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The title compound, [Zr2(C18H15OSi)6(OH)2(H2O)2]·C7H8, is a dimeric ZrIV compound. The asymmetric unit consists of two half-molecules of the complex and a toluene solvent mol­ecule. The zirconium centres are bridged by two μ-hydroxo ligands. Each Zr is octa­hedrally coordinated by the hydroxo groups, three triphenyl­silanolato groups and an additional water ligand. The centres of both Zr2O2 rings are located on crystallographic centres of inversion. The two independent monomeric units differ significantly with respect to the Zr—O—Si bond angles which is most probably due to the high steric demands of three triphenyl­silanolato ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806004156/bt6813sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806004156/bt6813Isup2.hkl
Contains datablock I

CCDC reference: 601126

Key indicators

  • Single-crystal X-ray study
  • T = 183 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.039
  • wR factor = 0.106
  • Data-to-parameter ratio = 10.7

checkCIF/PLATON results

No syntax errors found



Datablock: tt586


Alert level A THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4941
Author Response: The title compound is a minor product from a reaction and crystals were obtained after a complicated procedure lasting several days. All operations had to be performed under strict inert conditions in anhydrous solvents, since it had to be sure that the only water source was the amount of water added deliberately (cf. _publ_section_exptl_prep). The reaction as well as the crystallisation were done several times and only once crystalline material was obtained. The crystal was the best out of this badge, although it was very small and did nor diffract very well. The data set was recorded some years ago on a CAD4 diffractometer, so for the sake of time in combination with a weakly diffracting crystal, the theta(max) value is quite small leading to this problem as well as to several other level A, B and C alerts. Nevertheless, there are more than 9000 observed reflections and the important parts of the structure, i.e. the coordination spheres of the zirconium atoms, show a good resolution. The phenyl substituents as well as the solvent molecule are not improtant for the point that we would like to state with this strucure.
PLAT023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6].....      20.56 Deg.
Author Response: vide infra
PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............      20.56 Deg.
Author Response: vide infra
PLAT241_ALERT_2_A Check High      Ueq as Compared to Neighbors for       C101
Author Response: vide infra

Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.39 Ratio
Author Response: Several of the phenyl substituents of the triphenylsilanolate ligands might be more appropriatley resolved as disordered due to a rotation around the carbon silicon bond. Nevertheless, this would even have worsened the data parameter ratio, so we decided to refine only one conformation. This is also the reason for a number of additional A, B and C level alerts.
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for        C71
Author Response: vide infra
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for        C81
Author Response: vide infra
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for        C67
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for        C97
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for       C100
PLAT420_ALERT_2_B D-H Without Acceptor       O4     -   H4O    ...          ?
Author Response: The \m-hydroxo as well as the water ligands are situated in a hydrophobic cavity built up by the big number of phenyl groups of the triphenylsilanolato ligands.
PLAT420_ALERT_2_B D-H Without Acceptor       O5     -   H5A    ...          ?
Author Response: The \m-hydroxo as well as the water ligands are situated in a hydrophobic cavity built up by the big number of phenyl groups of the triphenylsilanolato ligands.
PLAT420_ALERT_2_B D-H Without Acceptor       O9     -   H9O    ...          ?
Author Response: The \m-hydroxo as well as the water ligands are situated in a hydrophobic cavity built up by the big number of phenyl groups of the triphenylsilanolato ligands.
PLAT420_ALERT_2_B D-H Without Acceptor       O10    -   H10B   ...          ?
Author Response: The \m-hydroxo as well as the water ligands are situated in a hydrophobic cavity built up by the big number of phenyl groups of the triphenylsilanolato ligands.

