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The title compound, [Cu8(C8H24O2Si)2(C3H7NO)8]·C4H4N2·C3H7NO, features a sandwich-like cage enclosing a pyrazine mol­ecule, both situated on a centre of inversion. In addition, the crystal structure contains one dimethyl­formamide mol­ecule which is disordered over a centre of inversion. The copper layer, containing eight atoms, is located between two siloxanolate fragments. The whole structure of Cu atoms and siloxanolate rings is distorted by the pyrazine mol­ecule, leading to an oval form. As a result, the angles between the Cu atoms differ at the copper layer. The difference in the angles could lead to some deviations in the Cu-Cu exchange inter­actions within the copper ring, which is of inter­est for mol­ecular magnetism.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106008924/sk3009sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106008924/sk3009Isup2.hkl
Contains datablock I

CCDC reference: 609403

Comment top

In recent years, the synthesis of metallaorganosiloxane compounds has attracted much attention due to the molecular magnetism of these compounds. A series of new crystalline copper-containing organosiloxanes has been synthesized and structurally characterized (Lindeman et al., 1997; Zucchi et al., 2000; Molodtsova et al., 1998; Abbati et al., 2003; Zucchi et al., 1998). We report here the structure of the title novel polyhedral methylsiloxane complex, (I), containing eight Cu atoms, with an encapsulated molecule of pyrazine.

A perspective view of (I) is shown in Fig. 1. The compound features a cage enclosing a pyrazine molecule, both located on a centre of inversion. The cage is composed of two [SiCH3O2]88− rings which are connected by eight Cu atoms. The coordination of the Cu atoms by the O atoms can be described as quadratically pyramidal, where the plane is composed of O atoms of the [SiCH3O2]88− rings. The Cu atoms deviate only slightly from this plane, by 0.2594 (18) Å for Cu1, 0.2170 (17) Å for Cu2, 0.1940 (15) Å for Cu3 and 0.2241 (17) Å for Cu4. The Cu—O distances in the quadratic plane range from 1.934 (3) to 1.973 (3) Å. In addition, each Cu atom is further bonded to the O atom of one dimethylformamide molecule, with Cu—O distances ranging from 2.265 (4) to 2.428 (4) Å. All dimethylformamide molecules are oriented in the same way around the cage. The longest diagonal in the plane of the eight Cu atoms is the distance from Cu3 to its symmetry equivalent [7.9677 (12) Å]. The shortest diagonal (between Cu1 and the symmetry equivalent of Cu4) is 6.5288 (10) Å.

In the centre of the cage, there is a pyrazine molecule oriented almost in the direction of the longest diagonal. The N atoms of the pyrazine molecule show two short contacts to two Cu atoms [N91···Cu3 2.644 (4) Å and N91···Cu2 2.772 (5) Å]. The bonds of the O atoms connecting two Si atoms are significantly longer [1.630 (7) Å] than the Si—O bonds of the O atoms connecting an Si and a Cu atom [1.610 (7) Å]. The only exceptions to this are the bonds Si4—O3 [1.617 (4) Å] and Si4—O41 [1.622 (3) Å].

The eight-membered ring of Cu atoms shows Cu—Cu distances ranging from 2.8150 (9) Å (Cu2—Cu3) to 2.9587 (7) Å [Cu1—Cu4i; symmetry code: (i) 1 − x, 1 − y, 1 − z]. The Cu—Cu—Cu angles at the Cu atoms which are bonded to the pyrazine molecule [131.93 (3)° for Cu2 and 128.69 (2)° for Cu3] are smaller than the remaining two [140.84 (3)° for Cu1 and 138.55 (3)° for Cu4].

In conclusion, it can be said that the title compound constitutes an ideal cage that has been designed to encapsulate a pyrazine guest molecule. The guest fits perfectly into the space offered by the host. Furthermore, attractive Cu···N interactions hold the guest tightly fixed in the cage.

Experimental top

A three-necked flask was charged with EtOH (25 ml). NaOH (0.4 g, 0.01 mol) and MeSi(OEt)3 (2.0 ml, 1.79 g, 0.01 mol) were added with vigorous stirring and the mixture was stirred for 1 h at room temperature. A solution of CuCl2 (0.45 g, 0.003 mol) in EtOH (25 ml) was added dropwise, and then a mixture of water (1.08 g, 0.06 mol) and EtOH (5 ml) was quickly added. The reaction was heated for 20 min at temperature slightly below the boiling point and then filtered hot through the twice-folded filter paper. The resulting blue solution was evaporated using a rotory evaporator and dried in vacuum (1 mm H g, 353 K). A bright-blue crystalline product was obtained (yield 1.68 g, 76.5%). This product was dissolved in dimethylformamide (15 ml) and the solution was then added to a mixture of pyrazine (0.16 g) in dimethylformamide (15 ml). In a few months, some greenish crystals of (I) were obtained which were suitable for X-ray diffraction analysis.

