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The structure of 1,1,3,3,5,5-hexaphenyltrisiloxane-1,5-diol–pyrazine (4/1), (C36H32O4Si3)4·C4H4N2 (1), contains finite centrosymmetric aggregates; the diol units form dimers, by means of O—H...O hydrogen bonds, and pairs of such dimers are linked to the pyrazine by means of O—H...N hydrogen bonds. In 1,1,3,3,5,5-hexaphenyltrisiloxane-1,5-diol–pyridine (2/3), (C36H32O4Si3)2·(C5H5N)3 (2), the diol units are linked into centrosymmetric pairs by means of disordered O—H...O hydrogen bonds: two of the three pyridine molecules are linked to the diol dimer by means of ordered O—H...N hydrogen bonds, while the third pyridine unit, which is disordered across a centre of inversion, links the diol dimers into a C33(9) chain by means of O—H...N and C—H...O hydrogen bonds. In 1,1,3,3-tetraphenyldisiloxane-1,3-diol–hexamethylenetetramine (1/1), (C24H22O3Si2)·C6H12N4 (3), the diol acts as a double donor and the hexamethylene­tetramine acts as a double acceptor in ordered O—H...N hydrogen bonds and the structure consists of C22(10) chains of alternating diol and amine units. In 1,1,3,3-tetraphenyldi­siloxane-1,3-diol–2,2′-bipyridyl (1/1), C24H22O3Si2·C10H8N2 (4), there are two independent diol molecules, both lying across centres of inversion and therefore both containing linear Si—O—Si groups: each diol acts as a double donor of hydrogen bonds and the unique 2,2′-bipyridyl molecule acts as a double acceptor, thus forming C22(11) chains of alternating diol and amine units. The structural motif in 1,1,3,3-tetra­phenyldisiloxane-1,3-diol–pyrazine (2/1), (C24H22O3Si2)2·C4H4N2 (5), is a chain-of-rings: pairs of diol molecules are linked by O—H...O hydrogen bonds into centrosymmetric R22(12) dimers and these dimers are linked into C22(13) chains by means of O—H...N hydrogen bonds to the pyrazine units. 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–pyridine (1/1), C24H22O3Si2·C5H5N (6), and 1,1,3,3-tetraphenyldisiloxane-1,3-diol–pyrimidine (1/1), C24H22O3Si2·C4H4N2 (7), are isomorphous: in each compound the amine unit is disordered across a centre of inversion. The diol molecules form C(6) chains, by means of disordered O—H...O hydrogen bonds, and these chains are linked into two-dimensional nets built from R66(26) rings, by a combination of O—H...N and C—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768199013051/cf0008sup1.cif
Contains datablocks global, sila1, sila2, sila3, sila4, sila5, sila6, sila7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila1sup2.hkl
Contains datablock sila1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila2sup3.hkl
Contains datablock sila2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila3sup4.hkl
Contains datablock sila3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila4sup5.hkl
Contains datablock 94809

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila5sup6.hkl
Contains datablock sila5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila6sup7.hkl
Contains datablock sila6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768199013051/cf0008sila7sup8.hkl
Contains datablock sila7

CCDC references: 144365; 144366; 144367; 144368; 144369; 144370; 144371

Computing details top

For all compounds, data collection: CAD-4-PC Software (Enraf-Nonius, 1992); cell refinement: SET4 & CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992); data reduction: DATRD2 in NRCVAX96 (Gabe et al., 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: NRCVAX96 and SHELXL97 (Sheldrick, 1997b); molecular graphics: NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998); software used to prepare material for publication: NRCVAX96, SHELXL97 and WORDPERFECT macro PREP8 (Ferguson, 1998).

(sila1) 1,1,3,3,5,5-Hexaphenyltrisiloxane-1,5-diol–pyrazine (4/1) top
Crystal data top
4(C36H32O4Si3)·C4H4N2F(000) = 1330
Mr = 2531.64? #Insert any comments here.
Triclinic, P1Dx = 1.235 Mg m3
a = 14.2354 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 15.2960 (14) ÅCell parameters from 25 reflections
c = 18.7470 (14) Åθ = 9.3–19.8°
α = 71.764 (6)°µ = 0.18 mm1
β = 88.862 (6)°T = 294 K
γ = 62.544 (7)°Block, colourless
V = 3402.7 (5) Å30.36 × 0.33 × 0.29 mm
Z = 1
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.1°
Graphite monochromatorh = 1618
θ/2θ scansk = 019
14788 measured reflectionsl = 2223
14788 independent reflections3 standard reflections every 120 min
10215 reflections with I > 2σ(I) intensity decay: no decay, variation 1.1%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.120 w = 1/[σ2(Fo2) + (0.0698P)2 + 0.0963P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.003
14788 reflectionsΔρmax = 0.26 e Å3
807 parametersΔρmin = 0.26 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0225 (9)
Special details top