Alert level C PLAT213_ALERT_2_C Atom C101 has ADP max/min Ratio ............. 3.30 prolat PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.08 Ratio
Author Response: Several of the phenyl substituents of the triphenylsilanolate ligands might be more appropriatley resolved as disordered due to a rotation around the carbon silicon bond. Nevertheless, this would even have worsened the data parameter ratio, so we decided to refine only one conformation. This is also the reason for a number of additional A, B and C level alerts.
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.66 Ratio
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zr2    -   O9      ..       9.52 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C57
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C65
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C69
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C72
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C94
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C95
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for       C102
Author Response: vide infra
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for       C107
Author Response: vide infra
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Zr1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Zr2
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C70
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C79
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       C113
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C109
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         13

4 ALERT level A = In general: serious problem 10 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 26 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: SET4 (de Boer & Duisenberg, 1984); data reduction: MolEN (Nonius, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: SHELXL97.

Di-µ-hydroxo-κ4O:O-bis[aquatris(triphenylsilanolato-κO)zirconium(IV)] toluene solvate top
Crystal data top
[Zr2(C18H15OSi)6(OH)2(H2O)2]·C7H8Z = 2
Mr = 1996.96F(000) = 2076
Triclinic, P1Dx = 1.283 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.693 (4) ÅCell parameters from 25 reflections
b = 16.324 (3) Åθ = 8.3–14.5°
c = 24.794 (4) ŵ = 0.33 mm1
α = 90.08 (1)°T = 183 K
β = 105.32 (2)°Cuboid, colorless
γ = 114.70 (2)°0.05 × 0.04 × 0.04 mm
V = 5168 (2) Å3
Data collection top
Enraf–Nonius CAD-4
diffractometer
9107 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.016
Graphite monochromatorθmax = 20.6°, θmin = 2.5°
ω/2θ scansh = 1414
Absorption correction: ψ scan
(North et al., 1968)
k = 1616
Tmin = 0.925, Tmax = 0.988l = 240
10711 measured reflections3 standard reflections every 600 min
10400 independent reflections intensity decay: 0.9%
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) = 0.106H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.051P)2 + 9.3505P]
where P = (Fo2 + 2Fc2)/3
10400 reflections(Δ/σ)max < 0.001
971 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.36 e Å3
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*/Ueq
Zr10.45605 (3)0.89723 (2)0.455713 (15)0.02346 (13)
O10.3123 (2)0.88082 (18)0.41853 (12)0.0392 (7)
Si10.18904 (9)0.84723 (8)0.38681 (5)0.0332 (3)
C10.1211 (2)0.8576 (2)0.43948 (11)0.0393 (11)
C20.1309 (2)0.94264 (17)0.45671 (13)0.0493 (12)
H20.16620.99380.43960.059*
C30.0889 (3)0.9528 (2)0.49898 (14)0.0664 (16)
H30.09561.01100.51080.080*
C40.0373 (3)0.8779 (3)0.52401 (12)0.0781 (19)
H40.00860.88490.55290.094*
C50.0275 (2)0.7928 (3)0.50677 (13)0.0734 (17)
H50.00780.74170.52390.088*
C60.0694 (2)0.78265 (18)0.46451 (14)0.0536 (13)
H60.06280.72450.45270.064*
C70.1266 (2)0.72672 (16)0.35179 (12)0.0392 (11)
C80.0183 (2)0.6793 (2)0.33117 (15)0.0602 (14)
H80.02510.70540.33800.072*
C90.0265 (2)0.5935 (2)0.30055 (15)0.0754 (17)
H90.10050.56110.28650.091*
C100.0370 (3)0.55521 (17)0.29054 (15)0.0755 (17)
H100.00640.49660.26960.091*
C110.1453 (3)0.6027 (2)0.31116 (16)0.0797 (18)
H110.18870.57650.30430.096*
C120.19007 (18)0.6884 (2)0.34178 (15)0.0602 (14)
H120.26410.72090.35590.072*
C130.1756 (2)0.92305 (19)0.33128 (11)0.0362 (10)
C140.07764 (18)0.9191 (2)0.30465 (14)0.0601 (14)
H140.01880.88190.31670.072*
C150.0658 (2)0.9696 (3)0.26045 (14)0.0778 (18)
H150.00120.96690.24220.093*
C160.1518 (3)1.0240 (2)0.24288 (12)0.0729 (17)
H160.14371.05850.21270.087*
C170.2498 (3)1.0280 (2)0.26951 (15)0.0772 (18)
H170.30861.06520.25750.093*
C180.26169 (19)0.9775 (2)0.31371 (14)0.0597 (14)
H180.32870.98020.33190.072*
O20.42527 (19)0.77309 (17)0.47514 (10)0.0318 (6)
Si20.43787 (9)0.67988 (7)0.48546 (5)0.0321 (3)
