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Acta Crystallogr Sect E Struct Rep Online. 2008 January 1; 64(Pt 1): m106.
Published online 2007 December 6. doi:  10.1107/S1600536807062903
PMCID: PMC2915059

An ionic organic–inorganic hybrid: tetra­kis[bis­(1,10-phenanthroline)copper(I)] dodeca­tungstophosphate(V)

Abstract

Single crystals of the title polyoxometallate-based organic–inorganic hybrid, [Cu(C12H8N2)2]4[SiW12O40], were grown under hydro­thermal conditions. The discrete [SiW12O40]4− anions are of the Keggin type and are packed in a slightly distorted ortho­rhom­bic F-centred mode, with the complex [CuI(phen)2]+ cations (phen is 1,10-phenanthroline) located in the voids of this arrangement. The four independent CuI cations are situated in the centres of more or less distorted tetra­hedra made up of N atoms from the phen ligands. The anions and cations are linked together via weak hydrogen-bonding inter­actions, forming an extended three-dimensional network. Additional stabilization is achieved via π–π inter­actions between different phen mol­ecules of adjacent [CuI(phen)2]+ cations with shortest distances between 3.416 and 3.499 Å.

Related literature

The educt H4SiW12O40 . nH2O was prepared according to literature procedures (Rocchiccioli-Deltcheff et al., 1983 [triangle]). A review of polyoxometallates was given recently by Kurth et al. (2001 [triangle]). For the bond-valence model, see: Brown (2002 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m106-scheme1.jpg

Experimental

Crystal data

  • [Cu(C12H8N2)2]4[SiW12O40]
  • M r = 4570.08
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m106-efi1.jpg
  • a = 18.332 (3) Å
  • b = 21.173 (3) Å
  • c = 27.901 (4) Å
  • V = 10830 (3) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 13.55 mm−1
  • T = 293 (2) K
  • 0.23 × 0.21 × 0.20 mm

Data collection

  • Bruker SMART APEX CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2001 [triangle]) T min = 0.066, T max = 0.072 (expected range = 0.061–0.066)
  • 66617 measured reflections
  • 24930 independent reflections
  • 20506 reflections with I > 2σ(I)
  • R int = 0.065

Refinement

  • R[F 2 > 2σ(F 2)] = 0.041
  • wR(F 2) = 0.072
  • S = 0.99
  • 24930 reflections
  • 1523 parameters
  • 2431 restraints
  • H-atom parameters constrained
  • Δρmax = 1.29 e Å−3
  • Δρmin = −1.37 e Å−3
  • Absolute structure: Flack (1983 [triangle]), with 11091 Friedel pairs
  • Flack parameter: −0.006 (6)

Data collection: SMART (Bruker, 2001 [triangle]); cell refinement: SAINT (Bruker, 2001 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 [triangle]); molecular graphics: Mercury (Version 1.4.2; Macrae et al., 2006 [triangle]); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807062903/wm2165sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807062903/wm2165Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Analysis and Testing Foundation of Northeast Normal University.

supplementary crystallographic information

Comment

The structure of the title compound is built from four independent complex coordination cations [Cu(phen)2]+ and one Keggin-type anion [SiW12O40]4-. The Keggin anions are arranged in a slightly distorted orthorhombic F-centred packing mode (Fig. 1) with the [Cu(phen)2]+ cations enclosing the Keggin anion, as shown in Fig. 2. In the Keggin anion, the Si—O and W—O distances as well as the corresponding angles are very similar to those of H4SiW12O40 (Kurth et al., 2001). The four Cu+ centres are surrounded in a distorted tetrahedral manner by N atoms from two phen molecules each, with Cu—N distances ranging from 1.982 (10) Å to 2.097 (12) Å, and N—Cu—N bond angles ranging from 81.0 (4)° to 149.3 (4)°.

The structure is held together by weak hydrogen bonding interactions between the phen H atoms of the cations and the terminal and bridging O atoms of the anions (Table 2). Additional stabilization of the structure is reached viaπ–π interactions between adjacent phen molecules with shortest distances between 3.416 Å and 3.499 Å (Fig. 3).

Results of bond valence sum (BVS) calculations (Brown, 2002) are in accordance with expected values for hexavalent tungsten (average for the 12 W atoms 6.19 valence units) and monovalent copper (average for the 4 Cu atoms 0.99 valence units). The presence of Cu+ was also confirmed by ESR experiments.

Experimental

H4SiW12O40.nH2O was prepared according to the method given by Rocchiccioli-Deltcheff et al. (1983). The starting mixture of H4SiW12O40.nH2O (1.15 g), Cu(OAc)2.2H2O (0.16 g), phen (0.065 g), oxalic acid dihydrate (0.25 g) and H2O (10 ml) was adjusted to pH = 2.5 by addition of HCl under stirring for 30 min. The final solution was transferred into a 25 ml Teflon lined autoclave and was heated at 443 K for 72 h. Then the autoclave was cooled with a rate of 10 K.h-1 to room temperature. Deep-black block-like crystals were filtered off, washed with distilled water, and dried at ambient temperature (45% yield on W).

Refinement

The Uij parameters of all C atoms were restrained to be approximately equal by using the SIMU instruction in SHELXL97. Hydrogen atoms were placed geometrically and refined in the riding model with Uiso(H) = 1.2Ueq(C) of the parent C atom. In the final Fourier map, the distance of the highest peak is 0.90 Å away from W2 and the distance of the deepest hole is 0.90 Å from W12.

Figures

Fig. 1.
The packing of the [SiW12O40]4- heteropolyanions leading to a slightly distorted F-centred orthorhombic lattice. All other atoms are omitted for clarity.
Fig. 2.
The Keggin-type SiW12O404- anions with surrounding [Cu(phen)2]+ cations displayed with aniostropic displacement parameters at the 30% probability level. H atoms are omitted for clarity.
Fig. 3.
Packing of the structure viewed down the a axis. H atoms are omitted for clarity.

Crystal data

[Cu(C12H8N2)2]4[SiW12O40]F000 = 8360
Mr = 4570.08Dx = 2.803 Mg m3
Orthorhombic, P212121Mo Kα radiation λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 5100 reflections
a = 18.332 (3) Åθ = 1.5–28.4º
b = 21.173 (3) ŵ = 13.55 mm1
c = 27.901 (4) ÅT = 293 (2) K
V = 10830 (3) Å3Block, black
Z = 40.23 × 0.21 × 0.20 mm

Data collection

Bruker SMART APEX CCD diffractometer24930 independent reflections
Radiation source: fine-focus sealed tube20506 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.065
T = 293(2) K Kθmax = 28.4º
[var phi] and ω scansθmin = 1.5º
Absorption correction: multi-scan(SADABS; Bruker, 2001)h = −24→19
Tmin = 0.066, Tmax = 0.072k = −23→27
66617 measured reflectionsl = −37→37