Experimental. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si1A0.29021 (4)0.53513 (3)0.18928 (3)0.03773 (12)
Si2A0.13743 (4)0.51451 (4)0.32153 (3)0.04133 (12)
Si3A0.09299 (4)0.35125 (4)0.29901 (3)0.03925 (12)
Si1B0.07340 (4)0.15162 (3)0.21510 (3)0.03586 (11)
Si2B0.15574 (4)0.00347 (3)0.18326 (3)0.03728 (11)
Si3B0.30942 (4)0.01307 (3)0.30607 (3)0.03684 (11)
O1A0.20313 (10)0.46157 (9)0.14727 (8)0.0508 (3)
O2A0.23442 (9)0.54187 (9)0.25990 (7)0.0474 (3)
O3A0.02525 (10)0.44306 (10)0.29805 (8)0.0582 (4)
O4A0.08677 (10)0.24898 (9)0.29516 (8)0.0509 (3)
O1B0.06255 (10)0.25705 (9)0.20295 (7)0.0471 (3)
O2B0.04558 (9)0.06121 (9)0.21527 (7)0.0471 (3)
O3B0.25270 (9)0.00910 (9)0.22272 (6)0.0434 (3)
O4B0.22186 (10)0.03294 (9)0.35922 (7)0.0500 (3)
N10.07241 (13)0.50084 (14)0.05058 (9)0.0563 (4)
C10.01144 (17)0.41275 (17)0.05138 (12)0.0587 (5)
C20.08330 (17)0.41179 (17)0.00135 (12)0.0613 (5)
C11A0.37651 (14)0.47437 (13)0.22276 (10)0.0449 (4)
C12A0.41822 (19)0.4464 (2)0.17311 (14)0.0724 (6)
C13A0.4852 (2)0.4033 (2)0.19395 (19)0.0938 (9)
C14A0.5135 (2)0.38892 (19)0.2647 (2)0.0854 (8)
C15A0.4738 (2)0.41493 (19)0.31524 (16)0.0778 (7)
C16A0.40473 (16)0.45738 (16)0.29482 (12)0.0587 (5)
C21A0.37001 (13)0.67029 (13)0.11973 (10)0.0402 (4)
C22A0.36296 (17)0.69381 (16)0.04289 (11)0.0579 (5)
C23A0.4234 (2)0.79405 (19)0.00820 (13)0.0749 (7)
C24A0.4926 (2)0.87212 (17)0.01618 (15)0.0744 (7)
C25A0.50178 (19)0.85193 (17)0.09120 (16)0.0746 (7)
C26A0.44072 (16)0.75179 (15)0.14270 (12)0.0596 (5)
C31A0.15287 (14)0.44000 (15)0.41592 (11)0.0489 (4)
C32A0.14016 (18)0.33945 (17)0.42920 (13)0.0633 (5)
C33A0.1555 (2)0.28331 (19)0.49781 (15)0.0754 (7)
C34A0.1838 (2)0.3251 (2)0.55428 (14)0.0799 (7)
C35A0.1959 (2)0.4225 (2)0.54290 (13)0.0784 (7)
C36A0.18118 (17)0.48019 (17)0.47472 (11)0.0613 (5)
C41A0.14497 (15)0.64019 (14)0.31843 (11)0.0501 (4)
C42A0.2221 (2)0.73561 (16)0.26823 (14)0.0699 (6)
C43A0.2283 (3)0.8292 (2)0.26712 (18)0.0922 (9)
C44A0.1594 (3)0.8296 (2)0.3151 (2)0.0937 (9)
C45A0.0825 (2)0.7373 (3)0.3656 (2)0.0997 (10)
C46A0.07521 (19)0.6433 (2)0.36637 (17)0.0805 (7)
C51A0.18702 (14)0.30000 (14)0.38685 (10)0.0452 (4)
C52A0.19497 (19)0.21731 (18)0.44886 (12)0.0667 (6)
C53A0.2716 (2)0.1721 (2)0.51145 (14)0.0880 (8)
C54A0.3416 (2)0.2094 (3)0.51427 (16)0.0954 (9)
C55A0.3345 (2)0.2916 (3)0.45519 (18)0.0931 (9)
C56A0.25877 (18)0.33666 (19)0.39094 (13)0.0667 (6)
C61A0.14572 (14)0.40720 (13)0.21583 (10)0.0428 (4)
C62A0.24038 (15)0.34197 (15)0.19480 (11)0.0534 (5)
C63A0.28403 (18)0.38056 (19)0.13500 (12)0.0655 (6)
C64A0.2350 (2)0.4853 (2)0.09420 (13)0.0707 (6)
C65A0.1424 (2)0.55220 (18)0.11311 (13)0.0713 (6)
C66A0.09807 (17)0.51370 (15)0.17336 (12)0.0568 (5)
C11B0.16849 (14)0.17588 (14)0.13594 (10)0.0431 (4)
C12B0.2055 (3)0.2623 (2)0.07157 (14)0.0976 (10)
C13B0.2701 (3)0.2735 (3)0.01125 (17)0.1393 (17)
C14B0.3012 (3)0.2022 (3)0.01472 (15)0.1030 (11)
C15B0.2649 (2)0.1144 (2)0.07748 (16)0.0856 (8)
C16B0.20009 (19)0.10159 (18)0.13850 (14)0.0691 (6)
C21B0.11381 (14)0.10753 (13)0.30860 (10)0.0413 (4)
C22B0.21299 (17)0.16967 (17)0.32513 (12)0.0622 (6)
C23B0.24637 (19)0.13990 (19)0.39395 (13)0.0705 (6)
C24B0.1821 (2)0.04757 (19)0.44788 (12)0.0705 (6)
C25B0.0848 (2)0.0160 (2)0.43357 (15)0.1070 (11)
C26B0.0502 (2)0.01271 (18)0.36483 (13)0.0833 (8)
C31B0.14038 (15)0.07032 (13)0.07919 (10)0.0447 (4)
C32B0.05654 (19)0.08463 (19)0.03146 (12)0.0653 (6)
C33B0.0422 (2)0.1334 (2)0.04631 (13)0.0794 (7)
C34B0.1125 (2)0.16736 (19)0.07809 (12)0.0758 (7)
C35B0.1952 (2)0.15487 (18)0.03319 (13)0.0702 (6)
C36B0.20868 (17)0.10732 (16)0.04497 (11)0.0572 (5)
C41B0.18565 (14)0.13460 (13)0.20550 (9)0.0424 (4)
C42B0.11069 (17)0.16837 (15)0.22626 (11)0.0537 (5)
C43B0.1345 (2)0.27125 (18)0.23927 (13)0.0685 (6)
C44B0.2334 (2)0.34217 (17)0.23230 (14)0.0737 (7)
C45B0.3098 (2)0.31232 (18)0.21287 (18)0.0926 (9)
C46B0.28572 (18)0.20889 (17)0.19972 (16)0.0763 (7)
C51B0.40153 (13)0.04417 (12)0.29025 (10)0.0416 (4)
C52B0.43255 (17)0.06786 (16)0.34878 (12)0.0599 (5)
C53B0.5081 (2)0.1019 (2)0.34176 (16)0.0785 (7)
C54B0.55305 (19)0.11414 (18)0.27655 (17)0.0763 (7)
C55B0.52334 (18)0.09292 (18)0.21826 (14)0.0689 (6)
C56B0.44805 (16)0.05826 (15)0.22482 (11)0.0535 (5)
C61B0.39011 (14)0.15617 (13)0.35743 (9)0.0406 (4)
C62B0.35785 (17)0.21069 (15)0.41777 (12)0.0612 (5)
C63B0.4203 (2)0.31738 (17)0.45463 (14)0.0745 (7)
C64B0.51559 (18)0.37158 (16)0.43196 (14)0.0677 (6)
C65B0.55036 (18)0.32093 (16)0.37351 (13)0.0666 (6)
C66B0.48829 (16)0.21326 (15)0.33675 (11)0.0537 (5)
H1A0.17200.49220.12300.076*
H4A0.03910.26760.26120.076*
H1B0.12200.30880.18930.071*
H4B0.18510.09650.33870.075*
H10.02210.34960.08680.070*
H20.14130.34800.00390.074*
H12A0.40060.45690.12420.087*
H13A0.51100.38400.15960.113*
H14A0.56000.36130.27840.102*
H15A0.49270.40440.36380.093*
H16A0.37750.47440.33010.070*
H22A0.31650.64090.02530.069*
H23A0.41670.80820.05950.090*
H24A0.53380.93940.01850.089*
H25A0.54910.90540.10790.090*
H26A0.44730.73900.19390.072*
H32A0.12110.31000.39120.076*
H33A0.14640.21660.50550.090*
H34A0.19480.28740.60020.096*
H35A0.21440.45050.58170.094*
H36A0.19030.54660.46810.074*
H42A0.27040.73680.23480.084*
H43A0.28050.89230.23290.111*
H44A0.16420.89280.31390.112*
H45A0.03540.73740.39920.120*
H46A0.02180.58070.40020.097*
H52A0.14730.19160.44820.080*
H53A0.27570.11600.55200.106*
H54A0.39370.17850.55640.114*
H55A0.38080.31830.45760.112*
H56A0.25630.39190.35040.080*
H62A0.27480.27040.22200.064*
H63A0.34710.33520.12230.079*
H64A0.26440.51120.05350.085*
H65A0.10930.62360.08550.086*
H66A0.03520.55990.18570.068*
H12B0.18720.31430.06810.117*
H13B0.29220.33200.03260.167*
H14B0.34700.21260.02530.124*
H15B0.28360.06290.07960.103*
H16B0.17750.04230.18180.083*
H22B0.25870.23380.28850.075*
H23B0.31340.18380.40300.085*
H24B0.20400.02750.49450.085*
H25B0.04060.08020.47070.128*
H26B0.01670.03240.35640.100*
H32B0.00930.06080.05240.078*
H33B0.01480.14320.07700.095*
H34B0.10370.19900.13040.091*
H35B0.24240.17820.05490.084*
H36B0.26470.10010.07510.069*
H42B0.04280.12090.23160.064*
H43B0.08270.29180.25280.082*
H44B0.24900.41100.24080.088*
H45B0.37770.36080.20840.111*
H46B0.33840.18930.18670.092*
H52B0.40200.06060.39310.072*
H53B0.52850.11660.38160.094*
H54B0.60390.13700.27220.092*
H55B0.55360.10160.17390.083*
H56B0.42830.04420.18450.064*
H62B0.29310.17480.43370.073*
H63B0.39730.35240.49500.089*
H64B0.55680.44350.45670.081*
H65B0.61520.35790.35810.080*
H66B0.51310.17880.29740.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si1A0.0343 (2)0.0294 (2)0.0421 (3)0.01229 (19)0.00732 (19)0.00781 (19)
Si2A0.0321 (2)0.0342 (2)0.0501 (3)0.01130 (19)0.0040 (2)0.0120 (2)
Si3A0.0322 (2)0.0333 (2)0.0501 (3)0.01246 (19)0.00212 (19)0.0163 (2)
Si1B0.0342 (2)0.0296 (2)0.0413 (2)0.01478 (19)0.00224 (18)0.00971 (18)
Si2B0.0366 (2)0.0321 (2)0.0378 (2)0.01360 (19)0.00205 (18)0.00969 (18)
Si3B0.0371 (2)0.0307 (2)0.0375 (2)0.01358 (19)0.00303 (18)0.00918 (18)
O1A0.0522 (8)0.0329 (6)0.0609 (8)0.0174 (6)0.0221 (6)0.0135 (6)
O2A0.0411 (7)0.0429 (7)0.0500 (7)0.0167 (6)0.0003 (5)0.0104 (6)
O3A0.0378 (7)0.0474 (8)0.0787 (10)0.0108 (6)0.0120 (6)0.0235 (7)
O4A0.0475 (7)0.0358 (6)0.0654 (9)0.0178 (6)0.0102 (6)0.0144 (6)
O1B0.0445 (7)0.0332 (6)0.0593 (8)0.0185 (5)0.0068 (6)0.0096 (6)
O2B0.0393 (6)0.0391 (6)0.0517 (7)0.0112 (5)0.0059 (5)0.0133 (5)
O3B0.0432 (7)0.0444 (7)0.0410 (6)0.0217 (6)0.0013 (5)0.0114 (5)
O4B0.0530 (8)0.0388 (7)0.0470 (7)0.0143 (6)0.0126 (6)0.0131 (6)
N10.0517 (10)0.0639 (11)0.0544 (10)0.0295 (9)0.0172 (8)0.0192 (8)
C10.0580 (12)0.0554 (12)0.0560 (12)0.0287 (10)0.0123 (10)0.0085 (9)
C20.0544 (12)0.0536 (12)0.0685 (14)0.0207 (10)0.0179 (10)0.0203 (10)
C11A0.0391 (9)0.0345 (9)0.0549 (11)0.0168 (8)0.0062 (8)0.0088 (8)
C12A0.0747 (15)0.0818 (16)0.0751 (15)0.0502 (14)0.0083 (12)0.0245 (13)
C13A0.093 (2)0.105 (2)0.118 (2)0.0729 (19)0.0130 (18)0.0402 (19)
C14A0.0599 (15)0.0601 (15)0.135 (3)0.0382 (12)0.0172 (16)0.0165 (16)
C15A0.0689 (15)0.0665 (15)0.0890 (18)0.0368 (13)0.0329 (13)0.0098 (13)
C16A0.0572 (12)0.0545 (12)0.0627 (13)0.0299 (10)0.0186 (10)0.0138 (10)
C21A0.0386 (9)0.0336 (8)0.0448 (9)0.0169 (7)0.0029 (7)0.0093 (7)
C22A0.0577 (12)0.0540 (12)0.0475 (11)0.0208 (10)0.0056 (9)0.0085 (9)
C23A0.0838 (17)0.0657 (15)0.0525 (13)0.0346 (14)0.0080 (11)0.0073 (11)
C24A0.0752 (16)0.0389 (11)0.0847 (17)0.0262 (11)0.0271 (13)0.0098 (11)
C25A0.0696 (15)0.0378 (11)0.0955 (19)0.0086 (10)0.0104 (13)0.0223 (12)
C26A0.0582 (12)0.0418 (10)0.0586 (12)0.0083 (9)0.0014 (10)0.0162 (9)
C31A0.0387 (9)0.0452 (10)0.0517 (11)0.0160 (8)0.0017 (8)0.0087 (8)
C32A0.0644 (13)0.0549 (12)0.0691 (14)0.0306 (11)0.0101 (11)0.0164 (11)
C33A0.0785 (16)0.0587 (14)0.0827 (17)0.0407 (13)0.0002 (13)0.0033 (12)
C34A0.0883 (18)0.0906 (19)0.0528 (13)0.0528 (16)0.0031 (12)0.0020 (13)
C35A0.0922 (18)0.0918 (19)0.0480 (13)0.0463 (16)0.0047 (12)0.0159 (12)
C36A0.0654 (13)0.0569 (12)0.0512 (12)0.0243 (11)0.0002 (10)0.0129 (10)
C41A0.0434 (10)0.0439 (10)0.0659 (12)0.0218 (8)0.0159 (9)0.0218 (9)
C42A0.0783 (16)0.0424 (11)0.0789 (15)0.0245 (11)0.0043 (12)0.0148 (11)
C43A0.114 (2)0.0453 (13)0.104 (2)0.0328 (15)0.0200 (18)0.0185 (13)
C44A0.110 (2)0.0693 (18)0.138 (3)0.0589 (18)0.052 (2)0.0576 (19)
C45A0.0852 (19)0.099 (2)0.158 (3)0.0592 (19)0.023 (2)0.074 (2)
C46A0.0566 (14)0.0658 (15)0.124 (2)0.0269 (12)0.0001 (14)0.0421 (15)
C51A0.0427 (10)0.0479 (10)0.0473 (10)0.0187 (8)0.0059 (8)0.0238 (8)
C52A0.0769 (15)0.0723 (15)0.0522 (12)0.0391 (13)0.0043 (11)0.0175 (11)
C53A0.108 (2)0.0908 (19)0.0518 (14)0.0416 (17)0.0107 (13)0.0153 (13)
C54A0.090 (2)0.110 (2)0.0689 (17)0.0287 (18)0.0239 (15)0.0365 (17)
C55A0.0821 (19)0.124 (3)0.097 (2)0.0584 (19)0.0083 (16)0.051 (2)
C56A0.0689 (14)0.0775 (15)0.0683 (14)0.0444 (13)0.0002 (11)0.0280 (12)
C61A0.0404 (9)0.0385 (9)0.0471 (10)0.0165 (8)0.0012 (7)0.0151 (8)
C62A0.0491 (11)0.0467 (11)0.0512 (11)0.0151 (9)0.0051 (9)0.0125 (9)
C63A0.0573 (13)0.0741 (15)0.0586 (13)0.0269 (12)0.0128 (10)0.0220 (11)
C64A0.0848 (17)0.0811 (17)0.0573 (13)0.0528 (15)0.0158 (12)0.0173 (12)
C65A0.0905 (18)0.0493 (12)0.0698 (15)0.0382 (13)0.0017 (13)0.0071 (11)
C66A0.0586 (12)0.0395 (10)0.0666 (13)0.0200 (9)0.0058 (10)0.0163 (9)
C11B0.0428 (9)0.0456 (10)0.0451 (10)0.0244 (8)0.0042 (7)0.0153 (8)
C12B0.145 (3)0.0882 (18)0.0668 (15)0.086 (2)0.0401 (16)0.0164 (13)
C13B0.213 (4)0.138 (3)0.0772 (19)0.134 (3)0.069 (2)0.0331 (18)
C14B0.134 (3)0.139 (3)0.0635 (16)0.100 (2)0.0204 (16)0.0136 (17)
C15B0.100 (2)0.099 (2)0.0944 (19)0.0744 (18)0.0001 (15)0.0348 (16)
C16B0.0727 (15)0.0646 (14)0.0756 (15)0.0447 (12)0.0091 (12)0.0113 (11)
C21B0.0441 (9)0.0367 (9)0.0424 (9)0.0199 (8)0.0039 (7)0.0117 (7)
C22B0.0521 (12)0.0526 (12)0.0554 (12)0.0126 (10)0.0100 (9)0.0053 (9)
C23B0.0631 (14)0.0714 (15)0.0655 (14)0.0251 (12)0.0261 (11)0.0212 (12)
C24B0.0877 (17)0.0691 (15)0.0515 (12)0.0402 (14)0.0241 (12)0.0133 (11)
C25B0.104 (2)0.0721 (17)0.0677 (16)0.0063 (16)0.0244 (16)0.0157 (13)
C26B0.0698 (15)0.0587 (14)0.0617 (14)0.0011 (12)0.0199 (12)0.0035 (11)
C31B0.0499 (10)0.0369 (9)0.0405 (9)0.0170 (8)0.0028 (8)0.0104 (7)
C32B0.0725 (14)0.0814 (16)0.0478 (11)0.0436 (13)0.0031 (10)0.0185 (11)
C33B0.0908 (18)0.0956 (19)0.0463 (12)0.0422 (16)0.0054 (12)0.0206 (12)
C34B0.1003 (19)0.0684 (15)0.0410 (11)0.0321 (14)0.0078 (12)0.0096 (10)
C35B0.0861 (17)0.0628 (14)0.0553 (13)0.0378 (13)0.0179 (12)0.0093 (11)
C36B0.0619 (13)0.0525 (11)0.0516 (11)0.0286 (10)0.0046 (9)0.0087 (9)
C41B0.0455 (10)0.0355 (9)0.0401 (9)0.0157 (8)0.0001 (7)0.0104 (7)
C42B0.0558 (11)0.0448 (10)0.0583 (12)0.0243 (9)0.0063 (9)0.0145 (9)
C43B0.0884 (17)0.0576 (13)0.0679 (14)0.0467 (13)0.0029 (12)0.0127 (11)
C44B0.0979 (19)0.0391 (11)0.0750 (15)0.0273 (13)0.0045 (13)0.0156 (10)
C45B0.0779 (18)0.0434 (13)0.141 (3)0.0120 (12)0.0135 (17)0.0388 (15)
C46B0.0557 (13)0.0474 (12)0.121 (2)0.0188 (11)0.0170 (13)0.0319 (13)
C51B0.0410 (9)0.0292 (8)0.0475 (10)0.0133 (7)0.0007 (7)0.0094 (7)
C52B0.0617 (13)0.0610 (13)0.0621 (13)0.0309 (11)0.0014 (10)0.0247 (10)
C53B0.0789 (17)0.0796 (17)0.0955 (19)0.0478 (14)0.0044 (14)0.0367 (15)
C54B0.0614 (14)0.0613 (14)0.112 (2)0.0395 (12)0.0015 (14)0.0201 (14)
C55B0.0619 (14)0.0626 (14)0.0776 (15)0.0355 (12)0.0133 (11)0.0095 (12)
C56B0.0534 (11)0.0510 (11)0.0560 (11)0.0280 (10)0.0057 (9)0.0133 (9)
C61B0.0417 (9)0.0338 (8)0.0419 (9)0.0157 (7)0.0002 (7)0.0110 (7)