C190.57771 (16)0.71258 (19)0.52936 (11)0.0365 (11)
C200.6191 (2)0.77384 (19)0.57814 (12)0.0467 (12)
H200.57570.79430.59080.056*
C210.7242 (2)0.80521 (19)0.60832 (11)0.0578 (14)
H210.75250.84710.64170.069*
C220.78777 (17)0.7753 (2)0.58973 (14)0.0691 (16)
H220.85960.79680.61040.083*
C230.7463 (2)0.7141 (2)0.54095 (15)0.0716 (17)
H230.78980.69360.52820.086*
C240.6413 (2)0.68269 (19)0.51077 (11)0.0497 (12)
H240.61300.64080.47740.060*
C250.3439 (2)0.60499 (18)0.52300 (12)0.0409 (11)
C260.2429 (2)0.5985 (2)0.50888 (14)0.0619 (14)
H260.22320.63400.48200.074*
C270.1706 (2)0.5399 (3)0.53402 (19)0.094 (2)
H270.10150.53550.52440.112*
C280.1994 (3)0.4880 (2)0.57328 (18)0.103 (3)
H280.15000.44800.59050.124*
C290.3005 (4)0.4945 (2)0.58741 (14)0.088 (2)
H290.32020.45890.61420.106*
C300.3727 (3)0.5530 (2)0.56226 (13)0.0577 (14)
H300.44180.55750.57190.069*
C310.4118 (2)0.61419 (16)0.41626 (9)0.0344 (10)
C320.4260 (2)0.65853 (13)0.36923 (11)0.0431 (11)
H320.44590.72210.37140.052*
C330.4112 (3)0.6099 (2)0.31909 (10)0.0554 (13)
H330.42090.64020.28700.067*
C340.3821 (3)0.51693 (19)0.31599 (10)0.0610 (14)
H340.37190.48370.28170.073*
C350.3678 (3)0.47259 (13)0.36302 (13)0.0573 (14)
H350.34790.40900.36090.069*
C360.3827 (2)0.52122 (16)0.41315 (11)0.0486 (12)
H360.37290.49090.44530.058*
O30.5050 (2)0.89467 (17)0.38942 (11)0.0335 (7)
Si30.56903 (8)0.93207 (7)0.34386 (5)0.0298 (3)
C370.68828 (17)0.90887 (19)0.36110 (12)0.0348 (10)
C380.68930 (19)0.83719 (18)0.39105 (12)0.0472 (12)
H380.63150.80200.40440.057*
C390.7749 (2)0.81704 (19)0.40148 (13)0.0565 (13)
H390.77560.76800.42200.068*
C400.85952 (19)0.8686 (2)0.38197 (14)0.0562 (14)
H400.91800.85480.38910.067*
C410.85850 (18)0.9402 (2)0.35202 (14)0.0565 (14)
H410.91630.97550.33870.068*
C420.7729 (2)0.96040 (17)0.34158 (12)0.0476 (12)
H420.77221.00940.32110.057*
C430.6110 (2)1.05869 (14)0.34694 (11)0.0336 (10)
C440.6961 (2)1.11748 (18)0.39053 (11)0.0444 (11)
H440.73891.09500.41560.053*
C450.7185 (2)1.20907 (17)0.39749 (12)0.0533 (13)
H450.77661.24920.42730.064*
C460.6558 (3)1.24189 (14)0.36085 (14)0.0593 (14)
H460.67111.30450.36560.071*
C470.5707 (2)1.18311 (19)0.31726 (13)0.0671 (15)
H470.52791.20550.29220.081*
C480.5483 (2)1.09151 (18)0.31030 (11)0.0523 (13)
H480.49021.05130.28050.063*
C490.47755 (19)0.87177 (19)0.27294 (9)0.0337 (10)
C500.5131 (2)0.8682 (2)0.22671 (13)0.0580 (14)
H500.58590.89760.23040.070*
C510.4421 (3)0.8214 (3)0.17514 (10)0.0786 (18)
H510.46640.81900.14350.094*
C520.3356 (3)0.7783 (2)0.16980 (11)0.0808 (19)
H520.28710.74640.13460.097*
C530.30006 (18)0.7819 (2)0.21603 (15)0.0783 (17)
H530.22730.75240.21240.094*
C540.3710 (2)0.8286 (2)0.26760 (12)0.0574 (14)
H540.34670.83110.29920.069*
O40.4683 (2)0.95509 (17)0.53601 (11)0.0378 (7)
H4O0.44430.92150.56380.057*
O50.6284 (2)0.9277 (2)0.50363 (13)0.0529 (8)
H5A0.64390.88400.52740.090*
H5B0.66180.97950.53130.090*
Zr20.42999 (3)0.39154 (3)0.021311 (16)0.03121 (13)
O60.5125 (2)0.4268 (2)0.10077 (11)0.0461 (8)
Si40.57004 (9)0.43463 (8)0.16733 (5)0.0370 (3)
C550.6754 (2)0.3953 (2)0.17556 (12)0.0411 (11)
C560.7085 (3)0.3613 (2)0.22449 (11)0.0657 (15)
H560.67840.35870.25440.079*
C570.7856 (3)0.3310 (3)0.22972 (15)0.092 (2)
H570.80820.30780.26320.111*
C580.8295 (3)0.3348 (3)0.1860 (2)0.087 (2)
H580.88220.31410.18960.104*
C590.7964 (3)0.3688 (3)0.13709 (17)0.0776 (17)
H590.82650.37140.10720.093*
C600.7194 (3)0.3991 (2)0.13186 (11)0.0553 (13)
H600.69680.42230.09840.066*
C610.4718 (2)0.36481 (19)0.20387 (11)0.0431 (11)
C620.4983 (2)0.37570 (19)0.26240 (11)0.0509 (13)
H620.56660.41770.28390.061*
C630.4250 (3)0.3251 (2)0.28944 (10)0.0598 (14)
H630.44320.33250.32940.072*
C640.3251 (3)0.2636 (2)0.25795 (15)0.0676 (16)
H640.27500.22900.27640.081*
C650.2986 (2)0.2527 (2)0.19942 (14)0.087 (2)
H650.23030.21070.17790.104*
C660.3719 (2)0.3033 (2)0.17238 (9)0.0687 (16)
H660.35380.29590.13240.082*
C670.6283 (3)0.55715 (18)0.19762 (15)0.0461 (12)
C680.7354 (2)0.6125 (3)0.21249 (18)0.0838 (19)
H680.78220.58790.20900.101*
C690.7740 (3)0.7039 (2)0.2324 (2)0.123 (3)
H690.84720.74170.24260.147*
C700.7055 (5)0.7398 (2)0.2375 (2)0.117 (3)
H700.73190.80230.25110.140*
C710.5985 (5)0.6845 (3)0.2226 (3)0.165 (5)
H710.55170.70900.22600.198*
C720.5599 (3)0.5931 (3)0.2027 (2)0.133 (4)
H720.48670.55530.19250.160*
O70.2880 (2)0.3482 (2)0.02876 (12)0.0491 (8)
Si50.16705 (9)0.31985 (9)0.02485 (5)0.0422 (3)
C730.1116 (2)0.20793 (17)0.05269 (14)0.0459 (12)
C740.0255 (3)0.1852 (2)0.07285 (16)0.0720 (16)
H740.00270.22770.07460.086*
C750.0195 (2)0.1004 (3)0.09039 (17)0.0835 (19)
H750.07840.08490.10420.100*