Refinement

Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.041  w = 1/[σ2(Fo2) + (0.0109P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.072(Δ/σ)max = 0.005
S = 0.99Δρmax = 1.29 e Å3
24930 reflectionsΔρmin = −1.37 e Å3
1523 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
2431 restraintsExtinction coefficient: 0.000046 (2)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), with 11091 Friedel pairs
Secondary atom site location: difference Fourier mapFlack parameter: −0.006 (6)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R- factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R- factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
W10.60792 (2)0.469201 (19)0.599936 (14)0.02241 (9)
W20.32235 (2)0.454247 (18)0.430751 (14)0.02309 (10)
W30.33999 (2)0.462793 (18)0.611797 (13)0.02199 (9)
W40.59085 (3)0.593174 (19)0.506810 (14)0.02581 (10)
W50.33766 (2)0.342912 (17)0.515962 (14)0.02335 (9)
W60.49097 (2)0.346761 (18)0.601527 (14)0.02234 (9)
W70.45059 (3)0.588793 (19)0.429200 (15)0.02552 (10)
W80.58799 (3)0.48431 (2)0.419501 (14)0.02656 (10)
W90.31693 (2)0.573911 (17)0.527752 (14)0.02169 (9)
W100.61225 (2)0.361745 (18)0.512450 (14)0.02279 (9)
W110.45668 (2)0.584345 (18)0.604974 (14)0.02361 (10)
W120.45954 (3)0.350016 (19)0.426112 (14)0.02600 (10)
O10.3909 (4)0.3035 (3)0.4642 (2)0.0284 (17)
O20.2948 (4)0.5093 (3)0.4823 (2)0.0216 (15)
O30.6255 (4)0.4287 (3)0.4668 (2)0.0260 (16)
O40.3142 (4)0.4051 (3)0.5611 (2)0.0225 (15)
O50.4766 (4)0.2962 (3)0.3830 (2)0.040 (2)
O60.6245 (4)0.5311 (3)0.5497 (2)0.0236 (16)
O70.5337 (4)0.3340 (3)0.4716 (2)0.0260 (17)
O80.3881 (4)0.5188 (3)0.4142 (2)0.0232 (16)
O90.3728 (4)0.6203 (3)0.5747 (2)0.0238 (16)
O100.4750 (4)0.6394 (3)0.6467 (2)0.0374 (19)
O110.2814 (5)0.4414 (3)0.6565 (2)0.036 (2)
O120.5174 (4)0.6098 (3)0.5539 (2)0.0268 (17)
O130.5669 (4)0.3141 (3)0.5628 (2)0.0273 (17)
O140.6356 (4)0.5528 (3)0.4537 (2)0.0280 (17)
O150.4233 (4)0.6430 (3)0.3883 (3)0.042 (2)
O160.4196 (4)0.4070 (3)0.6228 (2)0.0224 (16)
O170.6739 (4)0.4887 (3)0.6399 (2)0.0332 (18)
O180.2796 (4)0.5239 (3)0.5787 (2)0.0300 (17)
O190.4829 (4)0.2906 (3)0.6442 (2)0.0355 (19)
O200.6509 (4)0.6524 (3)0.5164 (3)0.0379 (19)
O210.5191 (4)0.4207 (3)0.4064 (2)0.0250 (16)
O220.5636 (4)0.4002 (3)0.6315 (2)0.0223 (16)
O230.5079 (4)0.5168 (3)0.4805 (2)0.0234 (15)
O240.2464 (4)0.6241 (3)0.5203 (2)0.0295 (17)
O250.4207 (4)0.3244 (3)0.5563 (2)0.0217 (16)
O260.5269 (4)0.6332 (3)0.4602 (2)0.0270 (17)
O270.2818 (4)0.3853 (3)0.4682 (2)0.0267 (17)
O280.2804 (4)0.2827 (3)0.5299 (3)0.037 (2)
O290.2543 (4)0.4644 (3)0.3904 (2)0.0330 (17)
O300.6607 (4)0.4099 (3)0.5607 (2)0.0292 (17)
O310.5301 (4)0.5235 (3)0.6190 (2)0.0259 (17)
O320.3781 (4)0.3922 (3)0.3966 (2)0.0276 (17)
O330.4139 (4)0.4206 (3)0.4838 (2)0.0205 (14)
O340.5262 (4)0.5471 (3)0.3917 (2)0.0321 (18)
O350.6791 (5)0.3106 (3)0.4969 (2)0.040 (2)
O360.5229 (4)0.4268 (3)0.54623 (19)0.0178 (15)
O370.3883 (4)0.5316 (3)0.6405 (2)0.0273 (16)
O380.4131 (4)0.5070 (3)0.55134 (19)0.0189 (15)
O390.6480 (5)0.4753 (4)0.3737 (2)0.041 (2)
O400.3867 (4)0.6033 (3)0.4805 (2)0.0236 (16)
Cu10.88189 (11)0.40331 (9)0.63125 (6)0.0666 (5)
Cu20.30068 (11)0.76365 (8)0.64680 (6)0.0582 (5)
Cu30.59060 (10)0.34318 (8)0.23805 (6)0.0546 (4)
Cu40.05409 (10)0.50611 (7)0.39601 (5)0.0526 (5)
C11.0407 (9)0.3619 (7)0.6296 (5)0.072 (2)
H1B1.03020.32880.65040.086*
C21.1133 (9)0.3724 (7)0.6121 (5)0.071 (2)
H2A1.14980.34420.62100.086*
C31.1301 (9)0.4181 (7)0.5850 (5)0.069 (2)
H3A1.17860.42320.57600.083*
C41.0785 (9)0.4612 (7)0.5681 (5)0.065 (2)
C51.0918 (9)0.5108 (6)0.5383 (5)0.066 (2)
H5A1.13910.51620.52690.079*
C61.0412 (9)0.5517 (6)0.5246 (5)0.066 (2)
H6A1.05360.58620.50570.079*
C70.9673 (9)0.5422 (6)0.5394 (5)0.062 (2)
C90.8384 (9)0.5662 (6)0.5374 (5)0.068 (2)
H9A0.79980.59130.52720.081*
C80.9082 (9)0.5781 (6)0.5241 (5)0.066 (2)
H8A0.91700.61200.50360.079*
C100.8276 (9)0.5136 (6)0.5677 (5)0.063 (2)
H10A0.78010.50410.57700.075*
C110.9506 (9)0.4910 (6)0.5695 (5)0.0620 (19)
C121.0077 (9)0.4502 (7)0.5854 (5)0.0626 (19)
C130.7946 (8)0.2880 (6)0.6035 (4)0.049 (2)
H13A0.82870.28100.57940.059*
C140.7347 (8)0.2466 (5)0.6062 (4)0.045 (2)
H14B0.72960.21310.58490.054*
C150.6849 (8)0.2574 (5)0.6408 (4)0.0461 (19)
H15B0.64450.23110.64350.055*
C160.6934 (8)0.3087 (5)0.6733 (4)0.0439 (18)
C170.6425 (8)0.3213 (6)0.7102 (4)0.0477 (18)
H17A0.60140.29610.71420.057*
C180.6554 (8)0.3721 (6)0.7402 (4)0.0481 (18)
H18A0.62160.38160.76390.058*
C190.7189 (8)0.4104 (6)0.7358 (4)0.0458 (18)
C200.7305 (8)0.4614 (6)0.7654 (4)0.0514 (19)
H20A0.69840.47080.79020.062*
C210.7909 (8)0.4981 (6)0.7570 (4)0.052 (2)
H21A0.80010.53320.77610.062*
C220.8385 (8)0.4825 (6)0.7197 (4)0.053 (2)
H22A0.87960.50740.71480.064*
C230.7675 (8)0.3979 (6)0.7000 (4)0.0473 (17)
C240.7557 (8)0.3461 (5)0.6675 (4)0.0426 (17)
C250.3226 (8)0.6457 (6)0.7115 (4)0.0485 (19)
H25A0.36210.63410.69250.058*
C260.3069 (8)0.6103 (6)0.7510 (4)0.050 (2)
H26A0.33740.57700.75940.060*
C270.2468 (7)0.6232 (5)0.7785 (4)0.0433 (18)
H27A0.23440.59730.80420.052*
C280.2046 (8)0.6761 (5)0.7673 (4)0.0414 (17)
C290.1423 (7)0.6931 (5)0.7939 (4)0.0403 (17)
