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Acta Cryst. (2008). E64, m616-m617    [ doi:10.1107/S1600536808008210 ]

[mu]-4,4'-Bipyridyl-1:2[kappa]2N:N'-methanol-2[kappa]O-tetrakis(tri-tert-butoxysilanethiolato)-1[kappa]4O,S;2[kappa]2S-dizinc(II)

A. Dolega and K. Baranowska

Abstract top

The title compound, [Zn2(C12H27O3SSi)4(C10H8N2)(CH4O)], is a binuclear complex with the two ZnII atoms linked via a bridging 4,4'-bipyridyl ligand. One of the ZnII atoms is penta-coordinated by two O,S-chelating tri-tert-butoxysilanethiolate units and one N atom of a 4,4'-bipyridine ligand, and the other ZnII atom is tetrahedrally coordinated by two tri-tert-butoxysilanethiolate anions acting as monodentate S ligands, the methanol O atom and the other N atom of the 4,4'-bipyridine ligand. This non-symmetrical coordination induces twisting and bending in the 4,4'-bipyridine ligand and introduces chirality into the system. The crystal studied exhibits inversion twinning. One tert-butyl group is disordered approximately equally over two positions.

Comment top

Two different coordination patterns are observed for zinc atoms in the title binuclear complex. Atom Zn1 is pentacoordinated by two O,S–chelating tri-tert-butoxysilanethiolate moieties and one N atom of a 4,4'-bipyridine ligand. Atom Zn2 is tetrahedrally coordinated by two tri-tert-butoxysilanethiolate anions acting as monodentate S-ligands, methanol oxygen and the other N of the 4,4'-bipyridine ligand (Table 1). This non-symmetric coordination results in a significant distortion of the pyridine rings of the 4,4'-bipyridine ligand; they are not only twisted [torsion angle C50—C51—C52—C53 = -28.8 (10)° and C58—C51—C52—C57 - 30.0 (9)°] but also bent [dihedral angle 31.7 (3)°] as well. The system is chiral and twinned by inversion with the Flack parameter of 0.462 (16) indicating almost equal shares of two crystal domains.

Coordination of methanol on zinc is strengthened by an intramolecular O—H···O hydrogen bonding with one of the adjacent tert-butoxy groups (Fig. 1).

Related literature top

For related literature, see: Bąkowicz et al. (2007); Becker et al. (2001); Pladzyk et al. (2007).

Experimental top

The title compound was obtained by the reaction of zinc acetyloacetonate (0.54 g, 2 mmol), 4,4'-bipyridine (0.312 g, 2 mmol) and tri-tert-butoxysilanethiol (0.9 ml, 3 mmol) in methanol (30 ml) and recrystallized from methanol at ambient temperature. For synthesis of substrates see, Becker et al. (2001).

Refinement top

The tBu group attached to O9 is disordered over two orientations with respect to rotation about O9—C33 bond. The site occupancies of the disordered atoms C34,C35,C36/C34A,C35A,C36A were refined to 0.52 (2)/0.48 (2). The same anisotropic displacement parameters were used for atoms C29, C30, C31 and C32, and for atoms C45, C46, C47 and C48. The hydroxyl H atom was located in a difference map and its positional parameters were refined with a O—H distance restraint of 0.99 (1) Å. The remaining H atoms were positioned geometrically and refined using a riding model, with C–H 0.95–0.98 Å and Uiso(H) = 1.2Ueq(C,O) or 1.5Ueq(methyl C). The highest residual electron-density peak is located 0.04 Å from atom C45.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of the title molecule, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. All H atoms except H13A have been omitted for clarity.
µ-4,4'-bipyridyl-1:2κ2N:N'-methanol-2κO-tetrakis(tri- tert-butoxysilanethiolato)-1κ4O,S;2κ2S-dizinc(II) top
Crystal data top
[Zn2(C12H27O3SSi)4(C10H8N2)(CH4O)]F000 = 3088
Mr = 1436.91Dx = 1.202 Mg m−3
Monoclinic, CcMo Kα radiation
λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 12077 reflections
a = 9.5897 (2) Åθ = 2.2–32.5º
b = 36.8378 (11) ŵ = 0.82 mm−1
c = 22.7611 (5) ÅT = 120 (2) K
β = 99.127 (2)ºPrism, colourless