Refinement top

H atoms were placed in calculated positions and refined with fixed individual displacement parameters [Uiso(H) = 1.2Ueq(C) or 1.5 Ueq(Cmethyl)] using a riding model, with C—H = 0.95 or 0.98 Å, for Caromatic or Cmethyl, respectively. The methyl groups of the non disordered dimethylformamide molecules were allowed to rotate but not to tip.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. A perspective view of the title compound, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms and the disordered dimethylformamide molecule have been omitted for clarity. Atoms with the suffix a were generated by the symmetry operator (1 − x, 1 − y, 1 − z).
Bis(µ6-cis-2,4,6,8,10,12,14,16-octamethylcyclooctasiloxane- 2,4,6,8,10,12,14,16-octolato)octakis[(dimethylformamide)copper(II)] dimethylformamide pyrazine solvate top
Crystal data top
[Cu8(C8H24O2Si)2(C3H7NO)8]·C4H4N2·C3H7NOF(000) = 2516
Mr = 2448.26Dx = 1.594 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 20012 reflections
a = 16.9402 (16) Åθ = 3.5–25.8°
b = 18.6388 (18) ŵ = 1.90 mm1
c = 17.2684 (16) ÅT = 173 K
β = 110.679 (7)°Block, light green
V = 5101.1 (9) Å30.22 × 0.20 × 0.18 mm
Z = 2
Data collection top
Stoe IPDS-II two-circle
diffractometer
9372 independent reflections
Radiation source: fine-focus sealed tube5221 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.084
ω scansθmax = 25.8°, θmin = 3.6°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 2020
Tmin = 0.679, Tmax = 0.726k = 2222
39433 measured reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-atom parameters constrained
S = 0.74 w = 1/[σ2(Fo2) + (0.0111P)2]
where P = (Fo2 + 2Fc2)/3
9372 reflections(Δ/σ)max = 0.004
573 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.45 e Å3
Crystal data top
[Cu8(C8H24O2Si)2(C3H7NO)8]·C4H4N2·C3H7NOV = 5101.1 (9) Å3
Mr = 2448.26Z = 2
Monoclinic, P21/nMo Kα radiation
a = 16.9402 (16) ŵ = 1.90 mm1
b = 18.6388 (18) ÅT = 173 K
c = 17.2684 (16) Å0.22 × 0.20 × 0.18 mm
β = 110.679 (7)°
Data collection top
Stoe IPDS-II two-circle
diffractometer
9372 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
5221 reflections with I > 2σ(I)
Tmin = 0.679, Tmax = 0.726Rint = 0.084
39433 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0390 restraints
wR(F2) = 0.069H-atom parameters constrained
S = 0.74Δρmax = 0.66 e Å3
9372 reflectionsΔρmin = 0.45 e Å3
573 parameters
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*/UeqOcc. (<1)
Cu10.61832 (3)0.58601 (3)0.68719 (4)0.02475 (13)
Cu20.45876 (4)0.54479 (3)0.70145 (4)0.02500 (14)
Cu30.31675 (4)0.47343 (3)0.59180 (4)0.02674 (14)
Cu40.29044 (4)0.42052 (3)0.43051 (4)0.02570 (14)
Si10.74894 (8)0.45479 (7)0.70793 (9)0.0270 (3)
C10.8515 (3)0.4746 (3)0.7893 (3)0.0382 (13)
H1A0.87810.42980.81520.057*
H1B0.84270.50580.83120.057*
H1C0.88820.49900.76460.057*
O10.6873 (2)0.41277 (17)0.7468 (2)0.0312 (8)
O110.70293 (19)0.52759 (15)0.6640 (2)0.0268 (7)
Si20.61954 (8)0.43980 (7)0.78820 (9)0.0279 (3)
C20.6729 (4)0.4518 (3)0.8994 (4)0.0420 (13)
H2A0.69880.40630.92420.063*
H2B0.63190.46690.92430.063*
H2C0.71680.48850.90930.063*
O20.5479 (2)0.37751 (17)0.7724 (2)0.0347 (9)
O210.57591 (19)0.51298 (15)0.7441 (2)0.0267 (8)
Si30.44505 (9)0.37552 (7)0.73938 (9)0.0273 (3)
C30.4120 (4)0.3537 (3)0.8286 (4)0.0420 (14)
H3A0.43680.30770.85270.063*
H3B0.35040.35040.80960.063*
H3C0.43150.39150.87050.063*
O30.4139 (2)0.31078 (16)0.6723 (2)0.0347 (8)
O310.40607 (19)0.45069 (16)0.6977 (2)0.0281 (7)
Si40.34807 (9)0.30198 (7)0.57851 (9)0.0285 (3)
C40.2652 (4)0.2386 (3)0.5796 (5)0.0536 (17)
H4A0.29110.19280.60320.080*
H4B0.22600.23090.52300.080*
H4C0.23450.25830.61340.080*
O40.4000 (2)0.26760 (17)0.5242 (2)0.0341 (9)
O410.3087 (2)0.37897 (16)0.5401 (2)0.0293 (8)
Si50.39066 (9)0.27406 (6)0.42748 (9)0.0267 (3)
C50.3174 (3)0.2040 (3)0.3677 (4)0.0426 (14)
H5A0.33930.15660.38960.064*
H5B0.31190.20710.30940.064*
H5C0.26190.21110.37250.064*
O50.4841 (2)0.26220 (16)0.4209 (2)0.0303 (8)
O510.35746 (19)0.35323 (15)0.3940 (2)0.0269 (8)
Si60.52381 (9)0.28975 (7)0.35316 (9)0.0282 (3)
C60.5001 (4)0.2226 (3)0.2700 (4)0.0409 (14)
H6A0.52360.17610.29350.061*
H6B0.52520.23760.22940.061*