H29A0.12770.66840.81980.048*
C300.1029 (7)0.7458 (5)0.7817 (4)0.0393 (17)
H30A0.06220.75720.79960.047*
C310.1247 (7)0.7838 (5)0.7411 (4)0.0366 (17)
C320.0865 (7)0.8380 (5)0.7277 (4)0.0385 (18)
H14A0.04580.85100.74490.046*
C330.1103 (7)0.8714 (5)0.6888 (4)0.0400 (19)
H16A0.08510.90720.67880.048*
C340.1701 (7)0.8522 (5)0.6651 (4)0.0397 (18)
H34A0.18490.87570.63870.048*
C350.1855 (7)0.7669 (5)0.7158 (4)0.0368 (16)
C360.2252 (7)0.7116 (5)0.7270 (4)0.0384 (16)
C370.2677 (8)0.7625 (5)0.5379 (4)0.0476 (19)
H37A0.21830.76170.54530.057*
C380.2869 (8)0.7594 (5)0.4894 (4)0.0471 (18)
H38A0.25150.75790.46560.057*
C390.3586 (8)0.7588 (5)0.4785 (5)0.0448 (18)
H39A0.37320.75550.44660.054*
C400.4112 (8)0.7631 (5)0.5146 (5)0.0451 (18)
C410.4874 (8)0.7642 (5)0.5053 (4)0.0459 (18)
H41A0.50460.75990.47410.055*
C420.5339 (8)0.7715 (5)0.5412 (4)0.0467 (18)
H42A0.58330.77500.53410.056*
C430.5124 (8)0.7743 (5)0.5898 (4)0.0456 (18)
C440.5599 (8)0.7797 (5)0.6280 (4)0.0485 (19)
H44A0.60990.78140.62260.058*
C450.5336 (8)0.7825 (5)0.6737 (5)0.050 (2)
H45A0.56530.78450.69970.060*
C460.4609 (8)0.7822 (5)0.6806 (5)0.050 (2)
H46A0.44370.78560.71180.059*
C470.4384 (8)0.7741 (5)0.6006 (4)0.0435 (17)
C480.3863 (8)0.7678 (5)0.5622 (4)0.0442 (17)
C490.6414 (9)0.3090 (6)0.3385 (5)0.061 (2)
H49A0.59280.30940.34800.073*
C500.6972 (9)0.2964 (6)0.3733 (5)0.063 (2)
H50A0.68420.28690.40470.075*
C510.7680 (9)0.2981 (6)0.3610 (5)0.064 (2)
H51A0.80330.28950.38400.077*
C520.7892 (9)0.3123 (6)0.3147 (5)0.060 (2)
C530.8624 (9)0.3151 (6)0.2967 (5)0.063 (2)
H53A0.90110.30680.31730.076*
C540.8755 (9)0.3289 (6)0.2527 (5)0.063 (2)
H54A0.92420.33110.24350.076*
C550.8217 (9)0.3411 (6)0.2166 (5)0.0580 (19)
C560.8319 (9)0.3553 (6)0.1692 (5)0.061 (2)
H56A0.87960.35800.15800.073*
C570.7777 (8)0.3655 (6)0.1375 (5)0.061 (2)
H57A0.78630.37480.10540.074*
C580.7073 (8)0.3612 (6)0.1566 (5)0.058 (2)
H58A0.66880.36790.13550.069*
C590.7477 (9)0.3377 (6)0.2328 (5)0.0572 (18)
C600.7295 (9)0.3230 (6)0.2810 (5)0.0576 (18)
C610.5135 (8)0.2694 (6)0.1586 (4)0.048 (2)
H1A0.55100.24000.16070.058*
C620.4621 (8)0.2602 (6)0.1238 (4)0.046 (2)
H62A0.46320.22460.10420.056*
C630.4092 (8)0.3049 (5)0.1186 (4)0.0469 (19)
H63A0.37480.30060.09430.056*
C640.4056 (7)0.3564 (5)0.1487 (4)0.0444 (18)
C650.3516 (8)0.4052 (6)0.1482 (4)0.0481 (18)
H65A0.31680.40470.12400.058*
C660.3484 (8)0.4517 (6)0.1809 (4)0.0500 (18)
H66A0.31140.48170.17960.060*
C670.4031 (8)0.4549 (6)0.2184 (4)0.0463 (18)
C680.4018 (8)0.5016 (6)0.2547 (4)0.0519 (19)
H68A0.36600.53270.25510.062*
C690.4542 (8)0.4994 (6)0.2886 (4)0.053 (2)
H69A0.45280.52800.31390.063*
C700.5103 (8)0.4552 (6)0.2865 (4)0.052 (2)
H70A0.54620.45560.31000.062*
C710.4595 (8)0.4115 (6)0.2193 (4)0.0429 (17)
C720.4605 (8)0.3609 (5)0.1850 (4)0.0434 (16)
C73−0.1100 (9)0.5450 (7)0.4033 (5)0.066 (2)
H73A−0.09980.58200.38660.079*
C74−0.1821 (9)0.5298 (7)0.4148 (5)0.074 (2)
H74A−0.22040.55600.40570.089*
C75−0.1952 (9)0.4752 (7)0.4400 (5)0.073 (2)
H75A−0.24320.46600.44820.087*
C76−0.1427 (8)0.4338 (7)0.4538 (5)0.067 (2)
C77−0.1518 (9)0.3792 (6)0.4788 (5)0.068 (2)
H77A−0.19890.36690.48670.081*
C78−0.0988 (8)0.3441 (6)0.4921 (5)0.064 (2)
H78A−0.10870.30880.51080.077*
C79−0.0279 (8)0.3566 (6)0.4796 (5)0.0593 (19)
C800.0324 (8)0.3194 (6)0.4883 (5)0.061 (2)
H80A0.02630.28160.50470.074*
C810.0987 (8)0.3358 (6)0.4742 (5)0.060 (2)
H81A0.13850.31130.48320.072*
C820.1090 (8)0.3875 (6)0.4468 (4)0.056 (2)
H82A0.15570.39570.43530.067*
C83−0.0138 (8)0.4125 (6)0.4504 (5)0.0576 (18)
C84−0.0728 (8)0.4543 (6)0.4398 (5)0.0598 (18)
C85−0.0082 (8)0.4836 (6)0.2937 (4)0.0522 (19)
H85A−0.03890.45300.30660.063*
C86−0.0169 (8)0.5001 (6)0.2456 (4)0.048 (2)
H86A−0.05230.48100.22670.057*
C870.0278 (8)0.5447 (6)0.2275 (4)0.0465 (19)
H15A0.02160.55750.19590.056*
C880.0838 (7)0.5724 (5)0.2551 (4)0.0419 (17)
C890.1332 (8)0.6190 (6)0.2394 (4)0.0470 (18)
H18B0.12820.63500.20850.056*
C900.1864 (8)0.6408 (6)0.2667 (4)0.0454 (18)
H90A0.22120.66770.25350.055*
C910.1912 (8)0.6234 (5)0.3175 (4)0.0436 (18)
C920.2425 (7)0.6472 (6)0.3489 (4)0.0458 (18)
H92A0.27990.67330.33820.055*
C930.2366 (8)0.6315 (5)0.3962 (4)0.0460 (18)
H93A0.27050.64690.41810.055*
C940.1804 (7)0.5925 (5)0.4119 (4)0.0446 (19)
H94A0.17670.58350.44450.054*
C950.1379 (7)0.5822 (6)0.3349 (4)0.0434 (16)
C960.0866 (8)0.5533 (5)0.3040 (4)0.0431 (16)
N10.6898 (6)0.3484 (5)0.2020 (3)0.044 (3)
N20.3141 (6)0.7663 (4)0.5743 (3)0.043 (3)
N30.5138 (5)0.4128 (4)0.2520 (3)0.036 (2)
N40.8272 (6)0.4339 (4)0.6915 (3)0.043 (3)
N50.8061 (6)0.3361 (4)0.6328 (3)0.039 (3)
N60.0418 (6)0.5093 (4)0.3219 (3)0.044 (3)
N70.5144 (5)0.3170 (4)0.1898 (3)0.035 (2)
N80.1326 (5)0.5681 (4)0.3827 (3)0.035 (2)
N90.8820 (6)0.4761 (5)0.5842 (3)0.049 (3)
N100.2100 (6)0.8014 (4)0.6771 (3)0.035 (2)
N110.0552 (6)0.4278 (4)0.4352 (3)0.039 (2)
N120.2834 (7)0.6967 (4)0.6987 (3)0.051 (3)
N13−0.0562 (7)0.5068 (5)0.4160 (3)0.057 (3)
N140.9886 (6)0.4021 (5)0.6146 (4)0.062 (3)
N150.4130 (6)0.7775 (5)0.6458 (3)0.048 (3)
N160.6579 (7)0.3203 (5)0.2926 (3)0.053 (3)
Si10.46447 (15)0.46771 (11)0.51552 (9)0.0146 (5)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