V = 7938.9 (3) Å30.31 × 0.12 × 0.10 mm
Z = 4
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer		8015 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.037
Detector resolution: 8.1883 pixels mm-1θmax = 25.1º
T = 120(2) Kθmin = 2.2º
ω scans, 0.70 deg widthh = −7→11
Absorption correction: nonek = −33→43
15025 measured reflectionsl = −27→27
9143 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH atoms treated by a mixture of
independent and constrained refinement
R[F2 > 2σ(F2)] = 0.044  w = 1/[σ2(Fo2) + (0.071P)2 + 7.4679P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.126(Δ/σ)max = 0.013
S = 1.19Δρmax = 1.13 e Å−3
9143 reflectionsΔρmin = −0.66 e Å−3
793 parametersExtinction correction: none
3 restraintsAbsolute structure: Flack (1983); 2104 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.462 (16)
Secondary atom site location: difference Fourier map
Crystal data top
[Zn2(C12H27O3SSi)4(C10H8N2)(CH4O)]V = 7938.9 (3) Å3
Mr = 1436.91Z = 4
Monoclinic, CcMo Kα
a = 9.5897 (2) ŵ = 0.82 mm−1
b = 36.8378 (11) ÅT = 120 (2) K
c = 22.7611 (5) Å0.31 × 0.12 × 0.10 mm
β = 99.127 (2)º
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer		9143 independent reflections
Absorption correction: none8015 reflections with I > 2σ(I)
15025 measured reflectionsRint = 0.037
Refinement top
R[F2 > 2σ(F2)] = 0.044H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.126Δρmax = 1.13 e Å−3
S = 1.19Δρmin = −0.66 e Å−3
9143 reflectionsAbsolute structure: Flack (1983); 2104 Friedel pairs
793 parametersFlack parameter: 0.462 (16)
3 restraints
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn10.87328 (8)0.419112 (17)0.52174 (3)0.02354 (17)
Zn20.02975 (8)0.208801 (17)0.49213 (3)0.02269 (17)
S10.75131 (17)0.47221 (4)0.50965 (7)0.0238 (3)
S21.08592 (17)0.39609 (4)0.50945 (7)0.0243 (3)
S3−0.13485 (16)0.22289 (4)0.54999 (7)0.0242 (3)
S40.12611 (17)0.15828 (4)0.45870 (7)0.0255 (3)
Si10.77984 (18)0.47450 (4)0.60187 (7)0.0198 (3)
Si21.02088 (18)0.39671 (4)0.41728 (7)0.0214 (4)
Si3−0.00917 (18)0.20566 (4)0.62862 (8)0.0222 (4)
Si4−0.04263 (19)0.14141 (4)0.39600 (8)0.0226 (4)
O10.8867 (5)0.43946 (11)0.62064 (18)0.0235 (9)
O20.6414 (5)0.46546 (11)0.6328 (2)0.0259 (10)
O30.8409 (5)0.51256 (11)0.63097 (18)0.0260 (10)
O40.8502 (4)0.40405 (11)0.41111 (18)0.0244 (9)
O51.1011 (5)0.42614 (11)0.38143 (19)0.0268 (10)
O61.0387 (5)0.35829 (11)0.3837 (2)0.0262 (10)
O7−0.0682 (5)0.17051 (12)0.6606 (2)0.0304 (10)
O80.0160 (5)0.23723 (12)0.6794 (2)0.0336 (11)
O90.1467 (5)0.19839 (12)0.6113 (2)0.0327 (11)
O10−0.0793 (5)0.17008 (11)0.3394 (2)0.0288 (10)
O11−0.0115 (5)0.10291 (10)0.36563 (19)0.0290 (10)
O12−0.1833 (5)0.14153 (12)0.42733 (19)0.0291 (10)
N10.7317 (5)0.37820 (12)0.5337 (2)0.0212 (11)
N20.1936 (6)0.24711 (13)0.5063 (2)0.0246 (12)
C10.9323 (8)0.42254 (17)0.6785 (3)0.0296 (15)
C20.9660 (11)0.4513 (2)0.7258 (4)0.052 (2)
H2A1.03650.46810.71440.078*
H2B1.00360.43980.76390.078*
H2C0.87980.46480.72990.078*
C31.0618 (8)0.4007 (2)0.6716 (4)0.0427 (19)
H3A1.03580.38140.64220.064*
H3B1.10150.38980.70990.064*
H3C1.13230.41660.6580.064*
C40.8154 (9)0.39783 (19)0.6933 (3)0.0400 (17)
H4A0.7320.41240.69740.06*
H4B0.84810.38510.73080.06*
H4C0.79080.38010.66130.06*
C50.5252 (8)0.48737 (18)0.6439 (3)0.0345 (16)
C60.5703 (10)0.5089 (2)0.7006 (4)0.048 (2)
H6A0.61280.49250.73240.072*
H6B0.48770.52080.71250.072*
H6C0.63960.52730.69370.072*
C70.4094 (9)0.4608 (2)0.6530 (5)0.053 (2)
H7A0.37490.44840.61540.08*
H7B0.33150.47390.66640.08*
H7C0.44730.44280.68310.08*
C80.4762 (8)0.5125 (2)0.5918 (4)0.0421 (18)
H8A0.55150.52980.58750.063*
H8B0.3920.52570.59910.063*
H8C0.45360.49820.55530.063*
C90.9372 (7)0.53963 (17)0.6156 (3)0.0288 (15)
C100.9754 (12)0.5622 (2)0.6713 (4)0.058 (3)
H10A0.88980.57330.68180.086*
H10B1.04190.58130.66410.086*
H10C1.01920.54660.7040.086*
C110.8618 (9)0.56240 (18)0.5651 (3)0.0369 (17)
H11A0.82970.54680.53080.055*