H6C0.43880.21820.24270.061*
O60.6260 (2)0.29511 (16)0.3997 (2)0.0311 (8)
O610.4872 (2)0.36741 (15)0.3195 (2)0.0273 (7)
Si70.69851 (8)0.35213 (7)0.39817 (9)0.0275 (3)
C70.7528 (4)0.3141 (3)0.3316 (4)0.0438 (14)
H7A0.77750.26760.35380.066*
H7B0.79760.34690.33040.066*
H7C0.71220.30770.27530.066*
O70.7651 (2)0.36052 (17)0.4918 (2)0.0312 (8)
O710.65712 (19)0.42832 (16)0.3644 (2)0.0277 (7)
Si80.79477 (8)0.42484 (7)0.56099 (9)0.0283 (3)
C80.9120 (3)0.4305 (3)0.6004 (4)0.0394 (13)
H8A0.93590.38430.62460.059*
H8B0.93060.46800.64280.059*
H8C0.93120.44210.55470.059*
O80.7646 (2)0.40367 (16)0.6376 (2)0.0300 (8)
O810.7529 (2)0.49986 (16)0.5205 (2)0.0307 (8)
O1010.7082 (2)0.63818 (18)0.8033 (2)0.0407 (9)
C1010.7708 (3)0.6642 (3)0.7925 (4)0.0366 (13)
H1010.77720.65530.74080.044*
N1010.8289 (3)0.7029 (2)0.8466 (3)0.0371 (11)
C1020.8231 (4)0.7203 (4)0.9262 (5)0.075 (2)
H10A0.78560.76160.92020.112*
H10B0.87930.73210.96560.112*
H10C0.80040.67900.94680.112*
C1030.8955 (4)0.7381 (3)0.8256 (5)0.0575 (18)
H10D0.89460.72070.77170.086*
H10E0.95040.72720.86800.086*
H10F0.88630.79010.82290.086*
O2010.4537 (2)0.5863 (2)0.8260 (2)0.0455 (9)
C2010.5187 (4)0.6185 (3)0.8639 (3)0.0377 (13)
H2010.56750.60650.85140.045*
N2010.5276 (3)0.6690 (2)0.9209 (3)0.0411 (11)
C2020.4545 (4)0.6934 (4)0.9384 (5)0.068 (2)
H20A0.40580.66350.90840.101*
H20B0.44250.74340.92080.101*
H20C0.46590.68990.99800.101*
C2030.6070 (4)0.7041 (4)0.9607 (4)0.0582 (18)
H20D0.62500.69711.02060.087*
H20E0.60090.75560.94820.087*
H20F0.64930.68380.94030.087*
O3010.2101 (3)0.4628 (2)0.6551 (3)0.0566 (11)
C3010.2419 (4)0.4876 (3)0.7256 (4)0.0475 (16)
H3010.28870.51900.73590.057*
N3010.2161 (3)0.4739 (3)0.7882 (3)0.0540 (14)
C3020.1487 (5)0.4250 (5)0.7797 (6)0.092 (3)
H30A0.11720.41640.72080.138*
H30B0.11080.44540.80560.138*
H30C0.17170.37950.80670.138*
C3030.2584 (5)0.5034 (4)0.8683 (5)0.076 (2)
H30D0.31250.52370.87080.114*
H30E0.26820.46550.91010.114*
H30F0.22340.54110.87930.114*
O4010.1560 (2)0.3710 (2)0.3667 (3)0.0464 (10)
C4010.1138 (3)0.3777 (3)0.4103 (4)0.0448 (15)
H4010.14270.38470.46790.054*
N4010.0290 (3)0.3760 (3)0.3827 (3)0.0493 (13)
C4020.0181 (4)0.3672 (5)0.2946 (5)0.075 (2)
H40A0.02130.36370.26470.112*
H40B0.05530.40860.27410.112*
H40C0.05210.32340.28560.112*
C4030.0165 (4)0.3885 (4)0.4370 (5)0.066 (2)
H40D0.02330.39300.49390.100*
H40E0.05470.34820.43340.100*
H40F0.04920.43280.42080.100*
N910.4476 (3)0.4976 (2)0.5457 (3)0.0432 (12)
C920.4465 (3)0.5524 (3)0.4952 (3)0.0339 (12)
H920.40870.59110.49100.041*
C930.4967 (3)0.5546 (3)0.4507 (3)0.0311 (12)
H930.49290.59440.41530.037*
O1L0.0819 (13)0.5343 (18)0.9088 (15)0.229 (12)0.50
C1L0.0413 (18)0.5546 (19)0.9504 (19)0.155 (13)0.50
H1L0.03320.60480.95430.186*0.50
N1L0.00000.50001.00000.218 (15)
C2L0.0427 (10)0.4476 (9)0.9813 (11)0.209 (9)
H2LA0.03060.40271.00450.313*
H2LB0.02540.44300.92110.313*
H2LC0.10340.45761.00490.313*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0241 (3)0.0223 (3)0.0263 (4)0.0001 (2)0.0070 (3)0.0001 (2)
Cu20.0230 (3)0.0235 (3)0.0261 (4)0.0002 (2)0.0057 (3)0.0007 (2)
Cu30.0272 (3)0.0252 (3)0.0253 (4)0.0005 (2)0.0061 (3)0.0013 (2)
Cu40.0258 (3)0.0246 (3)0.0251 (4)0.0002 (2)0.0069 (3)0.0012 (3)
Si10.0257 (7)0.0270 (6)0.0261 (8)0.0027 (5)0.0064 (7)0.0017 (6)
C10.032 (3)0.045 (3)0.034 (4)0.001 (2)0.007 (3)0.004 (3)
O10.0291 (17)0.0300 (17)0.033 (2)0.0040 (15)0.0087 (17)0.0032 (16)
O110.0282 (17)0.0255 (16)0.026 (2)0.0036 (14)0.0081 (17)0.0021 (14)
Si20.0271 (7)0.0270 (7)0.0276 (9)0.0009 (5)0.0072 (7)0.0034 (6)
C20.046 (3)0.042 (3)0.036 (4)0.005 (3)0.011 (3)0.001 (3)
O20.031 (2)0.0279 (17)0.044 (3)0.0012 (14)0.012 (2)0.0098 (16)
O210.0232 (17)0.0239 (16)0.031 (2)0.0023 (13)0.0065 (17)0.0043 (14)
Si30.0305 (8)0.0259 (7)0.0237 (8)0.0029 (5)0.0073 (7)0.0022 (6)
C30.051 (4)0.041 (3)0.036 (4)0.003 (3)0.019 (3)0.007 (3)
O30.046 (2)0.0283 (18)0.024 (2)0.0005 (15)0.005 (2)0.0034 (15)
O310.0274 (17)0.0256 (16)0.029 (2)0.0001 (14)0.0066 (17)0.0038 (15)
Si40.0331 (8)0.0249 (7)0.0270 (9)0.0028 (6)0.0101 (7)0.0002 (6)
C40.051 (4)0.041 (3)0.073 (5)0.016 (3)0.028 (4)0.001 (3)
O40.041 (2)0.0288 (18)0.036 (2)0.0024 (15)0.017 (2)0.0064 (15)