C62B0.0542 (12)0.0437 (11)0.0710 (14)0.0198 (9)0.0155 (10)0.0073 (10)
C63B0.0732 (15)0.0464 (12)0.0811 (16)0.0284 (12)0.0092 (13)0.0066 (11)
C64B0.0629 (14)0.0335 (10)0.0843 (16)0.0142 (10)0.0101 (12)0.0051 (10)
C65B0.0545 (12)0.0422 (11)0.0813 (15)0.0067 (10)0.0071 (11)0.0198 (11)
C66B0.0534 (11)0.0427 (10)0.0518 (11)0.0148 (9)0.0102 (9)0.0129 (9)
Geometric parameters (Å, º) top
Si1A—O2A1.611 (2)C45A—C46A1.387 (4)
Si1A—O1A1.629 (2)C51A—C52A1.385 (3)
Si1A—C11A1.8504 (18)C51A—C56A1.386 (3)
Si1A—C21A1.8630 (17)C52A—C53A1.375 (3)
Si2A—O3A1.613 (2)C53A—C54A1.366 (4)
Si2A—O2A1.626 (2)C54A—C55A1.355 (4)
Si2A—C31A1.853 (2)C55A—C56A1.391 (3)
Si2A—C41A1.8576 (19)C61A—C66A1.392 (2)
Si3A—O3A1.616 (2)C61A—C62A1.397 (2)
Si3A—O4A1.631 (2)C62A—C63A1.374 (3)
Si3A—C51A1.8519 (18)C63A—C64A1.364 (3)
Si3A—C61A1.8542 (19)C64A—C65A1.369 (3)
Si1B—O2B1.618 (2)C65A—C66A1.386 (3)
Si1B—O1B1.635 (2)C11B—C12B1.366 (3)
Si1B—C21B1.8536 (18)C11B—C16B1.390 (3)
Si1B—C11B1.8559 (18)C12B—C13B1.388 (3)
Si2B—O2B1.618 (2)C13B—C14B1.337 (4)
Si2B—O3B1.628 (2)C14B—C15B1.361 (4)
Si2B—C41B1.8553 (18)C15B—C16B1.391 (3)
Si2B—C31B1.8607 (18)C21B—C26B1.380 (3)
Si3B—O4B1.619 (2)C21B—C22B1.386 (3)
Si3B—O3B1.635 (2)C22B—C23B1.380 (3)
Si3B—C61B1.8558 (17)C23B—C24B1.344 (3)
Si3B—C51B1.8587 (18)C24B—C25B1.357 (3)
N1—C11.321 (3)C25B—C26B1.384 (3)
N1—C2i1.326 (3)C31B—C36B1.390 (3)
C1—C21.372 (3)C31B—C32B1.397 (3)
C11A—C16A1.382 (3)C32B—C33B1.384 (3)
C11A—C12A1.381 (3)C33B—C34B1.374 (4)
C12A—C13A1.378 (3)C34B—C35B1.364 (3)
C13A—C14A1.360 (4)C35B—C36B1.389 (3)
C14A—C15A1.356 (4)C41B—C46B1.382 (3)
C15A—C16A1.398 (3)C41B—C42B1.387 (3)
C21A—C26A1.384 (3)C42B—C43B1.386 (3)
C21A—C22A1.385 (3)C43B—C44B1.359 (3)
C22A—C23A1.381 (3)C44B—C45B1.365 (4)
C23A—C24A1.358 (4)C45B—C46B1.393 (3)
C24A—C25A1.359 (3)C51B—C56B1.387 (3)
C25A—C26A1.383 (3)C51B—C52B1.395 (3)
C31A—C36A1.390 (3)C52B—C53B1.384 (3)
C31A—C32A1.402 (3)C53B—C54B1.369 (4)
C32A—C33A1.382 (3)C54B—C55B1.358 (3)
C33A—C34A1.364 (4)C55B—C56B1.387 (3)
C34A—C35A1.364 (4)C61B—C62B1.389 (3)
C35A—C36A1.383 (3)C61B—C66B1.390 (2)
C41A—C46A1.379 (3)C62B—C63B1.383 (3)
C41A—C42A1.387 (3)C63B—C64B1.367 (3)
C42A—C43A1.387 (3)C64B—C65B1.359 (3)
C43A—C44A1.347 (4)C65B—C66B1.393 (3)
C44A—C45A1.366 (4)
O2A—Si1A—O1A112.36 (7)C43A—C42A—C41A121.1 (2)
O2A—Si1A—C11A110.14 (8)C44A—C43A—C42A120.6 (3)
O1A—Si1A—C11A105.84 (8)C43A—C44A—C45A120.1 (2)
O2A—Si1A—C21A108.42 (7)C44A—C45A—C46A119.5 (3)
O1A—Si1A—C21A109.26 (7)C41A—C46A—C45A121.9 (3)
C11A—Si1A—C21A110.82 (8)C52A—C51A—C56A117.07 (19)
O3A—Si2A—O2A108.61 (7)C52A—C51A—Si3A121.34 (15)
O3A—Si2A—C31A109.60 (8)C56A—C51A—Si3A121.37 (16)
O2A—Si2A—C31A108.07 (8)C53A—C52A—C51A121.7 (2)
O3A—Si2A—C41A109.97 (8)C54A—C53A—C52A120.2 (3)
O2A—Si2A—C41A107.80 (8)C55A—C54A—C53A119.5 (2)
C31A—Si2A—C41A112.68 (9)C54A—C55A—C56A120.9 (3)
O3A—Si3A—O4A110.21 (7)C51A—C56A—C55A120.6 (2)
O3A—Si3A—C51A114.40 (8)C66A—C61A—C62A116.55 (18)
O4A—Si3A—C51A104.14 (8)C66A—C61A—Si3A123.47 (15)
O3A—Si3A—C61A106.48 (8)C62A—C61A—Si3A119.93 (13)
O4A—Si3A—C61A111.81 (8)C63A—C62A—C61A121.87 (19)
C51A—Si3A—C61A109.93 (8)C64A—C63A—C62A120.1 (2)
O2B—Si1B—O1B105.69 (7)C63A—C64A—C65A120.0 (2)
O2B—Si1B—C21B107.39 (7)C64A—C65A—C66A120.1 (2)
O1B—Si1B—C21B111.50 (7)C65A—C66A—C61A121.3 (2)
O2B—Si1B—C11B110.77 (7)C12B—C11B—C16B116.96 (19)
O1B—Si1B—C11B109.76 (7)C12B—C11B—Si1B122.83 (15)
C21B—Si1B—C11B111.55 (8)C16B—C11B—Si1B120.10 (15)
O2B—Si2B—O3B110.70 (7)C11B—C12B—C13B121.0 (2)
O2B—Si2B—C41B106.89 (8)C14B—C13B—C12B121.5 (3)
O3B—Si2B—C41B110.81 (7)C13B—C14B—C15B119.3 (2)
O2B—Si2B—C31B110.26 (7)C14B—C15B—C16B120.0 (2)
O3B—Si2B—C31B107.04 (8)C11B—C16B—C15B121.2 (2)
C41B—Si2B—C31B111.19 (8)C26B—C21B—C22B116.05 (17)
O4B—Si3B—O3B111.82 (7)C26B—C21B—Si1B123.43 (15)
O4B—Si3B—C61B106.50 (7)C22B—C21B—Si1B120.51 (14)
O3B—Si3B—C61B110.42 (7)C23B—C22B—C21B122.44 (19)
O4B—Si3B—C51B112.47 (8)C24B—C23B—C22B120.1 (2)
O3B—Si3B—C51B107.51 (7)C23B—C24B—C25B119.3 (2)
C61B—Si3B—C51B108.07 (8)C24B—C25B—C26B121.3 (2)
Si1A—O2A—Si2A157.1 (1)C21B—C26B—C25B120.8 (2)
Si2A—O3A—Si3A164.0 (1)C36B—C31B—C32B116.95 (17)
Si2B—O2B—Si1B157.9 (1)C36B—C31B—Si2B123.66 (15)
Si2B—O3B—Si3B141.2 (1)C32B—C31B—Si2B119.39 (15)
C1—N1—C2i116.3 (2)C33B—C32B—C31B121.5 (2)
N1—C1—C2121.9 (2)C34B—C33B—C32B119.8 (2)
N1—C2—C1i121.9 (2)C35B—C34B—C33B120.3 (2)
C16A—C11A—C12A117.16 (19)C34B—C35B—C36B119.9 (2)
C16A—C11A—Si1A123.74 (15)C35B—C36B—C31B121.5 (2)
C12A—C11A—Si1A119.08 (15)C46B—C41B—C42B116.77 (18)
C13A—C12A—C11A121.9 (2)C46B—C41B—Si2B120.08 (15)
C14A—C13A—C12A120.0 (3)C42B—C41B—Si2B123.13 (14)
C15A—C14A—C13A119.9 (2)C43B—C42B—C41B121.5 (2)
C14A—C15A—C16A120.4 (2)C44B—C43B—C42B120.3 (2)
C11A—C16A—C15A120.6 (2)C43B—C44B—C45B120.0 (2)
C26A—C21A—C22A116.87 (17)C44B—C45B—C46B119.7 (2)
C26A—C21A—Si1A121.14 (14)C41B—C46B—C45B121.7 (2)
C22A—C21A—Si1A121.98 (14)C56B—C51B—C52B117.13 (18)
C23A—C22A—C21A121.4 (2)C56B—C51B—Si3B123.60 (14)
C24A—C23A—C22A120.2 (2)C52B—C51B—Si3B119.10 (15)
C23A—C24A—C25A120.0 (2)C53B—C52B—C51B120.9 (2)
C24A—C25A—C26A120.0 (2)C54B—C53B—C52B120.3 (2)
C25A—C26A—C21A121.5 (2)C55B—C54B—C53B120.0 (2)
C36A—C31A—C32A117.09 (19)C54B—C55B—C56B120.1 (2)
C36A—C31A—Si2A123.36 (16)C51B—C56B—C55B121.5 (2)
C32A—C31A—Si2A119.50 (16)C62B—C61B—C66B117.06 (16)
C33A—C32A—C31A121.1 (2)C62B—C61B—Si3B122.90 (14)
C34A—C33A—C32A120.4 (2)C66B—C61B—Si3B120.03 (14)
C33A—C34A—C35A119.5 (2)C63B—C62B—C61B121.2 (2)
C34A—C35A—C36A121.1 (2)C64B—C63B—C62B120.3 (2)
C35A—C36A—C31A120.7 (2)C65B—C64B—C63B120.32 (19)
C46A—C41A—C42A116.8 (2)C64B—C65B—C66B119.6 (2)
C46A—C41A—Si2A121.74 (16)C61B—C66B—C65B121.55 (19)
C42A—C41A—Si2A121.43 (16)
O1A—Si1A—O2A—Si2A5.7 (2)C51A—Si3A—C61A—C66A112.37 (16)
C11A—Si1A—O2A—Si2A112.0 (2)O3A—Si3A—C61A—C62A170.53 (14)
C21A—Si1A—O2A—Si2A126.6 (2)O4A—Si3A—C61A—C62A50.11 (16)
O3A—Si2A—O2A—Si1A8.9 (2)C51A—Si3A—C61A—C62A65.03 (16)
C31A—Si2A—O2A—Si1A110.0 (2)C66A—C61A—C62A—C63A0.4 (3)
C41A—Si2A—O2A—Si1A128.0 (2)Si3A—C61A—C62A—C63A177.99 (17)
O2A—Si2A—O3A—Si3A129.5 (4)C61A—C62A—C63A—C64A0.0 (3)
C31A—Si2A—O3A—Si3A11.7 (4)C62A—C63A—C64A—C65A0.4 (4)
C41A—Si2A—O3A—Si3A112.7 (4)C63A—C64A—C65A—C66A0.4 (4)
O4A—Si3A—O3A—Si2A78.0 (4)C64A—C65A—C66A—C61A0.0 (3)
C51A—Si3A—O3A—Si2A39.0 (4)C62A—C61A—C66A—C65A0.4 (3)
C61A—Si3A—O3A—Si2A160.6 (4)Si3A—C61A—C66A—C65A177.89 (17)
O3B—Si2B—O2B—Si1B105.7 (2)O2B—Si1B—C11B—C12B105.0 (2)
C41B—Si2B—O2B—Si1B133.6 (2)O1B—Si1B—C11B—C12B11.4 (2)
C31B—Si2B—O2B—Si1B12.6 (3)C21B—Si1B—C11B—C12B135.5 (2)
O1B—Si1B—O2B—Si2B60.6 (3)O2B—Si1B—C11B—C16B71.12 (18)
C21B—Si1B—O2B—Si2B179.7 (2)O1B—Si1B—C11B—C16B172.54 (17)
C11B—Si1B—O2B—Si2B58.3 (3)C21B—Si1B—C11B—C16B48.45 (19)
O2B—Si2B—O3B—Si3B49.6 (2)C16B—C11B—C12B—C13B1.2 (5)
C41B—Si2B—O3B—Si3B68.80 (14)Si1B—C11B—C12B—C13B175.0 (3)
C31B—Si2B—O3B—Si3B169.81 (12)C11B—C12B—C13B—C14B2.1 (6)
O4B—Si3B—O3B—Si2B44.7 (2)C12B—C13B—C14B—C15B2.9 (7)
C61B—Si3B—O3B—Si2B73.71 (14)C13B—C14B—C15B—C16B2.8 (5)
C51B—Si3B—O3B—Si2B168.61 (12)C12B—C11B—C16B—C15B1.1 (4)
O2A—Si1A—C11A—C16A11.88 (18)Si1B—C11B—C16B—C15B175.2 (2)
O1A—Si1A—C11A—C16A133.57 (16)C14B—C15B—C16B—C11B1.9 (4)
C21A—Si1A—C11A—C16A108.09 (17)O2B—Si1B—C21B—C26B1.1 (2)
O2A—Si1A—C11A—C12A169.91 (16)O1B—Si1B—C21B—C26B116.4 (2)
O1A—Si1A—C11A—C12A48.22 (18)C11B—Si1B—C21B—C26B120.5 (2)
C21A—Si1A—C11A—C12A70.12 (18)O2B—Si1B—C21B—C22B179.94 (16)
C16A—C11A—C12A—C13A0.0 (3)O1B—Si1B—C21B—C22B64.60 (18)
Si1A—C11A—C12A—C13A178.3 (2)C11B—Si1B—C21B—C22B58.51 (18)
C11A—C12A—C13A—C14A1.2 (4)C26B—C21B—C22B—C23B0.9 (3)
C12A—C13A—C14A—C15A1.5 (4)Si1B—C21B—C22B—C23B179.95 (19)
C13A—C14A—C15A—C16A0.6 (4)C21B—C22B—C23B—C24B0.2 (4)
C12A—C11A—C16A—C15A0.9 (3)C22B—C23B—C24B—C25B0.6 (4)
Si1A—C11A—C16A—C15A177.39 (16)C23B—C24B—C25B—C26B0.6 (5)
C14A—C15A—C16A—C11A0.6 (4)C22B—C21B—C26B—C25B0.9 (4)
O2A—Si1A—C21A—C26A49.21 (17)Si1B—C21B—C26B—C25B179.9 (2)
O1A—Si1A—C21A—C26A171.98 (16)C24B—C25B—C26B—C21B0.1 (5)
C11A—Si1A—C21A—C26A71.77 (18)O2B—Si2B—C31B—C36B125.95 (16)
O2A—Si1A—C21A—C22A131.84 (16)O3B—Si2B—C31B—C36B5.48 (18)
O1A—Si1A—C21A—C22A9.08 (18)C41B—Si2B—C31B—C36B115.67 (17)
C11A—Si1A—C21A—C22A107.17 (17)O2B—Si2B—C31B—C32B54.40 (18)
C26A—C21A—C22A—C23A0.3 (3)O3B—Si2B—C31B—C32B174.87 (15)
Si1A—C21A—C22A—C23A179.28 (18)C41B—Si2B—C31B—C32B63.97 (18)
C21A—C22A—C23A—C24A0.8 (4)C36B—C31B—C32B—C33B0.0 (3)
C22A—C23A—C24A—C25A0.7 (4)Si2B—C31B—C32B—C33B179.66 (19)
C23A—C24A—C25A—C26A0.1 (4)C31B—C32B—C33B—C34B1.0 (4)
C24A—C25A—C26A—C21A0.3 (4)C32B—C33B—C34B—C35B1.2 (4)
C22A—C21A—C26A—C25A0.3 (3)C33B—C34B—C35B—C36B0.2 (4)
Si1A—C21A—C26A—C25A178.73 (18)C34B—C35B—C36B—C31B0.9 (3)
O3A—Si2A—C31A—C36A130.85 (17)C32B—C31B—C36B—C35B1.0 (3)
O2A—Si2A—C31A—C36A110.95 (17)Si2B—C31B—C36B—C35B178.69 (16)
C41A—Si2A—C31A—C36A8.0 (2)O2B—Si2B—C41B—C46B166.26 (17)
O3A—Si2A—C31A—C32A51.93 (18)O3B—Si2B—C41B—C46B45.56 (19)
O2A—Si2A—C31A—C32A66.27 (17)C31B—Si2B—C41B—C46B73.35 (19)
C41A—Si2A—C31A—C32A174.73 (15)O2B—Si2B—C41B—C42B15.55 (17)
C36A—C31A—C32A—C33A0.1 (3)O3B—Si2B—C41B—C42B136.24 (15)
Si2A—C31A—C32A—C33A177.27 (17)C31B—Si2B—C41B—C42B104.84 (17)
C31A—C32A—C33A—C34A0.2 (4)C46B—C41B—C42B—C43B1.1 (3)
C32A—C33A—C34A—C35A0.7 (4)Si2B—C41B—C42B—C43B177.16 (16)
C33A—C34A—C35A—C36A0.8 (4)C41B—C42B—C43B—C44B0.4 (3)
C34A—C35A—C36A—C31A0.4 (4)C42B—C43B—C44B—C45B0.4 (4)
C32A—C31A—C36A—C35A0.1 (3)C43B—C44B—C45B—C46B0.5 (4)
Si2A—C31A—C36A—C35A177.23 (17)C42B—C41B—C46B—C45B1.0 (4)
O3A—Si2A—C41A—C46A64.0 (2)Si2B—C41B—C46B—C45B177.3 (2)
O2A—Si2A—C41A—C46A177.71 (18)C44B—C45B—C46B—C41B0.3 (4)
C31A—Si2A—C41A—C46A58.5 (2)O4B—Si3B—C51B—C56B149.49 (15)
O3A—Si2A—C41A—C42A116.72 (18)O3B—Si3B—C51B—C56B25.97 (17)
O2A—Si2A—C41A—C42A1.53 (19)C61B—Si3B—C51B—C56B93.23 (16)
C31A—Si2A—C41A—C42A120.69 (18)O4B—Si3B—C51B—C52B35.26 (16)
C46A—C41A—C42A—C43A0.3 (4)O3B—Si3B—C51B—C52B158.79 (14)
Si2A—C41A—C42A—C43A178.9 (2)C61B—Si3B—C51B—C52B82.02 (16)
C41A—C42A—C43A—C44A0.2 (4)C56B—C51B—C52B—C53B1.2 (3)
C42A—C43A—C44A—C45A0.0 (5)Si3B—C51B—C52B—C53B174.32 (17)
C43A—C44A—C45A—C46A0.7 (5)C51B—C52B—C53B—C54B0.7 (4)
C42A—C41A—C46A—C45A1.0 (4)C52B—C53B—C54B—C55B0.1 (4)
Si2A—C41A—C46A—C45A178.2 (2)C53B—C54B—C55B—C56B0.4 (4)
C44A—C45A—C46A—C41A1.2 (4)C52B—C51B—C56B—C55B0.9 (3)
O3A—Si3A—C51A—C52A89.11 (18)Si3B—C51B—C56B—C55B174.40 (16)
O4A—Si3A—C51A—C52A31.25 (19)C54B—C55B—C56B—C51B0.1 (3)
C61A—Si3A—C51A—C52A151.17 (17)O4B—Si3B—C61B—C62B15.78 (18)
O3A—Si3A—C51A—C56A96.52 (17)O3B—Si3B—C61B—C62B105.81 (17)
O4A—Si3A—C51A—C56A143.12 (17)C51B—Si3B—C61B—C62B136.85 (17)
C61A—Si3A—C51A—C56A23.20 (19)O4B—Si3B—C61B—C66B163.18 (15)
C56A—C51A—C52A—C53A1.0 (3)O3B—Si3B—C61B—C66B75.23 (16)
Si3A—C51A—C52A—C53A173.62 (19)C51B—Si3B—C61B—C66B42.11 (17)
C51A—C52A—C53A—C54A0.9 (4)C66B—C61B—C62B—C63B1.0 (3)
C52A—C53A—C54A—C55A0.5 (5)Si3B—C61B—C62B—C63B179.98 (18)
C53A—C54A—C55A—C56A1.7 (5)C61B—C62B—C63B—C64B0.2 (4)
C52A—C51A—C56A—C55A0.3 (3)C62B—C63B—C64B—C65B0.7 (4)
Si3A—C51A—C56A—C55A174.90 (19)C63B—C64B—C65B—C66B0.0 (4)
C54A—C55A—C56A—C51A1.7 (4)C62B—C61B—C66B—C65B1.7 (3)
O3A—Si3A—C61A—C66A12.06 (18)Si3B—C61B—C66B—C65B179.27 (17)
O4A—Si3A—C61A—C66A132.48 (16)C64B—C65B—C66B—C61B1.3 (3)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1A—H1A···N10.821.962.706 (2)150
O1B—H1B···O1A0.821.952.673 (2)146
O4A—H4A···O1B0.821.922.700 (2)157
O4B—H4B···O4A0.821.982.794 (2)174
(sila2) 1,1,3,3,5,5-Hexaphenyltrisiloxane-1,5-diol–pyridine (2/3) top
Crystal data top
2(C36H32O4Si3)·3(C5H5N)F(000) = 770
Mr = 1463.07? #Insert any comments here.
Triclinic, P1Dx = 1.234 Mg m3
a = 10.7764 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.8122 (12) ÅCell parameters from 25 reflections
c = 15.1733 (13) Åθ = 9.7–16.7°
α = 91.999 (11)°µ = 0.16 mm1
β = 94.851 (13)°T = 294 K
γ = 109.063 (7)°Block, colourless
V = 1968.6 (3) Å30.36 × 0.34 × 0.30 mm
Z = 1
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.0°
Graphite monochromatorh = 1312
θ/2θ scansk = 016
8519 measured reflectionsl = 1919
8519 independent reflections3 standard reflections every 120 min
5535 reflections with I > 2σ(I) intensity decay: 3.0%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.118 w = 1/[σ2(Fo2) + (0.0588P)2 + 0.1381P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
8519 reflectionsΔρmax = 0.34 e Å3
472 parametersΔρmin = 0.29 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0040 (7)
Special details top