H11B0.92670.58080.55410.055*
H11C0.78030.57440.57780.055*
C121.0658 (9)0.5221 (2)0.5975 (5)0.062 (3)
H12A1.11440.50750.63060.092*
H12B1.12980.5410.58710.092*
H12C1.03690.50640.56290.092*
C130.7380 (7)0.39982 (17)0.3603 (3)0.0274 (14)
C140.6177 (8)0.4239 (2)0.3728 (4)0.0407 (18)
H14A0.58510.41580.40930.061*
H14B0.53960.42250.33940.061*
H14C0.65070.44910.37770.061*
C150.6936 (8)0.35970 (18)0.3574 (3)0.0345 (16)
H15A0.77490.34450.35240.052*
H15B0.6180.3560.32360.052*
H15C0.65960.3530.39430.052*
C160.7898 (8)0.4118 (2)0.3033 (3)0.0407 (18)
H16A0.82730.43660.30830.061*
H16B0.71090.41130.27020.061*
H16C0.86430.39540.29490.061*
C171.1433 (8)0.46377 (18)0.3905 (3)0.0329 (16)
C181.0280 (10)0.4857 (2)0.4107 (5)0.062 (3)
H18A0.93990.48220.38290.093*
H18B1.05380.51150.41170.093*
H18C1.01490.47790.45060.093*
C191.2794 (10)0.4656 (2)0.4338 (4)0.053 (2)
H19A1.26370.45650.47270.08*
H19B1.31190.49080.43770.08*
H19C1.35110.45070.41910.08*
C201.1674 (12)0.4766 (2)0.3301 (4)0.061 (3)
H20A1.23570.46060.31520.091*
H20B1.20430.50140.33310.091*
H20C1.07790.47610.30250.091*
C211.1553 (7)0.34331 (16)0.3591 (3)0.0277 (14)
C221.2936 (8)0.3511 (2)0.3992 (4)0.0384 (17)
H22A1.3120.37720.39990.058*
H22B1.37030.33830.3840.058*
H22C1.28810.34260.43960.058*
C231.1565 (9)0.3581 (2)0.2971 (3)0.0420 (18)
H23A1.0710.35020.27080.063*
H23B1.240.3490.28190.063*
H23C1.15940.38470.29850.063*
C241.1282 (9)0.30224 (18)0.3556 (4)0.0389 (17)
H24A1.12680.29270.39570.058*
H24B1.20340.29030.33830.058*
H24C1.03690.29750.33070.058*
C25−0.1345 (7)0.13685 (15)0.6370 (3)0.0261 (14)
C26−0.0969 (9)0.10901 (19)0.6873 (3)0.0394 (18)
H26A0.00550.10510.69440.059*
H26B−0.1450.0860.67580.059*
H26C−0.12720.11820.72370.059*
C27−0.2920 (8)0.14394 (19)0.6247 (3)0.0350 (16)
H27A−0.32450.15160.66140.053*
H27B−0.34150.12170.60990.053*
H27C−0.31210.16310.59460.053*
C28−0.0792 (8)0.12438 (18)0.5822 (3)0.0333 (16)
H28A−0.10170.14250.55060.05*
H28B−0.12320.10120.56880.05*
H28C0.02350.12130.59130.05*
C29−0.0737 (11)0.2549 (3)0.7148 (5)0.0671 (14)
C30−0.2263 (10)0.2463 (3)0.6977 (5)0.0671 (14)
H30A−0.25870.25470.65690.101*
H30B−0.28030.25870.72490.101*
H30C−0.24040.22010.69990.101*
C31−0.0402 (11)0.2948 (3)0.7126 (5)0.0671 (14)
H31A0.06210.29840.72270.101*
H31B−0.08780.30790.74130.101*
H31C−0.07310.30420.67250.101*
C32−0.0275 (11)0.2409 (3)0.7777 (5)0.0671 (14)
H32A−0.06930.2170.78180.101*
H32B−0.05930.25780.80610.101*
H32C0.07570.2390.78560.101*
C330.2783 (7)0.1869 (2)0.6471 (4)0.0407 (18)
C340.399 (3)0.2111 (7)0.6362 (11)0.046 (5)0.52 (2)
H34A0.48240.2060.66610.07*0.52 (2)
H34B0.37190.23660.63910.07*0.52 (2)
H34C0.42180.20640.59640.07*0.52 (2)
C350.3074 (16)0.1498 (4)0.6381 (8)0.036 (4)0.52 (2)
H35A0.39880.14340.66150.054*0.52 (2)
H35B0.31040.14560.59580.054*0.52 (2)
H35C0.23320.13480.65070.054*0.52 (2)
C360.2727 (17)0.1917 (5)0.7189 (7)0.044 (5)0.52 (2)
H36A0.270.21750.72870.066*0.52 (2)
H36B0.35680.18060.74210.066*0.52 (2)
H36C0.18790.17970.72860.066*0.52 (2)
C34A0.365 (3)0.2192 (6)0.6588 (12)0.045 (6)0.48 (2)
H34D0.45570.21270.68250.067*0.48 (2)
H34E0.31620.23680.68080.067*0.48 (2)
H34F0.38050.22990.6210.067*0.48 (2)
C35A0.3435 (18)0.1624 (5)0.5985 (9)0.044 (6)0.48 (2)
H35D0.43110.15080.61770.065*0.48 (2)
H35E0.36360.1780.56590.065*0.48 (2)
H35F0.27510.14370.58270.065*0.48 (2)
C36A0.2532 (19)0.1649 (6)0.6954 (10)0.058 (7)0.48 (2)
H36D0.19230.1780.7190.088*0.48 (2)
H36E0.34330.15920.72060.088*0.48 (2)
H36F0.20670.14230.68020.088*0.48 (2)
C37−0.0162 (8)0.17337 (18)0.2852 (3)0.0321 (16)
C38−0.0609 (9)0.20988 (19)0.2604 (4)0.0411 (18)
H38A−0.16420.21110.25210.062*
H38B−0.02260.21380.22340.062*
H38C−0.0250.22870.28930.062*
C390.1417 (9)0.1706 (2)0.2994 (4)0.0427 (19)
H39A0.17780.18940.32830.064*
H39B0.18230.1740.26290.064*
H39C0.1680.14660.31610.064*
C40−0.0791 (11)0.1440 (2)0.2413 (3)0.051 (2)
H40A−0.05770.120.25910.077*
H40B−0.03830.14610.20460.077*