O410.0317 (19)0.0270 (16)0.030 (2)0.0039 (14)0.0113 (18)0.0051 (15)
Si50.0293 (7)0.0206 (6)0.0293 (9)0.0012 (5)0.0092 (7)0.0015 (5)
C50.032 (3)0.034 (3)0.054 (4)0.008 (2)0.006 (3)0.005 (3)
O50.0305 (19)0.0272 (17)0.034 (2)0.0022 (14)0.0121 (19)0.0012 (15)
O510.0295 (19)0.0240 (16)0.025 (2)0.0019 (13)0.0075 (18)0.0013 (14)
Si60.0280 (7)0.0234 (6)0.0318 (9)0.0030 (5)0.0086 (7)0.0004 (6)
C60.050 (3)0.027 (3)0.046 (4)0.002 (2)0.018 (3)0.003 (2)
O60.0246 (18)0.0270 (17)0.039 (2)0.0026 (14)0.0075 (18)0.0060 (15)
O610.0264 (18)0.0236 (16)0.031 (2)0.0009 (13)0.0085 (17)0.0034 (14)
Si70.0258 (7)0.0258 (7)0.0294 (9)0.0032 (5)0.0077 (7)0.0015 (6)
C70.034 (3)0.056 (4)0.044 (4)0.001 (3)0.017 (3)0.005 (3)
O70.0294 (19)0.0327 (18)0.026 (2)0.0090 (14)0.0023 (18)0.0004 (15)
O710.0259 (17)0.0283 (17)0.027 (2)0.0020 (13)0.0070 (17)0.0030 (14)
Si80.0262 (7)0.0296 (7)0.0246 (8)0.0047 (6)0.0033 (7)0.0008 (6)
C80.032 (3)0.040 (3)0.039 (4)0.004 (2)0.003 (3)0.003 (2)
O80.0311 (18)0.0285 (18)0.030 (2)0.0035 (14)0.0102 (18)0.0023 (14)
O810.0320 (19)0.0303 (17)0.030 (2)0.0038 (14)0.0108 (19)0.0015 (15)
O1010.038 (2)0.046 (2)0.038 (3)0.0120 (17)0.014 (2)0.0118 (18)
C1010.039 (3)0.038 (3)0.029 (4)0.003 (2)0.008 (3)0.003 (2)
N1010.030 (2)0.040 (2)0.036 (3)0.006 (2)0.007 (3)0.006 (2)
C1020.049 (4)0.112 (6)0.059 (5)0.018 (4)0.012 (4)0.050 (5)
C1030.046 (4)0.050 (4)0.071 (5)0.026 (3)0.014 (4)0.010 (3)
O2010.040 (2)0.056 (2)0.038 (3)0.011 (2)0.010 (2)0.018 (2)
C2010.039 (3)0.045 (3)0.026 (3)0.002 (3)0.008 (3)0.004 (2)
N2010.035 (3)0.047 (3)0.039 (3)0.002 (2)0.010 (3)0.009 (2)
C2020.064 (5)0.078 (5)0.066 (5)0.000 (4)0.030 (5)0.027 (4)
C2030.055 (4)0.069 (4)0.045 (5)0.022 (3)0.011 (4)0.020 (3)
O3010.054 (3)0.072 (3)0.047 (3)0.016 (2)0.022 (3)0.007 (2)
C3010.043 (4)0.058 (4)0.047 (5)0.007 (3)0.024 (4)0.009 (3)
N3010.054 (3)0.064 (3)0.051 (4)0.015 (3)0.027 (3)0.006 (3)
C3020.098 (6)0.105 (6)0.093 (7)0.043 (5)0.058 (6)0.012 (5)
C3030.089 (6)0.093 (6)0.054 (5)0.022 (4)0.035 (5)0.017 (4)
O4010.031 (2)0.067 (3)0.043 (3)0.0159 (18)0.015 (2)0.015 (2)
C4010.031 (3)0.054 (3)0.045 (4)0.005 (3)0.007 (3)0.005 (3)
N4010.035 (3)0.057 (3)0.056 (4)0.004 (2)0.016 (3)0.005 (3)
C4020.039 (4)0.115 (6)0.064 (6)0.013 (4)0.010 (4)0.014 (5)
C4030.043 (4)0.092 (5)0.077 (6)0.001 (3)0.036 (4)0.005 (4)
N910.044 (3)0.042 (3)0.050 (4)0.004 (2)0.026 (3)0.010 (2)
C920.032 (3)0.029 (2)0.040 (3)0.008 (2)0.011 (3)0.000 (2)
C930.029 (3)0.030 (3)0.031 (3)0.003 (2)0.007 (3)0.007 (2)
O1L0.148 (18)0.39 (4)0.17 (2)0.02 (2)0.082 (17)0.04 (2)
C1L0.10 (2)0.24 (4)0.10 (2)0.04 (2)0.003 (16)0.07 (2)
N1L0.087 (12)0.44 (4)0.074 (13)0.114 (19)0.038 (10)0.119 (19)
C2L0.157 (14)0.184 (16)0.160 (18)0.027 (12)0.100 (13)0.036 (13)
Geometric parameters (Å, º) top
Cu1—O111.951 (3)Si7—C71.849 (5)
Cu1—O61i1.953 (3)C7—H7A0.9800
Cu1—O51i1.956 (3)C7—H7B0.9800
Cu1—O211.958 (3)C7—H7C0.9800
Cu1—O1012.265 (4)O7—Si81.641 (4)
Cu1—Cu22.9030 (8)O71—Cu2i1.955 (3)
Cu1—Cu4i2.9587 (7)O71—Cu3i1.971 (3)
Cu2—O211.949 (3)Si8—O811.611 (3)
Cu2—O71i1.955 (3)Si8—O81.626 (3)
Cu2—O311.959 (3)Si8—C81.861 (5)
Cu2—O61i1.970 (3)C8—H8A0.9800
Cu2—O2012.316 (4)C8—H8B0.9800
Cu2—Cu32.8150 (9)C8—H8C0.9800
Cu3—O81i1.946 (4)O81—Cu3i1.946 (4)
Cu3—O411.957 (3)O81—Cu4i1.973 (3)
Cu3—O311.965 (3)O101—C1011.241 (6)
Cu3—O71i1.971 (3)C101—N1011.308 (7)
Cu3—O3012.428 (4)C101—H1010.9500
Cu3—Cu42.8377 (9)N101—C1021.449 (8)
Cu4—O11i1.934 (3)N101—C1031.459 (6)
Cu4—O511.940 (3)C102—H10A0.9800
Cu4—O411.966 (3)C102—H10B0.9800
Cu4—O81i1.973 (3)C102—H10C0.9800
Cu4—O4012.341 (4)C103—H10D0.9800
Cu4—Cu1i2.9586 (7)C103—H10E0.9800
Si1—O111.615 (3)C103—H10F0.9800
Si1—O11.629 (3)O201—C2011.223 (6)
Si1—O81.637 (3)C201—N2011.333 (7)
Si1—C11.846 (6)C201—H2010.9500
C1—H1A0.9800N201—C2031.434 (7)
C1—H1B0.9800N201—C2021.447 (7)
C1—H1C0.9800C202—H20A0.9800
O1—Si21.631 (3)C202—H20B0.9800
O11—Cu4i1.934 (3)C202—H20C0.9800
Si2—O211.609 (3)C203—H20D0.9800
Si2—O21.631 (3)C203—H20E0.9800
Si2—C21.824 (6)C203—H20F0.9800
C2—H2A0.9800O301—C3011.235 (7)
C2—H2B0.9800C301—N3011.326 (7)
C2—H2C0.9800C301—H3010.9500
O2—Si31.632 (4)N301—C3031.425 (9)
Si3—O311.607 (3)N301—C3021.427 (8)
Si3—O31.627 (4)C302—H30A0.9800