Experimental. ? #Insert any special details here.

Geometry. Mean-plane data from final SHELXL refinement run:-

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si10.02261 (5)0.19241 (4)0.07874 (3)0.03513 (14)
Si20.03287 (5)0.11951 (4)0.27774 (3)0.03263 (13)
Si30.11155 (5)0.33581 (4)0.39625 (3)0.03585 (14)
O10.06094 (13)0.07789 (12)0.02119 (9)0.0493 (4)
O20.04162 (13)0.17316 (11)0.18300 (8)0.0462 (3)
O30.10524 (13)0.21363 (11)0.35638 (8)0.0432 (3)
O40.01376 (13)0.36932 (13)0.35921 (10)0.0483 (4)
C110.18849 (19)0.24721 (16)0.03933 (13)0.0395 (4)
C120.2081 (2)0.2297 (2)0.04874 (14)0.0538 (6)
C130.3291 (3)0.2757 (2)0.07990 (17)0.0676 (7)
C140.4339 (3)0.3402 (2)0.0240 (2)0.0745 (8)
C150.4199 (2)0.3593 (2)0.0630 (2)0.0726 (8)
C160.2973 (2)0.31309 (19)0.09495 (16)0.0552 (6)
C210.06858 (18)0.29232 (17)0.06399 (13)0.0407 (4)
C220.0907 (2)0.3281 (2)0.01984 (15)0.0575 (6)
C230.1562 (3)0.4040 (2)0.0324 (2)0.0746 (8)
C240.2016 (3)0.4450 (2)0.0381 (2)0.0748 (8)
C250.1817 (2)0.4117 (2)0.1205 (2)0.0716 (8)
C260.1150 (2)0.3367 (2)0.13396 (15)0.0546 (6)
C310.11714 (18)0.01450 (15)0.28134 (12)0.0368 (4)
C320.1654 (2)0.0222 (2)0.20868 (15)0.0583 (6)
C330.2199 (3)0.1059 (2)0.21429 (19)0.0725 (8)
C340.2272 (2)0.1551 (2)0.2920 (2)0.0681 (7)
C350.1820 (3)0.1203 (2)0.36493 (18)0.0669 (7)
C360.1277 (2)0.03702 (19)0.35971 (15)0.0539 (6)
C410.14281 (18)0.05439 (15)0.29744 (13)0.0376 (4)
C420.2404 (2)0.00355 (19)0.22878 (15)0.0527 (6)
C430.3691 (2)0.0495 (2)0.24485 (19)0.0697 (7)
C440.4035 (2)0.0540 (2)0.3303 (2)0.0742 (8)
C450.3098 (2)0.0052 (2)0.39944 (18)0.0649 (7)
C460.1815 (2)0.04832 (18)0.38326 (14)0.0492 (5)
C510.25739 (19)0.44002 (16)0.35667 (13)0.0405 (4)
C520.2462 (2)0.5100 (2)0.29102 (16)0.0590 (6)
C530.3555 (3)0.5823 (2)0.25863 (18)0.0747 (8)
C540.4790 (3)0.5866 (3)0.29122 (19)0.0815 (9)
C550.4935 (3)0.5208 (3)0.3563 (2)0.0897 (10)
C560.3844 (2)0.4486 (2)0.38911 (18)0.0711 (8)
C610.12489 (18)0.32885 (15)0.51849 (12)0.0374 (4)
C620.0915 (2)0.40361 (19)0.57214 (14)0.0534 (6)
C630.0987 (3)0.4004 (2)0.66322 (15)0.0625 (7)
C640.1389 (2)0.3212 (2)0.70321 (15)0.0609 (6)
C650.1735 (2)0.24595 (19)0.65260 (15)0.0560 (6)
C660.1662 (2)0.24943 (17)0.56169 (14)0.0468 (5)
N710.2711 (2)0.28949 (19)0.39229 (19)0.0741 (6)
C720.3176 (3)0.2957 (2)0.4693 (2)0.0823 (8)
C730.4493 (4)0.2525 (3)0.4809 (3)0.1019 (11)
C740.5356 (4)0.2009 (3)0.4102 (4)0.1111 (13)
C750.4904 (3)0.1931 (3)0.3316 (3)0.1031 (11)
C760.3584 (3)0.2379 (3)0.3250 (2)0.0862 (9)
N810.3582 (3)0.0318 (2)0.00099 (19)0.0942 (9)0.50
C810.3582 (3)0.0318 (2)0.00099 (19)0.0942 (9)0.50
C820.4419 (5)0.0687 (3)0.0302 (2)0.1026 (12)
C830.5773 (5)0.1005 (3)0.0301 (2)0.1144 (15)
H10.01450.03870.01730.074*0.50
H20.13980.07000.01820.074*0.50
H40.08080.32750.37700.072*
H120.13750.18560.08760.065*
H130.33940.26280.13910.081*
H140.51550.37140.04520.089*
H150.49180.40310.10100.087*
H160.28830.32650.15430.066*
H220.06100.30040.06830.069*
H230.16940.42720.08880.090*
H240.24610.49560.02950.090*
H250.21300.43930.16830.086*
H260.10100.31560.19100.066*
H320.16090.01010.15510.070*
H330.25180.12890.16470.087*
H340.26290.21210.29520.082*
H350.18790.15290.41820.080*
H360.09710.01440.41000.065*
H420.21820.00540.17080.063*
H430.43280.08240.19790.084*
H440.49040.09010.34100.089*
H450.33280.00830.45720.078*
H460.11880.08140.43070.059*
H520.16260.50810.26820.071*
H530.34490.62820.21450.090*
H540.55280.63450.26890.098*
H550.57770.52410.37910.108*
H560.39660.40470.43430.085*
H620.06340.45760.54580.064*
H630.07630.45200.69730.075*
H640.14290.31830.76450.073*
H650.20180.19260.67970.067*
H660.18940.19770.52820.056*
H720.25840.33090.51800.099*
H730.47850.25860.53610.122*
H740.62530.17130.41620.133*
H750.54810.15760.28230.124*
H760.32810.23190.27010.103*
H810.26710.05270.00160.113*0.50
H820.40640.12030.05200.123*
H830.62760.17190.05200.137*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0358 (3)0.0350 (3)0.0334 (3)0.0093 (2)0.0058 (2)0.0055 (2)
Si20.0370 (3)0.0302 (3)0.0309 (3)0.0111 (2)0.0042 (2)0.0038 (2)
Si30.0377 (3)0.0321 (3)0.0370 (3)0.0115 (2)0.0010 (2)0.0001 (2)
O10.0416 (8)0.0436 (8)0.0580 (9)0.0090 (7)0.0054 (7)0.0072 (7)
O20.0565 (9)0.0466 (9)0.0376 (7)0.0178 (7)0.0087 (6)0.0142 (6)
O30.0505 (8)0.0351 (8)0.0422 (8)0.0137 (6)0.0008 (6)0.0052 (6)
O40.0435 (8)0.0550 (9)0.0496 (8)0.0205 (7)0.0038 (7)0.0090 (7)
C110.0393 (10)0.0378 (11)0.0428 (11)0.0132 (9)0.0071 (8)0.0100 (9)
C120.0486 (12)0.0652 (15)0.0475 (13)0.0162 (11)0.0108 (10)0.0134 (11)
C130.0608 (16)0.086 (2)0.0608 (15)0.0232 (15)0.0281 (13)0.0212 (14)
C140.0538 (15)0.0747 (19)0.097 (2)0.0156 (14)0.0359 (15)0.0233 (16)
C150.0406 (13)0.0650 (17)0.101 (2)0.0029 (12)0.0055 (13)0.0000 (15)
C160.0472 (12)0.0546 (14)0.0595 (14)0.0114 (11)0.0054 (10)0.0016 (11)
C210.0349 (10)0.0410 (11)0.0442 (11)0.0111 (9)0.0013 (8)0.0044 (9)
C220.0563 (14)0.0665 (16)0.0501 (13)0.0215 (12)0.0009 (11)0.0139 (11)
C230.0619 (16)0.0750 (19)0.0824 (19)0.0191 (14)0.0148 (14)0.0354 (16)
C240.0542 (15)0.0556 (16)0.115 (3)0.0243 (13)0.0169 (16)0.0075 (16)
C250.0600 (16)0.0671 (17)0.093 (2)0.0336 (14)0.0072 (14)0.0182 (15)
C260.0546 (13)0.0619 (15)0.0523 (13)0.0284 (12)0.0016 (10)0.0020 (11)
C310.0367 (10)0.0331 (10)0.0389 (10)0.0102 (8)0.0021 (8)0.0007 (8)
C320.0718 (16)0.0692 (16)0.0462 (12)0.0401 (13)0.0071 (11)0.0007 (11)
C330.0807 (19)0.0772 (19)0.0742 (18)0.0473 (16)0.0109 (14)0.0149 (15)
C340.0626 (16)0.0526 (15)0.098 (2)0.0347 (13)0.0027 (14)0.0005 (14)
C350.0728 (17)0.0621 (16)0.0780 (18)0.0371 (14)0.0078 (14)0.0230 (14)
C360.0678 (15)0.0524 (14)0.0525 (13)0.0317 (12)0.0139 (11)0.0129 (11)
C410.0383 (10)0.0319 (10)0.0435 (11)0.0119 (8)0.0054 (8)0.0083 (8)
C420.0445 (12)0.0578 (14)0.0507 (13)0.0103 (11)0.0009 (10)0.0094 (11)
C430.0433 (13)0.0746 (18)0.0786 (18)0.0049 (12)0.0069 (12)0.0107 (14)
C440.0439 (14)0.0758 (19)0.099 (2)0.0091 (13)0.0213 (14)0.0247 (16)
C450.0588 (15)0.0701 (17)0.0677 (16)0.0175 (13)0.0266 (13)0.0189 (13)
C460.0492 (12)0.0495 (13)0.0485 (12)0.0138 (10)0.0098 (10)0.0091 (10)
C510.0442 (11)0.0349 (11)0.0401 (11)0.0108 (9)0.0015 (9)0.0009 (8)
C520.0514 (13)0.0622 (16)0.0595 (14)0.0135 (12)0.0013 (11)0.0169 (12)
C530.0727 (18)0.0783 (19)0.0634 (16)0.0078 (15)0.0114 (13)0.0323 (14)
C540.0586 (17)0.091 (2)0.0760 (19)0.0051 (15)0.0142 (14)0.0222 (16)
C550.0424 (14)0.109 (3)0.107 (2)0.0091 (15)0.0024 (14)0.038 (2)
C560.0503 (14)0.0777 (19)0.0813 (18)0.0144 (13)0.0013 (13)0.0334 (15)
C610.0381 (10)0.0323 (10)0.0398 (10)0.0097 (8)0.0022 (8)0.0017 (8)
C620.0746 (15)0.0500 (13)0.0435 (12)0.0343 (12)0.0041 (11)0.0008 (10)
C630.0836 (18)0.0706 (17)0.0433 (13)0.0415 (14)0.0004 (12)0.0052 (12)
C640.0731 (16)0.0699 (17)0.0386 (12)0.0233 (14)0.0000 (11)0.0070 (11)
C650.0677 (15)0.0483 (14)0.0522 (13)0.0206 (12)0.0024 (11)0.0153 (11)
C660.0539 (12)0.0367 (11)0.0520 (13)0.0186 (10)0.0030 (10)0.0031 (9)
N710.0574 (13)0.0603 (14)0.108 (2)0.0224 (11)0.0157 (13)0.0109 (13)
C720.087 (2)0.071 (2)0.094 (2)0.0338 (17)0.0051 (18)0.0088 (17)
C730.112 (3)0.102 (3)0.116 (3)0.054 (2)0.058 (2)0.039 (2)
C740.064 (2)0.096 (3)0.179 (4)0.025 (2)0.041 (3)0.028 (3)
C750.060 (2)0.097 (3)0.144 (3)0.0199 (18)0.005 (2)0.012 (2)
C760.075 (2)0.087 (2)0.100 (2)0.0287 (18)0.0195 (18)0.0012 (19)
N810.133 (3)0.0558 (17)0.0725 (18)0.0071 (18)0.0086 (17)0.0056 (14)
C810.133 (3)0.0558 (17)0.0725 (18)0.0071 (18)0.0086 (17)0.0056 (14)
C820.161 (4)0.058 (2)0.078 (2)0.024 (2)0.000 (2)0.0049 (16)
C830.150 (4)0.057 (2)0.085 (2)0.025 (2)0.024 (2)0.0032 (17)
Geometric parameters (Å, º) top
Si1—O21.616 (2)C35—C361.376 (3)
Si1—O11.625 (2)C41—C421.391 (3)
Si1—C111.854 (2)C41—C461.398 (3)
Si1—C211.860 (2)C42—C431.378 (3)
Si2—O21.612 (2)C43—C441.376 (4)
Si2—O31.617 (2)C44—C451.370 (4)
Si2—C311.853 (2)C45—C461.375 (3)
Si2—C411.8577 (19)C51—C561.382 (3)
Si3—O41.610 (2)C51—C521.387 (3)
Si3—O31.637 (2)C52—C531.380 (3)
Si3—C611.8557 (19)C53—C541.363 (4)
Si3—C511.860 (2)C54—C551.352 (4)
C11—C161.392 (3)C55—C561.381 (3)
C11—C121.393 (3)C61—C621.389 (3)
C12—C131.376 (3)C61—C661.399 (3)
C13—C141.363 (4)C62—C631.380 (3)
C14—C151.364 (4)C63—C641.368 (3)
C15—C161.395 (3)C64—C651.374 (3)
C21—C261.391 (3)C65—C661.378 (3)
C21—C221.395 (3)N71—C721.319 (4)
C22—C231.386 (4)N71—C761.323 (4)
C23—C241.369 (4)C72—C731.374 (4)
C24—C251.359 (4)C73—C741.353 (5)
C25—C261.385 (3)C74—C751.339 (5)
C31—C321.388 (3)C75—C761.363 (4)
C31—C361.394 (3)N81—C83i1.382 (5)
C32—C331.382 (3)C82—C831.381 (5)
C33—C341.365 (4)C83—C81i1.382 (5)
C34—C351.363 (4)
O2—Si1—O1111.66 (8)C36—C31—Si2119.38 (15)
O2—Si1—C11108.06 (8)C33—C32—C31121.4 (2)
O1—Si1—C11108.93 (8)C34—C33—C32120.5 (2)
O2—Si1—C21108.90 (8)C35—C34—C33119.7 (2)
O1—Si1—C21108.41 (8)C34—C35—C36120.1 (2)
C11—Si1—C21110.89 (9)C35—C36—C31122.0 (2)
O2—Si2—O3110.39 (8)C42—C41—C46116.81 (19)
O2—Si2—C31110.36 (8)C42—C41—Si2122.00 (15)
O3—Si2—C31107.60 (8)C46—C41—Si2121.07 (15)
O2—Si2—C41109.77 (8)C43—C42—C41121.4 (2)
O3—Si2—C41108.93 (8)C44—C43—C42120.2 (2)
C31—Si2—C41109.76 (8)C45—C44—C43119.9 (2)
O4—Si3—O3112.66 (8)C44—C45—C46119.9 (2)
O4—Si3—C61112.55 (8)C45—C46—C41121.8 (2)
O3—Si3—C61105.34 (8)C56—C51—C52116.1 (2)
O4—Si3—C51105.53 (9)C56—C51—Si3121.23 (17)
O3—Si3—C51107.75 (8)C52—C51—Si3122.59 (16)
C61—Si3—C51113.05 (9)C53—C52—C51121.9 (2)
Si2—O2—Si1163.8 (1)C54—C53—C52120.1 (2)
Si2—O3—Si3142.5 (1)C55—C54—C53119.6 (2)
C16—C11—C12116.94 (19)C54—C55—C56120.5 (3)
C16—C11—Si1121.60 (16)C55—C56—C51121.8 (2)
C12—C11—Si1121.35 (16)C62—C61—C66116.40 (18)
C13—C12—C11121.8 (2)C62—C61—Si3120.40 (15)
C14—C13—C12120.0 (2)C66—C61—Si3123.20 (15)
C13—C14—C15120.5 (2)C63—C62—C61122.2 (2)
C14—C15—C16119.8 (2)C64—C63—C62119.9 (2)
C11—C16—C15121.0 (2)C63—C64—C65119.8 (2)
C26—C21—C22116.8 (2)C64—C65—C66120.1 (2)
C26—C21—Si1123.01 (16)C65—C66—C61121.6 (2)
C22—C21—Si1120.15 (17)C72—N71—C76116.5 (3)
C23—C22—C21121.3 (2)N71—C72—C73123.0 (3)
C24—C23—C22120.2 (2)C74—C73—C72118.7 (3)
C25—C24—C23119.9 (2)C75—C74—C73119.3 (3)
C24—C25—C26120.4 (3)C74—C75—C76118.9 (4)
C25—C26—C21121.4 (2)N71—C76—C75123.7 (3)
C32—C31—C36116.35 (19)C82—C83—C81i123.4 (3)
C32—C31—Si2124.17 (16)
O3—Si2—O2—Si1172.2 (3)C34—C35—C36—C310.2 (4)
C31—Si2—O2—Si169.0 (4)C32—C31—C36—C350.5 (3)
C41—Si2—O2—Si152.1 (4)Si2—C31—C36—C35176.00 (19)
O1—Si1—O2—Si26.6 (4)O2—Si2—C41—C4234.10 (19)
C11—Si1—O2—Si2126.4 (3)O3—Si2—C41—C42155.08 (17)
C21—Si1—O2—Si2113.1 (4)C31—Si2—C41—C4287.36 (18)
O2—Si2—O3—Si351.0 (2)O2—Si2—C41—C46149.95 (16)
C31—Si2—O3—Si3171.53 (14)O3—Si2—C41—C4628.97 (18)
C41—Si2—O3—Si369.55 (16)C31—Si2—C41—C4688.60 (18)
O4—Si3—O3—Si216.7 (2)C46—C41—C42—C430.4 (3)
C61—Si3—O3—Si2139.70 (15)Si2—C41—C42—C43176.54 (19)
C51—Si3—O3—Si299.35 (16)C41—C42—C43—C440.6 (4)
O2—Si1—C11—C1631.1 (2)C42—C43—C44—C450.2 (4)
O1—Si1—C11—C16152.56 (17)C43—C44—C45—C460.2 (4)
C21—Si1—C11—C1688.21 (19)C44—C45—C46—C410.3 (4)
O2—Si1—C11—C12152.77 (17)C42—C41—C46—C450.0 (3)
O1—Si1—C11—C1231.3 (2)Si2—C41—C46—C45176.14 (18)
C21—Si1—C11—C1287.94 (19)O4—Si3—C51—C56168.4 (2)
C16—C11—C12—C130.4 (3)O3—Si3—C51—C5671.1 (2)
Si1—C11—C12—C13175.91 (19)C61—Si3—C51—C5644.9 (2)
C11—C12—C13—C140.2 (4)O4—Si3—C51—C5214.4 (2)
C12—C13—C14—C150.2 (4)O3—Si3—C51—C52106.22 (19)
C13—C14—C15—C160.4 (4)C61—Si3—C51—C52137.79 (18)
C12—C11—C16—C150.3 (3)C56—C51—C52—C531.3 (4)
Si1—C11—C16—C15176.07 (19)Si3—C51—C52—C53176.1 (2)
C14—C15—C16—C110.1 (4)C51—C52—C53—C540.1 (4)
O2—Si1—C21—C262.4 (2)C52—C53—C54—C551.0 (5)
O1—Si1—C21—C26119.25 (18)C53—C54—C55—C560.7 (5)
C11—Si1—C21—C26121.21 (18)C54—C55—C56—C510.7 (5)
O2—Si1—C21—C22176.13 (16)C52—C51—C56—C551.6 (4)
O1—Si1—C21—C2262.18 (19)Si3—C51—C56—C55175.8 (2)
C11—Si1—C21—C2257.35 (19)O4—Si3—C61—C6236.68 (19)
C26—C21—C22—C230.1 (3)O3—Si3—C61—C62159.81 (17)
Si1—C21—C22—C23178.79 (18)C51—Si3—C61—C6282.78 (19)
C21—C22—C23—C240.5 (4)O4—Si3—C61—C66142.42 (16)
C22—C23—C24—C250.4 (4)O3—Si3—C61—C6619.29 (18)
C23—C24—C25—C260.3 (4)C51—Si3—C61—C6698.12 (18)
C24—C25—C26—C211.0 (4)C66—C61—C62—C630.1 (3)
C22—C21—C26—C250.9 (3)Si3—C61—C62—C63179.27 (19)
Si1—C21—C26—C25179.47 (18)C61—C62—C63—C640.4 (4)
O2—Si2—C31—C327.7 (2)C62—C63—C64—C650.8 (4)
O3—Si2—C31—C32128.22 (18)C63—C64—C65—C660.7 (4)
C41—Si2—C31—C32113.39 (19)C64—C65—C66—C610.4 (3)
O2—Si2—C31—C36176.14 (16)C62—C61—C66—C650.1 (3)
O3—Si2—C31—C3655.63 (18)Si3—C61—C66—C65179.23 (17)
C41—Si2—C31—C3662.76 (18)C76—N71—C72—C730.6 (4)
C36—C31—C32—C330.4 (3)N71—C72—C73—C740.2 (5)
Si2—C31—C32—C33175.84 (19)C72—C73—C74—C750.3 (6)
C31—C32—C33—C340.2 (4)C73—C74—C75—C760.3 (6)
C32—C33—C34—C350.9 (4)C72—N71—C76—C750.5 (5)
C33—C34—C35—C360.9 (4)C74—C75—C76—N710.1 (6)
Symmetry code: (i) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N710.821.982.722 (3)150
C81—H81···O10.932.133.048 (4)167
O1—H1···O1ii0.822.012.809 (2)164
O1—H2···N810.822.233.048 (4)173
Symmetry code: (ii) x, y, z.
(sila3) 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–hexamethylenetetramine (1/1) top
Crystal data top
C24H22O3Si2·C6H12N4? #Insert any comments here.
Mr = 554.79Dx = 1.244 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 16.1555 (9) ÅCell parameters from 25 reflections
b = 8.4622 (10) Åθ = 9.4–14.2°
c = 21.8427 (16) ŵ = 0.16 mm1
β = 97.386 (5)°T = 294 K
V = 2961.4 (4) Å3Block, colourless
Z = 40.34 × 0.32 × 0.20 mm
F(000) = 1176
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.012
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.1°
Graphite monochromatorh = 2020
θ/2θ scansk = 010
6651 measured reflectionsl = 027
6436 independent reflections3 standard reflections every 120 min
3416 reflections with I > 2σ(I) intensity decay: 6.9%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.044H-atom parameters constrained
wR(F2) = 0.116 w = 1/[σ2(Fo2) + (0.0585P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.95(Δ/σ)max = 0.048
6436 reflectionsΔρmax = 0.26 e Å3
409 parametersΔρmin = 0.24 e Å3
58 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0027 (6)
Special details top

Experimental. ? #Insert any special details here.