H40C−0.18170.14720.23220.077*
C410.0531 (8)0.06921 (17)0.3891 (3)0.0327 (16)
C420.2117 (9)0.0722 (2)0.3932 (4)0.046 (2)
H42A0.2350.07910.35430.069*
H42B0.25540.04880.40540.069*
H42C0.24750.09080.42270.069*
C43−0.0073 (12)0.04046 (19)0.3439 (4)0.058 (2)
H43A−0.11030.03970.34130.087*
H43B0.03250.01670.35660.087*
H43C0.01690.04650.30480.087*
C440.0133 (9)0.06086 (18)0.4498 (3)0.0386 (18)
H44A0.0510.07980.47810.058*
H44B0.0530.03730.46380.058*
H44C−0.08980.06010.44660.058*
C45−0.3318 (11)0.1365 (3)0.4069 (5)0.0726 (15)
C46−0.3974 (10)0.1729 (3)0.4057 (5)0.0726 (15)
H46A−0.36830.1850.44410.109*
H46B−0.50050.17050.39820.109*
H46C−0.36690.18750.3740.109*
C47−0.3877 (10)0.1155 (3)0.4557 (5)0.0726 (15)
H47A−0.33790.09230.46210.109*
H47B−0.4890.1110.44380.109*
H47C−0.37240.12970.49260.109*
C48−0.3621 (10)0.1192 (3)0.3481 (5)0.0726 (15)
H48A−0.32310.13410.31890.109*
H48B−0.46450.1170.33620.109*
H48C−0.31890.09510.34990.109*
C490.7655 (7)0.34292 (15)0.5319 (3)0.0252 (14)
H490.86070.33660.530.03*
C500.6686 (7)0.31558 (16)0.5325 (3)0.0256 (14)
H500.69690.29090.53130.031*
C510.5279 (7)0.32437 (15)0.5350 (3)0.0232 (13)
C520.4154 (7)0.29640 (16)0.5279 (3)0.0251 (14)
C530.4244 (7)0.26550 (17)0.4945 (3)0.0294 (15)
H530.50770.26070.47820.035*
C540.3124 (7)0.24173 (17)0.4849 (3)0.0272 (15)
H540.32080.22050.46190.033*
C560.1850 (7)0.27639 (16)0.5404 (3)0.0272 (14)
H560.10140.280.55720.033*
C570.2920 (7)0.30154 (16)0.5523 (3)0.0286 (15)
H570.28210.32210.57650.034*
C580.4954 (7)0.36096 (15)0.5397 (3)0.0222 (13)
H580.40230.36810.54380.027*
C590.5983 (7)0.38676 (16)0.5385 (3)0.0265 (14)
H590.57390.41160.5410.032*
C60−0.1725 (9)0.2591 (2)0.4021 (4)0.0415 (18)
H60A−0.25620.24930.41630.062*
H60B−0.19690.26580.36010.062*
H60C−0.13880.28060.42550.062*
O13−0.0646 (5)0.23231 (11)0.4085 (2)0.0299 (10)
H13A−0.076 (8)0.2162 (16)0.3734 (19)0.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0201 (4)0.0164 (3)0.0347 (4)−0.0013 (3)0.0061 (3)0.0003 (3)
Zn20.0219 (4)0.0166 (3)0.0305 (4)−0.0032 (3)0.0070 (3)−0.0025 (3)
S10.0293 (8)0.0179 (7)0.0232 (8)0.0019 (6)0.0014 (7)0.0007 (6)
S20.0197 (7)0.0307 (8)0.0220 (8)0.0022 (7)0.0015 (6)−0.0003 (6)
S30.0215 (8)0.0227 (7)0.0289 (8)0.0030 (6)0.0053 (6)0.0010 (6)
S40.0224 (8)0.0201 (7)0.0344 (9)−0.0028 (6)0.0052 (7)−0.0070 (6)
Si10.0220 (8)0.0161 (7)0.0213 (8)−0.0018 (7)0.0037 (7)0.0007 (6)
Si20.0199 (8)0.0228 (8)0.0213 (9)−0.0025 (7)0.0024 (7)0.0000 (6)
Si30.0190 (8)0.0197 (8)0.0286 (9)0.0022 (7)0.0057 (7)−0.0007 (7)
Si40.0254 (9)0.0191 (8)0.0242 (9)−0.0060 (7)0.0068 (7)−0.0028 (7)
O10.025 (2)0.023 (2)0.020 (2)−0.0015 (18)−0.0018 (18)0.0022 (17)
O20.028 (2)0.018 (2)0.032 (2)−0.0014 (18)0.008 (2)0.0051 (17)
O30.032 (3)0.021 (2)0.026 (2)−0.0078 (19)0.007 (2)−0.0009 (17)
O40.021 (2)0.030 (2)0.022 (2)0.0007 (19)0.0027 (18)−0.0019 (18)
O50.031 (2)0.024 (2)0.025 (2)−0.0058 (19)0.003 (2)0.0005 (18)
O60.023 (2)0.025 (2)0.031 (2)−0.0030 (19)0.0070 (19)−0.0006 (18)
O70.034 (3)0.029 (2)0.029 (2)−0.004 (2)0.006 (2)0.0001 (19)
O80.026 (2)0.036 (3)0.038 (3)0.000 (2)0.005 (2)−0.010 (2)
O90.024 (2)0.037 (3)0.039 (3)0.007 (2)0.009 (2)0.008 (2)
O100.034 (3)0.022 (2)0.031 (2)−0.004 (2)0.007 (2)−0.0002 (18)
O110.042 (3)0.021 (2)0.024 (2)−0.005 (2)0.004 (2)−0.0030 (17)
O120.027 (2)0.035 (2)0.027 (2)−0.009 (2)0.008 (2)−0.0058 (19)
N10.019 (3)0.017 (2)0.027 (3)−0.001 (2)0.004 (2)−0.004 (2)
N20.025 (3)0.021 (3)0.028 (3)−0.006 (2)0.005 (2)0.003 (2)
C10.033 (4)0.032 (3)0.022 (3)0.000 (3)0.000 (3)0.005 (3)
C20.078 (6)0.039 (4)0.032 (4)−0.003 (4)−0.013 (4)0.004 (3)
C30.039 (4)0.049 (4)0.041 (4)0.017 (4)0.006 (4)0.022 (3)
C40.047 (5)0.037 (4)0.037 (4)−0.002 (4)0.008 (4)0.013 (3)
C50.032 (4)0.028 (3)0.048 (4)0.003 (3)0.020 (3)0.010 (3)
C60.070 (6)0.037 (4)0.045 (5)0.007 (4)0.031 (4)0.004 (3)
C70.031 (4)0.049 (5)0.085 (7)0.000 (4)0.025 (4)0.024 (4)
C80.029 (4)0.040 (4)0.059 (5)0.009 (3)0.012 (4)0.010 (4)