W10.0197 (2)0.0235 (2)0.0241 (2)0.00063 (17)−0.00485 (19)−0.00050 (17)
W20.0207 (3)0.0237 (2)0.0249 (2)0.00116 (17)−0.00588 (19)−0.00199 (17)
W30.0197 (2)0.0234 (2)0.0228 (2)0.00076 (17)0.00518 (18)0.00090 (17)
W40.0210 (3)0.0235 (2)0.0330 (2)−0.00702 (18)−0.0007 (2)0.00533 (17)
W50.0222 (3)0.01697 (19)0.0309 (2)−0.00510 (17)−0.0021 (2)−0.00112 (17)
W60.0226 (3)0.0199 (2)0.0245 (2)0.00215 (17)−0.00037 (19)0.00576 (17)
W70.0222 (3)0.0258 (2)0.0286 (2)0.00014 (18)0.0001 (2)0.01133 (18)
W80.0213 (3)0.0362 (2)0.0221 (2)0.00214 (19)0.00498 (19)0.00588 (18)
W90.0189 (2)0.01701 (19)0.0292 (2)0.00386 (16)0.00012 (19)0.00018 (16)
W100.0198 (2)0.0225 (2)0.0260 (2)0.00685 (17)0.00054 (19)−0.00064 (17)
W110.0233 (3)0.0192 (2)0.0283 (2)0.00003 (17)−0.00081 (19)−0.00737 (17)
W120.0264 (3)0.0262 (2)0.0254 (2)0.00377 (19)−0.0027 (2)−0.00968 (18)
O10.031 (5)0.025 (4)0.029 (4)−0.003 (3)−0.004 (4)0.004 (3)
O20.014 (4)0.019 (3)0.031 (3)0.002 (3)0.002 (3)0.004 (3)
O30.016 (4)0.027 (4)0.036 (4)0.005 (3)0.004 (3)−0.005 (3)
O40.013 (4)0.021 (3)0.034 (4)−0.003 (3)−0.001 (3)0.002 (3)
O50.026 (5)0.054 (5)0.039 (4)0.012 (4)−0.006 (4)−0.023 (4)
O60.017 (4)0.023 (4)0.030 (4)−0.002 (3)0.005 (3)0.001 (3)
O70.029 (5)0.022 (4)0.026 (4)0.003 (3)0.001 (3)−0.003 (3)
O80.019 (4)0.021 (3)0.030 (3)0.006 (3)−0.002 (3)0.004 (3)
O90.022 (4)0.016 (3)0.033 (4)0.003 (3)−0.005 (3)0.003 (3)
O100.027 (5)0.040 (5)0.045 (4)−0.002 (4)0.008 (4)−0.023 (4)
O110.039 (6)0.043 (5)0.026 (4)0.003 (4)0.009 (4)0.006 (3)
O120.027 (5)0.014 (3)0.039 (4)−0.003 (3)0.004 (3)0.005 (3)
O130.033 (5)0.021 (4)0.028 (4)0.006 (3)−0.006 (3)−0.006 (3)
O140.019 (5)0.035 (4)0.030 (4)0.003 (3)0.006 (3)0.009 (3)
O150.034 (5)0.043 (5)0.048 (5)−0.007 (4)0.000 (4)0.022 (4)
O160.030 (5)0.009 (3)0.028 (3)−0.008 (3)0.003 (3)0.000 (3)
O170.029 (5)0.035 (4)0.036 (4)0.000 (3)−0.017 (4)−0.003 (3)
O180.023 (5)0.032 (4)0.035 (4)0.007 (3)0.002 (3)−0.001 (3)
O190.034 (5)0.032 (4)0.041 (4)0.005 (4)−0.001 (4)0.014 (3)
O200.032 (5)0.030 (4)0.052 (4)−0.005 (3)−0.003 (4)0.004 (4)
O210.025 (5)0.025 (4)0.024 (3)0.002 (3)0.005 (3)0.000 (3)
O220.014 (4)0.023 (4)0.030 (4)0.006 (3)−0.005 (3)−0.007 (3)
O230.012 (4)0.033 (4)0.024 (3)−0.003 (3)−0.004 (3)−0.002 (3)
O240.031 (5)0.016 (3)0.041 (4)0.007 (3)0.005 (4)0.008 (3)
O250.020 (4)0.015 (3)0.030 (4)0.006 (3)0.001 (3)−0.003 (3)
O260.030 (5)0.022 (4)0.028 (4)−0.003 (3)−0.002 (3)0.008 (3)
O270.015 (4)0.026 (4)0.039 (4)−0.002 (3)−0.010 (3)0.000 (3)
O280.032 (5)0.016 (4)0.064 (5)−0.006 (3)−0.015 (4)0.004 (3)
O290.027 (5)0.035 (4)0.037 (4)−0.002 (3)−0.006 (4)0.006 (3)
O300.028 (5)0.031 (4)0.029 (4)0.005 (3)0.007 (3)−0.001 (3)
O310.030 (5)0.018 (3)0.030 (4)0.000 (3)0.005 (3)−0.008 (3)
O320.026 (5)0.034 (4)0.023 (3)0.000 (3)−0.012 (3)−0.008 (3)
O330.020 (4)0.020 (3)0.021 (3)0.002 (3)−0.001 (3)0.004 (3)
O340.025 (5)0.042 (4)0.030 (4)0.002 (3)0.010 (3)0.021 (3)
O350.031 (5)0.035 (4)0.053 (5)0.020 (4)−0.009 (4)−0.007 (3)
O360.021 (4)0.012 (3)0.020 (3)0.003 (3)0.003 (3)−0.005 (2)
O370.024 (5)0.030 (4)0.029 (4)0.005 (3)−0.003 (3)0.001 (3)
O380.019 (4)0.017 (3)0.020 (3)−0.001 (3)0.000 (3)0.007 (3)
O390.036 (6)0.059 (5)0.027 (4)0.004 (4)0.004 (4)0.010 (4)
O400.023 (4)0.015 (3)0.033 (4)0.002 (3)−0.005 (3)−0.001 (3)
Cu10.0489 (13)0.0670 (12)0.0838 (13)−0.0113 (10)0.0172 (10)0.0242 (10)
Cu20.0609 (14)0.0582 (11)0.0555 (10)0.0017 (9)0.0334 (10)0.0065 (8)
Cu30.0314 (11)0.0685 (11)0.0638 (10)0.0077 (9)−0.0003 (9)0.0088 (9)
Cu40.0629 (13)0.0515 (10)0.0432 (8)−0.0153 (8)−0.0030 (9)0.0243 (7)
C10.057 (5)0.066 (5)0.093 (5)−0.007 (4)0.003 (4)0.011 (4)
C20.053 (5)0.068 (5)0.094 (5)−0.002 (4)0.002 (4)0.008 (4)
C30.053 (4)0.065 (4)0.089 (4)−0.007 (4)0.005 (4)0.008 (4)
C40.052 (4)0.060 (4)0.083 (4)−0.009 (4)0.006 (4)0.007 (4)
C50.050 (4)0.063 (4)0.085 (4)−0.014 (4)0.010 (4)0.003 (4)
C60.057 (4)0.058 (4)0.083 (4)−0.013 (4)0.009 (4)0.008 (4)
C70.052 (4)0.054 (4)0.081 (4)−0.009 (4)0.011 (4)0.005 (4)
C90.057 (5)0.058 (4)0.087 (5)−0.001 (4)0.010 (4)0.010 (4)
C80.058 (4)0.057 (4)0.084 (4)−0.007 (4)0.008 (4)0.011 (4)
C100.054 (4)0.055 (4)0.079 (4)−0.003 (4)0.010 (4)0.008 (3)
C110.050 (4)0.055 (4)0.080 (4)−0.010 (3)0.009 (4)0.006 (3)
C120.050 (4)0.057 (4)0.081 (4)−0.011 (3)0.008 (4)0.006 (3)
C130.054 (5)0.043 (4)0.050 (4)0.003 (4)0.000 (4)0.004 (4)
C140.054 (5)0.036 (4)0.045 (4)−0.001 (4)−0.002 (4)0.001 (4)
C150.052 (4)0.043 (4)0.043 (4)0.000 (3)−0.004 (4)0.004 (3)
C160.051 (4)0.039 (3)0.041 (3)0.004 (3)−0.003 (3)0.005 (3)
C170.054 (4)0.045 (4)0.044 (3)0.002 (3)−0.003 (3)0.002 (3)
C180.055 (4)0.045 (4)0.044 (3)0.005 (3)0.000 (3)0.001 (3)
C190.055 (4)0.040 (3)0.042 (3)0.001 (3)−0.006 (3)0.006 (3)
C200.059 (4)0.048 (4)0.047 (4)0.003 (3)−0.003 (4)0.001 (3)
C210.062 (5)0.041 (4)0.051 (4)0.001 (4)−0.008 (4)0.003 (4)
C220.059 (4)0.044 (4)0.056 (4)−0.004 (4)−0.004 (4)0.006 (3)
C230.054 (4)0.040 (3)0.048 (3)0.001 (3)−0.004 (3)0.006 (3)
C240.050 (4)0.036 (3)0.041 (3)0.004 (3)−0.004 (3)0.008 (3)
C250.052 (4)0.041 (4)0.053 (4)0.007 (4)0.012 (4)0.005 (3)
C260.055 (4)0.044 (4)0.052 (4)0.007 (4)0.007 (4)0.007 (4)
C270.048 (4)0.038 (3)0.044 (4)0.002 (3)0.006 (3)0.008 (3)