Geometry. Mean-plane data from final SHELXL refinement run:-

Least-squares planes(x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

14.2027(0.0081) x - 3.2188(0.0052) y - 8.6886(0.0177) z = 0.9369(0.0055)

* 0.0247(0.0017) C11 * 0.0157(0.0018) C12 * -0.0058(0.0019) C13 * -0.0171(0.0023) C14 * -0.0045(0.0020) C15 * 0.0130(0.0019) C16 * -0.0261(0.0011) Si1

Rms deviation of fitted atoms = 0.0171

5.2635(0.0659) x + 5.5485(0.0271) y + 13.8394(0.1000) z = 4.9455(0.0067)

Angle to previous plane(with approximate e.s.d.) = 80.9 (2)

* 0.0113(0.0159) C21A_a * 0.0181(0.0119) C22A_a * -0.0044(0.0113) C23A_a * -0.0177(0.0134) C24A_a * 0.0011(0.0068) C25A_a * 0.0111(0.0059) C26A_a * -0.0194(0.0079) Si1

Rms deviation of fitted atoms = 0.0136

6.7330(0.0453) x + 7.4296(0.0124) y + 3.9310(0.1282) z = 4.3812(0.0115)

Angle to previous plane(with approximate e.s.d.) = 29.3 (5)

* -0.0262(0.0117) C21B_b * -0.0442(0.0119) C22B_b * 0.0325(0.0111) C23B_b * 0.0165(0.0114) C24B_b * -0.0083(0.0061) C25B_b * -0.0033(0.0052) C26B_b * 0.0329(0.0065) Si1

Rms deviation of fitted atoms = 0.0271

1.1860(0.0156) x + 3.1749(0.0037) y + 19.8099(0.0050) z = 1.4147(0.0045)

Angle to previous plane(with approximate e.s.d.) = 54.7 (4)

* 0.0162(0.0017) C31 * 0.0066(0.0017) C32 * -0.0066(0.0017) C33 * -0.0053(0.0019) C34 * 0.0024(0.0017) C35 * -0.0024(0.0018) C36 * -0.0110(0.0010) Si2

Rms deviation of fitted atoms = 0.0085

7.0084(0.0151) x - 7.3162(0.0029) y + 4.2761(0.0214) z = 0.1794(0.0045)

Angle to previous plane(with approximate e.s.d.) = 86.7 (1)

* 0.0057(0.0018) C41 * 0.0005(0.0019) C42 * 0.0029(0.0020) C43 * -0.0062(0.0025) C44 * -0.0017(0.0023) C45 * 0.0047(0.0022) C46 * -0.0059(0.0012) Si2

Rms deviation of fitted atoms = 0.0045

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si10.22392 (4)0.31469 (8)0.14462 (3)0.04133 (17)
Si20.28447 (4)0.25625 (8)0.01276 (3)0.04079 (17)
O10.29915 (11)0.4140 (2)0.18159 (8)0.0673 (5)
O20.37426 (9)0.1708 (2)0.02328 (8)0.0564 (5)
O30.24148 (10)0.2692 (2)0.07552 (7)0.0587 (5)
C110.21525 (13)0.1337 (3)0.19166 (10)0.0404 (5)
C120.25093 (15)0.1275 (3)0.25329 (10)0.0514 (6)
C130.24281 (19)0.0013 (4)0.29021 (13)0.0704 (8)
C140.1991 (2)0.1278 (4)0.26689 (17)0.0825 (10)
C150.16268 (19)0.1306 (3)0.20698 (18)0.0785 (9)
C160.17047 (15)0.0017 (3)0.16868 (13)0.0612 (7)
C21A0.1279 (4)0.4384 (11)0.1338 (10)0.046 (3)0.50
C22A0.0688 (13)0.404 (2)0.1707 (6)0.092 (5)0.50
C23A0.0097 (12)0.488 (2)0.1652 (7)0.120 (5)0.50
C24A0.0184 (9)0.6014 (19)0.1219 (9)0.096 (4)0.50
C25A0.0403 (6)0.6339 (9)0.0880 (4)0.087 (2)0.50
C26A0.1149 (4)0.5492 (8)0.0943 (3)0.067 (2)0.50
C21B0.1183 (4)0.4053 (13)0.1393 (9)0.035 (2)0.50
C22B0.0726 (11)0.418 (2)0.1892 (5)0.056 (2)0.50
C23B0.0007 (11)0.496 (2)0.1867 (5)0.073 (3)0.50
C24B0.0405 (8)0.559 (2)0.1316 (7)0.078 (4)0.50
C25B0.0009 (5)0.5469 (10)0.0802 (4)0.094 (3)0.50
C26B0.0752 (4)0.4766 (10)0.0841 (4)0.086 (3)0.50
C310.30472 (14)0.4549 (3)0.01892 (9)0.0394 (5)
C320.38366 (14)0.5001 (3)0.03138 (10)0.0462 (6)
C330.39802 (16)0.6462 (3)0.05631 (11)0.0532 (6)
C340.33444 (18)0.7512 (3)0.06926 (11)0.0571 (6)
C350.25573 (17)0.7113 (3)0.05777 (11)0.0573 (7)
C360.24109 (15)0.5645 (3)0.03362 (10)0.0496 (6)
C410.20864 (14)0.1489 (3)0.04388 (10)0.0457 (6)
C420.22557 (18)0.1305 (3)0.10434 (12)0.0585 (7)
C430.1721 (2)0.0532 (4)0.14836 (14)0.0783 (9)
C440.0994 (3)0.0064 (4)0.13337 (18)0.0905 (11)
C450.07920 (18)0.0083 (4)0.07411 (18)0.0879 (10)
C460.13420 (17)0.0859 (3)0.02995 (14)0.0684 (8)
N10.39060 (11)0.6835 (2)0.15747 (8)0.0460 (5)
N20.41673 (11)0.9250 (2)0.10210 (8)0.0412 (4)
N30.46530 (12)0.9039 (2)0.21221 (8)0.0518 (5)
N40.53223 (11)0.7498 (2)0.13822 (8)0.0489 (5)
C10.35860 (14)0.7942 (3)0.10849 (10)0.0463 (6)
C20.40625 (16)0.7743 (3)0.21555 (10)0.0557 (7)
C30.43149 (15)1.0078 (3)0.16200 (11)0.0521 (6)
C40.49663 (14)0.8582 (3)0.08957 (10)0.0482 (6)
C50.47230 (15)0.6238 (3)0.14330 (11)0.0531 (6)
C60.54306 (15)0.8364 (3)0.19647 (11)0.0584 (7)
H10.31090.48870.16040.081*
H20.37190.09330.04550.068*
H120.28140.21410.27000.062*
H130.26740.00120.33110.085*
H140.19360.21480.29210.099*
H150.13290.21900.19140.094*
H160.14550.00050.12790.073*
H22A0.07910.32400.20010.111*0.50
H23A0.05110.46460.18980.145*0.50
H24A0.06780.65890.11600.115*0.50
H25A0.03210.71490.05910.105*0.50
H26A0.15570.57390.06940.081*0.50
H22B0.09380.36980.22630.067*0.50
H23B0.02530.50800.22260.088*0.50
H24B0.09230.60760.13000.094*0.50
H25B0.02590.58680.04260.113*0.50
H26B0.10150.47410.04860.103*0.50
H320.42800.43010.02270.055*
H330.45150.67280.06430.064*
H340.34440.84950.08580.069*
H350.21210.78300.06620.069*
H360.18710.53820.02700.059*
H420.27490.17200.11530.070*
H430.18570.04190.18820.094*
H440.06280.05760.16330.109*
H450.02950.03320.06390.105*
H460.12070.09580.01000.082*
H1A0.30580.83700.11750.056*
H1B0.34840.73760.06960.056*
H2A0.35380.81700.22540.067*
H2B0.42790.70360.24870.067*
H3A0.47011.09430.15880.062*
H3B0.37931.05240.17140.062*
H4A0.48840.80210.05050.058*
H4B0.53580.94350.08580.058*
H5A0.49490.55130.17560.064*
H5B0.46400.56540.10480.064*
H6A0.58310.92080.19390.070*
H6B0.56590.76550.22930.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0434 (4)0.0415 (4)0.0392 (3)0.0010 (3)0.0058 (3)0.0063 (3)
Si20.0443 (3)0.0410 (4)0.0380 (3)0.0115 (3)0.0089 (2)0.0104 (3)
O10.0679 (12)0.0627 (13)0.0660 (11)0.0223 (10)0.0110 (9)0.0225 (10)
O20.0491 (9)0.0543 (11)0.0678 (11)0.0157 (8)0.0154 (8)0.0306 (9)
O30.0669 (11)0.0688 (12)0.0438 (9)0.0069 (9)0.0198 (8)0.0079 (8)
C110.0389 (12)0.0396 (13)0.0454 (12)0.0009 (10)0.0153 (10)0.0040 (10)
C120.0588 (15)0.0528 (15)0.0450 (13)0.0092 (12)0.0158 (11)0.0090 (12)
C130.092 (2)0.063 (2)0.0609 (17)0.0151 (18)0.0301 (15)0.0214 (16)
C140.099 (2)0.064 (2)0.094 (2)0.016 (2)0.048 (2)0.0309 (19)
C150.072 (2)0.0449 (17)0.124 (3)0.0143 (15)0.037 (2)0.0066 (18)
C160.0554 (16)0.0558 (17)0.0738 (18)0.0065 (14)0.0135 (13)0.0009 (15)
C21A0.055 (4)0.034 (5)0.047 (6)0.006 (3)0.006 (4)0.006 (4)
C22A0.066 (6)0.096 (9)0.117 (11)0.021 (6)0.019 (8)0.051 (8)
C23A0.055 (7)0.128 (10)0.182 (14)0.020 (6)0.032 (10)0.049 (10)
C24A0.061 (8)0.067 (8)0.154 (11)0.028 (7)0.003 (6)0.002 (6)
C25A0.120 (7)0.065 (5)0.072 (5)0.047 (5)0.004 (5)0.001 (4)
C26A0.076 (5)0.071 (5)0.057 (4)0.037 (4)0.013 (4)0.014 (3)
C21B0.044 (4)0.026 (4)0.037 (4)0.003 (3)0.014 (3)0.011 (4)
C22B0.041 (4)0.092 (5)0.035 (3)0.007 (3)0.007 (3)0.001 (4)
C23B0.046 (4)0.114 (7)0.061 (4)0.011 (4)0.011 (4)0.021 (5)
C24B0.040 (5)0.097 (11)0.097 (5)0.017 (5)0.007 (4)0.010 (6)
C25B0.076 (6)0.131 (9)0.076 (5)0.052 (5)0.012 (4)0.022 (6)
C26B0.059 (5)0.144 (9)0.057 (4)0.035 (4)0.021 (4)0.036 (5)
C310.0490 (13)0.0377 (13)0.0315 (11)0.0087 (11)0.0046 (9)0.0028 (9)
C320.0527 (14)0.0421 (13)0.0455 (13)0.0117 (12)0.0124 (11)0.0030 (11)
C330.0589 (15)0.0479 (16)0.0549 (15)0.0003 (13)0.0160 (12)0.0063 (12)
C340.0814 (19)0.0368 (13)0.0532 (14)0.0012 (14)0.0086 (13)0.0056 (12)
C350.0649 (17)0.0427 (16)0.0623 (15)0.0194 (13)0.0007 (13)0.0087 (12)
C360.0465 (13)0.0500 (15)0.0524 (14)0.0120 (12)0.0069 (11)0.0104 (12)
C410.0512 (14)0.0355 (13)0.0501 (14)0.0124 (11)0.0054 (11)0.0091 (10)
C420.0824 (19)0.0365 (13)0.0553 (15)0.0056 (13)0.0038 (14)0.0066 (12)
C430.117 (3)0.0515 (18)0.0610 (18)0.0080 (19)0.0089 (19)0.0014 (15)
C440.100 (3)0.067 (2)0.092 (3)0.009 (2)0.033 (2)0.0094 (19)
C450.0512 (18)0.089 (2)0.120 (3)0.0063 (17)0.0021 (19)0.000 (2)
C460.0547 (16)0.076 (2)0.0735 (18)0.0058 (15)0.0056 (14)0.0010 (17)
N10.0518 (11)0.0424 (11)0.0440 (10)0.0023 (10)0.0074 (9)0.0020 (9)
N20.0449 (10)0.0355 (10)0.0421 (10)0.0064 (9)0.0019 (8)0.0029 (8)
N30.0546 (12)0.0568 (14)0.0420 (11)0.0039 (11)0.0011 (9)0.0097 (10)
N40.0438 (11)0.0483 (12)0.0548 (12)0.0128 (10)0.0068 (9)0.0058 (10)
C10.0400 (12)0.0495 (15)0.0474 (13)0.0005 (11)0.0024 (10)0.0020 (11)
C20.0615 (16)0.0687 (18)0.0382 (12)0.0051 (14)0.0117 (11)0.0038 (12)
C30.0532 (15)0.0407 (14)0.0610 (15)0.0061 (12)0.0018 (12)0.0105 (12)
C40.0514 (14)0.0461 (14)0.0486 (14)0.0022 (12)0.0129 (11)0.0041 (11)
C50.0682 (17)0.0390 (14)0.0527 (14)0.0143 (13)0.0097 (12)0.0045 (11)
C60.0467 (14)0.0662 (18)0.0575 (15)0.0030 (13)0.0113 (11)0.0037 (13)
Geometric parameters (Å, º) top
Si1—O11.607 (2)C25B—C26B1.359 (11)
Si1—O31.618 (2)C31—C361.391 (3)
Si1—C111.860 (2)C31—C321.391 (3)
Si1—C21A1.8610 (1)C32—C331.382 (3)
Si1—C21B1.8610 (1)C33—C341.360 (3)
Si2—O21.611 (2)C34—C351.370 (3)
Si2—O31.618 (2)C35—C361.381 (3)
Si2—C411.862 (2)C41—C461.385 (3)
Si2—C311.863 (2)C41—C421.391 (3)
C11—C161.389 (3)C42—C431.373 (4)
C11—C121.396 (3)C43—C441.357 (5)
C12—C131.372 (3)C44—C451.381 (5)
C13—C141.346 (4)C45—C461.390 (4)
C14—C151.364 (4)N1—C11.465 (3)
C15—C161.413 (4)N1—C21.477 (3)
C21A—C26A1.273 (15)N1—C51.483 (3)
C21A—C22A1.359 (19)N2—C41.467 (3)
C22A—C23A1.45 (3)N2—C11.470 (3)
C23A—C24A1.34 (2)N2—C31.476 (3)
C24A—C25A1.306 (15)N3—C31.456 (3)
C25A—C26A1.395 (10)N3—C61.461 (3)
C21B—C22B1.397 (18)N3—C21.461 (3)
C21B—C26B1.445 (17)N4—C51.454 (3)
C22B—C23B1.35 (2)N4—C61.459 (3)
C23B—C24B1.39 (2)N4—C41.464 (3)
C24B—C25B1.366 (15)
O1—Si1—O3112.41 (10)C25B—C24B—C23B117.9 (12)
O1—Si1—C11105.01 (10)C26B—C25B—C24B119.8 (9)
O3—Si1—C11110.74 (10)C25B—C26B—C21B124.7 (8)
O1—Si1—C21A109.5 (5)C36—C31—C32116.1 (2)
O3—Si1—C21A105.0 (7)C36—C31—Si2121.85 (17)
C11—Si1—C21A114.4 (4)C32—C31—Si2121.99 (16)
O1—Si1—C21B116.4 (5)C33—C32—C31121.8 (2)
O3—Si1—C21B108.1 (6)C34—C33—C32120.4 (2)
C11—Si1—C21B103.9 (4)C33—C34—C35119.7 (2)
C21A—Si1—C21B10.8 (6)C34—C35—C36120.0 (2)
O2—Si2—O3112.71 (9)C35—C36—C31122.0 (2)
O2—Si2—C41112.30 (10)C46—C41—C42116.6 (2)
O3—Si2—C41106.17 (10)C46—C41—Si2123.90 (19)
O2—Si2—C31105.08 (9)C42—C41—Si2119.50 (19)
O3—Si2—C31111.63 (10)C43—C42—C41122.4 (3)
C41—Si2—C31108.99 (10)C44—C43—C42119.6 (3)
Si1—O3—Si2162.3 (2)C43—C44—C45120.6 (3)
C16—C11—C12116.8 (2)C44—C45—C46119.1 (3)
C16—C11—Si1122.36 (18)C41—C46—C45121.7 (3)
C12—C11—Si1120.83 (18)C1—N1—C2107.46 (18)
C13—C12—C11122.5 (3)C1—N1—C5107.79 (17)
C14—C13—C12119.6 (3)C2—N1—C5107.34 (18)
C13—C14—C15121.2 (3)C4—N2—C1108.42 (17)
C14—C15—C16119.6 (3)C4—N2—C3107.61 (17)
C11—C16—C15120.3 (3)C1—N2—C3107.80 (17)
C26A—C21A—C22A119.7 (8)C3—N3—C6108.04 (19)
C26A—C21A—Si1124.2 (9)C3—N3—C2107.86 (18)
C22A—C21A—Si1116.1 (12)C6—N3—C2107.8 (2)
C21A—C22A—C23A121.3 (14)C5—N4—C6107.94 (19)
C24A—C23A—C22A114.9 (15)C5—N4—C4108.16 (18)
C25A—C24A—C23A122.2 (14)C6—N4—C4108.08 (19)
C24A—C25A—C26A121.2 (10)N1—C1—N2112.39 (17)
C21A—C26A—C25A120.7 (8)N3—C2—N1112.85 (17)
C22B—C21B—C26B112.0 (7)N3—C3—N2112.51 (18)
C22B—C21B—Si1123.8 (13)N4—C4—N2112.26 (17)
C26B—C21B—Si1124.2 (10)N4—C5—N1112.64 (18)
C23B—C22B—C21B123.6 (12)N4—C6—N3113.03 (18)
C22B—C23B—C24B121.8 (11)
O1—Si1—O3—Si23.7 (4)Si1—C21B—C26B—C25B178.1 (6)
C11—Si1—O3—Si2120.9 (4)O2—Si2—C31—C36179.58 (17)
C21A—Si1—O3—Si2115.2 (5)O3—Si2—C31—C3657.1 (2)
C21B—Si1—O3—Si2126.0 (5)C41—Si2—C31—C3659.9 (2)
O2—Si2—O3—Si162.2 (4)O2—Si2—C31—C322.8 (2)
C41—Si2—O3—Si1174.5 (4)O3—Si2—C31—C32125.32 (18)
C31—Si2—O3—Si155.8 (4)C41—Si2—C31—C32117.72 (18)
O1—Si1—C11—C16165.14 (19)C36—C31—C32—C330.7 (3)
O3—Si1—C11—C1643.6 (2)Si2—C31—C32—C33178.37 (17)
C21A—Si1—C11—C1674.8 (8)C31—C32—C33—C340.3 (4)
C21B—Si1—C11—C1672.2 (7)C32—C33—C34—C350.3 (4)
O1—Si1—C11—C1217.8 (2)C33—C34—C35—C360.5 (4)
O3—Si1—C11—C12139.36 (17)C34—C35—C36—C311.5 (4)
C21A—Si1—C11—C12102.3 (7)C32—C31—C36—C351.5 (3)
C21B—Si1—C11—C12104.9 (7)Si2—C31—C36—C35179.25 (18)
C16—C11—C12—C130.1 (3)O2—Si2—C41—C46119.3 (2)
Si1—C11—C12—C13177.13 (19)O3—Si2—C41—C464.3 (2)
C11—C12—C13—C140.1 (4)C31—Si2—C41—C46124.7 (2)
C12—C13—C14—C150.2 (5)O2—Si2—C41—C4261.4 (2)
C13—C14—C15—C160.4 (5)O3—Si2—C41—C42174.95 (17)
C12—C11—C16—C150.1 (3)C31—Si2—C41—C4254.6 (2)
Si1—C11—C16—C15177.30 (19)C46—C41—C42—C430.4 (4)
C14—C15—C16—C110.4 (4)Si2—C41—C42—C43179.7 (2)
O1—Si1—C21A—C26A76.3 (17)C41—C42—C43—C440.8 (4)
O3—Si1—C21A—C26A44.6 (16)C42—C43—C44—C450.8 (5)
C11—Si1—C21A—C26A166.2 (12)C43—C44—C45—C460.4 (5)
C21B—Si1—C21A—C26A153 (8)C42—C41—C46—C450.0 (4)
O1—Si1—C21A—C22A104.5 (13)Si2—C41—C46—C45179.3 (2)
O3—Si1—C21A—C22A134.6 (14)C44—C45—C46—C410.0 (5)
C11—Si1—C21A—C22A13.0 (17)C2—N1—C1—N258.2 (2)
C21B—Si1—C21A—C22A27 (6)C5—N1—C1—N257.3 (2)
C26A—C21A—C22A—C23A1 (3)C4—N2—C1—N157.8 (2)
Si1—C21A—C22A—C23A177.9 (12)C3—N2—C1—N158.4 (2)
C21A—C22A—C23A—C24A1 (2)C3—N3—C2—N158.5 (2)
C22A—C23A—C24A—C25A1 (3)C6—N3—C2—N157.9 (2)
C23A—C24A—C25A—C26A1 (2)C1—N1—C2—N358.4 (2)
C22A—C21A—C26A—C25A1 (2)C5—N1—C2—N357.3 (2)
Si1—C21A—C26A—C25A178.4 (8)C6—N3—C3—N257.9 (2)
C24A—C25A—C26A—C21A0.5 (16)C2—N3—C3—N258.3 (2)
O1—Si1—C21B—C22B71.4 (13)C4—N2—C3—N358.4 (2)
O3—Si1—C21B—C22B161.1 (12)C1—N2—C3—N358.4 (2)
C11—Si1—C21B—C22B43.4 (14)C5—N4—C4—N258.4 (2)
C21A—Si1—C21B—C22B124 (8)C6—N4—C4—N258.2 (2)
O1—Si1—C21B—C26B105.9 (12)C1—N2—C4—N458.1 (2)
O3—Si1—C21B—C26B21.6 (12)C3—N2—C4—N458.3 (2)
C11—Si1—C21B—C26B139.3 (10)C6—N4—C5—N158.3 (2)
C21A—Si1—C21B—C26B53 (6)C4—N4—C5—N158.4 (2)
C26B—C21B—C22B—C23B4 (2)C1—N1—C5—N457.9 (2)
Si1—C21B—C22B—C23B173.9 (12)C2—N1—C5—N457.5 (2)
C21B—C22B—C23B—C24B6 (3)C5—N4—C6—N358.9 (3)
C22B—C23B—C24B—C25B3 (2)C4—N4—C6—N357.9 (3)
C23B—C24B—C25B—C26B0.6 (17)C3—N3—C6—N457.8 (3)
C24B—C25B—C26B—C21B2.6 (13)C2—N3—C6—N458.5 (3)
C22B—C21B—C26B—C25B0.5 (16)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···N10.822.102.804 (2)144
O2—H2···N2i0.821.962.731 (2)156
Symmetry code: (i) x, y1, z.
(sila4) 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–2,2'-bipyridyl (1/1) top
Crystal data top
C24H22O3Si2·C10H8N2F(000) = 600
Mr = 570.78? #Insert any comments here.
Triclinic, P1Dx = 1.244 Mg m3
a = 8.9245 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.1900 (17) ÅCell parameters from 25 reflections
c = 17.3660 (19) Åθ = 9.3–19.3°
α = 99.57 (2)°µ = 0.15 mm1
β = 100.519 (13)°T = 294 K
γ = 93.80 (3)°Block, colourless
V = 1523.5 (3) Å30.38 × 0.36 × 0.33 mm
Z = 2
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.0°
Graphite monochromatorh = 1111
θ/2θ scansk = 013
6633 measured reflectionsl = 2221
6633 independent reflections3 standard reflections every 120 min
5141 reflections with I > 2σ(I) intensity decay: 2.8%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.117 w = 1/[σ2(Fo2) + (0.0593P)2 + 0.2883P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
6633 reflectionsΔρmax = 0.28 e Å3
376 parametersΔρmin = 0.21 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0078 (14)
Special details top