C90.033 (4)0.024 (3)0.028 (4)−0.011 (3)0.000 (3)0.003 (3)
C100.088 (7)0.048 (5)0.034 (4)−0.043 (5)0.003 (4)−0.003 (4)
C110.043 (4)0.026 (4)0.041 (4)−0.005 (3)0.003 (3)0.002 (3)
C120.029 (4)0.047 (5)0.109 (8)−0.009 (4)0.013 (5)0.020 (5)
C130.023 (3)0.028 (3)0.028 (4)−0.002 (3)−0.005 (3)−0.003 (3)
C140.023 (4)0.054 (5)0.042 (4)0.010 (3)−0.004 (3)−0.011 (4)
C150.034 (4)0.042 (4)0.026 (4)−0.007 (3)0.000 (3)−0.007 (3)
C160.036 (4)0.058 (5)0.027 (4)−0.010 (4)−0.001 (3)0.002 (3)
C170.034 (4)0.028 (3)0.036 (4)−0.011 (3)0.007 (3)0.002 (3)
C180.057 (6)0.023 (4)0.110 (8)−0.007 (4)0.024 (6)−0.003 (4)
C190.053 (5)0.052 (5)0.050 (5)−0.028 (4)−0.003 (4)−0.001 (4)
C200.082 (7)0.056 (5)0.042 (5)−0.035 (5)0.005 (5)0.011 (4)
C210.027 (3)0.025 (3)0.034 (4)−0.002 (3)0.014 (3)0.001 (3)
C220.032 (4)0.036 (4)0.047 (4)0.001 (3)0.005 (3)−0.003 (3)
C230.047 (5)0.049 (4)0.032 (4)0.001 (4)0.013 (4)−0.002 (3)
C240.040 (4)0.031 (4)0.049 (5)0.004 (3)0.017 (4)−0.005 (3)
C250.030 (4)0.017 (3)0.033 (4)−0.004 (3)0.011 (3)0.007 (2)
C260.051 (5)0.033 (4)0.037 (4)0.005 (3)0.014 (4)0.008 (3)
C270.031 (4)0.032 (4)0.044 (4)0.001 (3)0.012 (3)0.008 (3)
C280.036 (4)0.029 (4)0.036 (4)0.000 (3)0.009 (3)0.000 (3)
C290.052 (3)0.074 (3)0.081 (3)0.000 (3)0.026 (3)−0.025 (3)
C300.052 (3)0.074 (3)0.081 (3)0.000 (3)0.026 (3)−0.025 (3)
C310.052 (3)0.074 (3)0.081 (3)0.000 (3)0.026 (3)−0.025 (3)
C320.052 (3)0.074 (3)0.081 (3)0.000 (3)0.026 (3)−0.025 (3)
C330.017 (3)0.041 (4)0.063 (5)0.008 (3)0.002 (3)0.004 (4)
C340.036 (12)0.041 (12)0.059 (16)−0.009 (9)0.000 (10)0.004 (10)
C350.034 (8)0.026 (7)0.045 (11)0.007 (6)−0.005 (7)−0.003 (6)
C360.033 (8)0.057 (11)0.038 (9)0.010 (8)−0.003 (7)−0.005 (8)
C34A0.044 (15)0.036 (12)0.046 (15)−0.004 (10)−0.019 (11)0.000 (10)
C35A0.029 (9)0.040 (10)0.058 (13)0.018 (7)−0.003 (8)−0.021 (9)
C36A0.028 (9)0.072 (16)0.069 (15)0.001 (9)−0.012 (9)0.033 (13)
C370.039 (4)0.032 (4)0.028 (4)−0.004 (3)0.014 (3)0.004 (3)
C380.043 (5)0.041 (4)0.041 (4)0.002 (4)0.013 (4)0.009 (3)
C390.049 (5)0.035 (4)0.050 (5)0.001 (4)0.026 (4)0.014 (3)
C400.087 (7)0.044 (4)0.027 (4)−0.018 (4)0.021 (4)−0.005 (3)
C410.046 (4)0.021 (3)0.031 (4)−0.001 (3)0.009 (3)−0.004 (3)
C420.051 (5)0.031 (4)0.059 (5)0.005 (4)0.021 (4)−0.002 (3)
C430.092 (7)0.026 (4)0.052 (5)0.000 (4)0.002 (5)−0.015 (4)
C440.049 (5)0.025 (3)0.043 (4)0.003 (3)0.011 (4)0.008 (3)
C450.040 (3)0.106 (4)0.068 (3)−0.020 (3)−0.002 (2)−0.009 (3)
C460.040 (3)0.106 (4)0.068 (3)−0.020 (3)−0.002 (2)−0.009 (3)
C470.040 (3)0.106 (4)0.068 (3)−0.020 (3)−0.002 (2)−0.009 (3)
C480.040 (3)0.106 (4)0.068 (3)−0.020 (3)−0.002 (2)−0.009 (3)
C490.024 (3)0.022 (3)0.028 (3)0.001 (3)0.001 (3)−0.001 (2)
C500.022 (3)0.017 (3)0.036 (4)0.003 (3)0.001 (3)−0.001 (3)
C510.022 (3)0.019 (3)0.028 (3)−0.007 (3)0.001 (3)0.000 (2)
C520.025 (3)0.019 (3)0.031 (4)−0.006 (3)0.006 (3)0.004 (2)
C530.023 (3)0.028 (3)0.038 (4)−0.002 (3)0.008 (3)−0.005 (3)
C540.030 (4)0.021 (3)0.033 (4)−0.004 (3)0.011 (3)−0.004 (3)
C560.028 (4)0.021 (3)0.035 (4)−0.002 (3)0.012 (3)0.001 (3)
C570.032 (4)0.016 (3)0.039 (4)−0.001 (3)0.009 (3)−0.001 (3)
C580.019 (3)0.020 (3)0.029 (3)−0.001 (3)0.006 (3)−0.003 (2)
C590.027 (4)0.017 (3)0.036 (4)0.002 (3)0.006 (3)−0.009 (3)
C600.044 (4)0.039 (4)0.043 (4)0.011 (4)0.011 (4)0.009 (3)
O130.036 (3)0.024 (2)0.030 (3)0.001 (2)0.007 (2)0.0027 (18)
Geometric parameters (Å, °) top
Zn1—N12.075 (5)C24—H24A0.98
Zn1—S22.2664 (18)C24—H24B0.98
Zn1—S12.2732 (16)C24—H24C0.98
Zn1—O12.357 (4)C25—C281.504 (9)
Zn1—O42.554 (4)C25—C271.515 (10)
Zn2—N22.098 (5)C25—C261.536 (9)
Zn2—O132.156 (5)C26—H26A0.98
Zn2—S42.2627 (16)C26—H26B0.98
Zn2—S32.2704 (17)C26—H26C0.98
S1—Si12.075 (2)C27—H27A0.98
S2—Si22.092 (2)C27—H27B0.98
S3—Si32.091 (2)C27—H27C0.98
S4—Si42.076 (2)C28—H28A0.98
Si1—O31.620 (4)C28—H28B0.98
Si1—O21.633 (5)C28—H28C0.98
Si1—O11.661 (4)C29—C301.487 (14)
Si2—O51.622 (5)C29—C311.510 (14)
Si2—O61.630 (4)C29—C321.520 (16)