Si3—C31.860 (5)C302—H30B0.9800
C3—H3A0.9800C302—H30C0.9800
C3—H3B0.9800C303—H30D0.9800
C3—H3C0.9800C303—H30E0.9800
O3—Si41.617 (4)C303—H30F0.9800
Si4—O411.622 (3)O401—C4011.213 (6)
Si4—O41.627 (3)C401—N4011.345 (7)
Si4—C41.840 (5)C401—H4010.9500
C4—H4A0.9800N401—C4031.425 (7)
C4—H4B0.9800N401—C4021.458 (9)
C4—H4C0.9800C402—H40A0.9800
O4—Si51.625 (4)C402—H40B0.9800
Si5—O511.612 (3)C402—H40C0.9800
Si5—O51.641 (3)C403—H40D0.9800
Si5—C51.846 (5)C403—H40E0.9800
C5—H5A0.9800C403—H40F0.9800
C5—H5B0.9800N91—C93i1.341 (6)
C5—H5C0.9800N91—C921.340 (7)
O5—Si61.625 (3)C92—C931.333 (6)
O51—Cu1i1.956 (3)C92—H920.9500
Si6—O611.601 (3)C93—N91i1.341 (6)
Si6—O61.635 (4)C93—H930.9500
Si6—C61.840 (5)O1L—C1L1.22 (3)
C6—H6A0.9800C1L—N1L1.64 (4)
C6—H6B0.9800C1L—H1L0.9500
C6—H6C0.9800N1L—C2Lii1.322 (19)
O6—Si71.631 (3)N1L—C2L1.322 (19)
O61—Cu1i1.953 (3)N1L—C1Lii1.64 (4)
O61—Cu2i1.970 (3)C2L—H2LA0.9800
Si7—O711.600 (3)C2L—H2LB0.9800
Si7—O71.619 (4)C2L—H2LC0.9800
O11—Cu1—O61i163.57 (15)Si5—C5—H5B109.5
O11—Cu1—O51i79.65 (12)H5A—C5—H5B109.5
O61i—Cu1—O51i96.87 (12)Si5—C5—H5C109.5
O11—Cu1—O2198.15 (12)H5A—C5—H5C109.5
O61i—Cu1—O2181.28 (12)H5B—C5—H5C109.5
O51i—Cu1—O21165.86 (15)Si6—O5—Si5131.4 (2)
O11—Cu1—O10196.26 (13)Si5—O51—Cu4130.22 (18)
O61i—Cu1—O101100.14 (13)Si5—O51—Cu1i130.70 (17)
O51i—Cu1—O10198.10 (13)Cu4—O51—Cu1i98.83 (13)
O21—Cu1—O10196.02 (13)O61—Si6—O5109.96 (16)
O11—Cu1—Cu2130.04 (9)O61—Si6—O6109.32 (17)
O61i—Cu1—Cu242.50 (8)O5—Si6—O6107.51 (19)
O51i—Cu1—Cu2130.65 (10)O61—Si6—C6112.5 (2)
O21—Cu1—Cu241.91 (9)O5—Si6—C6108.4 (2)
O101—Cu1—Cu2113.15 (8)O6—Si6—C6109.1 (2)
O11—Cu1—Cu4i40.17 (9)Si6—C6—H6A109.5
O61i—Cu1—Cu4i131.82 (10)Si6—C6—H6B109.5
O51i—Cu1—Cu4i40.39 (8)H6A—C6—H6B109.5
O21—Cu1—Cu4i133.60 (9)Si6—C6—H6C109.5
O101—Cu1—Cu4i105.98 (8)H6A—C6—H6C109.5
Cu2—Cu1—Cu4i140.84 (3)H6B—C6—H6C109.5
O21—Cu2—O71i167.67 (14)Si7—O6—Si6134.8 (2)
O21—Cu2—O3197.55 (13)Si6—O61—Cu1i130.72 (17)
O71i—Cu2—O3181.85 (13)Si6—O61—Cu2i132.21 (18)
O21—Cu2—O61i81.07 (12)Cu1i—O61—Cu2i95.45 (13)
O71i—Cu2—O61i96.69 (13)O71—Si7—O7109.81 (18)
O31—Cu2—O61i166.85 (13)O71—Si7—O6110.41 (17)
O21—Cu2—O20196.73 (14)O7—Si7—O6108.05 (19)
O71i—Cu2—O20195.51 (13)O71—Si7—C7111.4 (2)
O31—Cu2—O20199.40 (13)O7—Si7—C7109.5 (2)
O61i—Cu2—O20193.75 (13)O6—Si7—C7107.6 (2)
O21—Cu2—Cu3128.66 (10)Si7—C7—H7A109.5
O71i—Cu2—Cu344.42 (9)Si7—C7—H7B109.5
O31—Cu2—Cu344.24 (10)H7A—C7—H7B109.5
O61i—Cu2—Cu3127.69 (11)Si7—C7—H7C109.5
O201—Cu2—Cu3118.63 (9)H7A—C7—H7C109.5
O21—Cu2—Cu142.13 (8)H7B—C7—H7C109.5
O71i—Cu2—Cu1131.03 (9)Si7—O7—Si8136.3 (2)
O31—Cu2—Cu1131.40 (9)Si7—O71—Cu2i131.33 (19)
O61i—Cu2—Cu142.05 (8)Si7—O71—Cu3i132.5 (2)
O201—Cu2—Cu1109.37 (9)Cu2i—O71—Cu3i91.62 (12)
Cu3—Cu2—Cu1131.93 (3)O81—Si8—O8110.27 (16)
O81i—Cu3—O4181.68 (14)O81—Si8—O7110.10 (19)
O81i—Cu3—O31168.45 (12)O8—Si8—O7108.18 (17)
O41—Cu3—O3197.90 (14)O81—Si8—C8111.1 (2)
O81i—Cu3—O71i96.86 (13)O8—Si8—C8108.5 (2)
O41—Cu3—O71i168.80 (12)O7—Si8—C8108.7 (2)
O31—Cu3—O71i81.30 (13)Si8—C8—H8A109.5
O81i—Cu3—O301100.61 (14)Si8—C8—H8B109.5
O41—Cu3—O301100.87 (13)H8A—C8—H8B109.5
O31—Cu3—O30190.82 (14)Si8—C8—H8C109.5
O71i—Cu3—O30190.33 (13)H8A—C8—H8C109.5
O81i—Cu3—Cu2128.53 (10)H8B—C8—H8C109.5
O41—Cu3—Cu2129.59 (10)Si8—O8—Si1129.9 (2)
O31—Cu3—Cu244.06 (9)Si8—O81—Cu3i132.3 (2)
O71i—Cu3—Cu243.97 (9)Si8—O81—Cu4i129.8 (2)
O301—Cu3—Cu2109.34 (11)Cu3i—O81—Cu4i92.77 (14)
O81i—Cu3—Cu443.99 (9)C101—O101—Cu1112.2 (3)
O41—Cu3—Cu443.78 (10)O101—C101—N101125.0 (5)
O31—Cu3—Cu4129.88 (9)O101—C101—H101117.5
O71i—Cu3—Cu4129.45 (9)N101—C101—H101117.5
O301—Cu3—Cu4121.96 (11)C101—N101—C102121.1 (5)
Cu2—Cu3—Cu4128.69 (2)C101—N101—C103121.5 (5)
O11i—Cu4—O5180.48 (12)C102—N101—C103116.9 (5)
O11i—Cu4—O41166.69 (14)N101—C102—H10A109.5
O51—Cu4—O4198.44 (13)N101—C102—H10B109.5
O11i—Cu4—O81i97.26 (13)H10A—C102—H10B109.5
O51—Cu4—O81i166.93 (14)N101—C102—H10C109.5
O41—Cu4—O81i80.78 (13)H10A—C102—H10C109.5
O11i—Cu4—O40197.87 (14)H10B—C102—H10C109.5
O51—Cu4—O401100.15 (13)N101—C103—H10D109.5
O41—Cu4—O40195.38 (14)N101—C103—H10E109.5
O81i—Cu4—O40192.90 (13)H10D—C103—H10E109.5
O11i—Cu4—Cu3128.20 (9)N101—C103—H10F109.5
O51—Cu4—Cu3129.51 (10)H10D—C103—H10F109.5
O41—Cu4—Cu343.54 (9)H10E—C103—H10F109.5