Experimental. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si10.00191 (5)0.13409 (5)0.03771 (3)0.04547 (13)
O10.13995 (15)0.24650 (18)0.00920 (8)0.0738 (4)
O110.00000.00000.00000.0714 (6)
C110.18819 (19)0.19901 (16)0.03637 (9)0.0429 (3)
C120.2040 (2)0.33553 (19)0.02731 (11)0.0592 (5)
C130.3478 (3)0.3823 (2)0.03004 (13)0.0745 (7)
C140.4758 (3)0.2943 (3)0.04242 (12)0.0715 (6)
C150.4643 (2)0.1607 (2)0.05257 (12)0.0657 (5)
C160.3217 (2)0.11319 (19)0.04927 (11)0.0527 (4)
C210.02804 (18)0.09050 (17)0.14238 (9)0.0432 (3)
C220.1184 (2)0.16923 (19)0.17716 (11)0.0570 (4)
C230.1272 (3)0.1356 (2)0.25698 (12)0.0672 (5)
C240.0457 (2)0.0233 (2)0.30313 (11)0.0607 (5)
C250.0425 (3)0.0569 (3)0.27068 (12)0.0806 (7)
C260.0515 (3)0.0233 (2)0.19123 (12)0.0755 (7)
Si20.51135 (5)0.15958 (4)0.50421 (2)0.03834 (12)
O20.37954 (13)0.20373 (15)0.43891 (7)0.0568 (3)
O210.50000.00000.50000.0591 (5)
C310.70562 (17)0.21275 (15)0.48905 (8)0.0384 (3)
C320.7307 (2)0.31973 (18)0.45099 (11)0.0521 (4)
C330.8749 (2)0.3591 (2)0.43949 (12)0.0638 (5)
C340.9986 (2)0.2944 (2)0.46699 (12)0.0614 (5)
C350.9780 (2)0.1913 (2)0.50675 (13)0.0625 (5)
C360.8331 (2)0.15012 (17)0.51706 (11)0.0518 (4)
C410.48447 (18)0.24066 (15)0.60393 (9)0.0417 (3)
C420.3939 (2)0.34604 (17)0.61450 (11)0.0489 (4)
C430.3845 (2)0.41157 (19)0.69001 (12)0.0591 (5)
C440.4647 (3)0.3724 (2)0.75592 (12)0.0646 (5)
C450.5552 (3)0.2696 (2)0.74780 (11)0.0684 (6)
C460.5651 (2)0.2043 (2)0.67257 (10)0.0574 (5)
N510.16478 (18)0.37404 (17)0.17185 (8)0.0571 (4)
C520.26252 (18)0.36046 (16)0.23786 (9)0.0417 (3)
C530.2507 (2)0.42609 (17)0.31315 (10)0.0479 (4)
C540.1361 (2)0.5081 (2)0.32035 (12)0.0590 (5)
C550.0351 (3)0.5219 (2)0.25331 (14)0.0760 (6)
C560.0536 (3)0.4527 (3)0.18126 (13)0.0791 (7)
N610.43930 (18)0.20755 (15)0.28378 (8)0.0520 (3)
C620.38977 (18)0.27737 (15)0.22664 (9)0.0416 (3)
C630.4577 (2)0.27739 (19)0.16098 (10)0.0538 (4)
C640.5822 (3)0.2065 (2)0.15477 (12)0.0712 (6)
C650.6319 (3)0.1337 (3)0.21174 (13)0.0790 (7)
C660.5572 (3)0.1357 (2)0.27439 (12)0.0687 (6)
H10.13310.26550.05610.111*
H120.11760.39610.01940.071*
H130.35670.47370.02340.089*
H140.57140.32620.04390.086*
H150.55190.10110.06170.079*
H160.31510.02140.05590.063*
H220.17460.24640.14640.068*
H230.18910.19010.27900.081*
H240.05050.00180.35670.073*
H250.09690.13460.30180.097*
H260.11310.07910.17000.091*
H20.40650.19540.39580.085*
H320.64870.36570.43290.063*
H330.88840.42980.41300.077*
H341.09540.32040.45870.074*
H351.06170.14880.52690.075*
H360.82070.07890.54330.062*
H420.33850.37300.57000.059*
H430.32390.48200.69580.071*
H440.45780.41580.80650.078*
H450.60990.24370.79280.082*
H460.62700.13460.66770.069*
H530.31950.41450.35810.057*
H540.12730.55370.37010.071*
H550.04370.57650.25650.091*
H560.01620.46140.13600.095*
H630.41960.32480.12160.065*
H640.63170.20830.11220.085*
H650.71470.08360.20830.095*
H660.59050.08430.31250.082*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0433 (2)0.0596 (3)0.0335 (2)0.0127 (2)0.00451 (17)0.00873 (19)
O10.0525 (8)0.1118 (12)0.0437 (7)0.0059 (8)0.0041 (6)0.0127 (7)
O110.0912 (15)0.0838 (14)0.0579 (11)0.0484 (12)0.0265 (10)0.0374 (10)
C110.0495 (9)0.0480 (9)0.0318 (7)0.0137 (7)0.0067 (6)0.0075 (6)
C120.0720 (12)0.0496 (10)0.0523 (10)0.0128 (9)0.0028 (9)0.0064 (8)
C130.1020 (18)0.0605 (12)0.0607 (12)0.0433 (13)0.0076 (12)0.0052 (10)
C140.0649 (13)0.0980 (17)0.0502 (11)0.0396 (13)0.0061 (9)0.0030 (11)
C150.0501 (10)0.0913 (15)0.0557 (11)0.0140 (10)0.0131 (9)0.0081 (10)
C160.0527 (10)0.0557 (10)0.0513 (10)0.0110 (8)0.0135 (8)0.0085 (8)
C210.0412 (8)0.0510 (9)0.0363 (8)0.0062 (7)0.0051 (6)0.0075 (7)
C220.0690 (12)0.0477 (9)0.0517 (10)0.0042 (8)0.0111 (9)0.0062 (8)
C230.0882 (15)0.0656 (12)0.0551 (11)0.0006 (11)0.0257 (10)0.0220 (10)
C240.0702 (12)0.0759 (13)0.0363 (9)0.0107 (10)0.0100 (8)0.0100 (9)
C250.0882 (16)0.0886 (16)0.0502 (11)0.0314 (13)0.0147 (11)0.0146 (11)
C260.0819 (15)0.0854 (15)0.0518 (11)0.0341 (12)0.0233 (10)0.0031 (10)
Si20.0414 (2)0.0377 (2)0.0343 (2)0.00102 (16)0.00259 (16)0.00945 (16)
O20.0459 (7)0.0848 (9)0.0418 (6)0.0098 (6)0.0035 (5)0.0216 (6)
O210.0738 (12)0.0375 (9)0.0633 (11)0.0090 (8)0.0142 (9)0.0065 (8)
C310.0433 (8)0.0359 (7)0.0336 (7)0.0009 (6)0.0036 (6)0.0050 (6)
C320.0460 (9)0.0498 (9)0.0604 (10)0.0018 (7)0.0012 (8)0.0224 (8)
C330.0587 (11)0.0665 (12)0.0662 (12)0.0150 (9)0.0064 (9)0.0269 (10)
C340.0469 (10)0.0735 (13)0.0606 (11)0.0080 (9)0.0126 (8)0.0063 (10)
C350.0468 (10)0.0673 (12)0.0726 (13)0.0142 (9)0.0077 (9)0.0111 (10)
C360.0520 (10)0.0488 (9)0.0569 (10)0.0091 (8)0.0084 (8)0.0174 (8)
C410.0450 (8)0.0409 (8)0.0382 (8)0.0029 (6)0.0064 (6)0.0095 (6)
C420.0475 (9)0.0492 (9)0.0488 (9)0.0015 (7)0.0065 (7)0.0103 (7)
C430.0615 (11)0.0524 (10)0.0632 (12)0.0029 (9)0.0201 (9)0.0028 (9)
C440.0857 (14)0.0605 (11)0.0470 (10)0.0048 (10)0.0230 (10)0.0018 (9)
C450.0896 (15)0.0760 (14)0.0385 (9)0.0046 (12)0.0060 (9)0.0162 (9)
C460.0719 (12)0.0587 (11)0.0442 (9)0.0138 (9)0.0095 (8)0.0161 (8)
N510.0582 (9)0.0700 (10)0.0404 (8)0.0175 (8)0.0021 (7)0.0064 (7)
C520.0455 (8)0.0418 (8)0.0358 (7)0.0015 (6)0.0056 (6)0.0062 (6)
C530.0526 (9)0.0506 (9)0.0387 (8)0.0009 (7)0.0090 (7)0.0051 (7)
C540.0671 (12)0.0604 (11)0.0520 (10)0.0085 (9)0.0238 (9)0.0032 (8)
C550.0739 (14)0.0882 (16)0.0736 (14)0.0366 (12)0.0235 (12)0.0155 (12)
C560.0741 (14)0.1085 (19)0.0555 (12)0.0406 (13)0.0031 (10)0.0157 (12)
N610.0610 (9)0.0542 (8)0.0396 (7)0.0101 (7)0.0031 (6)0.0104 (6)
C620.0468 (8)0.0407 (8)0.0323 (7)0.0000 (6)0.0010 (6)0.0015 (6)
C630.0619 (11)0.0624 (11)0.0367 (8)0.0130 (9)0.0088 (8)0.0067 (7)
C640.0728 (13)0.0978 (16)0.0442 (10)0.0313 (12)0.0147 (9)0.0039 (10)
C650.0822 (15)0.0992 (17)0.0531 (11)0.0483 (13)0.0058 (10)0.0005 (11)
C660.0835 (14)0.0713 (13)0.0501 (11)0.0312 (11)0.0001 (10)0.0132 (9)
Geometric parameters (Å, º) top
Si1—O111.6108 (6)C32—C331.382 (3)
Si1—O11.622 (2)C33—C341.375 (3)
Si1—C211.8589 (16)C34—C351.370 (3)
Si1—C111.8640 (17)C35—C361.386 (3)
O11—Si1i1.6108 (6)C41—C421.394 (2)
C11—C161.390 (3)C41—C461.395 (2)
C11—C121.393 (2)C42—C431.389 (3)
C12—C131.394 (3)C43—C441.368 (3)
C13—C141.365 (3)C44—C451.368 (3)
C14—C151.357 (3)C45—C461.385 (3)
C15—C161.387 (3)N51—C561.332 (3)
C21—C261.383 (3)N51—C521.341 (2)
C21—C221.383 (2)C52—C531.392 (2)
C22—C231.389 (3)C52—C621.482 (2)
C23—C241.361 (3)C53—C541.372 (3)
C24—C251.355 (3)C54—C551.370 (3)
C25—C261.384 (3)C55—C561.373 (3)
Si2—O211.6111 (5)N61—C661.340 (3)
Si2—O21.620 (2)N61—C621.343 (2)
Si2—C411.8551 (17)C62—C631.386 (2)
Si2—C311.8597 (16)C63—C641.375 (3)
O21—Si2ii1.6111 (5)C64—C651.362 (3)
C31—C361.391 (2)C65—C661.374 (3)
C31—C321.392 (2)
O11—Si1—O1113.09 (7)C36—C31—Si2121.71 (12)
O11—Si1—C21108.80 (6)C32—C31—Si2121.37 (12)
O1—Si1—C21107.43 (8)C33—C32—C31121.41 (17)
O11—Si1—C11106.97 (6)C34—C33—C32120.45 (18)
O1—Si1—C11111.04 (8)C35—C34—C33119.40 (18)
C21—Si1—C11109.46 (7)C34—C35—C36120.22 (18)
Si1i—O11—Si1180.0C35—C36—C31121.58 (17)
C16—C11—C12117.00 (17)C42—C41—C46116.98 (16)
C16—C11—Si1121.52 (13)C42—C41—Si2122.49 (12)
C12—C11—Si1121.37 (15)C46—C41—Si2120.35 (13)
C11—C12—C13120.7 (2)C43—C42—C41121.39 (17)
C14—C13—C12120.25 (19)C44—C43—C42119.89 (18)
C15—C14—C13120.38 (19)C43—C44—C45120.32 (18)
C14—C15—C16119.8 (2)C44—C45—C46119.95 (19)
C15—C16—C11121.80 (18)C45—C46—C41121.47 (18)
C26—C21—C22116.31 (16)C56—N51—C52117.0 (2)
C26—C21—Si1119.76 (13)N51—C52—C53122.07 (16)
C22—C21—Si1123.86 (13)N51—C52—C62116.73 (14)
C21—C22—C23121.48 (17)C53—C52—C62121.12 (14)
C24—C23—C22120.25 (18)C54—C53—C52119.21 (17)
C25—C24—C23119.78 (18)C55—C54—C53119.12 (17)
C24—C25—C26119.95 (19)C54—C55—C56118.17 (19)
C21—C26—C25122.22 (19)N51—C56—C55124.4 (2)
O21—Si2—O2112.31 (6)C66—N61—C62117.1 (2)
O21—Si2—C41108.72 (5)N61—C62—C63122.06 (16)
O2—Si2—C41107.23 (7)N61—C62—C52117.40 (14)
O21—Si2—C31107.35 (6)C63—C62—C52120.48 (15)
O2—Si2—C31111.05 (7)C64—C63—C62119.26 (18)
C41—Si2—C31110.17 (7)C65—C64—C63119.1 (2)
Si2ii—O21—Si2180.0C64—C65—C66118.58 (19)
C36—C31—C32116.90 (15)N61—C66—C65123.81 (19)
O11—Si1—C11—C1635.46 (14)C33—C34—C35—C361.9 (3)
O1—Si1—C11—C16159.29 (13)C34—C35—C36—C311.2 (3)
C21—Si1—C11—C1682.26 (15)C32—C31—C36—C350.7 (3)
O11—Si1—C11—C12148.58 (13)Si2—C31—C36—C35178.99 (15)
O1—Si1—C11—C1224.76 (16)O21—Si2—C41—C42137.12 (13)
C21—Si1—C11—C1293.70 (15)O2—Si2—C41—C4215.47 (16)
C16—C11—C12—C130.9 (3)C31—Si2—C41—C42105.50 (14)
Si1—C11—C12—C13177.06 (15)O21—Si2—C41—C4647.88 (15)
C11—C12—C13—C140.6 (3)O2—Si2—C41—C46169.53 (14)
C12—C13—C14—C150.3 (3)C31—Si2—C41—C4669.50 (15)
C13—C14—C15—C160.9 (3)C46—C41—C42—C430.0 (3)
C14—C15—C16—C110.5 (3)Si2—C41—C42—C43175.19 (13)
C12—C11—C16—C150.4 (3)C41—C42—C43—C440.3 (3)
Si1—C11—C16—C15176.50 (14)C42—C43—C44—C450.5 (3)
O11—Si1—C21—C2642.59 (18)C43—C44—C45—C460.4 (3)
O1—Si1—C21—C26165.35 (17)C44—C45—C46—C410.0 (3)
C11—Si1—C21—C2673.98 (18)C42—C41—C46—C450.2 (3)
O11—Si1—C21—C22140.67 (14)Si2—C41—C46—C45175.49 (16)
O1—Si1—C21—C2217.92 (18)C56—N51—C52—C530.6 (3)
C11—Si1—C21—C22102.76 (16)C56—N51—C52—C62177.51 (19)
C26—C21—C22—C230.5 (3)N51—C52—C53—C540.4 (3)
Si1—C21—C22—C23176.36 (16)C62—C52—C53—C54176.30 (16)
C21—C22—C23—C240.2 (3)C52—C53—C54—C550.9 (3)
C22—C23—C24—C251.0 (4)C53—C54—C55—C560.2 (4)
C23—C24—C25—C261.1 (4)C52—N51—C56—C551.4 (4)
C22—C21—C26—C250.3 (3)C54—C55—C56—N510.9 (4)
Si1—C21—C26—C25176.6 (2)C66—N61—C62—C630.8 (3)
C24—C25—C26—C210.5 (4)C66—N61—C62—C52178.11 (16)
O21—Si2—C31—C3634.24 (14)N51—C52—C62—N61147.35 (16)
O2—Si2—C31—C36157.37 (13)C53—C52—C62—N6135.7 (2)
C41—Si2—C31—C3683.98 (15)N51—C52—C62—C6335.2 (2)
O21—Si2—C31—C32147.56 (13)C53—C52—C62—C63141.66 (17)
O2—Si2—C31—C3224.43 (16)N61—C62—C63—C641.6 (3)
C41—Si2—C31—C3294.22 (15)C52—C62—C63—C64175.66 (18)
C36—C31—C32—C331.9 (3)C62—C63—C64—C652.6 (3)
Si2—C31—C32—C33179.81 (15)C63—C64—C65—C661.2 (4)
C31—C32—C33—C341.2 (3)C62—N61—C66—C652.3 (3)
C32—C33—C34—C350.7 (3)C64—C65—C66—N611.3 (4)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···N510.822.092.869 (2)159
O2—H2···N610.822.042.846 (2)167
(sila5) 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–pyrazine (2/1) top
Crystal data top
2(C24H22O3Si2)·C4H4N2F(000) = 478
Mr = 909.28? #Insert any comments here.
Triclinic, P1Dx = 1.258 Mg m3
a = 8.8365 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.8028 (10) ÅCell parameters from 25 reflections
c = 13.3231 (16) Åθ = 14.5–20.5°
α = 108.740 (11)°µ = 0.18 mm1
β = 89.774 (14)°T = 294 K
γ = 94.792 (10)°Plate, colourless
V = 1199.8 (2) Å30.39 × 0.39 × 0.10 mm
Z = 1
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.0°
Graphite monochromatorh = 1111
θ/2θ scansk = 013
5200 measured reflectionsl = 1616
5200 independent reflections3 standard reflections every 120 min
3278 reflections with I > 2σ(I) intensity decay: no decay, variation 0.6%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H-atom parameters constrained
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0577P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
5200 reflectionsΔρmax = 0.25 e Å3
292 parametersΔρmin = 0.21 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.010 (2)
Special details top