Si2—O41.643 (5)C30—H30A0.98
Si3—O91.628 (5)C30—H30B0.98
Si3—O81.630 (5)C30—H30C0.98
Si3—O71.631 (5)C31—H31A0.98
Si4—O121.623 (5)C31—H31B0.98
Si4—O111.626 (4)C31—H31C0.98
Si4—O101.660 (5)C32—H32A0.98
O1—C11.460 (7)C32—H32B0.98
O2—C51.430 (8)C32—H32C0.98
O3—C91.439 (7)C33—C351.417 (15)
O4—C131.457 (8)C33—C36A1.42 (2)
O5—C171.450 (8)C33—C34A1.45 (3)
O6—C211.438 (8)C33—C341.51 (2)
O7—C251.456 (8)C33—C35A1.627 (18)
O8—C291.425 (10)C33—C361.654 (18)
O9—C331.453 (9)C34—H34A0.98
O10—C371.462 (8)C34—H34B0.98
O11—C411.451 (8)C34—H34C0.98
O12—C451.438 (11)C35—H35A0.98
N1—C591.338 (8)C35—H35B0.98
N1—C491.342 (8)C35—H35C0.98
N2—C541.323 (9)C36—H36A0.98
N2—C561.339 (8)C36—H36B0.98
C1—C21.510 (10)C36—H36C0.98
C1—C31.510 (10)C34A—H34D0.98
C1—C41.523 (10)C34A—H34E0.98
C2—H2A0.98C34A—H34F0.98
C2—H2B0.98C35A—H35D0.98
C2—H2C0.98C35A—H35E0.98
C3—H3A0.98C35A—H35F0.98
C3—H3B0.98C36A—H36D0.98
C3—H3C0.98C36A—H36E0.98
C4—H4A0.98C36A—H36F0.98
C4—H4B0.98C37—C381.495 (10)
C4—H4C0.98C37—C391.501 (11)
C5—C81.518 (10)C37—C401.529 (10)
C5—C61.519 (11)C38—H38A0.98
C5—C71.520 (10)C38—H38B0.98
C6—H6A0.98C38—H38C0.98
C6—H6B0.98C39—H39A0.98
C6—H6C0.98C39—H39B0.98
C7—H7A0.98C39—H39C0.98
C7—H7B0.98C40—H40A0.98
C7—H7C0.98C40—H40B0.98
C8—H8A0.98C40—H40C0.98
C8—H8B0.98C41—C421.513 (11)
C8—H8C0.98C41—C441.523 (10)
C9—C121.507 (11)C41—C431.525 (10)
C9—C101.510 (10)C42—H42A0.98
C9—C111.511 (10)C42—H42B0.98
C10—H10A0.98C42—H42C0.98
C10—H10B0.98C43—H43A0.98
C10—H10C0.98C43—H43B0.98
C11—H11A0.98C43—H43C0.98
C11—H11B0.98C44—H44A0.98
C11—H11C0.98C44—H44B0.98
C12—H12A0.98C44—H44C0.98
C12—H12B0.98C45—C481.469 (14)
C12—H12C0.98C45—C461.482 (15)
C13—C141.518 (9)C45—C471.519 (15)
C13—C161.527 (10)C46—H46A0.98
C13—C151.537 (9)C46—H46B0.98
C14—H14A0.98C46—H46C0.98
C14—H14B0.98C47—H47A0.98
C14—H14C0.98C47—H47B0.98
C15—H15A0.98C47—H47C0.98
C15—H15B0.98C48—H48A0.98
C15—H15C0.98C48—H48B0.98
C16—H16A0.98C48—H48C0.98
C16—H16B0.98C49—C501.372 (9)
C16—H16C0.98C49—H490.95
C17—C181.499 (11)C50—C511.398 (9)
C17—C191.506 (11)C50—H500.95
C17—C201.508 (10)C51—C581.392 (8)
C18—H18A0.98C51—C521.482 (8)
C18—H18B0.98C52—C531.380 (9)
C18—H18C0.98C52—C571.396 (9)
C19—H19A0.98C53—C541.376 (9)
C19—H19B0.98C53—H530.95
C19—H19C0.98C54—H540.95
C20—H20A0.98C56—C571.378 (9)
C20—H20B0.98C56—H560.95
C20—H20C0.98C57—H570.95
C21—C221.513 (10)C58—C591.373 (9)
C21—C231.513 (10)C58—H580.95
C21—C241.535 (9)C59—H590.95
C22—H22A0.98C60—O131.419 (9)
C22—H22B0.98C60—H60A0.98
C22—H22C0.98C60—H60B0.98
C23—H23A0.98C60—H60C0.98
C23—H23B0.98O13—H13A0.988 (10)
C23—H23C0.98
N1—Zn1—S2111.39 (14)H24A—C24—H24B109.5
N1—Zn1—S1107.81 (15)C21—C24—H24C109.5
S2—Zn1—S1139.71 (7)H24A—C24—H24C109.5
N1—Zn1—O192.46 (17)H24B—C24—H24C109.5
S2—Zn1—O1108.85 (12)O7—C25—C28112.0 (5)
S1—Zn1—O177.94 (11)O7—C25—C27106.6 (5)
N1—Zn1—O490.91 (17)C28—C25—C27111.8 (6)
S2—Zn1—O474.68 (10)O7—C25—C26104.9 (5)
S1—Zn1—O496.04 (11)C28—C25—C26110.0 (5)
O1—Zn1—O4173.77 (14)C27—C25—C26111.3 (6)
N2—Zn2—O1393.72 (19)C25—C26—H26A109.5
N2—Zn2—S4105.61 (15)C25—C26—H26B109.5
O13—Zn2—S499.79 (13)H26A—C26—H26B109.5
N2—Zn2—S3109.24 (15)C25—C26—H26C109.5
O13—Zn2—S3100.81 (13)H26A—C26—H26C109.5
S4—Zn2—S3137.87 (6)H26B—C26—H26C109.5
Si1—S1—Zn185.98 (7)C25—C27—H27A109.5
Si2—S2—Zn189.35 (8)C25—C27—H27B109.5
Si3—S3—Zn293.88 (8)H27A—C27—H27B109.5
Si4—S4—Zn299.32 (8)C25—C27—H27C109.5
O3—Si1—O2105.5 (2)H27A—C27—H27C109.5
O3—Si1—O1113.5 (2)H27B—C27—H27C109.5
O2—Si1—O1104.0 (2)C25—C28—H28A109.5
O3—Si1—S1115.46 (17)C25—C28—H28B109.5
O2—Si1—S1116.22 (19)H28A—C28—H28B109.5
O1—Si1—S1101.86 (16)C25—C28—H28C109.5
O5—Si2—O6104.6 (2)H28A—C28—H28C109.5
O5—Si2—O4113.1 (2)H28B—C28—H28C109.5
O6—Si2—O4106.3 (2)O8—C29—C30114.4 (8)
O5—Si2—S2114.96 (19)O8—C29—C31106.0 (8)
O6—Si2—S2115.06 (18)C30—C29—C31113.8 (9)
O4—Si2—S2102.83 (17)O8—C29—C32105.5 (8)
O9—Si3—O8104.5 (3)C30—C29—C32107.6 (9)
O9—Si3—O7112.0 (2)C31—C29—C32109.2 (9)
O8—Si3—O7105.8 (2)C29—C30—H30A109.5