O81i—Cu4—Cu343.23 (10)C201—O201—Cu2109.8 (3)
O401—Cu4—Cu3112.84 (9)O201—C201—N201126.0 (5)
O11i—Cu4—Cu1i40.62 (8)O201—C201—H201117.0
O51—Cu4—Cu1i40.78 (9)N201—C201—H201117.0
O41—Cu4—Cu1i134.63 (9)C201—N201—C203121.1 (5)
O81i—Cu4—Cu1i133.53 (9)C201—N201—C202119.7 (5)
O401—Cu4—Cu1i108.55 (9)C203—N201—C202118.9 (5)
Cu3—Cu4—Cu1i138.55 (3)N201—C202—H20A109.5
O11—Si1—O1108.95 (16)N201—C202—H20B109.5
O11—Si1—O8108.54 (18)H20A—C202—H20B109.5
O1—Si1—O8108.77 (17)N201—C202—H20C109.5
O11—Si1—C1111.0 (2)H20A—C202—H20C109.5
O1—Si1—C1110.6 (2)H20B—C202—H20C109.5
O8—Si1—C1109.0 (2)N201—C203—H20D109.5
Si1—C1—H1A109.5N201—C203—H20E109.5
Si1—C1—H1B109.5H20D—C203—H20E109.5
H1A—C1—H1B109.5N201—C203—H20F109.5
Si1—C1—H1C109.5H20D—C203—H20F109.5
H1A—C1—H1C109.5H20E—C203—H20F109.5
H1B—C1—H1C109.5C301—O301—Cu3106.1 (3)
Si1—O1—Si2133.3 (2)O301—C301—N301125.2 (6)
Si1—O11—Cu4i130.91 (17)O301—C301—H301117.4
Si1—O11—Cu1129.78 (17)N301—C301—H301117.4
Cu4i—O11—Cu199.21 (14)C301—N301—C303121.3 (5)
O21—Si2—O2109.52 (18)C301—N301—C302121.4 (6)
O21—Si2—O1109.36 (16)C303—N301—C302117.2 (5)
O2—Si2—O1107.65 (18)N301—C302—H30A109.5
O21—Si2—C2111.6 (2)N301—C302—H30B109.5
O2—Si2—C2109.1 (2)H30A—C302—H30B109.5
O1—Si2—C2109.5 (2)N301—C302—H30C109.5
Si2—C2—H2A109.5H30A—C302—H30C109.5
Si2—C2—H2B109.5H30B—C302—H30C109.5
H2A—C2—H2B109.5N301—C303—H30D109.5
Si2—C2—H2C109.5N301—C303—H30E109.5
H2A—C2—H2C109.5H30D—C303—H30E109.5
H2B—C2—H2C109.5N301—C303—H30F109.5
Si2—O2—Si3135.6 (2)H30D—C303—H30F109.5
Si2—O21—Cu2132.29 (17)H30E—C303—H30F109.5
Si2—O21—Cu1129.66 (17)C401—O401—Cu4110.8 (4)
Cu2—O21—Cu195.96 (14)O401—C401—N401124.6 (6)
O31—Si3—O3110.43 (19)O401—C401—H401117.7
O31—Si3—O2110.85 (17)N401—C401—H401117.7
O3—Si3—O2107.67 (18)C401—N401—C403121.4 (6)
O31—Si3—C3111.4 (2)C401—N401—C402119.7 (5)
O3—Si3—C3108.1 (2)C403—N401—C402118.8 (5)
O2—Si3—C3108.2 (2)N401—C402—H40A109.5
Si3—C3—H3A109.5N401—C402—H40B109.5
Si3—C3—H3B109.5H40A—C402—H40B109.5
H3A—C3—H3B109.5N401—C402—H40C109.5
Si3—C3—H3C109.5H40A—C402—H40C109.5
H3A—C3—H3C109.5H40B—C402—H40C109.5
H3B—C3—H3C109.5N401—C403—H40D109.5
Si4—O3—Si3136.4 (2)N401—C403—H40E109.5
Si3—O31—Cu2131.0 (2)H40D—C403—H40E109.5
Si3—O31—Cu3131.7 (2)N401—C403—H40F109.5
Cu2—O31—Cu391.70 (13)H40D—C403—H40F109.5
O3—Si4—O41110.98 (18)H40E—C403—H40F109.5
O3—Si4—O4107.20 (19)C93i—N91—C92115.5 (4)
O41—Si4—O4109.91 (17)C93—C92—N91122.2 (4)
O3—Si4—C4108.2 (3)C93—C92—H92118.9
O41—Si4—C4111.6 (3)N91—C92—H92118.9
O4—Si4—C4108.8 (2)C92—C93—N91i122.2 (5)
Si4—C4—H4A109.5C92—C93—H93118.9
Si4—C4—H4B109.5N91i—C93—H93118.9
H4A—C4—H4B109.5O1L—C1L—N1L123 (3)
Si4—C4—H4C109.5O1L—C1L—H1L118.3
H4A—C4—H4C109.5N1L—C1L—H1L118.3
H4B—C4—H4C109.5C2Lii—N1L—C2L179.998 (8)
Si5—O4—Si4133.4 (2)C2Lii—N1L—C1L92.3 (12)
Si4—O41—Cu3131.1 (2)C2L—N1L—C1L87.7 (12)
Si4—O41—Cu4130.11 (18)C2Lii—N1L—C1Lii87.7 (12)
Cu3—O41—Cu492.68 (13)C2L—N1L—C1Lii92.3 (12)
O51—Si5—O4109.32 (17)C1L—N1L—C1Lii180.0 (16)
O51—Si5—O5108.77 (16)N1L—C2L—H2LA108.6
O4—Si5—O5108.34 (19)N1L—C2L—H2LB109.8
O51—Si5—C5111.5 (2)H2LA—C2L—H2LB109.5
O4—Si5—C5108.9 (2)N1L—C2L—H2LC110.0
O5—Si5—C5109.9 (2)H2LA—C2L—H2LC109.5
Si5—C5—H5A109.5H2LB—C2L—H2LC109.5
O11—Cu1—Cu2—O2148.76 (19)O2—Si3—O31—Cu214.4 (3)
O61i—Cu1—Cu2—O21151.6 (2)C3—Si3—O31—Cu2106.2 (3)
O51i—Cu1—Cu2—O21163.10 (19)O3—Si3—O31—Cu312.0 (3)
O101—Cu1—Cu2—O2172.20 (18)O2—Si3—O31—Cu3131.2 (2)
Cu4i—Cu1—Cu2—O21105.48 (15)C3—Si3—O31—Cu3108.2 (3)
O11—Cu1—Cu2—O71i116.83 (18)O21—Cu2—O31—Si314.9 (3)
O61i—Cu1—Cu2—O71i42.8 (2)O71i—Cu2—O31—Si3177.5 (3)
O51i—Cu1—Cu2—O71i2.48 (18)O61i—Cu2—O31—Si398.0 (6)
O21—Cu1—Cu2—O71i165.6 (2)O201—Cu2—O31—Si383.2 (2)
O101—Cu1—Cu2—O71i122.22 (16)Cu3—Cu2—O31—Si3155.0 (3)
Cu4i—Cu1—Cu2—O71i60.11 (13)Cu1—Cu2—O31—Si343.2 (3)
O11—Cu1—Cu2—O314.29 (19)O21—Cu2—O31—Cu3140.10 (12)
O61i—Cu1—Cu2—O31163.9 (2)O71i—Cu2—O31—Cu327.47 (12)
O51i—Cu1—Cu2—O31118.63 (18)O61i—Cu2—O31—Cu357.1 (6)
O21—Cu1—Cu2—O3144.5 (2)O201—Cu2—O31—Cu3121.75 (13)
O101—Cu1—Cu2—O31116.67 (17)Cu1—Cu2—O31—Cu3111.80 (10)
Cu4i—Cu1—Cu2—O3161.01 (14)O81i—Cu3—O31—Si3100.4 (7)
O11—Cu1—Cu2—O61i159.6 (2)O41—Cu3—O31—Si313.3 (2)
O51i—Cu1—Cu2—O61i45.27 (19)O71i—Cu3—O31—Si3178.0 (2)
O21—Cu1—Cu2—O61i151.6 (2)O301—Cu3—O31—Si387.8 (2)