Experimental. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si10.00473 (6)0.14967 (5)0.72883 (4)0.03606 (15)
Si20.04689 (6)0.14748 (5)0.67098 (4)0.03861 (16)
O10.07033 (16)0.13766 (14)0.61441 (10)0.0463 (3)
O20.05509 (17)0.19021 (15)0.56249 (11)0.0511 (4)
O30.06639 (16)0.01107 (12)0.72750 (11)0.0452 (3)
C110.1689 (2)0.27509 (18)0.74879 (14)0.0372 (4)
C120.2993 (2)0.2748 (2)0.80669 (17)0.0487 (5)
C130.4209 (3)0.3684 (2)0.81805 (19)0.0584 (6)
C140.4140 (3)0.4631 (2)0.77039 (19)0.0567 (6)
C150.2877 (3)0.4666 (2)0.71350 (19)0.0577 (6)
C160.1668 (3)0.37365 (19)0.70291 (17)0.0473 (5)
C210.1357 (2)0.19493 (19)0.83585 (15)0.0407 (5)
C220.2647 (3)0.1114 (2)0.83562 (19)0.0576 (6)
C230.3645 (3)0.1394 (3)0.9179 (2)0.0684 (7)
C240.3388 (3)0.2516 (3)1.0029 (2)0.0718 (7)
C250.2146 (3)0.3371 (3)1.0042 (2)0.0754 (8)
C260.1142 (3)0.3093 (2)0.92177 (18)0.0564 (6)
C310.2394 (2)0.2068 (2)0.64417 (18)0.0471 (5)
C320.2742 (3)0.2936 (3)0.5476 (2)0.0748 (8)
C330.4167 (5)0.3389 (4)0.5279 (3)0.1140 (14)
C340.5267 (4)0.2986 (4)0.6043 (4)0.1137 (16)
C350.4971 (3)0.2149 (3)0.7014 (4)0.0990 (12)
C360.3540 (3)0.1686 (2)0.7213 (3)0.0740 (8)
C410.0547 (2)0.2233 (2)0.76202 (17)0.0459 (5)
C420.0981 (3)0.3570 (2)0.7281 (2)0.0603 (6)
C430.1722 (3)0.4163 (3)0.7953 (3)0.0750 (8)
C440.2048 (3)0.3436 (3)0.8952 (3)0.0801 (9)
C450.1638 (3)0.2120 (3)0.9311 (2)0.0818 (9)
C460.0874 (3)0.1523 (3)0.86541 (19)0.0627 (6)
N510.3588 (2)0.0340 (2)0.55076 (15)0.0563 (5)
C520.4776 (3)0.1004 (3)0.5848 (2)0.0800 (9)
C530.6168 (3)0.0660 (3)0.5346 (2)0.0751 (8)
H10.15640.10100.60890.069*
H20.00820.16730.51730.077*
H120.30510.21020.83850.058*
H130.50670.36690.85770.070*
H140.49600.52520.77700.068*
H150.28300.53150.68190.069*
H160.08120.37700.66380.057*
H220.28380.03480.77850.069*
H230.44980.08190.91570.082*
H240.40500.26951.05920.086*
H250.19790.41441.06100.090*
H260.03050.36840.92390.068*
H320.19970.32250.49410.090*
H330.43690.39730.46190.137*
H340.62290.32820.59040.136*
H350.57230.18860.75440.119*
H360.33500.11080.78790.089*
H420.07710.40780.65950.072*
H430.19960.50610.77160.090*
H440.25530.38370.93960.096*
H450.18720.16230.99960.098*
H460.05750.06290.89120.075*
H520.46630.17360.64540.096*
H530.69680.11610.56270.090*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0392 (3)0.0347 (3)0.0347 (3)0.0019 (2)0.0022 (2)0.0121 (2)
Si20.0406 (3)0.0352 (3)0.0418 (3)0.0031 (2)0.0032 (2)0.0150 (2)
O10.0439 (9)0.0551 (9)0.0414 (8)0.0060 (7)0.0030 (6)0.0201 (7)
O20.0520 (9)0.0549 (9)0.0468 (9)0.0038 (7)0.0030 (7)0.0190 (7)
O30.0517 (9)0.0366 (7)0.0479 (8)0.0054 (6)0.0023 (6)0.0142 (6)
C110.0402 (11)0.0361 (10)0.0334 (10)0.0039 (8)0.0045 (8)0.0084 (8)
C120.0507 (13)0.0510 (12)0.0480 (12)0.0026 (10)0.0035 (10)0.0212 (10)
C130.0414 (13)0.0638 (15)0.0654 (15)0.0015 (11)0.0095 (11)0.0157 (12)
C140.0468 (13)0.0490 (13)0.0655 (15)0.0088 (10)0.0077 (11)0.0093 (11)
C150.0658 (16)0.0434 (12)0.0652 (15)0.0035 (11)0.0063 (12)0.0213 (11)
C160.0498 (13)0.0393 (11)0.0533 (13)0.0001 (9)0.0035 (10)0.0162 (9)
C210.0422 (11)0.0433 (11)0.0399 (11)0.0084 (9)0.0027 (9)0.0167 (9)
C220.0545 (14)0.0544 (14)0.0593 (14)0.0001 (11)0.0100 (11)0.0134 (11)
C230.0595 (16)0.0733 (17)0.0756 (18)0.0001 (13)0.0205 (13)0.0300 (15)
C240.0684 (18)0.091 (2)0.0583 (16)0.0187 (15)0.0275 (13)0.0239 (15)
C250.0758 (19)0.0799 (18)0.0527 (15)0.0074 (15)0.0158 (13)0.0033 (13)
C260.0530 (14)0.0558 (14)0.0526 (13)0.0017 (11)0.0120 (11)0.0074 (11)
C310.0446 (12)0.0391 (11)0.0640 (14)0.0055 (9)0.0088 (10)0.0252 (10)
C320.088 (2)0.088 (2)0.0644 (17)0.0457 (16)0.0267 (14)0.0365 (15)
C330.124 (3)0.150 (3)0.106 (3)0.093 (3)0.065 (2)0.075 (3)
C340.068 (2)0.131 (3)0.194 (5)0.047 (2)0.057 (3)0.115 (3)
C350.0472 (17)0.076 (2)0.192 (4)0.0065 (15)0.022 (2)0.070 (3)
C360.0553 (16)0.0498 (14)0.115 (2)0.0002 (12)0.0134 (16)0.0243 (15)
C410.0412 (12)0.0489 (12)0.0552 (13)0.0047 (9)0.0027 (10)0.0273 (10)
C420.0564 (15)0.0521 (13)0.0790 (17)0.0025 (11)0.0109 (13)0.0308 (12)
C430.0607 (17)0.0672 (17)0.113 (2)0.0071 (13)0.0036 (16)0.0535 (17)
C440.0654 (18)0.110 (2)0.092 (2)0.0015 (16)0.0080 (16)0.072 (2)
C450.093 (2)0.105 (2)0.0618 (17)0.0070 (18)0.0160 (15)0.0471 (17)
C460.0760 (18)0.0667 (16)0.0514 (14)0.0015 (13)0.0037 (12)0.0286 (12)
N510.0447 (11)0.0709 (13)0.0515 (11)0.0023 (9)0.0009 (9)0.0192 (10)
C520.0667 (18)0.0811 (19)0.0647 (17)0.0087 (15)0.0041 (14)0.0155 (14)
C530.0503 (15)0.0838 (19)0.0746 (18)0.0197 (14)0.0068 (13)0.0008 (15)
Geometric parameters (Å, º) top
Si1—O11.627 (2)C24—C251.371 (4)
Si1—O31.630 (2)C25—C261.382 (3)
Si1—C211.858 (2)C31—C321.378 (3)
Si1—C111.858 (2)C31—C361.385 (3)
Si2—O21.621 (2)C32—C331.383 (4)
Si2—O31.629 (2)C33—C341.349 (6)
Si2—C411.858 (2)C34—C351.358 (5)
Si2—C311.861 (2)C35—C361.392 (4)
C11—C161.389 (3)C41—C461.387 (3)
C11—C121.390 (3)C41—C421.389 (3)
C12—C131.386 (3)C42—C431.391 (3)
C13—C141.372 (3)C43—C441.354 (4)
C14—C151.362 (3)C44—C451.364 (4)
C15—C161.379 (3)C45—C461.387 (3)
C21—C261.388 (3)N51—C53i1.296 (3)
C21—C221.392 (3)N51—C521.317 (3)
C22—C231.377 (3)C52—C531.367 (4)
C23—C241.370 (4)C53—N51i1.296 (3)
O1—Si1—O3111.09 (8)C23—C22—C21121.6 (2)
O1—Si1—C21111.29 (8)C24—C23—C22120.3 (2)
O3—Si1—C21107.67 (8)C23—C24—C25119.4 (2)
O1—Si1—C11105.09 (8)C24—C25—C26120.4 (2)
O3—Si1—C11109.02 (8)C25—C26—C21121.3 (2)
C21—Si1—C11112.71 (9)C32—C31—C36116.6 (2)
O2—Si2—O3112.15 (8)C32—C31—Si2121.79 (19)
O2—Si2—C41106.63 (9)C36—C31—Si2121.61 (19)
O3—Si2—C41108.78 (9)C31—C32—C33121.8 (3)
O2—Si2—C31110.63 (10)C34—C33—C32120.2 (4)
O3—Si2—C31108.30 (9)C33—C34—C35120.1 (3)
C41—Si2—C31110.34 (9)C34—C35—C36119.9 (3)
Si2—O3—Si1144.7 (1)C31—C36—C35121.4 (3)
C16—C11—C12116.67 (19)C46—C41—C42117.2 (2)
C16—C11—Si1120.19 (15)C46—C41—Si2122.84 (17)
C12—C11—Si1123.13 (15)C42—C41—Si2119.96 (17)
C13—C12—C11121.5 (2)C41—C42—C43121.0 (3)
C14—C13—C12119.6 (2)C44—C43—C42120.3 (3)
C15—C14—C13120.4 (2)C43—C44—C45120.3 (2)
C14—C15—C16119.8 (2)C44—C45—C46119.9 (3)
C15—C16—C11122.0 (2)C45—C46—C41121.3 (3)
C26—C21—C22116.9 (2)C53i—N51—C52115.1 (2)
C26—C21—Si1122.10 (16)N51—C52—C53122.6 (2)
C22—C21—Si1120.91 (16)N51i—C53—C52122.3 (2)
O2—Si2—O3—Si112.8 (2)C22—C21—C26—C251.4 (3)
C41—Si2—O3—Si1104.87 (17)Si1—C21—C26—C25175.6 (2)
C31—Si2—O3—Si1135.19 (16)O2—Si2—C31—C3210.1 (2)
O1—Si1—O3—Si224.8 (2)O3—Si2—C31—C32133.43 (19)
C21—Si1—O3—Si297.33 (17)C41—Si2—C31—C32107.6 (2)
C11—Si1—O3—Si2140.10 (16)O2—Si2—C31—C36171.55 (18)
O1—Si1—C11—C1628.44 (18)O3—Si2—C31—C3648.3 (2)
O3—Si1—C11—C16147.59 (16)C41—Si2—C31—C3670.7 (2)
C21—Si1—C11—C1692.92 (17)C36—C31—C32—C330.9 (4)
O1—Si1—C11—C12150.02 (17)Si2—C31—C32—C33179.3 (2)
O3—Si1—C11—C1230.87 (19)C31—C32—C33—C340.1 (5)
C21—Si1—C11—C1288.61 (19)C32—C33—C34—C351.0 (6)
C16—C11—C12—C130.1 (3)C33—C34—C35—C361.3 (5)
Si1—C11—C12—C13178.61 (17)C32—C31—C36—C350.6 (4)
C11—C12—C13—C140.7 (3)Si2—C31—C36—C35179.0 (2)
C12—C13—C14—C151.0 (4)C34—C35—C36—C310.5 (4)
C13—C14—C15—C160.6 (4)O2—Si2—C41—C46128.7 (2)
C14—C15—C16—C110.0 (4)O3—Si2—C41—C467.6 (2)
C12—C11—C16—C150.2 (3)C31—Si2—C41—C46111.1 (2)
Si1—C11—C16—C15178.33 (17)O2—Si2—C41—C4252.8 (2)
O1—Si1—C21—C26119.46 (18)O3—Si2—C41—C42173.99 (17)
O3—Si1—C21—C26118.58 (18)C31—Si2—C41—C4267.3 (2)
C11—Si1—C21—C261.7 (2)C46—C41—C42—C430.5 (4)
O1—Si1—C21—C2263.71 (19)Si2—C41—C42—C43179.06 (19)
O3—Si1—C21—C2258.25 (19)C41—C42—C43—C440.6 (4)
C11—Si1—C21—C22178.52 (17)C42—C43—C44—C450.6 (4)
C26—C21—C22—C231.4 (3)C43—C44—C45—C460.5 (5)
Si1—C21—C22—C23175.6 (2)C44—C45—C46—C411.7 (4)
C21—C22—C23—C240.0 (4)C42—C41—C46—C451.7 (4)
C22—C23—C24—C251.5 (4)Si2—C41—C46—C45179.8 (2)
C23—C24—C25—C261.5 (4)C53i—N51—C52—C530.6 (5)
C24—C25—C26—C210.0 (4)N51—C52—C53—N51i0.6 (5)
Symmetry code: (i) x1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···N510.821.942.720 (2)159
O2—H2···O1ii0.821.992.800 (2)167
Symmetry code: (ii) x, y, z+1.
(sila6) 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–pyridine (1/1) top
Crystal data top
C24H22O3Si2·C5H5NF(000) = 260
Mr = 493.70? #Insert any comments here.
Triclinic, P1Dx = 1.222 Mg m3
a = 6.4469 (15) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.2837 (15) ÅCell parameters from 25 reflections
c = 10.6088 (15) Åθ = 10.0–19.0°
α = 74.645 (11)°µ = 0.16 mm1
β = 81.968 (13)°T = 294 K
γ = 85.511 (11)°Block, colourless
V = 671.0 (2) Å30.35 × 0.35 × 0.33 mm
Z = 1
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.0°
Graphite monochromatorh = 88
θ/2θ scansk = 013
2899 measured reflectionsl = 1213
2899 independent reflections3 standard reflections every 120 min
2449 reflections with I > 2σ(I) intensity decay: no decay, variation 2.9%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.109 w = 1/[σ2(Fo2) + (0.0522P)2 + 0.1916P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
2899 reflectionsΔρmax = 0.30 e Å3
163 parametersΔρmin = 0.26 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.034 (5)
Special details top