C280.046 (4)0.036 (3)0.042 (3)0.006 (3)0.007 (3)0.004 (3)
C290.047 (4)0.037 (3)0.037 (3)0.002 (3)0.009 (3)0.007 (3)
C300.044 (4)0.035 (3)0.038 (3)0.004 (3)0.007 (3)0.001 (3)
C310.042 (4)0.032 (3)0.036 (3)0.003 (3)0.005 (3)0.004 (3)
C320.042 (4)0.036 (3)0.037 (3)0.004 (3)0.009 (3)0.000 (3)
C330.045 (4)0.033 (4)0.042 (4)0.004 (4)0.006 (4)0.006 (3)
C340.046 (4)0.033 (3)0.040 (4)−0.001 (3)0.008 (3)0.005 (3)
C350.044 (4)0.030 (3)0.036 (3)0.000 (3)0.005 (3)0.004 (3)
C360.044 (4)0.032 (3)0.040 (3)0.000 (3)0.010 (3)0.001 (3)
C370.052 (4)0.033 (3)0.057 (4)0.000 (3)0.014 (4)0.002 (3)
C380.053 (4)0.037 (3)0.052 (3)0.000 (3)0.006 (4)−0.001 (3)
C390.053 (4)0.030 (3)0.051 (3)0.003 (3)0.015 (3)0.001 (3)
C400.051 (4)0.029 (3)0.055 (3)0.001 (3)0.016 (3)0.000 (3)
C410.054 (4)0.031 (3)0.052 (4)0.003 (3)0.017 (3)−0.002 (3)
C420.052 (4)0.030 (3)0.058 (4)0.003 (3)0.020 (3)0.000 (3)
C430.053 (4)0.029 (3)0.054 (4)0.002 (3)0.015 (3)−0.001 (3)
C440.055 (4)0.031 (3)0.060 (4)0.002 (3)0.014 (4)−0.001 (3)
C450.058 (5)0.034 (4)0.058 (4)0.000 (4)0.009 (4)0.001 (4)
C460.058 (4)0.035 (3)0.057 (4)0.002 (4)0.014 (4)−0.001 (3)
C470.052 (4)0.026 (3)0.052 (3)0.000 (3)0.017 (3)0.000 (3)
C480.052 (4)0.026 (3)0.054 (3)0.004 (3)0.016 (3)0.000 (3)
C490.055 (4)0.064 (4)0.063 (4)0.001 (4)0.002 (4)0.000 (4)
C500.058 (5)0.066 (4)0.063 (4)0.005 (4)−0.001 (4)0.006 (4)
C510.056 (4)0.068 (4)0.069 (4)0.003 (4)−0.002 (4)0.003 (4)
C520.053 (4)0.061 (4)0.066 (4)0.004 (4)0.001 (4)0.000 (4)
C530.053 (4)0.067 (4)0.070 (4)0.002 (4)−0.002 (4)0.001 (4)
C540.052 (4)0.065 (4)0.073 (4)0.001 (4)0.005 (4)−0.001 (4)
C550.048 (4)0.058 (4)0.068 (4)−0.001 (4)0.008 (4)0.001 (4)
C560.051 (4)0.061 (4)0.070 (4)−0.002 (4)0.010 (4)0.005 (4)
C570.052 (5)0.064 (4)0.068 (4)0.000 (4)0.012 (4)0.002 (4)
C580.050 (4)0.060 (4)0.063 (4)0.000 (4)0.009 (4)0.001 (4)
C590.049 (4)0.058 (4)0.065 (4)0.001 (3)0.005 (3)0.001 (3)
C600.050 (4)0.060 (4)0.064 (4)0.003 (3)0.004 (3)0.001 (3)
C610.049 (4)0.048 (4)0.048 (4)0.000 (4)0.002 (4)−0.004 (3)
C620.051 (5)0.048 (4)0.041 (4)−0.007 (4)0.001 (4)−0.011 (4)
C630.049 (4)0.050 (4)0.042 (3)−0.008 (3)−0.005 (3)−0.005 (3)
C640.045 (4)0.044 (4)0.044 (3)−0.003 (3)−0.002 (3)−0.003 (3)
C650.050 (4)0.050 (4)0.045 (3)0.001 (3)−0.009 (3)−0.002 (3)
C660.049 (4)0.049 (4)0.053 (3)0.000 (3)−0.005 (3)−0.005 (3)
C670.048 (4)0.047 (4)0.044 (3)−0.006 (3)−0.004 (3)−0.007 (3)
C680.052 (4)0.050 (4)0.054 (4)0.002 (3)−0.001 (4)−0.009 (3)
C690.052 (5)0.052 (4)0.053 (4)−0.003 (4)−0.002 (4)−0.016 (4)
C700.050 (4)0.054 (4)0.051 (4)−0.003 (4)−0.005 (4)−0.009 (3)
C710.046 (4)0.043 (3)0.040 (3)−0.005 (3)−0.003 (3)−0.006 (3)
C720.044 (4)0.044 (3)0.042 (3)−0.006 (3)0.000 (3)−0.005 (3)
C730.053 (4)0.070 (4)0.076 (4)0.003 (4)0.000 (4)0.016 (4)
C740.055 (5)0.078 (5)0.089 (4)0.007 (4)−0.001 (4)0.017 (4)
C750.055 (4)0.073 (4)0.090 (4)0.002 (4)0.003 (4)0.015 (4)
C760.051 (4)0.069 (4)0.082 (4)0.004 (4)0.001 (4)0.014 (4)
C770.051 (4)0.069 (4)0.084 (4)−0.007 (4)0.004 (4)0.016 (4)
C780.052 (4)0.059 (4)0.081 (4)−0.002 (4)0.009 (4)0.012 (3)
C790.048 (4)0.056 (4)0.074 (4)−0.001 (3)0.010 (4)0.012 (3)
C800.050 (4)0.057 (4)0.077 (4)0.004 (4)0.008 (4)0.017 (4)
C810.050 (5)0.052 (4)0.078 (4)0.008 (4)0.004 (4)0.015 (4)
C820.045 (5)0.054 (4)0.068 (4)0.003 (4)0.006 (4)0.016 (4)
C830.045 (4)0.056 (4)0.072 (4)0.000 (3)0.005 (4)0.013 (3)
C840.047 (4)0.059 (4)0.073 (3)0.000 (3)0.003 (3)0.013 (3)
C850.049 (4)0.054 (4)0.053 (4)−0.003 (3)0.002 (3)0.006 (3)
C860.046 (4)0.052 (4)0.045 (4)−0.003 (4)0.003 (4)0.004 (4)
C870.047 (4)0.050 (4)0.042 (3)0.001 (3)0.005 (3)0.003 (3)
C880.043 (4)0.046 (3)0.036 (3)−0.001 (3)0.007 (3)0.003 (3)
C890.048 (4)0.050 (4)0.043 (3)−0.001 (3)0.007 (3)0.001 (3)
C900.045 (4)0.048 (3)0.044 (3)−0.003 (3)0.008 (3)−0.001 (3)
C910.043 (4)0.045 (3)0.042 (3)−0.001 (3)0.005 (3)0.003 (3)
C920.046 (4)0.048 (4)0.043 (3)−0.002 (3)0.006 (3)0.003 (3)
C930.047 (4)0.044 (3)0.046 (3)0.003 (3)0.002 (3)0.001 (3)
C940.044 (4)0.045 (4)0.044 (4)0.001 (3)0.001 (4)0.004 (3)
C950.044 (4)0.045 (3)0.041 (3)0.001 (3)0.002 (3)0.005 (3)
C960.043 (3)0.045 (3)0.041 (3)0.000 (3)0.002 (3)0.004 (3)
N10.045 (8)0.055 (7)0.031 (5)−0.008 (6)0.010 (5)0.005 (5)
N20.059 (8)0.029 (5)0.041 (6)−0.004 (5)0.017 (6)0.007 (4)
N30.034 (7)0.050 (6)0.024 (4)−0.001 (5)0.009 (4)−0.008 (4)
N40.044 (8)0.031 (5)0.055 (6)0.002 (5)−0.010 (6)−0.006 (4)
N50.037 (7)0.028 (5)0.053 (6)0.011 (4)0.017 (5)−0.001 (4)
N60.055 (8)0.047 (6)0.029 (5)−0.019 (5)−0.008 (5)0.006 (4)
N70.028 (6)0.041 (6)0.035 (5)0.005 (4)0.011 (5)−0.003 (4)
N80.038 (7)0.024 (5)0.044 (5)0.008 (4)−0.007 (5)0.002 (4)
N90.033 (7)0.042 (6)0.071 (7)0.010 (5)0.013 (6)0.016 (5)
N100.039 (7)0.037 (5)0.028 (5)−0.005 (5)0.013 (5)0.006 (4)
N110.035 (7)0.033 (5)0.049 (6)0.003 (4)0.007 (5)0.009 (4)
N120.064 (9)0.034 (6)0.056 (6)0.010 (5)0.021 (6)−0.002 (5)
N130.055 (9)0.066 (8)0.050 (6)0.027 (6)−0.019 (6)0.001 (5)
N140.037 (8)0.050 (7)0.099 (9)−0.005 (5)0.000 (7)0.019 (6)
N150.045 (8)0.053 (7)0.046 (6)0.012 (5)0.003 (6)0.005 (5)
N160.064 (9)0.052 (7)0.043 (6)−0.003 (6)0.005 (6)0.011 (5)
Si10.0176 (15)0.0133 (11)0.0129 (11)−0.0029 (10)0.0014 (11)0.0003 (10)