C760.0216 (3)0.03828 (19)0.08778 (17)0.0803 (18)
H760.00910.01970.09980.096*
C770.1078 (3)0.0610 (2)0.06762 (17)0.0795 (17)
H770.13590.01850.06580.095*
C780.1528 (2)0.1458 (2)0.05007 (15)0.0619 (14)
H780.21160.16130.03630.074*
C790.1574 (3)0.4100 (2)0.06724 (14)0.0500 (12)
C800.2331 (3)0.4506 (3)0.11861 (16)0.102 (2)
H800.29180.43710.12980.122*
C810.2230 (4)0.5110 (3)0.15354 (14)0.134 (3)
H810.27470.53870.18870.161*
C820.1371 (4)0.5308 (3)0.13710 (18)0.094 (2)
H820.13010.57200.16100.113*
C830.0613 (3)0.4902 (3)0.0857 (2)0.0831 (18)
H830.00260.50370.07450.100*
C840.0715 (2)0.4298 (2)0.05080 (14)0.0690 (16)
H840.01970.40210.01570.083*
C850.0907 (2)0.3068 (2)0.05188 (9)0.0449 (12)
C860.0180 (3)0.22133 (17)0.08002 (14)0.0691 (16)
H860.00190.17000.06000.083*
C870.0313 (3)0.2110 (2)0.13744 (14)0.0832 (18)
H870.08100.15260.15670.100*
C880.0077 (3)0.2862 (3)0.16673 (10)0.0712 (16)
H880.04140.27910.20600.085*
C890.0650 (3)0.3716 (2)0.13859 (12)0.0603 (14)
H890.08110.42300.15860.072*
C900.1143 (2)0.38192 (16)0.08117 (13)0.0489 (12)
H900.16400.44030.06190.059*
O80.4399 (2)0.2780 (2)0.00787 (13)0.0516 (8)
Si60.45447 (10)0.18605 (8)0.00069 (5)0.0456 (3)
C910.5942 (2)0.2182 (3)0.00177 (16)0.0602 (14)
C920.6445 (4)0.2911 (2)0.02508 (16)0.0801 (18)
H920.60890.32500.04330.096*
C930.7469 (4)0.3143 (3)0.0252 (2)0.106 (3)
H930.78130.36420.04360.128*
C940.7989 (3)0.2647 (4)0.0015 (2)0.139 (4)
H940.86890.28060.00140.166*
C950.7486 (4)0.1918 (4)0.0284 (2)0.137 (4)
H950.78420.15790.04660.165*
C960.6463 (4)0.1686 (3)0.02849 (18)0.097 (2)
H960.61190.11880.04680.117*
C970.4239 (3)0.1169 (2)0.05896 (12)0.0512 (13)
C980.3469 (3)0.0278 (2)0.04844 (11)0.0707 (16)
H980.30740.00070.01080.085*
C990.3277 (3)0.0217 (2)0.09303 (16)0.0866 (19)
H990.27500.08260.08580.104*
C1000.3855 (4)0.0178 (3)0.14814 (13)0.098 (2)
H1000.37240.01600.17860.118*
C1010.4626 (4)0.1069 (3)0.15867 (10)0.180 (5)
H1010.50210.13400.19630.216*
C1020.4818 (4)0.1565 (2)0.11408 (14)0.145 (4)
H1020.53440.21740.12130.174*
C1030.3640 (3)0.1188 (2)0.06846 (13)0.0584 (14)
C1040.2784 (3)0.1356 (3)0.09440 (19)0.086 (2)
H1040.26700.18100.07700.103*
C1050.2095 (3)0.0861 (4)0.14577 (19)0.127 (3)
H1050.15100.09760.16350.152*
C1060.2262 (4)0.0198 (3)0.17120 (13)0.147 (5)
H1060.17910.01400.20630.176*
C1070.3118 (5)0.0029 (3)0.1453 (2)0.136 (4)
H1070.32320.04240.16260.163*
C1080.3807 (3)0.0524 (3)0.09389 (19)0.087 (2)
H1080.43910.04090.07620.104*
O90.5621 (2)0.47012 (18)0.01227 (12)0.0466 (8)
H9O0.60800.44850.02140.070*
O100.3424 (3)0.3690 (2)0.07450 (12)0.0606 (9)
H10A0.37290.40160.10020.103*
H10B0.27330.36980.09150.103*
C1090.9759 (5)0.6742 (4)0.6573 (2)0.101 (2)
C1101.0499 (4)0.7645 (4)0.6689 (2)0.101 (2)
H1101.09800.78740.64740.121*
C1111.0536 (4)0.8214 (3)0.7120 (3)0.116 (3)
H1111.10420.88310.71990.139*
C1120.9832 (5)0.7880 (5)0.7435 (2)0.128 (3)
H1120.98570.82690.77290.154*
C1130.9092 (4)0.6977 (5)0.7319 (3)0.140 (4)
H1130.86110.67490.75340.167*
C1140.9055 (4)0.6408 (3)0.6888 (3)0.116 (3)
H1140.85500.57910.68080.139*
C1150.9734 (10)0.6133 (7)0.6133 (4)0.186 (5)
H11A1.00960.64920.58740.280*
H11B0.90050.57370.59250.280*
H11C1.00840.57620.63050.280*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0240 (2)0.0229 (2)0.0229 (2)0.01021 (17)0.00587 (17)0.00221 (16)
O10.0296 (16)0.0450 (18)0.0472 (18)0.0200 (14)0.0113 (14)0.0134 (14)
Si10.0269 (6)0.0388 (7)0.0364 (7)0.0169 (6)0.0087 (5)0.0088 (5)
C10.022 (2)0.060 (3)0.032 (2)0.019 (2)0.000 (2)0.008 (2)
C20.026 (3)0.062 (3)0.053 (3)0.019 (2)0.003 (2)0.011 (3)
C30.037 (3)0.095 (4)0.061 (4)0.030 (3)0.003 (3)0.029 (3)
C40.050 (4)0.149 (6)0.039 (3)0.047 (4)0.011 (3)0.000 (4)
C50.058 (4)0.116 (5)0.055 (4)0.040 (4)0.027 (3)0.035 (4)
C60.044 (3)0.078 (4)0.047 (3)0.033 (3)0.018 (3)0.023 (3)
C70.041 (3)0.041 (3)0.037 (3)0.018 (2)0.013 (2)0.014 (2)
C80.048 (3)0.047 (3)0.073 (4)0.019 (3)0.001 (3)0.005 (3)
C90.057 (4)0.052 (4)0.084 (4)0.013 (3)0.015 (3)0.004 (3)
C100.095 (5)0.045 (3)0.064 (4)0.022 (4)0.004 (3)0.003 (3)
C110.080 (5)0.053 (4)0.111 (5)0.028 (3)0.036 (4)0.006 (3)
C120.054 (3)0.043 (3)0.080 (4)0.018 (3)0.022 (3)0.003 (3)
C130.038 (3)0.039 (3)0.037 (3)0.022 (2)0.010 (2)0.005 (2)
C140.050 (3)0.062 (3)0.060 (3)0.024 (3)0.002 (3)0.020 (3)
C150.068 (4)0.076 (4)0.066 (4)0.031 (3)0.017 (3)0.018 (3)
C160.113 (5)0.068 (4)0.044 (3)0.051 (4)0.014 (3)0.020 (3)
C170.094 (5)0.084 (4)0.090 (4)0.055 (4)0.058 (4)0.049 (4)
C180.059 (3)0.069 (4)0.076 (4)0.041 (3)0.036 (3)0.040 (3)
O20.0318 (15)0.0296 (16)0.0338 (16)0.0143 (13)0.0078 (13)0.0033 (12)
Si20.0343 (7)0.0263 (6)0.0361 (7)0.0138 (5)0.0098 (5)0.0063 (5)
C190.041 (3)0.031 (2)0.037 (3)0.016 (2)0.011 (2)0.016 (2)