Experimental. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si10.33028 (7)0.62363 (4)0.49582 (4)0.03472 (15)
O10.50000.50000.50000.0533 (5)
O20.1014 (2)0.57049 (15)0.56521 (11)0.0543 (3)
C110.4150 (3)0.73920 (16)0.58522 (15)0.0395 (3)
C120.6050 (3)0.7218 (2)0.63580 (19)0.0547 (5)
C130.6656 (4)0.8117 (2)0.6995 (2)0.0713 (6)
C140.5397 (5)0.9205 (2)0.7125 (2)0.0729 (7)
C150.3511 (5)0.9413 (2)0.6639 (2)0.0752 (7)
C160.2877 (4)0.85129 (19)0.60049 (19)0.0582 (5)
C210.3102 (3)0.71147 (15)0.32045 (15)0.0404 (4)
C220.4845 (3)0.72227 (19)0.22522 (17)0.0532 (4)
C230.4705 (4)0.7935 (2)0.0954 (2)0.0717 (6)
C240.2840 (5)0.8548 (2)0.0595 (2)0.0811 (8)
C250.1106 (4)0.8451 (3)0.1507 (2)0.0807 (7)
C260.1224 (3)0.7743 (2)0.28057 (19)0.0600 (5)
N310.0305 (4)0.5302 (3)0.8578 (3)0.0952 (8)0.50
C320.1757 (5)0.5528 (3)0.9314 (4)0.1131 (12)
C330.1445 (5)0.5239 (3)1.0681 (4)0.1077 (11)
C310.0305 (4)0.5302 (3)0.8578 (3)0.0952 (8)0.50
H10.05470.52870.52020.081*0.50
H20.09540.55760.64530.081*0.50
H120.69390.64830.62680.066*
H130.79330.79720.73350.086*
H140.58170.98090.75450.087*
H150.26471.01580.67320.090*
H160.15880.86620.56800.070*
H220.61210.68120.24880.064*
H230.58820.79960.03280.086*
H240.27530.90310.02730.097*
H250.01620.88620.12570.097*
H260.00320.76860.34190.072*
H310.04900.54850.77320.114*0.50
H320.30150.58940.88770.136*
H330.25040.54291.11100.129*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0367 (2)0.0342 (2)0.0326 (2)0.00223 (16)0.00517 (16)0.00672 (16)
O10.0660 (12)0.0377 (9)0.0603 (11)0.0112 (8)0.0217 (9)0.0166 (8)
O20.0482 (7)0.0757 (9)0.0396 (6)0.0232 (6)0.0002 (5)0.0126 (6)
C110.0467 (9)0.0371 (8)0.0333 (7)0.0037 (7)0.0001 (6)0.0089 (6)
C120.0529 (11)0.0593 (11)0.0603 (11)0.0020 (9)0.0121 (9)0.0274 (9)
C130.0743 (15)0.0833 (16)0.0683 (14)0.0214 (12)0.0143 (11)0.0327 (12)
C140.111 (2)0.0614 (13)0.0537 (12)0.0303 (13)0.0022 (12)0.0263 (10)
C150.117 (2)0.0453 (11)0.0634 (13)0.0074 (12)0.0043 (13)0.0247 (10)
C160.0680 (13)0.0508 (10)0.0562 (11)0.0107 (9)0.0066 (9)0.0186 (9)
C210.0498 (9)0.0368 (8)0.0348 (8)0.0023 (7)0.0074 (7)0.0082 (6)
C220.0581 (11)0.0557 (11)0.0431 (9)0.0072 (9)0.0006 (8)0.0093 (8)
C230.0943 (18)0.0727 (14)0.0424 (10)0.0192 (13)0.0090 (11)0.0095 (10)
C240.125 (2)0.0705 (15)0.0404 (11)0.0011 (14)0.0210 (13)0.0040 (10)
C250.0962 (19)0.0791 (16)0.0592 (13)0.0225 (14)0.0325 (13)0.0003 (11)
C260.0623 (12)0.0640 (12)0.0491 (10)0.0133 (10)0.0143 (9)0.0076 (9)
N310.0744 (16)0.0770 (16)0.130 (2)0.0169 (13)0.0008 (15)0.0234 (15)
C320.078 (2)0.097 (2)0.146 (3)0.0284 (17)0.024 (2)0.012 (2)
C330.084 (2)0.090 (2)0.151 (3)0.0225 (17)0.018 (2)0.027 (2)
C310.0744 (16)0.0770 (16)0.130 (2)0.0169 (13)0.0008 (15)0.0234 (15)
Geometric parameters (Å, º) top
Si1—O11.6067 (5)C21—C261.392 (3)
Si1—O21.621 (2)C21—C221.392 (2)
Si1—C211.8582 (16)C22—C231.390 (3)
Si1—C111.8584 (16)C23—C241.368 (4)
O1—Si1i1.6067 (5)C24—C251.364 (4)
C11—C121.385 (2)C25—C261.387 (3)
C11—C161.394 (2)N31—C33ii1.349 (4)
C12—C131.387 (3)N31—C321.369 (5)
C13—C141.356 (3)C32—C331.390 (5)
C14—C151.366 (4)C33—C31ii1.349 (4)
C15—C161.394 (3)C33—N31ii1.349 (4)
O1—Si1—O2111.11 (6)C15—C16—C11120.8 (2)
O1—Si1—C21108.16 (6)C26—C21—C22117.52 (16)
O2—Si1—C21108.49 (7)C26—C21—Si1121.15 (14)
O1—Si1—C11109.18 (6)C22—C21—Si1121.27 (13)
O2—Si1—C11108.64 (7)C23—C22—C21121.0 (2)
C21—Si1—C11111.27 (7)C24—C23—C22120.1 (2)
Si1—O1—Si1i180.0C25—C24—C23120.1 (2)
C12—C11—C16117.12 (17)C24—C25—C26120.4 (2)
C12—C11—Si1122.93 (13)C25—C26—C21121.0 (2)
C16—C11—Si1119.93 (14)C33ii—N31—C32113.0 (3)
C11—C12—C13121.49 (19)N31—C32—C33123.3 (3)
C14—C13—C12120.3 (2)C31ii—C33—N31ii0.0 (2)
C13—C14—C15120.0 (2)C31ii—C33—C32123.7 (3)
C14—C15—C16120.3 (2)N31ii—C33—C32123.7 (3)
O1—Si1—C11—C124.84 (16)C11—Si1—C21—C2691.62 (17)
O2—Si1—C11—C12126.16 (15)O1—Si1—C21—C2234.52 (15)
C21—Si1—C11—C12114.47 (16)O2—Si1—C21—C22155.15 (14)
O1—Si1—C11—C16176.98 (13)C11—Si1—C21—C2285.40 (15)
O2—Si1—C11—C1655.66 (16)C26—C21—C22—C230.2 (3)
C21—Si1—C11—C1663.71 (16)Si1—C21—C22—C23176.97 (15)
C16—C11—C12—C130.3 (3)C21—C22—C23—C240.2 (3)
Si1—C11—C12—C13178.55 (16)C22—C23—C24—C250.6 (4)
C11—C12—C13—C140.7 (3)C23—C24—C25—C260.6 (4)
C12—C13—C14—C150.7 (3)C24—C25—C26—C210.2 (4)
C13—C14—C15—C160.3 (4)C22—C21—C26—C250.2 (3)
C14—C15—C16—C110.2 (3)Si1—C21—C26—C25176.96 (18)
C12—C11—C16—C150.1 (3)C33ii—N31—C32—C330.5 (5)
Si1—C11—C16—C15178.17 (16)N31—C32—C33—C31ii0.5 (6)
O1—Si1—C21—C26148.46 (15)N31—C32—C33—N31ii0.5 (6)
O2—Si1—C21—C2627.83 (17)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H1···O2iii0.821.942.755 (2)170
O2—H2···N310.822.182.995 (3)172
C31—H31···O20.862.142.995 (3)174
Symmetry code: (iii) x, y+1, z+1.
(sila7) 1,1,3,3-Tetraphenyldisiloxane-1,3-diol–pyrimidine (1/1) top
Crystal data top
C24H22O3Si2·C4H4N2F(000) = 260
Mr = 494.69? #Insert any comments here.
Triclinic, P1Dx = 1.240 Mg m3
a = 6.4358 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.2497 (12) ÅCell parameters from 25 reflections
c = 10.4056 (10) Åθ = 9.5–17.0°
α = 76.000 (7)°µ = 0.17 mm1
β = 84.438 (9)°T = 294 K
γ = 86.372 (12)°Block, colourless
V = 662.32 (11) Å30.38 × 0.38 × 0.36 mm
Z = 1
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Radiation source: X-ray tubeθmax = 26.9°, θmin = 2.0°
Graphite monochromatorh = 88
θ/2θ scansk = 013
2876 measured reflectionsl = 1213
2876 independent reflections3 standard reflections every 60 min
2389 reflections with I > 2σ(I) intensity decay: no decay, variation 0.6%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.131 w = 1/[σ2(Fo2) + (0.0802P)2 + 0.1328P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
2876 reflectionsΔρmax = 0.32 e Å3
162 parametersΔρmin = 0.39 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.028 (6)
Special details top

Experimental. ? #Insert any special details here.

Geometry. Mean-plane data from final SHELXL refinement run:-

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si10.33183 (7)0.62355 (4)0.49509 (4)0.03787 (17)
O10.50000.50000.50000.0586 (5)
O20.1068 (2)0.57096 (15)0.56611 (12)0.0587 (4)
C110.4219 (3)0.74260 (16)0.58478 (16)0.0421 (4)
C120.6167 (3)0.7299 (2)0.6341 (2)0.0606 (5)
C130.6794 (4)0.8222 (3)0.6996 (3)0.0790 (7)
C140.5506 (5)0.9287 (2)0.7148 (2)0.0777 (7)
C150.3589 (5)0.9449 (2)0.6665 (2)0.0782 (7)
C160.2941 (4)0.8528 (2)0.6024 (2)0.0612 (5)
C210.2984 (3)0.70585 (16)0.31810 (16)0.0439 (4)
C220.4665 (4)0.7173 (2)0.22184 (19)0.0601 (5)
C230.4423 (5)0.7836 (3)0.0905 (2)0.0811 (7)
C240.2534 (6)0.8397 (3)0.0542 (2)0.0866 (8)
C250.0845 (5)0.8300 (3)0.1465 (2)0.0834 (8)
C260.1064 (4)0.7636 (2)0.2780 (2)0.0619 (5)
C310.0314 (7)0.5298 (3)0.8579 (4)0.1176 (11)0.50
N310.0314 (7)0.5298 (3)0.8579 (4)0.1176 (11)0.50
C320.1845 (6)0.5240 (4)0.9357 (5)0.1137 (10)0.75
N320.1845 (6)0.5240 (4)0.9357 (5)0.1137 (10)0.25
N330.1605 (8)0.4972 (4)1.0694 (5)0.1304 (15)0.25
C330.1605 (8)0.4972 (4)1.0694 (5)0.1304 (15)0.75
H10.05580.52780.52100.088*0.50
H20.09740.57560.64410.088*0.50
H120.70720.65830.62320.073*
H130.80990.81100.73310.095*
H140.59330.99050.75820.093*
H150.27121.01800.67660.094*
H160.16250.86490.57040.073*
H220.59680.68000.24570.072*
H230.55590.78970.02730.097*
H240.23860.88480.03370.104*
H250.04480.86790.12110.100*
H260.00870.75770.34010.074*
H310.04860.54810.77260.141*0.50
H320.30860.53850.89800.136*0.75
H330.27770.49671.11530.156*0.75
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0418 (3)0.0352 (2)0.0357 (2)0.00002 (16)0.00378 (16)0.00693 (16)
O10.0737 (13)0.0396 (9)0.0648 (11)0.0157 (8)0.0203 (10)0.0159 (8)
O20.0567 (8)0.0806 (10)0.0407 (7)0.0245 (7)0.0025 (6)0.0151 (6)
C110.0510 (9)0.0366 (8)0.0378 (8)0.0023 (6)0.0003 (6)0.0087 (6)
C120.0566 (11)0.0621 (12)0.0703 (13)0.0015 (9)0.0107 (9)0.0278 (10)
C130.0832 (16)0.0856 (17)0.0786 (16)0.0235 (13)0.0159 (13)0.0309 (13)
C140.122 (2)0.0599 (13)0.0584 (13)0.0284 (14)0.0014 (13)0.0255 (10)
C150.123 (2)0.0483 (11)0.0650 (13)0.0084 (12)0.0069 (14)0.0248 (10)
C160.0721 (13)0.0517 (11)0.0608 (12)0.0116 (9)0.0039 (10)0.0195 (9)
C210.0534 (9)0.0382 (8)0.0393 (8)0.0019 (7)0.0058 (7)0.0075 (6)
C220.0674 (12)0.0604 (12)0.0478 (10)0.0011 (9)0.0040 (9)0.0076 (8)
C230.107 (2)0.0822 (17)0.0455 (11)0.0082 (15)0.0151 (12)0.0061 (11)
C240.135 (3)0.0733 (15)0.0436 (11)0.0053 (16)0.0175 (14)0.0040 (10)
C250.0995 (19)0.0772 (16)0.0670 (15)0.0206 (14)0.0328 (14)0.0004 (12)
C260.0648 (12)0.0621 (12)0.0533 (11)0.0120 (10)0.0109 (9)0.0047 (9)
C310.122 (3)0.093 (2)0.145 (3)0.017 (2)0.033 (2)0.033 (2)
N310.122 (3)0.093 (2)0.145 (3)0.017 (2)0.033 (2)0.033 (2)
C320.106 (2)0.099 (2)0.140 (3)0.0061 (18)0.013 (2)0.034 (2)
N320.106 (2)0.099 (2)0.140 (3)0.0061 (18)0.013 (2)0.034 (2)
N330.160 (4)0.093 (2)0.153 (4)0.001 (2)0.090 (3)0.029 (2)
C330.160 (4)0.093 (2)0.153 (4)0.001 (2)0.090 (3)0.029 (2)
Geometric parameters (Å, º) top
Si1—O11.6074 (5)C21—C221.391 (3)
Si1—O21.623 (2)C21—C261.393 (3)
Si1—C111.8550 (17)C22—C231.390 (3)
Si1—C211.8579 (16)C23—C241.359 (4)
O1—Si1i1.6074 (5)C24—C251.371 (4)
C11—C121.387 (3)C25—C261.389 (3)
C11—C161.393 (2)C31—C321.324 (5)
C12—C131.391 (3)C31—C33ii1.391 (6)
C13—C141.359 (4)C31—N33ii1.391 (6)
C14—C151.362 (4)N33—N31ii1.391 (6)
C15—C161.384 (3)
O1—Si1—O2110.91 (6)C14—C15—C16120.3 (2)
O1—Si1—C11109.66 (6)C15—C16—C11121.4 (2)
O2—Si1—C11108.03 (7)C22—C21—C26117.58 (17)
O1—Si1—C21108.34 (6)C22—C21—Si1121.17 (14)
O2—Si1—C21108.17 (8)C26—C21—Si1121.19 (14)
C11—Si1—C21111.73 (7)C23—C22—C21120.9 (2)
Si1i—O1—Si1180.0C24—C23—C22120.3 (2)
C12—C11—C16116.80 (18)C23—C24—C25120.2 (2)
C12—C11—Si1123.06 (14)C24—C25—C26120.0 (2)
C16—C11—Si1120.12 (15)C25—C26—C21120.9 (2)
C11—C12—C13121.4 (2)C32—C31—C33ii112.1 (4)
C14—C13—C12120.2 (2)C32—C31—N33ii112.1 (4)
C13—C14—C15120.0 (2)C33ii—C31—N33ii0.002 (1)
O1—Si1—C11—C126.43 (17)O1—Si1—C21—C2236.21 (16)
O2—Si1—C11—C12127.41 (16)O2—Si1—C21—C22156.51 (15)
C21—Si1—C11—C12113.72 (17)C11—Si1—C21—C2284.71 (17)
O1—Si1—C11—C16175.23 (13)O1—Si1—C21—C26146.69 (15)
O2—Si1—C11—C1654.24 (16)O2—Si1—C21—C2626.39 (18)
C21—Si1—C11—C1664.63 (17)C11—Si1—C21—C2692.39 (17)
C16—C11—C12—C130.9 (3)C26—C21—C22—C230.2 (3)
Si1—C11—C12—C13179.28 (17)Si1—C21—C22—C23177.43 (18)
C11—C12—C13—C141.0 (4)C21—C22—C23—C240.6 (4)
C12—C13—C14—C150.4 (4)C22—C23—C24—C250.7 (4)
C13—C14—C15—C160.3 (4)C23—C24—C25—C260.5 (4)
C14—C15—C16—C110.4 (4)C24—C25—C26—C210.2 (4)
C12—C11—C16—C150.2 (3)C22—C21—C26—C250.1 (3)
Si1—C11—C16—C15178.64 (17)Si1—C21—C26—C25177.26 (18)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H1···O2iii0.821.922.736 (2)170
O2—H2···N310.822.172.959 (4)163
C31—H31···O20.862.102.959 (4)174
Symmetry code: (iii) x, y+1, z+1.
 

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