O9—Si3—S3105.60 (19)C29—C30—H30B109.5
O8—Si3—S3112.98 (19)H30A—C30—H30B109.5
O7—Si3—S3115.4 (2)C29—C30—H30C109.5
O12—Si4—O11114.3 (2)H30A—C30—H30C109.5
O12—Si4—O10104.5 (2)H30B—C30—H30C109.5
O11—Si4—O10104.8 (2)C29—C31—H31A109.5
O12—Si4—S4107.98 (19)C29—C31—H31B109.5
O11—Si4—S4112.2 (2)H31A—C31—H31B109.5
O10—Si4—S4112.91 (18)C29—C31—H31C109.5
C1—O1—Si1130.4 (4)H31A—C31—H31C109.5
C1—O1—Zn1133.6 (3)H31B—C31—H31C109.5
Si1—O1—Zn193.64 (18)C29—C32—H32A109.5
C5—O2—Si1132.1 (4)C29—C32—H32B109.5
C9—O3—Si1134.8 (4)H32A—C32—H32B109.5
C13—O4—Si2130.6 (4)C29—C32—H32C109.5
C13—O4—Zn1138.0 (4)H32A—C32—H32C109.5
Si2—O4—Zn191.27 (19)H32B—C32—H32C109.5
C17—O5—Si2135.3 (4)C35—C33—C36A67.8 (13)
C21—O6—Si2131.4 (4)C35—C33—C34A134.3 (13)
C25—O7—Si3132.4 (4)C36A—C33—C34A119.3 (15)
C29—O8—Si3133.7 (5)C35—C33—O9111.9 (8)
C33—O9—Si3131.4 (5)C36A—C33—O9111.3 (9)
C37—O10—Si4129.9 (4)C34A—C33—O9106.5 (11)
C41—O11—Si4133.4 (4)C35—C33—C34111.8 (12)
C45—O12—Si4135.0 (6)C36A—C33—C34133.8 (14)
C59—N1—C49118.0 (5)O9—C33—C34110.8 (11)
C59—N1—Zn1119.5 (4)C36A—C33—C35A110.0 (13)
C49—N1—Zn1122.2 (4)C34A—C33—C35A108.0 (13)
C54—N2—C56118.0 (6)O9—C33—C35A100.0 (8)
C54—N2—Zn2120.7 (4)C35—C33—C36106.5 (10)
C56—N2—Zn2121.2 (4)C34A—C33—C3680.7 (13)
O1—C1—C2110.1 (5)O9—C33—C36111.3 (7)
O1—C1—C3105.5 (5)C34—C33—C36104.2 (12)
C2—C1—C3111.3 (7)C33—C34—H34A109.5
O1—C1—C4109.2 (6)C33—C34—H34B109.5
C2—C1—C4110.1 (6)C33—C34—H34C109.5
C3—C1—C4110.5 (6)C33—C35—H35A109.5
C1—C2—H2A109.5C33—C35—H35B109.5
C1—C2—H2B109.5C33—C35—H35C109.5
H2A—C2—H2B109.5C33—C36—H36A109.5
C1—C2—H2C109.5C33—C36—H36B109.5
H2A—C2—H2C109.5C33—C36—H36C109.5
H2B—C2—H2C109.5C33—C34A—H34D109.5
C1—C3—H3A109.5C33—C34A—H34E109.5
C1—C3—H3B109.5H34D—C34A—H34E109.5
H3A—C3—H3B109.5C33—C34A—H34F109.5
C1—C3—H3C109.5H34D—C34A—H34F109.5
H3A—C3—H3C109.5H34E—C34A—H34F109.5
H3B—C3—H3C109.5C33—C35A—H35D109.5
C1—C4—H4A109.5C33—C35A—H35E109.5
C1—C4—H4B109.5H35D—C35A—H35E109.5
H4A—C4—H4B109.5C33—C35A—H35F109.5
C1—C4—H4C109.5H35D—C35A—H35F109.5
H4A—C4—H4C109.5H35E—C35A—H35F109.5
H4B—C4—H4C109.5C33—C36A—H36D109.5
O2—C5—C8111.1 (5)C33—C36A—H36E109.5
O2—C5—C6108.7 (6)H36D—C36A—H36E109.5
C8—C5—C6110.9 (6)C33—C36A—H36F109.5
O2—C5—C7105.5 (5)H36D—C36A—H36F109.5
C8—C5—C7110.9 (7)H36E—C36A—H36F109.5
C6—C5—C7109.6 (7)O10—C37—C38105.1 (5)
C5—C6—H6A109.5O10—C37—C39110.6 (6)
C5—C6—H6B109.5C38—C37—C39111.1 (6)
H6A—C6—H6B109.5O10—C37—C40108.6 (5)
C5—C6—H6C109.5C38—C37—C40109.2 (7)
H6A—C6—H6C109.5C39—C37—C40111.8 (7)
H6B—C6—H6C109.5C37—C38—H38A109.5
C5—C7—H7A109.5C37—C38—H38B109.5
C5—C7—H7B109.5H38A—C38—H38B109.5
H7A—C7—H7B109.5C37—C38—H38C109.5
C5—C7—H7C109.5H38A—C38—H38C109.5
H7A—C7—H7C109.5H38B—C38—H38C109.5
H7B—C7—H7C109.5C37—C39—H39A109.5
C5—C8—H8A109.5C37—C39—H39B109.5
C5—C8—H8B109.5H39A—C39—H39B109.5
H8A—C8—H8B109.5C37—C39—H39C109.5
C5—C8—H8C109.5H39A—C39—H39C109.5
H8A—C8—H8C109.5H39B—C39—H39C109.5
H8B—C8—H8C109.5C37—C40—H40A109.5
O3—C9—C12110.7 (5)C37—C40—H40B109.5
O3—C9—C10104.9 (5)H40A—C40—H40B109.5
C12—C9—C10111.4 (7)C37—C40—H40C109.5
O3—C9—C11108.7 (6)H40A—C40—H40C109.5
C12—C9—C11110.0 (6)H40B—C40—H40C109.5
C10—C9—C11110.8 (6)O11—C41—C42109.1 (5)
C9—C10—H10A109.5O11—C41—C44110.7 (5)
C9—C10—H10B109.5C42—C41—C44110.6 (7)
H10A—C10—H10B109.5O11—C41—C43104.6 (6)
C9—C10—H10C109.5C42—C41—C43111.4 (7)
H10A—C10—H10C109.5C44—C41—C43110.4 (6)
H10B—C10—H10C109.5C41—C42—H42A109.5
C9—C11—H11A109.5C41—C42—H42B109.5
C9—C11—H11B109.5H42A—C42—H42B109.5
H11A—C11—H11B109.5C41—C42—H42C109.5
C9—C11—H11C109.5H42A—C42—H42C109.5
H11A—C11—H11C109.5H42B—C42—H42C109.5
H11B—C11—H11C109.5C41—C43—H43A109.5
C9—C12—H12A109.5C41—C43—H43B109.5
C9—C12—H12B109.5H43A—C43—H43B109.5
H12A—C12—H12B109.5C41—C43—H43C109.5
C9—C12—H12C109.5H43A—C43—H43C109.5
H12A—C12—H12C109.5H43B—C43—H43C109.5
H12B—C12—H12C109.5C41—C44—H44A109.5
O4—C13—C14106.1 (5)C41—C44—H44B109.5
O4—C13—C16110.1 (5)H44A—C44—H44B109.5
C14—C13—C16110.4 (6)C41—C44—H44C109.5