Geometric parameters (Å, °)

W1—O171.695 (7)C25—H25A0.9300
W1—O221.888 (6)C26—C271.371 (17)
W1—O311.908 (7)C26—H26A0.9300
W1—O301.927 (6)C27—C281.396 (16)
W1—O61.943 (6)C27—H27A0.9300
W1—O362.341 (6)C28—C361.405 (15)
W2—O291.695 (7)C28—C291.409 (17)
W2—O81.880 (7)C29—C301.373 (15)
W2—O321.917 (7)C29—H29A0.9300
W2—O21.920 (6)C30—C311.445 (14)
W2—O271.943 (6)C30—H30A0.9300
W2—O332.349 (6)C31—C351.367 (16)
W3—O111.706 (7)C31—C321.394 (15)
W3—O371.885 (7)C32—C331.368 (14)
W3—O161.903 (7)C32—H14A0.9300
W3—O41.928 (6)C33—C341.343 (16)
W3—O181.937 (7)C33—H16A0.9300
W3—O382.349 (6)C34—N101.342 (14)
W4—O201.690 (7)C34—H34A0.9300
W4—O61.882 (6)C35—N101.378 (12)
W4—O141.897 (6)C35—C361.413 (15)
W4—O121.913 (7)C36—N121.365 (15)
W4—O261.946 (6)C37—N21.327 (16)
W4—O232.339 (6)C37—C381.399 (16)
W5—O281.697 (7)C37—H37A0.9300
W5—O41.872 (6)C38—C391.350 (17)
W5—O271.905 (6)C38—H38A0.9300
W5—O251.932 (7)C39—C401.398 (18)
W5—O11.933 (7)C39—H39A0.9300
W5—O332.338 (6)C40—C481.408 (16)
W6—O191.690 (6)C40—C411.421 (18)
W6—O251.865 (7)C41—C421.324 (17)
W6—O131.893 (7)C41—H41A0.9300
W6—O161.921 (7)C42—C431.413 (15)
W6—O221.938 (6)C42—H42A0.9300
W6—O362.366 (6)C43—C441.382 (17)
W7—O151.695 (7)C43—C471.390 (18)
W7—O401.875 (7)C44—C451.365 (15)
W7—O261.895 (7)C44—H44A0.9300
W7—O81.918 (7)C45—C461.345 (19)
W7—O341.948 (7)C45—H45A0.9300
W7—O232.339 (6)C46—N151.313 (16)
W8—O391.698 (7)C46—H46A0.9300
W8—O211.882 (7)C47—N151.347 (13)
W8—O31.898 (6)C47—C481.441 (18)
W8—O341.911 (7)C48—N21.366 (16)
W8—O141.943 (7)C49—N161.337 (14)
W8—O232.350 (6)C49—C501.437 (19)
W9—O241.687 (7)C49—H49A0.9300
W9—O181.901 (7)C50—C511.34 (2)
W9—O21.908 (6)C50—H50A0.9300
W9—O91.932 (6)C51—C521.380 (18)
W9—O401.939 (7)C51—H51A0.9300
W9—O382.356 (6)C52—C531.43 (2)
W10—O351.691 (7)C52—C601.46 (2)
W10—O301.908 (7)C53—C541.284 (16)
W10—O31.921 (6)C53—H53A0.9300
W10—O131.919 (7)C54—C551.433 (19)
W10—O71.929 (7)C54—H54A0.9300
W10—O362.339 (6)C55—C561.369 (16)
W11—O101.681 (6)C55—C591.43 (2)
W11—O121.888 (6)C56—C571.349 (19)
W11—O311.904 (7)C56—H56A0.9300
W11—O91.913 (6)C57—C581.398 (19)
W11—O371.949 (7)C57—H57A0.9300
W11—O382.358 (6)C58—N11.334 (14)
W12—O51.687 (6)C58—H58A0.9300
W12—O71.890 (7)C59—N11.384 (17)
W12—O11.919 (7)C59—C601.420 (17)
W12—O321.924 (7)C60—N161.353 (18)
W12—O211.933 (7)C61—N71.330 (13)
W12—O332.351 (6)C61—C621.368 (17)
O23—Si11.634 (7)C61—H1A0.9300
O33—Si11.623 (6)C62—C631.363 (17)
O36—Si11.621 (7)C62—H62A0.9300
O38—Si11.605 (7)C63—C641.377 (15)
Cu1—N51.990 (10)C63—H63A0.9300
Cu1—N142.011 (12)C64—C651.432 (17)
Cu1—N92.023 (9)C64—C721.431 (16)
Cu1—N42.062 (10)C65—C661.344 (15)
Cu2—N102.030 (10)C65—H65A0.9300
Cu2—N22.037 (9)C66—C671.450 (17)
Cu2—N122.050 (10)C66—H66A0.9300
Cu2—N152.080 (12)C67—C711.383 (18)
Cu3—N162.018 (11)C67—C681.415 (15)
Cu3—N72.019 (10)C68—C691.351 (17)
Cu3—N12.081 (10)C68—H68A0.9300
Cu3—N32.074 (10)C69—C701.391 (18)
Cu4—N111.988 (8)C69—H69A0.9300
Cu4—N81.982 (10)C70—N31.319 (13)
Cu4—N62.082 (8)C70—H70A0.9300
Cu4—N132.097 (12)C71—N31.350 (14)
C1—N141.347 (17)C71—C721.437 (14)
C1—C21.43 (2)C72—N71.364 (15)
C1—H1B0.9300C73—N131.324 (17)
C2—C31.267 (17)C73—C741.40 (2)
C2—H2A0.9300C73—H73A0.9300
C3—C41.396 (19)C74—C751.374 (18)
C3—H3A0.9300C74—H74A0.9300
C4—C51.360 (17)C75—C761.356 (19)
C4—C121.41 (2)C75—H75A0.9300
C5—C61.326 (18)C76—C771.361 (17)
C5—H5A0.9300C76—C841.408 (14)
C6—C71.430 (19)C77—C781.278 (18)
C6—H6A0.9300C77—H77A0.9300
C7—C111.405 (17)C78—C791.372 (19)
C7—C81.389 (19)C78—H78A0.9300
C9—C81.36 (2)C79—C801.378 (18)
C9—C101.411 (16)C79—C831.459 (17)
C9—H9A0.9300C80—C811.324 (18)
C8—H8A0.9300C80—H80A0.9300
C10—N91.356 (16)C81—C821.349 (15)
C10—H10A0.9300C81—H81A0.9300
C11—N91.360 (17)C82—N111.342 (15)
C11—C121.43 (2)C82—H82A0.9300
C12—N141.349 (15)C83—N111.373 (16)
C13—N51.321 (14)C83—C841.428 (18)
C13—C141.408 (17)C84—N131.329 (15)
C13—H13A0.9300C85—N61.324 (15)
C14—C151.349 (17)C85—C861.396 (14)
C14—H14B0.9300C85—H85A0.9300
C15—C161.422 (15)C86—C871.348 (16)
C15—H15B0.9300C86—H86A0.9300
C16—C241.399 (17)C87—C881.411 (17)
C16—C171.415 (17)C87—H15A0.9300
C17—C181.384 (15)C88—C961.425 (14)
C17—H17A0.9300C88—C891.409 (16)
C18—C191.423 (18)C89—C901.320 (17)
C18—H18A0.9300C89—H18B0.9300
C19—C231.364 (17)C90—C911.468 (15)
C19—C201.376 (16)C90—H90A0.9300
C20—C211.372 (18)C91—C921.382 (17)
C20—H20A0.9300C91—C951.396 (17)
C21—C221.397 (17)C92—C931.364 (15)
C21—H21A0.9300C92—H92A0.9300
C22—N41.312 (13)C93—C941.393 (16)
C22—H22A0.9300C93—H93A0.9300
C23—N41.354 (16)C94—N81.303 (14)
C23—C241.441 (16)C94—H94A0.9300
C24—N51.356 (14)C95—N81.371 (13)
C25—N121.345 (15)C95—C961.416 (17)
C25—C261.364 (15)C96—N61.338 (14)
O17—W1—O22100.9 (3)C24—C16—C17121.0 (12)
O17—W1—O31101.7 (3)C24—C16—C15116.6 (12)
O22—W1—O3190.8 (3)C17—C16—C15122.4 (13)
O17—W1—O30100.0 (3)C18—C17—C16118.3 (13)
O22—W1—O3088.7 (3)C18—C17—H17A120.9
O31—W1—O30157.9 (3)C16—C17—H17A120.9
O17—W1—O6101.4 (3)C17—C18—C19122.1 (13)
O22—W1—O6157.7 (3)C17—C18—H18A118.9
O31—W1—O685.0 (3)C19—C18—H18A118.9
O30—W1—O687.2 (3)C23—C19—C20119.3 (13)
O17—W1—O36171.5 (3)C23—C19—C18119.1 (12)
O22—W1—O3673.5 (2)C20—C19—C18121.4 (13)
O31—W1—O3684.9 (2)C21—C20—C19117.8 (13)
O30—W1—O3673.8 (3)C21—C20—H20A121.1
O6—W1—O3684.3 (2)C19—C20—H20A121.1
O29—W2—O8102.5 (3)C20—C21—C22119.9 (13)
O29—W2—O3298.6 (3)C20—C21—H21A120.1
O8—W2—O3292.0 (3)C22—C21—H21A120.1
O29—W2—O2103.1 (3)N4—C22—C21122.2 (13)
O8—W2—O284.8 (3)N4—C22—H22A118.9
O32—W2—O2158.2 (3)C21—C22—H22A118.9
O29—W2—O2799.9 (3)N4—C23—C19123.2 (12)
O8—W2—O27157.4 (3)N4—C23—C24116.1 (12)
O32—W2—O2787.5 (3)C19—C23—C24120.7 (13)
O2—W2—O2787.3 (3)N5—C24—C16123.4 (11)
O29—W2—O33169.7 (3)N5—C24—C23117.8 (12)
O8—W2—O3385.2 (2)C16—C24—C23118.8 (12)
O32—W2—O3374.0 (2)N12—C25—C26123.0 (13)
O2—W2—O3384.3 (2)N12—C25—H25A118.5