C200.047 (3)0.048 (3)0.041 (3)0.021 (2)0.004 (2)0.014 (2)
C210.059 (4)0.055 (3)0.038 (3)0.013 (3)0.000 (3)0.015 (2)
C220.042 (3)0.088 (4)0.059 (4)0.018 (3)0.003 (3)0.036 (3)
C230.050 (4)0.102 (5)0.078 (4)0.044 (3)0.024 (3)0.038 (4)
C240.045 (3)0.058 (3)0.055 (3)0.029 (3)0.017 (3)0.017 (2)
C250.047 (3)0.029 (2)0.039 (3)0.009 (2)0.013 (2)0.001 (2)
C260.044 (3)0.066 (4)0.062 (3)0.010 (3)0.018 (3)0.003 (3)
C270.055 (4)0.097 (5)0.098 (5)0.004 (4)0.035 (4)0.012 (4)
C280.110 (6)0.073 (5)0.085 (5)0.016 (4)0.056 (5)0.001 (4)
C290.124 (6)0.052 (4)0.061 (4)0.006 (4)0.038 (4)0.018 (3)
C300.075 (4)0.040 (3)0.053 (3)0.016 (3)0.025 (3)0.013 (3)
C310.029 (2)0.030 (3)0.043 (3)0.014 (2)0.006 (2)0.001 (2)
C320.047 (3)0.038 (3)0.044 (3)0.017 (2)0.014 (2)0.004 (2)
C330.075 (4)0.052 (3)0.043 (3)0.028 (3)0.021 (3)0.003 (3)
C340.073 (4)0.058 (4)0.055 (4)0.033 (3)0.017 (3)0.012 (3)
C350.075 (4)0.036 (3)0.064 (4)0.025 (3)0.024 (3)0.004 (3)
C360.064 (3)0.034 (3)0.051 (3)0.023 (2)0.019 (3)0.005 (2)
O30.0343 (16)0.0349 (16)0.0347 (16)0.0161 (13)0.0138 (13)0.0058 (13)
Si30.0285 (6)0.0339 (7)0.0303 (6)0.0150 (5)0.0112 (5)0.0059 (5)
C370.030 (2)0.041 (3)0.033 (2)0.016 (2)0.009 (2)0.000 (2)
C380.038 (3)0.057 (3)0.052 (3)0.027 (2)0.014 (2)0.016 (3)
C390.057 (3)0.065 (3)0.058 (3)0.039 (3)0.011 (3)0.016 (3)
C400.042 (3)0.071 (4)0.059 (3)0.035 (3)0.002 (3)0.007 (3)
C410.033 (3)0.064 (4)0.073 (4)0.018 (3)0.023 (3)0.000 (3)
C420.042 (3)0.050 (3)0.057 (3)0.022 (3)0.021 (2)0.007 (2)
C430.032 (2)0.040 (3)0.033 (2)0.016 (2)0.016 (2)0.009 (2)
C440.039 (3)0.040 (3)0.051 (3)0.016 (2)0.010 (2)0.005 (2)
C450.045 (3)0.044 (3)0.060 (3)0.012 (3)0.010 (3)0.003 (3)
C460.080 (4)0.037 (3)0.063 (4)0.025 (3)0.026 (3)0.007 (3)
C470.092 (4)0.051 (4)0.058 (4)0.040 (3)0.005 (3)0.013 (3)
C480.060 (3)0.039 (3)0.047 (3)0.020 (3)0.002 (3)0.006 (2)
C490.037 (3)0.032 (2)0.035 (3)0.018 (2)0.011 (2)0.0066 (19)
C500.061 (3)0.063 (3)0.041 (3)0.017 (3)0.017 (3)0.004 (3)
C510.099 (5)0.077 (4)0.045 (4)0.025 (4)0.020 (3)0.005 (3)
C520.101 (5)0.062 (4)0.045 (4)0.022 (4)0.009 (3)0.008 (3)
C530.047 (3)0.088 (4)0.067 (4)0.013 (3)0.007 (3)0.006 (3)
C540.044 (3)0.068 (3)0.048 (3)0.016 (3)0.006 (3)0.001 (3)
O40.0537 (18)0.0282 (16)0.0281 (15)0.0117 (14)0.0168 (14)0.0062 (12)
O50.0318 (17)0.0507 (19)0.057 (2)0.0108 (15)0.0045 (15)0.0126 (16)
Zr20.0303 (2)0.0344 (3)0.0276 (2)0.0132 (2)0.00774 (19)0.01103 (18)
O60.0401 (18)0.061 (2)0.0329 (17)0.0210 (16)0.0061 (14)0.0133 (15)
Si40.0404 (7)0.0398 (7)0.0293 (7)0.0176 (6)0.0071 (6)0.0091 (5)
C550.038 (3)0.037 (3)0.040 (3)0.015 (2)0.001 (2)0.000 (2)
C560.068 (4)0.088 (4)0.052 (3)0.052 (3)0.006 (3)0.017 (3)
C570.096 (5)0.113 (5)0.086 (5)0.075 (5)0.004 (4)0.022 (4)
C580.055 (4)0.080 (4)0.122 (6)0.040 (3)0.002 (4)0.014 (4)
C590.061 (4)0.079 (4)0.093 (5)0.028 (3)0.027 (3)0.011 (4)
C600.049 (3)0.056 (3)0.060 (3)0.021 (3)0.018 (3)0.003 (3)
C610.050 (3)0.044 (3)0.045 (3)0.028 (3)0.016 (2)0.019 (2)
C620.074 (4)0.045 (3)0.040 (3)0.027 (3)0.024 (3)0.009 (2)
C630.095 (4)0.054 (3)0.053 (3)0.044 (3)0.039 (3)0.021 (3)
C640.080 (4)0.071 (4)0.073 (4)0.039 (4)0.046 (3)0.045 (3)
C650.057 (4)0.102 (5)0.071 (4)0.008 (3)0.015 (3)0.046 (4)
C660.056 (4)0.082 (4)0.048 (3)0.012 (3)0.013 (3)0.031 (3)
C670.062 (3)0.046 (3)0.037 (3)0.028 (3)0.018 (2)0.012 (2)
C680.073 (4)0.056 (4)0.089 (4)0.027 (3)0.028 (3)0.011 (3)
C690.124 (6)0.056 (5)0.116 (6)0.025 (4)0.054 (5)0.022 (4)
C700.208 (10)0.055 (4)0.095 (5)0.060 (6)0.049 (6)0.002 (4)
C710.204 (10)0.059 (5)0.308 (14)0.059 (6)0.193 (11)0.036 (6)
C720.115 (6)0.050 (4)0.278 (11)0.038 (4)0.120 (7)0.022 (5)
O70.0347 (18)0.061 (2)0.0419 (18)0.0118 (15)0.0108 (14)0.0144 (15)
Si50.0317 (7)0.0464 (8)0.0426 (8)0.0120 (6)0.0099 (6)0.0108 (6)
C730.034 (3)0.052 (3)0.044 (3)0.013 (2)0.007 (2)0.010 (2)
C740.055 (3)0.073 (4)0.098 (5)0.028 (3)0.037 (3)0.040 (3)
C750.072 (4)0.078 (4)0.108 (5)0.025 (4)0.050 (4)0.048 (4)
C760.088 (5)0.060 (4)0.075 (4)0.016 (4)0.022 (4)0.030 (3)
C770.095 (5)0.063 (4)0.091 (5)0.042 (4)0.031 (4)0.025 (3)
C780.063 (3)0.056 (3)0.071 (4)0.025 (3)0.027 (3)0.016 (3)
C790.049 (3)0.045 (3)0.049 (3)0.014 (2)0.016 (3)0.010 (2)
C800.123 (6)0.112 (5)0.067 (4)0.079 (5)0.026 (4)0.023 (4)
C810.183 (9)0.139 (7)0.079 (5)0.111 (7)0.033 (5)0.038 (5)
C820.133 (6)0.083 (5)0.079 (5)0.052 (5)0.045 (5)0.008 (4)
C830.064 (4)0.079 (4)0.108 (5)0.028 (3)0.034 (4)0.002 (4)
C840.048 (3)0.076 (4)0.076 (4)0.023 (3)0.014 (3)0.011 (3)
C850.033 (3)0.049 (3)0.050 (3)0.018 (2)0.008 (2)0.004 (3)
C860.067 (4)0.056 (4)0.057 (4)0.016 (3)0.007 (3)0.007 (3)
C870.081 (4)0.067 (4)0.068 (4)0.019 (3)0.010 (3)0.011 (3)