O101—Cu1—Cu2—O61i79.44 (18)Cu2—Cu3—O31—Si3154.7 (3)
Cu4i—Cu1—Cu2—O61i102.89 (16)Cu4—Cu3—O31—Si346.8 (3)
O11—Cu1—Cu2—O201127.02 (17)O81i—Cu3—O31—Cu254.4 (7)
O61i—Cu1—Cu2—O20173.36 (19)O41—Cu3—O31—Cu2141.43 (11)
O51i—Cu1—Cu2—O201118.63 (16)O71i—Cu3—O31—Cu227.27 (11)
O21—Cu1—Cu2—O20178.27 (18)O301—Cu3—O31—Cu2117.48 (13)
O101—Cu1—Cu2—O2016.07 (15)Cu4—Cu3—O31—Cu2107.94 (10)
Cu4i—Cu1—Cu2—O201176.25 (11)Si3—O3—Si4—O415.6 (4)
O11—Cu1—Cu2—Cu356.24 (14)Si3—O3—Si4—O4125.6 (3)
O61i—Cu1—Cu2—Cu3103.37 (15)Si3—O3—Si4—C4117.2 (3)
O51i—Cu1—Cu2—Cu358.10 (13)O3—Si4—O4—Si5149.9 (3)
O21—Cu1—Cu2—Cu3105.00 (14)O41—Si4—O4—Si529.2 (4)
O101—Cu1—Cu2—Cu3177.20 (11)C4—Si4—O4—Si593.3 (4)
Cu4i—Cu1—Cu2—Cu30.48 (6)O3—Si4—O41—Cu38.8 (3)
O21—Cu2—Cu3—O81i113.47 (15)O4—Si4—O41—Cu3127.2 (2)
O71i—Cu2—Cu3—O81i52.73 (16)C4—Si4—O41—Cu3112.0 (3)
O31—Cu2—Cu3—O81i168.00 (17)O3—Si4—O41—Cu4135.8 (2)
O61i—Cu2—Cu3—O81i1.96 (15)O4—Si4—O41—Cu417.4 (3)
O201—Cu2—Cu3—O81i119.09 (16)C4—Si4—O41—Cu4103.4 (3)
Cu1—Cu2—Cu3—O81i57.39 (12)O81i—Cu3—O41—Si4179.8 (2)
O21—Cu2—Cu3—O411.26 (17)O31—Cu3—O41—Si411.4 (2)
O71i—Cu2—Cu3—O41167.47 (17)O71i—Cu3—O41—Si496.5 (8)
O31—Cu2—Cu3—O4153.26 (17)O301—Cu3—O41—Si481.0 (2)
O61i—Cu2—Cu3—O41112.78 (16)Cu2—Cu3—O41—Si445.6 (3)
O201—Cu2—Cu3—O41126.17 (17)Cu4—Cu3—O41—Si4153.7 (3)
Cu1—Cu2—Cu3—O4157.35 (12)O81i—Cu3—O41—Cu426.08 (12)
O21—Cu2—Cu3—O3154.52 (16)O31—Cu3—O41—Cu4142.26 (12)
O71i—Cu2—Cu3—O31139.27 (17)O71i—Cu3—O41—Cu457.2 (8)
O61i—Cu2—Cu3—O31166.04 (16)O301—Cu3—O41—Cu4125.37 (14)
O201—Cu2—Cu3—O3172.91 (17)Cu2—Cu3—O41—Cu4108.03 (12)
Cu1—Cu2—Cu3—O31110.60 (12)O11i—Cu4—O41—Si497.3 (6)
O21—Cu2—Cu3—O71i166.21 (17)O51—Cu4—O41—Si413.0 (3)
O31—Cu2—Cu3—O71i139.27 (17)O81i—Cu4—O41—Si4179.8 (3)
O61i—Cu2—Cu3—O71i54.69 (16)O401—Cu4—O41—Si488.1 (3)
O201—Cu2—Cu3—O71i66.36 (17)Cu3—Cu4—O41—Si4154.1 (3)
Cu1—Cu2—Cu3—O71i110.13 (13)Cu1i—Cu4—O41—Si434.7 (3)
O21—Cu2—Cu3—O301124.60 (16)O11i—Cu4—O41—Cu356.7 (6)
O71i—Cu2—Cu3—O30169.20 (17)O51—Cu4—O41—Cu3141.04 (13)
O31—Cu2—Cu3—O30170.08 (16)O81i—Cu4—O41—Cu325.76 (13)
O61i—Cu2—Cu3—O301123.88 (16)O401—Cu4—O41—Cu3117.83 (13)
O201—Cu2—Cu3—O3012.83 (17)Cu1i—Cu4—O41—Cu3119.34 (10)
Cu1—Cu2—Cu3—O301179.32 (12)Si4—O4—Si5—O5133.3 (3)
O21—Cu2—Cu3—Cu456.19 (12)Si4—O4—Si5—O5151.7 (3)
O71i—Cu2—Cu3—Cu4110.02 (13)Si4—O4—Si5—C588.7 (3)
O31—Cu2—Cu3—Cu4110.71 (12)O51—Si5—O5—Si635.4 (3)
O61i—Cu2—Cu3—Cu455.33 (11)O4—Si5—O5—Si6154.1 (3)
O201—Cu2—Cu3—Cu4176.38 (12)C5—Si5—O5—Si687.0 (3)
Cu1—Cu2—Cu3—Cu40.11 (5)O4—Si5—O51—Cu426.7 (3)
O81i—Cu3—Cu4—O11i52.96 (17)O5—Si5—O51—Cu4144.8 (2)
O41—Cu3—Cu4—O11i165.82 (18)C5—Si5—O51—Cu493.8 (3)
O31—Cu3—Cu4—O11i113.63 (16)O4—Si5—O51—Cu1i146.3 (2)
O71i—Cu3—Cu4—O11i1.97 (17)O5—Si5—O51—Cu1i28.2 (3)
O301—Cu3—Cu4—O11i123.45 (18)C5—Si5—O51—Cu1i93.2 (3)
Cu2—Cu3—Cu4—O11i55.67 (12)O11i—Cu4—O51—Si5175.0 (3)
O81i—Cu3—Cu4—O51165.05 (17)O41—Cu4—O51—Si518.4 (3)
O41—Cu3—Cu4—O5153.73 (17)O81i—Cu4—O51—Si5103.9 (6)
O31—Cu3—Cu4—O511.54 (16)O401—Cu4—O51—Si578.7 (3)
O71i—Cu3—Cu4—O51114.06 (16)Cu3—Cu4—O51—Si552.5 (3)
O301—Cu3—Cu4—O51124.46 (17)Cu1i—Cu4—O51—Si5174.6 (4)
Cu2—Cu3—Cu4—O5156.42 (12)O11i—Cu4—O51—Cu1i10.32 (14)
O81i—Cu3—Cu4—O41141.22 (18)O41—Cu4—O51—Cu1i156.25 (14)
O31—Cu3—Cu4—O4152.18 (17)O81i—Cu4—O51—Cu1i70.7 (7)
O71i—Cu3—Cu4—O41167.79 (18)O401—Cu4—O51—Cu1i106.69 (15)
O301—Cu3—Cu4—O4170.73 (19)Cu3—Cu4—O51—Cu1i122.09 (10)
Cu2—Cu3—Cu4—O41110.14 (14)Si5—O5—Si6—O6134.4 (3)
O41—Cu3—Cu4—O81i141.22 (18)Si5—O5—Si6—O6153.3 (3)
O31—Cu3—Cu4—O81i166.59 (17)Si5—O5—Si6—C688.9 (3)
O71i—Cu3—Cu4—O81i50.99 (17)O61—Si6—O6—Si719.7 (4)
O301—Cu3—Cu4—O81i70.49 (18)O5—Si6—O6—Si7139.0 (3)
Cu2—Cu3—Cu4—O81i108.63 (13)C6—Si6—O6—Si7103.7 (3)
O81i—Cu3—Cu4—O40168.41 (17)O5—Si6—O61—Cu1i25.6 (3)
O41—Cu3—Cu4—O40172.81 (17)O6—Si6—O61—Cu1i143.4 (2)
O31—Cu3—Cu4—O401125.00 (16)C6—Si6—O61—Cu1i95.3 (3)
O71i—Cu3—Cu4—O401119.40 (16)O5—Si6—O61—Cu2i136.2 (2)
O301—Cu3—Cu4—O4012.08 (17)O6—Si6—O61—Cu2i18.4 (3)
Cu2—Cu3—Cu4—O401177.04 (11)C6—Si6—O61—Cu2i102.9 (3)
O81i—Cu3—Cu4—Cu1i108.34 (13)Si6—O6—Si7—O7120.6 (4)
O41—Cu3—Cu4—Cu1i110.43 (14)Si6—O6—Si7—O7140.7 (3)
O31—Cu3—Cu4—Cu1i58.25 (12)Si6—O6—Si7—C7101.1 (3)
O71i—Cu3—Cu4—Cu1i57.36 (12)O71—Si7—O7—Si85.4 (3)