O27—W2—O3373.0 (2)C26—C25—H25A118.5
O11—W3—O37101.0 (3)C25—C26—C27120.8 (13)
O11—W3—O16101.6 (3)C25—C26—H26A119.6
O37—W3—O1692.9 (3)C27—C26—H26A119.6
O11—W3—O4102.3 (3)C26—C27—C28118.7 (11)
O37—W3—O4156.6 (3)C26—C27—H27A120.7
O16—W3—O485.0 (3)C28—C27—H27A120.7
O11—W3—O1899.5 (3)C27—C28—C36117.4 (12)
O37—W3—O1887.4 (3)C27—C28—C29122.4 (11)
O16—W3—O18158.4 (3)C36—C28—C29120.2 (11)
O4—W3—O1886.2 (3)C30—C29—C28120.2 (11)
O11—W3—O38171.7 (3)C30—C29—H29A119.9
O37—W3—O3874.3 (2)C28—C29—H29A119.9
O16—W3—O3885.7 (2)C29—C30—C31120.1 (12)
O4—W3—O3882.3 (2)C29—C30—H30A119.9
O18—W3—O3873.6 (3)C31—C30—H30A119.9
O20—W4—O6101.8 (3)C35—C31—C32119.1 (10)
O20—W4—O14100.2 (3)C35—C31—C30119.0 (11)
O6—W4—O1492.3 (3)C32—C31—C30121.9 (11)
O20—W4—O12102.3 (3)C33—C32—C31118.6 (11)
O6—W4—O1285.6 (3)C33—C32—H14A120.7
O14—W4—O12157.4 (3)C31—C32—H14A120.7
O20—W4—O26100.0 (3)C34—C33—C32119.6 (11)
O6—W4—O26158.0 (3)C34—C33—H16A120.2
O14—W4—O2686.3 (3)C32—C33—H16A120.2
O12—W4—O2687.4 (3)N10—C34—C33124.4 (10)
O20—W4—O23170.6 (3)N10—C34—H34A117.8
O6—W4—O2386.0 (3)C33—C34—H34A117.8
O14—W4—O2374.0 (3)N10—C35—C31122.1 (11)
O12—W4—O2383.4 (3)N10—C35—C36116.4 (11)
O26—W4—O2372.5 (2)C31—C35—C36121.5 (10)
O28—W5—O4103.3 (3)N12—C36—C28123.4 (11)
O28—W5—O27100.5 (3)N12—C36—C35117.8 (10)
O4—W5—O2790.9 (3)C28—C36—C35118.8 (11)
O28—W5—O25101.6 (3)N2—C37—C38125.6 (14)
O4—W5—O2586.1 (3)N2—C37—H37A117.2
O27—W5—O25157.8 (3)C38—C37—H37A117.2
O28—W5—O199.2 (3)C39—C38—C37117.6 (14)
O4—W5—O1157.3 (3)C39—C38—H38A121.2
O27—W5—O187.3 (3)C37—C38—H38A121.2
O25—W5—O187.1 (3)C38—C39—C40120.5 (12)
O28—W5—O33170.7 (3)C38—C39—H39A119.8
O4—W5—O3384.3 (2)C40—C39—H39A119.8
O27—W5—O3373.8 (3)C39—C40—C48117.5 (13)
O25—W5—O3383.9 (2)C39—C40—C41123.2 (12)
O1—W5—O3373.5 (2)C48—C40—C41119.3 (13)
O19—W6—O25103.8 (3)C42—C41—C40119.8 (12)
O19—W6—O13102.1 (3)C42—C41—H41A120.1
O25—W6—O1391.7 (3)C40—C41—H41A120.1
O19—W6—O16101.0 (3)C41—C42—C43123.3 (14)
O25—W6—O1684.7 (3)C41—C42—H42A118.3
O13—W6—O16156.9 (3)C43—C42—H42A118.3
O19—W6—O2299.7 (3)C44—C43—C47116.5 (12)
O25—W6—O22156.2 (3)C44—C43—C42124.6 (14)
O13—W6—O2287.4 (3)C47—C43—C42118.8 (13)
O16—W6—O2287.0 (3)C43—C44—C45120.2 (14)
O19—W6—O36170.4 (3)C43—C44—H44A119.9
O25—W6—O3684.9 (2)C45—C44—H44A119.9
O13—W6—O3673.0 (2)C46—C45—C44118.8 (14)
O16—W6—O3683.9 (2)C46—C45—H45A120.6
O22—W6—O3672.1 (2)C44—C45—H45A120.6
O15—W7—O40102.6 (3)N15—C46—C45123.9 (13)
O15—W7—O26100.9 (3)N15—C46—H46A118.1
O40—W7—O2691.8 (3)C45—C46—H46A118.1
O15—W7—O8101.6 (3)N15—C47—C43122.7 (13)
O40—W7—O885.4 (3)N15—C47—C48118.2 (12)
O26—W7—O8157.5 (3)C43—C47—C48119.0 (12)
O15—W7—O3498.9 (3)N2—C48—C40123.1 (13)
O40—W7—O34158.3 (2)N2—C48—C47117.4 (11)
O26—W7—O3486.9 (3)C40—C48—C47119.5 (13)
O8—W7—O3487.6 (3)N16—C49—C50121.3 (15)
O15—W7—O23170.4 (3)N16—C49—H49A119.3
O40—W7—O2385.5 (2)C50—C49—H49A119.3
O26—W7—O2373.3 (2)C51—C50—C49120.6 (14)
O8—W7—O2384.1 (2)C51—C50—H50A119.7
O34—W7—O2373.4 (2)C49—C50—H50A119.7
O39—W8—O21102.0 (3)C50—C51—C52121.2 (15)
O39—W8—O3102.7 (3)C50—C51—H51A119.4
O21—W8—O386.3 (3)C52—C51—H51A119.4
O39—W8—O3499.1 (3)C51—C52—C53126.9 (15)
O21—W8—O3491.2 (3)C51—C52—C60115.2 (15)
O3—W8—O34158.2 (3)C53—C52—C60117.8 (13)
O39—W8—O1499.4 (3)C54—C53—C52121.4 (16)
O21—W8—O14158.6 (3)C54—C53—H53A119.3
O3—W8—O1487.6 (3)C52—C53—H53A119.3
O34—W8—O1487.0 (3)C53—C54—C55125.7 (16)
O39—W8—O23169.5 (3)C53—C54—H54A117.1
O21—W8—O2386.0 (2)C55—C54—H54A117.1
O3—W8—O2384.5 (2)C56—C55—C59116.4 (15)
O34—W8—O2373.7 (2)C56—C55—C54128.7 (15)
O14—W8—O2372.9 (2)C59—C55—C54114.9 (13)
O24—W9—O1899.6 (3)C57—C56—C55124.7 (15)
O24—W9—O2101.9 (3)C57—C56—H56A117.6
O18—W9—O291.3 (3)C55—C56—H56A117.6
O24—W9—O999.8 (3)C56—C57—C58114.7 (14)
O18—W9—O988.1 (3)C56—C57—H57A122.7
O2—W9—O9158.1 (3)C58—C57—H57A122.7
O24—W9—O40102.7 (3)N1—C58—C57126.8 (14)
O18—W9—O40157.7 (3)N1—C58—H58A116.6
O2—W9—O4085.3 (3)C57—C58—H58A116.6
O9—W9—O4087.1 (3)N1—C59—C55121.6 (12)
O24—W9—O38170.8 (3)N1—C59—C60116.3 (13)
O18—W9—O3874.1 (3)C55—C59—C60122.2 (14)
O2—W9—O3885.1 (2)N16—C60—C59117.7 (14)
O9—W9—O3873.7 (2)N16—C60—C52124.4 (13)
O40—W9—O3883.7 (2)C59—C60—C52117.9 (15)
O35—W10—O30100.7 (3)N7—C61—C62125.5 (13)
O35—W10—O3102.2 (3)N7—C61—H1A117.2
O30—W10—O390.8 (3)C62—C61—H1A117.2
O35—W10—O1399.5 (3)C61—C62—C63117.8 (12)
O30—W10—O1388.0 (3)C61—C62—H62A121.1
O3—W10—O13158.1 (3)C63—C62—H62A121.1
O35—W10—O7101.2 (3)C62—C63—C64121.3 (12)
O30—W10—O7158.1 (3)C62—C63—H63A119.4
O3—W10—O785.8 (3)C64—C63—H63A119.4
O13—W10—O787.1 (3)C63—C64—C65126.8 (12)
O35—W10—O36171.0 (3)C63—C64—C72116.8 (12)
O30—W10—O3674.2 (3)C65—C64—C72116.4 (11)
O3—W10—O3685.4 (2)C66—C65—C64123.5 (12)
O13—W10—O3673.2 (2)C66—C65—H65A118.2
O7—W10—O3684.0 (2)C64—C65—H65A118.2
O10—W11—O12102.0 (3)C65—C66—C67119.6 (13)
O10—W11—O31100.7 (3)C65—C66—H66A120.2
O12—W11—O3186.1 (3)C67—C66—H66A120.2
O10—W11—O9100.9 (3)C71—C67—C68117.6 (12)
O12—W11—O991.5 (3)C71—C67—C66120.0 (11)
O31—W11—O9158.2 (3)C68—C67—C66122.4 (13)
O10—W11—O37100.0 (3)C69—C68—C67117.8 (13)
O12—W11—O37158.0 (3)C69—C68—H68A121.1
O31—W11—O3787.8 (3)C67—C68—H68A121.1
O9—W11—O3786.3 (3)C68—C69—C70121.2 (12)
O10—W11—O38171.3 (3)C68—C69—H69A119.4
O12—W11—O3885.3 (2)C70—C69—H69A119.4
O31—W11—O3884.2 (2)N3—C70—C69121.8 (12)
O9—W11—O3874.0 (2)N3—C70—H70A119.1
O37—W11—O3873.0 (2)C69—C70—H70A119.1
O5—W12—O7103.0 (3)N3—C71—C67123.4 (10)
O5—W12—O199.8 (3)N3—C71—C72117.0 (12)
O7—W12—O190.5 (3)C67—C71—C72119.5 (12)
O5—W12—O3298.8 (3)N7—C72—C71116.9 (11)
O7—W12—O32158.2 (3)N7—C72—C64122.2 (10)
O1—W12—O3288.1 (3)C71—C72—C64120.8 (12)
O5—W12—O21102.4 (3)N13—C73—C74120.1 (14)
O7—W12—O2185.6 (3)N13—C73—H73A120.0
O1—W12—O21157.8 (3)C74—C73—H73A120.0
O32—W12—O2187.5 (3)C73—C74—C75118.4 (15)
O5—W12—O33169.9 (3)C73—C74—H74A120.8
O7—W12—O3384.9 (2)C75—C74—H74A120.8