C880.067 (4)0.100 (5)0.047 (3)0.044 (4)0.004 (3)0.002 (4)
C890.056 (3)0.072 (4)0.054 (4)0.032 (3)0.012 (3)0.018 (3)
C900.044 (3)0.051 (3)0.048 (3)0.020 (2)0.008 (2)0.010 (2)
O80.063 (2)0.0402 (18)0.052 (2)0.0233 (16)0.0164 (17)0.0134 (15)
Si60.0557 (8)0.0332 (7)0.0431 (8)0.0159 (6)0.0125 (6)0.0033 (6)
C910.062 (3)0.043 (3)0.060 (3)0.011 (3)0.012 (3)0.021 (3)
C920.082 (5)0.068 (4)0.079 (4)0.009 (3)0.045 (4)0.017 (3)
C930.091 (6)0.094 (5)0.100 (6)0.006 (5)0.050 (5)0.034 (4)
C940.073 (5)0.129 (8)0.166 (9)0.003 (6)0.027 (6)0.078 (7)
C950.062 (5)0.112 (7)0.208 (10)0.036 (5)0.002 (6)0.047 (7)
C960.059 (4)0.067 (4)0.145 (7)0.025 (4)0.002 (4)0.012 (4)
C970.071 (3)0.040 (3)0.047 (3)0.030 (3)0.015 (3)0.008 (2)
C980.086 (4)0.058 (4)0.053 (3)0.018 (3)0.019 (3)0.012 (3)
C990.111 (5)0.058 (4)0.072 (4)0.016 (4)0.030 (4)0.026 (3)
C1000.176 (7)0.074 (5)0.055 (4)0.058 (5)0.042 (4)0.025 (3)
C1010.342 (14)0.057 (5)0.044 (4)0.012 (6)0.027 (6)0.011 (4)
C1020.257 (11)0.051 (4)0.040 (4)0.004 (5)0.012 (5)0.006 (3)
C1030.056 (3)0.048 (3)0.049 (3)0.002 (3)0.020 (3)0.012 (3)
C1040.070 (4)0.070 (4)0.071 (4)0.001 (3)0.002 (4)0.014 (3)
C1050.080 (5)0.126 (7)0.069 (5)0.032 (5)0.017 (4)0.025 (5)
C1060.127 (8)0.135 (8)0.053 (5)0.064 (6)0.032 (5)0.026 (5)
C1070.134 (7)0.112 (6)0.090 (6)0.032 (6)0.065 (6)0.046 (5)
C1080.100 (5)0.068 (4)0.068 (4)0.005 (4)0.039 (4)0.017 (3)
O90.056 (2)0.0290 (16)0.0470 (18)0.0118 (15)0.0133 (15)0.0186 (14)
O100.070 (2)0.072 (2)0.0330 (18)0.0303 (19)0.0055 (16)0.0164 (16)
C1090.106 (6)0.083 (6)0.106 (6)0.058 (5)0.010 (5)0.020 (5)
C1100.086 (5)0.100 (6)0.098 (6)0.031 (5)0.011 (4)0.039 (5)
C1110.102 (6)0.102 (6)0.101 (6)0.003 (5)0.030 (5)0.006 (5)
C1120.121 (7)0.115 (7)0.133 (7)0.043 (6)0.027 (6)0.034 (6)
C1130.100 (7)0.110 (7)0.239 (12)0.065 (6)0.065 (7)0.078 (8)
C1140.076 (5)0.077 (5)0.201 (10)0.040 (4)0.039 (6)0.051 (6)
C1150.298 (15)0.155 (9)0.121 (8)0.123 (10)0.042 (9)0.043 (7)
Geometric parameters (Å, º) top
Zr1—O31.967 (3)Si4—C551.875 (3)
Zr1—O11.970 (3)Si4—C611.877 (2)
Zr1—O21.974 (3)Si4—C671.877 (3)
Zr1—O42.133 (3)C55—C561.3900
Zr1—O4i2.174 (3)C55—C601.3900
Zr1—O52.329 (3)C56—C571.3900
Zr1—Zr1i3.5506 (11)C56—H560.9500
O1—Si11.617 (3)C57—C581.3900
Si1—C131.879 (2)C57—H570.9500
Si1—C71.879 (3)C58—C591.3900
Si1—C11.886 (2)C58—H580.9500
C1—C21.3900C59—C601.3900
C1—C61.3900C59—H590.9500
C2—C31.3900C60—H600.9500
C2—H20.9500C61—C621.3900
C3—C41.3900C61—C661.3900
C3—H30.9500C62—C631.3900
C4—C51.3900C62—H620.9500
C4—H40.9500C63—C641.3900
C5—C61.3900C63—H630.9500
C5—H50.9500C64—C651.3900
C6—H60.9500C64—H640.9500
C7—C81.3900C65—C661.3900
C7—C121.3900C65—H650.9500
C8—C91.3900C66—H660.9500
C8—H80.9500C67—C681.3900
C9—C101.3900C67—C721.3900
C9—H90.9500C68—C691.3900
C10—C111.3900C68—H680.9500
C10—H100.9500C69—C701.3900
C11—C121.3900C69—H690.9500
C11—H110.9500C70—C711.3900
C12—H120.9500C70—H700.9500
C13—C141.3900C71—C721.3900
C13—C181.3900C71—H710.9500
C14—C151.3900C72—H720.9500
C14—H140.9500O7—Si51.613 (3)
C15—C161.3900Si5—C731.880 (3)
C15—H150.9500Si5—C791.882 (3)
C16—C171.3900Si5—C851.896 (2)
C16—H160.9500C73—C741.3900
C17—C181.3900C73—C781.3900
C17—H170.9500C74—C751.3900
C18—H180.9500C74—H740.9500
O2—Si21.621 (3)C75—C761.3900
Si2—C251.881 (2)C75—H750.9500
Si2—C311.883 (2)C76—C771.3900
Si2—C191.895 (2)C76—H760.9500
C19—C201.3900C77—C781.3900
C19—C241.3900C77—H770.9500
C20—C211.3900C78—H780.9500
C20—H200.9500C79—C801.3900
C21—C221.3900C79—C841.3900
C21—H210.9500C80—C811.3900
C22—C231.3900C80—H800.9500
C22—H220.9500C81—C821.3900
C23—C241.3900C81—H810.9500
C23—H230.9500C82—C831.3900
C24—H240.9500C82—H820.9500
C25—C261.3900C83—C841.3900
C25—C301.3900C83—H830.9500
C26—C271.3900C84—H840.9500
C26—H260.9500C85—C861.3900
C27—C281.3900C85—C901.3900
C27—H270.9500C86—C871.3900
C28—C291.3900C86—H860.9500
C28—H280.9500C87—C881.3900
C29—C301.3900C87—H870.9500
C29—H290.9500C88—C891.3900
C30—H300.9500C88—H880.9500
C31—C321.3900C89—C901.3900
C31—C361.3900C89—H890.9500
C32—C331.3900C90—H900.9500
C32—H320.9500O8—Si61.617 (3)
C33—C341.3900Si6—C1031.866 (3)
C33—H330.9500Si6—C971.868 (3)
C34—C351.3900Si6—C911.887 (3)
C34—H340.9500C91—C921.3900
C35—C361.3900C91—C961.3900
C35—H350.9500C92—C931.3900
C36—H360.9500C92—H920.9500
O3—Si31.618 (3)C93—C941.3900
Si3—C491.873 (2)C93—H930.9500
Si3—C371.885 (2)C94—C951.3900
Si3—C431.889 (2)C94—H940.9500
C37—C381.3900C95—C961.3900
C37—C421.3900C95—H950.9500
C38—C391.3900C96—H960.9500
C38—H380.9500C97—C981.3900
C39—C401.3900C97—C1021.3900
C39—H390.9500C98—C991.3900
C40—C411.3900C98—H980.9500
C40—H400.9500C99—C1001.3900
C41—C421.3900C99—H990.9500
C41—H410.9500C100—C1011.3900
C42—H420.9500C100—H1000.9500
