3377 [|Fo| > 3σ(|Fo|)]9728, 8692, 6024 [I > 1.5σ(I)]
Rint0.0170.0090.0170.040
(sin θ/λ)max1)0.6500.7560.6500.756
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.068, 0.053, 1.34 0.051, 0.079, 1.39 0.064, 0.054, 1.23 0.048, 0.069, 1.18
No. of reflections5122535233776191
No. of parameters415253217244
No. of restraints?0?0
H-atom treatmentH-atom parameters constrainedH-atom parameters not refinedH-atom parameters constrainedH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.80, 0.570.45, 0.320.66, 0.510.53, 0.26


(V)
Crystal data
Chemical formula[Cu2(C5H11O2Si)4]
Mr652.00
Crystal system, space groupMonoclinic, P21/a
Temperature (K)298
a, b, c (Å)10.288 (6), 24.692 (5), 13.116 (5)
α, β, γ (°)90, 97.71 (4), 90
V3)3302 (2)
Z4
Radiation typeMo Kα
µ (mm1)1.47
Crystal size (mm)0.3 × 0.1 × 0.05
Data collection
DiffractometerRigaku AFC7R
diffractometer
Absorption correctionΨ-scan
(North et al., 1968)
Tmin, Tmax0.852, 0.929
No. of measured, independent and
observed reflections
7986, 7574, 3260 [I > 1.5σ(I)]
Rint0.042
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.068, 0.100, 1.48
No. of reflections3309
No. of parameters247
No. of restraints0
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.78, 0.60

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, local programs, TEXSAN (Molecular Structure Corporation, 1998), CRYSTAN-GM (Edwards et al., 1996), CRYSTAN-GM, TEXSAN.

Selected geometric parameters (Å, º) for (I) top
Cu1—Cu1i2.632 (1)Cu2—O14ii1.972 (4)
Cu1—O71.962 (4)Cu2—N162.198 (6)
Cu1—O8i1.961 (4)O7—C171.263 (7)
Cu1—O91.982 (4)O8—C171.276 (7)
Cu1—O10i1.972 (4)O9—C221.255 (7)
Cu1—N152.194 (5)O10—C221.268 (7)
Cu2—Cu2ii2.635 (1)O11—C321.252 (10)
Cu2—O111.961 (4)O12—C321.271 (8)
Cu2—O12ii1.965 (4)O13—C371.276 (8)
Cu2—O131.959 (4)O14—C371.258 (8)
O7—Cu1—O8i168.3 (2)O7—C17—O8123.6 (6)
O9—Cu1—O10i168.7 (2)O9—C22—O10125.5 (5)
O11—Cu2—O12ii168.3 (2)O11—C32—O12125.0 (6)
O13—Cu2—O14ii168.5 (2)O13—C37—O14124.6 (6)
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y+2, z+1.
Selected geometric parameters (Å, º) for (II) top
Cu1—Cu1i2.664 (1)Cu1—N12.244 (3)
Cu1—O11.977 (2)O1—C11.243 (4)
Cu1—O2i1.960 (2)O2—C11.261 (4)
Cu1—O31.953 (2)O3—C61.264 (4)
Cu1—O4i1.965 (2)O4—C61.254 (4)
O1—Cu1—O2i167.1 (1)O1—C1—O2125.4 (3)
O3—Cu1—O4i167.2 (1)O3—C6—O4124.8 (3)
Symmetry code: (i) x, y, z2.
Selected geometric parameters (Å, º) for (III) top
Cu1—Cu1i2.638 (3)Cu1—N82.176 (3)
Cu1—O41.971 (3)O4—C91.273 (5)
Cu1—O5i1.958 (3)O5—C91.240 (5)
Cu1—O61.976 (3)O6—C141.249 (4)
Cu1—O7i1.973 (3)O7—C141.267 (5)
O4—Cu1—O5i168.2 (2)O4—C9—O5125.5 (4)
O6—Cu1—O7i168.1 (1)O6—C14—O7125.3 (4)
Symmetry code: (i) x+2, y, z+1.
Selected geometric parameters (Å, º) for (IV) top
Cu1—Cu1i2.665 (1)Cu1—N12.274 (2)
Cu1—O11.969 (2)O1—C11.259 (3)
Cu1—O2i1.965 (2)O2—C11.254 (3)
Cu1—O31.973 (2)O3—C61.258 (3)
Cu1—O4i1.959 (2)O4—C61.251 (3)
O1—Cu1—O2i167.3 (1)O1—C1—O2125.3 (2)
O3—Cu1—O4i166.9 (1)O3—C6—O4124.3 (2)
Symmetry code: (i) x, y+1, z+1.
Selected geometric parameters (Å, º) for (V) top
Cu1—Cu22.618 (2)Cu2—O82.003 (6)
Cu1—O11.988 (6)O1—C11.25 (1)
Cu1—O31.916 (7)O2—C11.28 (1)
Cu1—O51.997 (6)O3—C61.26 (1)
Cu1—O6i2.291 (6)O4—C61.25 (1)
Cu1—O71.950 (6)O5—C111.24 (1)
Cu2—O21.892 (6)O6—C111.28 (1)
Cu2—O41.970 (7)O7—C161.27 (1)
Cu2—O61.935 (6)O8—C161.25 (1)
Cu2—O7ii2.261 (6)
O1—Cu1—O5159.0 (3)Cu1—O7—Cu2i101.3 (2)
O3—Cu1—O7178.5 (3)O1—C1—O2124.2 (9)
O2—Cu2—O6178.0 (3)O3—C6—O4124.1 (9)
O4—Cu2—O8158.0 (3)O5—C11—O6123.5 (9)
Cu1—O6i—Cu2i100.7 (2)O7—C16—O8123.4 (8)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x+1/2, y+1/2, z.
 

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