O1—W12—O3373.4 (2)C76—C75—C74124.4 (16)
O32—W12—O3373.8 (2)C76—C75—H75A117.8
O21—W12—O3384.4 (2)C74—C75—H75A117.8
W12—O1—W5121.5 (3)C75—C76—C77127.4 (15)
W9—O2—W2151.3 (4)C75—C76—C84111.6 (14)
W8—O3—W10150.8 (4)C77—C76—C84121.0 (14)
W5—O4—W3152.0 (4)C78—C77—C76123.3 (16)
W4—O6—W1151.5 (4)C78—C77—H77A118.3
W12—O7—W10151.6 (3)C76—C77—H77A118.3
W2—O8—W7153.0 (3)C77—C78—C79122.3 (15)
W11—O9—W9121.5 (3)C77—C78—H78A118.8
W11—O12—W4151.7 (3)C79—C78—H78A118.8
W6—O13—W10123.0 (3)C80—C79—C78127.2 (14)
W4—O14—W8121.7 (4)C80—C79—C83114.8 (14)
W3—O16—W6152.3 (3)C78—C79—C83117.7 (13)
W9—O18—W3121.5 (4)C81—C80—C79122.3 (13)
W8—O21—W12151.3 (3)C81—C80—H80A118.9
W1—O22—W6123.1 (3)C79—C80—H80A118.9
Si1—O23—W7124.2 (4)C80—C81—C82120.7 (14)
Si1—O23—W4124.6 (3)C80—C81—H81A119.7
W7—O23—W491.9 (2)C82—C81—H81A119.7
Si1—O23—W8123.5 (3)N11—C82—C81123.3 (14)
W7—O23—W891.6 (2)N11—C82—H82A118.4
W4—O23—W891.3 (2)C81—C82—H82A118.4
W6—O25—W5152.5 (3)N11—C83—C84119.2 (12)
W7—O26—W4122.2 (3)N11—C83—C79121.7 (12)
W5—O27—W2121.6 (3)C84—C83—C79119.0 (14)
W10—O30—W1121.0 (4)N13—C84—C76127.2 (14)
W1—O31—W11151.5 (3)N13—C84—C83116.6 (13)
W2—O32—W12121.3 (3)C76—C84—C83116.2 (13)
Si1—O33—W5124.4 (3)N6—C85—C86123.1 (12)
Si1—O33—W2124.4 (3)N6—C85—H85A118.4
W5—O33—W291.6 (2)C86—C85—H85A118.4
Si1—O33—W12124.1 (4)C87—C86—C85117.8 (13)
W5—O33—W1291.6 (2)C87—C86—H86A121.1
W2—O33—W1290.9 (2)C85—C86—H86A121.1
W8—O34—W7121.3 (3)C86—C87—C88121.9 (11)
Si1—O36—W1125.0 (3)C86—C87—H15A119.0
Si1—O36—W10124.3 (3)C88—C87—H15A119.0
W1—O36—W1091.0 (2)C87—C88—C96115.5 (11)
Si1—O36—W6124.3 (4)C87—C88—C89126.1 (11)
W1—O36—W691.2 (2)C96—C88—C89118.3 (12)
W10—O36—W690.8 (2)C90—C89—C88122.8 (12)
W3—O37—W11121.9 (3)C90—C89—H18B118.6
Si1—O38—W3125.1 (3)C88—C89—H18B118.6
Si1—O38—W9125.2 (3)C89—C90—C91120.8 (12)
W3—O38—W990.7 (2)C89—C90—H90A119.6
Si1—O38—W11123.8 (4)C91—C90—H90A119.6
W3—O38—W1190.82 (19)C92—C91—C95118.8 (11)
W9—O38—W1190.7 (2)C92—C91—C90124.2 (12)
W7—O40—W9151.4 (3)C95—C91—C90116.9 (12)
N5—Cu1—N14132.5 (4)C93—C92—C91118.1 (12)
N5—Cu1—N9124.0 (4)C93—C92—H92A120.9
N14—Cu1—N981.9 (4)C91—C92—H92A120.9
N5—Cu1—N482.4 (4)C92—C93—C94120.5 (13)
N14—Cu1—N4131.7 (5)C92—C93—H93A119.7
N9—Cu1—N4106.9 (4)C94—C93—H93A119.7
N10—Cu2—N2120.1 (4)N8—C94—C93122.4 (11)
N10—Cu2—N1281.5 (4)N8—C94—H94A118.8
N2—Cu2—N12137.6 (4)C93—C94—H94A118.8
N10—Cu2—N15139.5 (4)N8—C95—C91121.7 (11)
N2—Cu2—N1582.2 (4)N8—C95—C96116.8 (11)
N12—Cu2—N15105.1 (4)C91—C95—C96121.5 (11)
N16—Cu3—N7149.3 (4)N6—C96—C88122.2 (11)
N16—Cu3—N181.0 (4)N6—C96—C95118.9 (10)
N7—Cu3—N1107.3 (4)C88—C96—C95119.0 (11)
N16—Cu3—N3116.4 (4)C58—N1—C59115.9 (12)
N7—Cu3—N381.4 (4)C58—N1—Cu3132.9 (10)
N1—Cu3—N3130.2 (4)C59—N1—Cu3111.2 (8)
N11—Cu4—N8130.4 (4)C37—N2—C48115.6 (11)
N11—Cu4—N6125.1 (4)C37—N2—Cu2132.9 (10)
N8—Cu4—N682.6 (4)C48—N2—Cu2111.3 (9)
N11—Cu4—N1382.5 (4)C70—N3—C71118.0 (11)
N8—Cu4—N13138.2 (4)C70—N3—Cu3130.9 (9)
N6—Cu4—N1399.2 (4)C71—N3—Cu3111.1 (7)
N14—C1—C2117.0 (14)C22—N4—C23117.6 (12)
N14—C1—H1B121.5C22—N4—Cu1131.2 (9)
C2—C1—H1B121.5C23—N4—Cu1111.0 (8)
C3—C2—C1123.1 (16)C13—N5—C24117.0 (11)
C3—C2—H2A118.4C13—N5—Cu1130.5 (9)
C1—C2—H2A118.4C24—N5—Cu1112.3 (8)
C2—C3—C4122.5 (17)C85—N6—C96119.3 (10)
C2—C3—H3A118.8C85—N6—Cu4130.7 (9)
C4—C3—H3A118.8C96—N6—Cu4109.0 (8)
C5—C4—C12120.3 (15)C61—N7—C72116.3 (11)
C5—C4—C3126.1 (16)C61—N7—Cu3130.8 (9)
C12—C4—C3113.7 (14)C72—N7—Cu3112.2 (7)
C4—C5—C6123.7 (16)C94—N8—C95118.3 (11)
C4—C5—H5A118.2C94—N8—Cu4129.3 (8)
C6—C5—H5A118.2C95—N8—Cu4112.2 (8)
C5—C6—C7119.2 (14)C11—N9—C10116.1 (12)
C5—C6—H6A120.4C11—N9—Cu1112.0 (9)
C7—C6—H6A120.4C10—N9—Cu1131.8 (10)
C11—C7—C8115.8 (15)C34—N10—C35116.2 (10)
C11—C7—C6119.1 (14)C34—N10—Cu2131.2 (7)
C8—C7—C6125.0 (14)C35—N10—Cu2112.6 (8)
C8—C9—C10116.3 (15)C82—N11—C83117.0 (11)
C8—C9—H9A121.9C82—N11—Cu4132.1 (9)
C10—C9—H9A121.9C83—N11—Cu4110.9 (8)
C9—C8—C7123.3 (14)C25—N12—C36116.7 (10)
C9—C8—H8A118.3C25—N12—Cu2131.3 (9)
C7—C8—H8A118.3C36—N12—Cu2111.7 (8)
N9—C10—C9124.3 (14)C73—N13—C84118.3 (14)
N9—C10—H10A117.9C73—N13—Cu4130.5 (11)
C9—C10—H10A117.9C84—N13—Cu4110.4 (9)
N9—C11—C7124.2 (14)C1—N14—C12118.7 (14)
N9—C11—C12116.2 (12)C1—N14—Cu1128.8 (10)
C7—C11—C12119.6 (15)C12—N14—Cu1112.5 (10)
N14—C12—C4125.0 (15)C46—N15—C47117.7 (13)
N14—C12—C11117.0 (14)C46—N15—Cu2131.6 (9)
C4—C12—C11118.0 (13)C47—N15—Cu2110.3 (9)
N5—C13—C14124.9 (13)C49—N16—C60117.2 (13)
N5—C13—H13A117.6C49—N16—Cu3128.8 (11)
C14—C13—H13A117.6C60—N16—Cu3113.7 (9)
C15—C14—C13117.4 (12)O38—Si1—O33108.8 (4)
C15—C14—H14B121.3O38—Si1—O36109.5 (3)
C13—C14—H14B121.3O33—Si1—O36109.7 (3)
C14—C15—C16120.8 (13)O38—Si1—O23109.2 (3)
C14—C15—H15B119.6O33—Si1—O23110.0 (3)
C16—C15—H15B119.6O36—Si1—O23109.5 (4)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C10—H10A···O170.932.643.503 (17)154
C41—H41A···O260.932.743.131 (13)106
C25—H25A···O100.932.433.329 (16)162
C50—H50A···O350.932.623.477 (16)153
C69—H69A···O340.932.593.322 (14)136
C49—H49A···O50.932.363.276 (18)169
C92—H92A···O150.933.043.491 (16)111
C94—H94A···O240.932.623.326 (14)134

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2165).

References

  • Brown, I. D. (2002). The Chemical Bond in Inorganic Chemistry: The Bond Valence Model Oxford University Press.
  • Bruker (2001). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Kurth, D. G., Volkmer, D., Pope, M. T. & Müller, A. (2001). Editors. Polyoxometalate Chemistry, p. 301. Dordrecht: Kluwer.
  • Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst.39, 453–457.
  • Rocchiccioli-Deltcheff, C., Fournier, M., Franck, R. & Thouvenot, R. (1983). Inorg. Chem.22, 207–216.
  • Sheldrick, G. M. (1997). SHELXS97 and SHELXL97 University of Göttingen, Germany.

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