C43—C441.3900C101—C1021.3900
C43—C481.3900C101—H1010.9500
C44—C451.3900C102—H1020.9500
C44—H440.9500C103—C1041.3900
C45—C461.3900C103—C1081.3900
C45—H450.9500C104—C1051.3900
C46—C471.3900C104—H1040.9500
C46—H460.9500C105—C1061.3900
C47—C481.3900C105—H1050.9500
C47—H470.9500C106—C1071.3900
C48—H480.9500C106—H1060.9500
C49—C501.3900C107—C1081.3900
C49—C541.3900C107—H1070.9500
C50—C511.3900C108—H1080.9500
C50—H500.9500O9—Zr2ii2.227 (3)
C51—C521.3900O9—H9O0.9532
C51—H510.9500O10—H10A0.9178
C52—C531.3900O10—H10B0.9971
C52—H520.9500C109—C1101.3900
C53—C541.3900C109—C1141.3900
C53—H530.9500C109—C1151.457 (11)
C54—H540.9500C110—C1111.3900
O4—Zr1i2.174 (3)C110—H1100.9500
O4—H4O0.9314C111—C1121.3900
O5—H5A0.9872C111—H1110.9500
O5—H5B0.9486C112—C1131.3900
Zr2—O81.954 (3)C112—H1120.9500
Zr2—O61.958 (3)C113—C1141.3900
Zr2—O71.964 (3)C113—H1130.9500
Zr2—O92.210 (3)C114—H1140.9500
Zr2—O9ii2.227 (3)C115—H11A0.9800
Zr2—O102.328 (3)C115—H11B0.9800
Zr2—Zr2ii3.5999 (11)C115—H11C0.9800
O6—Si41.621 (3)
O3—Zr1—O1100.27 (11)O7—Zr2—O1083.02 (12)
O3—Zr1—O2100.74 (11)O9—Zr2—O1079.52 (11)
O1—Zr1—O299.31 (11)O9ii—Zr2—O1081.26 (11)
O3—Zr1—O4153.66 (11)O8—Zr2—Zr2ii127.81 (9)
O1—Zr1—O496.26 (11)O6—Zr2—Zr2ii94.71 (9)
O2—Zr1—O496.62 (10)O7—Zr2—Zr2ii124.29 (9)
O3—Zr1—O4i88.58 (10)O9—Zr2—Zr2ii35.93 (8)
O1—Zr1—O4i97.28 (11)O9ii—Zr2—Zr2ii35.61 (8)
O2—Zr1—O4i159.15 (10)O10—Zr2—Zr2ii78.13 (9)
O4—Zr1—O4i68.98 (11)Si4—O6—Zr2168.6 (2)
O3—Zr1—O582.28 (11)O6—Si4—C55109.00 (15)
O1—Zr1—O5175.30 (12)O6—Si4—C61109.96 (15)
O2—Zr1—O584.01 (11)C55—Si4—C61110.98 (15)
O4—Zr1—O580.00 (12)O6—Si4—C67107.60 (17)
O4i—Zr1—O578.78 (11)C55—Si4—C67110.33 (16)
O3—Zr1—Zr1i121.56 (8)C61—Si4—C67108.90 (16)
O1—Zr1—Zr1i98.22 (9)C56—C55—C60120.0
O2—Zr1—Zr1i129.91 (8)C56—C55—Si4120.56 (19)
O4—Zr1—Zr1i34.86 (7)C60—C55—Si4119.44 (19)
O4i—Zr1—Zr1i34.12 (7)C57—C56—C55120.0
O5—Zr1—Zr1i77.08 (8)C57—C56—H56120.0
Si1—O1—Zr1169.22 (18)C55—C56—H56120.0
O1—Si1—C13108.28 (14)C56—C57—C58120.0
O1—Si1—C7111.54 (15)C56—C57—H57120.0
C13—Si1—C7108.61 (15)C58—C57—H57120.0
O1—Si1—C1109.24 (15)C59—C58—C57120.0
C13—Si1—C1109.09 (14)C59—C58—H58120.0
C7—Si1—C1110.02 (14)C57—C58—H58120.0
C2—C1—C6120.0C58—C59—C60120.0
C2—C1—Si1119.19 (18)C58—C59—H59120.0
C6—C1—Si1120.58 (18)C60—C59—H59120.0
C1—C2—C3120.0C59—C60—C55120.0
C1—C2—H2120.0C59—C60—H60120.0
C3—C2—H2120.0C55—C60—H60120.0
C4—C3—C2120.0C62—C61—C66120.0
C4—C3—H3120.0C62—C61—Si4120.00 (17)
C2—C3—H3120.0C66—C61—Si4120.00 (17)
C5—C4—C3120.0C63—C62—C61120.0
C5—C4—H4120.0C63—C62—H62120.0
C3—C4—H4120.0C61—C62—H62120.0
C4—C5—C6120.0C62—C63—C64120.0
C4—C5—H5120.0C62—C63—H63120.0
C6—C5—H5120.0C64—C63—H63120.0
C5—C6—C1120.0C65—C64—C63120.0
C5—C6—H6120.0C65—C64—H64120.0
C1—C6—H6120.0C63—C64—H64120.0
C8—C7—C12120.0C64—C65—C66120.0
C8—C7—Si1120.66 (17)C64—C65—H65120.0
C12—C7—Si1119.05 (18)C66—C65—H65120.0
C7—C8—C9120.0C65—C66—C61120.0
C7—C8—H8120.0C65—C66—H66120.0
C9—C8—H8120.0C61—C66—H66120.0
C10—C9—C8120.0C68—C67—C72120.0
C10—C9—H9120.0C68—C67—Si4122.4 (2)
C8—C9—H9120.0C72—C67—Si4117.6 (2)
C9—C10—C11120.0C69—C68—C67120.0
C9—C10—H10120.0C69—C68—H68120.0
C11—C10—H10120.0C67—C68—H68120.0
C12—C11—C10120.0C70—C69—C68120.0
C12—C11—H11120.0C70—C69—H69120.0
C10—C11—H11120.0C68—C69—H69120.0
C11—C12—C7120.0C69—C70—C71120.0
C11—C12—H12120.0C69—C70—H70120.0
C7—C12—H12120.0C71—C70—H70120.0
C14—C13—C18120.0C72—C71—C70120.0
C14—C13—Si1119.73 (17)C72—C71—H71120.0
C18—C13—Si1120.07 (17)C70—C71—H71120.0
C15—C14—C13120.0C71—C72—C67120.0
C15—C14—H14120.0C71—C72—H72120.0
C13—C14—H14120.0C67—C72—H72120.0
C16—C15—C14120.0Si5—O7—Zr2170.06 (19)
C16—C15—H15120.0O7—Si5—C73109.55 (16)
C14—C15—H15120.0O7—Si5—C79109.75 (17)
C15—C16—C17120.0C73—Si5—C79109.86 (16)
C15—C16—H16120.0O7—Si5—C85108.64 (15)
C17—C16—H16120.0C73—Si5—C85108.79 (15)
C18—C17—C16120.0C79—Si5—C85110.22 (16)
C18—C17—H17120.0C74—C73—C78120.0
C16—C17—H17120.0C74—C73—Si5119.85 (19)
C17—C18—C13120.0C78—C73—Si5120.04 (19)
C17—C18—H18120.0C73—C74—C75120.0
C13—C18—H18120.0C73—C74—H74120.0
Si2—O2—Zr1159.77 (16)C75—C74—H74120.0
O2—Si2—C25111.36 (14)C76—C75—C74120.0
O2—Si2—C31110.47 (13)C76—C75—H75120.0
C25—Si2—C31108.17 (14)C74—C75—H75120.0
O2—Si2—C19107.47 (14)C75—C76—C77120.0
C25—Si2—C19110.10 (14)C75—C76—H76120.0
C31—Si2—C19109.27 (14)C77—C76—H76120.0
C20—C19—C24120.0C76—C77—C78120.0
C20—C19—Si2118.88 (17)C76—C77—H77120.0
C24—C19—Si2120.86 (17)C78—C77—H77120.0
C19—C20—C21120.0C77—C78—C73120.0
C19—C20—H20120.0C77—C78—H78120.0
C21—C20—H20120.0C73—C78—H78120.0
C22—C21—C20120.0C80—C79—C84120.0
C22—C21—H21120.0C80—C79—Si5118.4 (2)
C20—C21—H21120.0C84—C79—Si5121.3 (2)
C21—C22—C23120.0C79—C80—C81120.0