O301—Cu3—Cu4—Cu1i178.83 (13)O6—Si7—O7—Si8115.1 (3)
Cu2—Cu3—Cu4—Cu1i0.29 (6)C7—Si7—O7—Si8128.0 (3)
O11—Si1—O1—Si233.6 (4)O7—Si7—O71—Cu2i139.2 (2)
O8—Si1—O1—Si2151.8 (3)O6—Si7—O71—Cu2i20.2 (3)
C1—Si1—O1—Si288.6 (4)C7—Si7—O71—Cu2i99.4 (3)
O1—Si1—O11—Cu4i149.0 (2)O7—Si7—O71—Cu3i9.6 (3)
O8—Si1—O11—Cu4i30.7 (3)O6—Si7—O71—Cu3i128.7 (2)
C1—Si1—O11—Cu4i89.0 (3)C7—Si7—O71—Cu3i111.8 (3)
O1—Si1—O11—Cu126.7 (3)Si7—O7—Si8—O817.7 (3)
O8—Si1—O11—Cu1145.0 (2)Si7—O7—Si8—O8112.8 (3)
C1—Si1—O11—Cu195.2 (3)Si7—O7—Si8—C8129.6 (3)
O61i—Cu1—O11—Si1108.0 (5)O81—Si8—O8—Si137.9 (3)
O51i—Cu1—O11—Si1172.9 (3)O7—Si8—O8—Si1158.3 (3)
O21—Cu1—O11—Si121.2 (3)C8—Si8—O8—Si183.9 (3)
O101—Cu1—O11—Si175.8 (3)O11—Si1—O8—Si840.6 (3)
Cu2—Cu1—O11—Si151.7 (3)O1—Si1—O8—Si8159.0 (3)
Cu4i—Cu1—O11—Si1176.8 (4)C1—Si1—O8—Si880.4 (3)
O61i—Cu1—O11—Cu4i68.8 (5)O8—Si8—O81—Cu3i123.8 (2)
O51i—Cu1—O11—Cu4i10.30 (14)O7—Si8—O81—Cu3i4.5 (3)
O21—Cu1—O11—Cu4i155.55 (14)C8—Si8—O81—Cu3i115.9 (3)
O101—Cu1—O11—Cu4i107.43 (14)O8—Si8—O81—Cu4i23.8 (3)
Cu2—Cu1—O11—Cu4i125.07 (9)O7—Si8—O81—Cu4i143.1 (2)
Si1—O1—Si2—O2133.1 (4)C8—Si8—O81—Cu4i96.5 (3)
Si1—O1—Si2—O2152.0 (3)O11—Cu1—O101—C10150.6 (4)
Si1—O1—Si2—C289.5 (4)O61i—Cu1—O101—C101128.3 (3)
O21—Si2—O2—Si314.1 (4)O51i—Cu1—O101—C10129.8 (3)
O1—Si2—O2—Si3132.9 (3)O21—Cu1—O101—C101149.5 (3)
C2—Si2—O2—Si3108.4 (4)Cu2—Cu1—O101—C101170.7 (3)
O2—Si2—O21—Cu216.3 (3)Cu4i—Cu1—O101—C10110.8 (3)
O1—Si2—O21—Cu2134.1 (2)Cu1—O101—C101—N101173.6 (4)
C2—Si2—O21—Cu2104.6 (3)O101—C101—N101—C1021.4 (9)
O2—Si2—O21—Cu1143.1 (2)O101—C101—N101—C103173.0 (5)
O1—Si2—O21—Cu125.4 (3)O21—Cu2—O201—C20141.7 (4)
C2—Si2—O21—Cu196.0 (3)O71i—Cu2—O201—C201136.8 (4)
O71i—Cu2—O21—Si2102.6 (6)O31—Cu2—O201—C201140.6 (4)
O31—Cu2—O21—Si216.2 (3)O61i—Cu2—O201—C20139.7 (4)
O61i—Cu2—O21—Si2177.0 (3)Cu3—Cu2—O201—C201176.9 (3)
O201—Cu2—O21—Si284.2 (3)Cu1—Cu2—O201—C2010.3 (4)
Cu3—Cu2—O21—Si251.2 (3)Cu2—O201—C201—N201155.5 (5)
Cu1—Cu2—O21—Si2164.2 (3)O201—C201—N201—C203179.1 (6)
O71i—Cu2—O21—Cu161.6 (6)O201—C201—N201—C2024.4 (9)
O31—Cu2—O21—Cu1147.99 (13)O81i—Cu3—O301—C301141.2 (4)
O61i—Cu2—O21—Cu118.79 (13)O41—Cu3—O301—C301135.3 (4)
O201—Cu2—O21—Cu1111.55 (14)O31—Cu3—O301—C30137.1 (4)
Cu3—Cu2—O21—Cu1113.03 (10)O71i—Cu3—O301—C30144.2 (4)
O11—Cu1—O21—Si220.4 (3)Cu2—Cu3—O301—C3013.7 (4)
O61i—Cu1—O21—Si2176.2 (3)Cu4—Cu3—O301—C301177.0 (4)
O51i—Cu1—O21—Si2100.3 (5)Cu3—O301—C301—N301159.4 (5)
O101—Cu1—O21—Si276.8 (3)O301—C301—N301—C303178.1 (7)
Cu2—Cu1—O21—Si2164.9 (3)O301—C301—N301—C3022.7 (11)
Cu4i—Cu1—O21—Si242.0 (3)O11i—Cu4—O401—C401134.2 (4)
O11—Cu1—O21—Cu2144.44 (14)O51—Cu4—O401—C401144.1 (4)
O61i—Cu1—O21—Cu218.95 (14)O41—Cu4—O401—C40144.5 (4)
O51i—Cu1—O21—Cu264.5 (5)O81i—Cu4—O401—C40136.5 (4)
O101—Cu1—O21—Cu2118.32 (14)Cu3—Cu4—O401—C4013.2 (4)
Cu4i—Cu1—O21—Cu2122.81 (9)Cu1i—Cu4—O401—C401174.6 (4)
Si2—O2—Si3—O3113.4 (4)Cu4—O401—C401—N401158.2 (5)
Si2—O2—Si3—O3134.3 (3)O401—C401—N401—C403176.3 (6)
Si2—O2—Si3—C3109.0 (3)O401—C401—N401—C4021.5 (9)
O31—Si3—O3—Si46.9 (4)C93i—N91—C92—C930.8 (9)
O2—Si3—O3—Si4128.1 (3)N91—C92—C93—N91i0.9 (10)
C3—Si3—O3—Si4115.2 (3)O1L—C1L—N1L—C2Lii171 (2)
O3—Si3—O31—Cu2133.6 (2)O1L—C1L—N1L—C2L9 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+2.

Experimental details

Crystal data
Chemical formula[Cu8(C8H24O2Si)2(C3H7NO)8]·C4H4N2·C3H7NO
Mr2448.26
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)16.9402 (16), 18.6388 (18), 17.2684 (16)
β (°) 110.679 (7)
V3)5101.1 (9)
Z2
Radiation typeMo Kα
µ (mm1)1.90
Crystal size (mm)0.22 × 0.20 × 0.18
Data collection
DiffractometerStoe IPDS-II two-circle
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 2003; Blessing, 1995)
Tmin, Tmax0.679, 0.726
No. of measured, independent and
observed [I > 2σ(I)] reflections
39433, 9372, 5221
Rint0.084
(sin θ/λ)max1)0.613
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.069, 0.74
No. of reflections9372
No. of parameters573
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.66, 0.45

Computer programs: X-AREA (Stoe & Cie, 2001), X-AREA, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991), SHELXL97 and PLATON (Spek, 2003).

 

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