C21—C22—H22120.0C79—C80—H80120.0
C23—C22—H22120.0C81—C80—H80120.0
C24—C23—C22120.0C82—C81—C80120.0
C24—C23—H23120.0C82—C81—H81120.0
C22—C23—H23120.0C80—C81—H81120.0
C23—C24—C19120.0C83—C82—C81120.0
C23—C24—H24120.0C83—C82—H82120.0
C19—C24—H24120.0C81—C82—H82120.0
C26—C25—C30120.0C82—C83—C84120.0
C26—C25—Si2119.09 (19)C82—C83—H83120.0
C30—C25—Si2120.83 (19)C84—C83—H83120.0
C25—C26—C27120.0C83—C84—C79120.0
C25—C26—H26120.0C83—C84—H84120.0
C27—C26—H26120.0C79—C84—H84120.0
C28—C27—C26120.0C86—C85—C90120.0
C28—C27—H27120.0C86—C85—Si5120.24 (18)
C26—C27—H27120.0C90—C85—Si5119.54 (18)
C27—C28—C29120.0C85—C86—C87120.0
C27—C28—H28120.0C85—C86—H86120.0
C29—C28—H28120.0C87—C86—H86120.0
C28—C29—C30120.0C88—C87—C86120.0
C28—C29—H29120.0C88—C87—H87120.0
C30—C29—H29120.0C86—C87—H87120.0
C29—C30—C25120.0C87—C88—C89120.0
C29—C30—H30120.0C87—C88—H88120.0
C25—C30—H30120.0C89—C88—H88120.0
C32—C31—C36120.0C88—C89—C90120.0
C32—C31—Si2120.57 (15)C88—C89—H89120.0
C36—C31—Si2119.37 (15)C90—C89—H89120.0
C33—C32—C31120.0C89—C90—C85120.0
C33—C32—H32120.0C89—C90—H90120.0
C31—C32—H32120.0C85—C90—H90120.0
C32—C33—C34120.0Si6—O8—Zr2176.1 (2)
C32—C33—H33120.0O8—Si6—C103108.62 (18)
C34—C33—H33120.0O8—Si6—C97110.57 (17)
C35—C34—C33120.0C103—Si6—C97109.62 (16)
C35—C34—H34120.0O8—Si6—C91108.74 (17)
C33—C34—H34120.0C103—Si6—C91109.54 (17)
C34—C35—C36120.0C97—Si6—C91109.73 (19)
C34—C35—H35120.0C92—C91—C96120.0
C36—C35—H35120.0C92—C91—Si6119.7 (3)
C35—C36—C31120.0C96—C91—Si6120.3 (3)
C35—C36—H36120.0C93—C92—C91120.0
C31—C36—H36120.0C93—C92—H92120.0
Si3—O3—Zr1158.70 (17)C91—C92—H92120.0
O3—Si3—C49107.00 (14)C92—C93—C94120.0
O3—Si3—C37110.19 (13)C92—C93—H93120.0
C49—Si3—C37110.91 (14)C94—C93—H93120.0
O3—Si3—C43108.20 (14)C95—C94—C93120.0
C49—Si3—C43110.94 (13)C95—C94—H94120.0
C37—Si3—C43109.54 (13)C93—C94—H94120.0
C38—C37—C42120.0C94—C95—C96120.0
C38—C37—Si3119.78 (15)C94—C95—H95120.0
C42—C37—Si3120.15 (15)C96—C95—H95120.0
C37—C38—C39120.0C95—C96—C91120.0
C37—C38—H38120.0C95—C96—H96120.0
C39—C38—H38120.0C91—C96—H96120.0
C38—C39—C40120.0C98—C97—C102120.0
C38—C39—H39120.0C98—C97—Si6121.86 (19)
C40—C39—H39120.0C102—C97—Si6118.13 (19)
C41—C40—C39120.0C99—C98—C97120.0
C41—C40—H40120.0C99—C98—H98120.0
C39—C40—H40120.0C97—C98—H98120.0
C40—C41—C42120.0C98—C99—C100120.0
C40—C41—H41120.0C98—C99—H99120.0
C42—C41—H41120.0C100—C99—H99120.0
C41—C42—C37120.0C101—C100—C99120.0
C41—C42—H42120.0C101—C100—H100120.0
C37—C42—H42120.0C99—C100—H100120.0
C44—C43—C48120.0C102—C101—C100120.0
C44—C43—Si3119.81 (15)C102—C101—H101120.0
C48—C43—Si3119.59 (15)C100—C101—H101120.0
C43—C44—C45120.0C101—C102—C97120.0
C43—C44—H44120.0C101—C102—H102120.0
C45—C44—H44120.0C97—C102—H102120.0
C46—C45—C44120.0C104—C103—C108120.0
C46—C45—H45120.0C104—C103—Si6118.9 (3)
C44—C45—H45120.0C108—C103—Si6121.1 (3)
C45—C46—C47120.0C105—C104—C103120.0
C45—C46—H46120.0C105—C104—H104120.0
C47—C46—H46120.0C103—C104—H104120.0
C48—C47—C46120.0C104—C105—C106120.0
C48—C47—H47120.0C104—C105—H105120.0
C46—C47—H47120.0C106—C105—H105120.0
C47—C48—C43120.0C107—C106—C105120.0
C47—C48—H48120.0C107—C106—H106120.0
C43—C48—H48120.0C105—C106—H106120.0
C50—C49—C54120.0C108—C107—C106120.0
C50—C49—Si3122.20 (17)C108—C107—H107120.0
C54—C49—Si3117.80 (17)C106—C107—H107120.0
C51—C50—C49120.0C107—C108—C103120.0
C51—C50—H50120.0C107—C108—H108120.0
C49—C50—H50120.0C103—C108—H108120.0
C50—C51—C52120.0Zr2—O9—Zr2ii108.46 (13)
C50—C51—H51120.0Zr2—O9—H9O125.8
C52—C51—H51120.0Zr2ii—O9—H9O125.8
C53—C52—C51120.0Zr2—O10—H10A123.0
C53—C52—H52120.0Zr2—O10—H10B126.3
C51—C52—H52120.0H10A—O10—H10B94.8
C52—C53—C54120.0C110—C109—C114120.0
C52—C53—H53120.0C110—C109—C115120.4 (7)
C54—C53—H53120.0C114—C109—C115119.6 (7)
C53—C54—C49120.0C109—C110—C111120.0
C53—C54—H54120.0C109—C110—H110120.0
C49—C54—H54120.0C111—C110—H110120.0
Zr1—O4—Zr1i111.02 (11)C112—C111—C110120.0
Zr1—O4—H4O124.5C112—C111—H111120.0
Zr1i—O4—H4O124.5C110—C111—H111120.0
Zr1—O5—H5A120.4C111—C112—C113120.0
Zr1—O5—H5B113.1C111—C112—H112120.0
H5A—O5—H5B98.5C113—C112—H112120.0
O8—Zr2—O699.13 (13)C114—C113—C112120.0
O8—Zr2—O7102.30 (13)C114—C113—H113120.0
O6—Zr2—O7100.24 (12)C112—C113—H113120.0
O8—Zr2—O992.52 (12)C113—C114—C109120.0
O6—Zr2—O995.46 (11)C113—C114—H114120.0
O7—Zr2—O9156.30 (11)C109—C114—H114120.0
O8—Zr2—O9ii161.33 (12)C109—C115—H11A109.5
O6—Zr2—O9ii92.19 (12)C109—C115—H11B109.5
O7—Zr2—O9ii90.12 (12)H11A—C115—H11B109.5
O9—Zr2—O9ii71.54 (13)C109—C115—H11C109.5
O8—Zr2—O1086.43 (12)H11A—C115—H11C109.5
O6—Zr2—O10172.72 (12)H11B—C115—H11C109.5
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z.
 

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