O4—C13—C15107.6 (5)H44A—C44—H44C109.5
C14—C13—C15110.9 (6)H44B—C44—H44C109.5
C16—C13—C15111.5 (6)O12—C45—C48113.2 (8)
C13—C14—H14A109.5O12—C45—C46106.5 (8)
C13—C14—H14B109.5C48—C45—C46110.7 (10)
H14A—C14—H14B109.5O12—C45—C47106.0 (8)
C13—C14—H14C109.5C48—C45—C47113.8 (9)
H14A—C14—H14C109.5C46—C45—C47106.1 (9)
H14B—C14—H14C109.5C45—C46—H46A109.5
C13—C15—H15A109.5C45—C46—H46B109.5
C13—C15—H15B109.5H46A—C46—H46B109.5
H15A—C15—H15B109.5C45—C46—H46C109.5
C13—C15—H15C109.5H46A—C46—H46C109.5
H15A—C15—H15C109.5H46B—C46—H46C109.5
H15B—C15—H15C109.5C45—C47—H47A109.5
C13—C16—H16A109.5C45—C47—H47B109.5
C13—C16—H16B109.5H47A—C47—H47B109.5
H16A—C16—H16B109.5C45—C47—H47C109.5
C13—C16—H16C109.5H47A—C47—H47C109.5
H16A—C16—H16C109.5H47B—C47—H47C109.5
H16B—C16—H16C109.5C45—C48—H48A109.5
O5—C17—C18110.9 (6)C45—C48—H48B109.5
O5—C17—C19109.3 (6)H48A—C48—H48B109.5
C18—C17—C19112.4 (7)C45—C48—H48C109.5
O5—C17—C20104.4 (6)H48A—C48—H48C109.5
C18—C17—C20109.7 (8)H48B—C48—H48C109.5
C19—C17—C20109.9 (7)N1—C49—C50122.9 (6)
C17—C18—H18A109.5N1—C49—H49118.5
C17—C18—H18B109.5C50—C49—H49118.5
H18A—C18—H18B109.5C49—C50—C51119.4 (5)
C17—C18—H18C109.5C49—C50—H50120.3
H18A—C18—H18C109.5C51—C50—H50120.3
H18B—C18—H18C109.5C58—C51—C50117.2 (5)
C17—C19—H19A109.5C58—C51—C52120.9 (6)
C17—C19—H19B109.5C50—C51—C52121.7 (5)
H19A—C19—H19B109.5C53—C52—C57117.5 (6)
C17—C19—H19C109.5C53—C52—C51121.6 (6)
H19A—C19—H19C109.5C57—C52—C51120.7 (6)
H19B—C19—H19C109.5C54—C53—C52119.8 (6)
C17—C20—H20A109.5C54—C53—H53120.1
C17—C20—H20B109.5C52—C53—H53120.1
H20A—C20—H20B109.5N2—C54—C53122.9 (6)
C17—C20—H20C109.5N2—C54—H54118.6
H20A—C20—H20C109.5C53—C54—H54118.6
H20B—C20—H20C109.5N2—C56—C57122.9 (6)
O6—C21—C22110.7 (5)N2—C56—H56118.6
O6—C21—C23110.3 (6)C57—C56—H56118.6
C22—C21—C23111.0 (6)C56—C57—C52118.9 (6)
O6—C21—C24105.2 (5)C56—C57—H57120.6
C22—C21—C24110.0 (6)C52—C57—H57120.6
C23—C21—C24109.5 (6)C59—C58—C51119.9 (6)
C21—C22—H22A109.5C59—C58—H58120
C21—C22—H22B109.5C51—C58—H58120
H22A—C22—H22B109.5N1—C59—C58122.5 (5)
C21—C22—H22C109.5N1—C59—H59118.7
H22A—C22—H22C109.5C58—C59—H59118.7
H22B—C22—H22C109.5O13—C60—H60A109.5
C21—C23—H23A109.5O13—C60—H60B109.5
C21—C23—H23B109.5H60A—C60—H60B109.5
H23A—C23—H23B109.5O13—C60—H60C109.5
C21—C23—H23C109.5H60A—C60—H60C109.5
H23A—C23—H23C109.5H60B—C60—H60C109.5
H23B—C23—H23C109.5C60—O13—Zn2124.5 (4)
C21—C24—H24A109.5C60—O13—H13A111 (5)
C21—C24—H24B109.5Zn2—O13—H13A117 (4)
N1—Zn1—S1—Si184.07 (16)O4—Zn1—N1—C59−102.5 (5)
S2—Zn1—S1—Si1−109.63 (11)S2—Zn1—N1—C49−2.2 (5)
O1—Zn1—S1—Si1−4.64 (12)S1—Zn1—N1—C49168.3 (4)
O4—Zn1—S1—Si1176.98 (12)O1—Zn1—N1—C49−113.6 (5)
N1—Zn1—S2—Si292.88 (17)O4—Zn1—N1—C4971.6 (5)
S1—Zn1—S2—Si2−73.10 (12)O13—Zn2—N2—C54−87.8 (5)
O1—Zn1—S2—Si2−166.61 (12)S4—Zn2—N2—C5413.4 (5)
O4—Zn1—S2—Si28.02 (11)S3—Zn2—N2—C54169.4 (5)
N2—Zn2—S3—Si3−73.62 (17)O13—Zn2—N2—C5696.7 (5)
O13—Zn2—S3—Si3−171.46 (13)S4—Zn2—N2—C56−162.1 (4)
S4—Zn2—S3—Si370.56 (12)S3—Zn2—N2—C56−6.1 (5)
N2—Zn2—S4—Si4−141.77 (16)Si1—O1—C1—C2−42.1 (8)
O13—Zn2—S4—Si4−45.08 (15)Zn1—O1—C1—C2160.4 (5)
S3—Zn2—S4—Si473.25 (12)Si1—O1—C1—C3−162.2 (5)
Zn1—S1—Si1—O3130.0 (2)Zn1—O1—C1—C340.3 (8)
Zn1—S1—Si1—O2−105.65 (18)Si1—O1—C1—C479.0 (6)
Zn1—S1—Si1—O16.58 (17)Zn1—O1—C1—C4−78.5 (7)
Zn1—S2—Si2—O5111.0 (2)Si1—O2—C5—C840.1 (9)
Zn1—S2—Si2—O6−127.46 (19)Si1—O2—C5—C6−82.2 (7)
Zn1—S2—Si2—O4−12.39 (17)Si1—O2—C5—C7160.4 (6)
Zn2—S3—Si3—O910.0 (2)Si1—O3—C9—C12−44.4 (9)
Zn2—S3—Si3—O8123.7 (2)Si1—O3—C9—C10−164.8 (6)
Zn2—S3—Si3—O7−114.32 (19)Si1—O3—C9—C1176.6 (7)
Zn2—S4—Si4—O12−49.28 (19)Si2—O4—C13—C14−158.0 (5)
Zn2—S4—Si4—O11−176.06 (18)Zn1—O4—C13—C1428.1 (8)
Zn2—S4—Si4—O1065.8 (2)Si2—O4—C13—C16−38.6 (7)
O3—Si1—O1—C165.0 (6)Zn1—O4—C13—C16147.6 (5)
O2—Si1—O1—C1−49.0 (6)Si2—O4—C13—C1583.2 (6)
S1—Si1—O1—C1−170.2 (5)Zn1—O4—C13—C15−90.7 (6)
O3—Si1—O1—Zn1−131.1 (2)Si2—O5—C17—C18−43.3 (9)
O2—Si1—O1—Zn1114.8 (2)Si2—O5—C17—C1981.1 (8)
S1—Si1—O1—Zn1−6.34 (16)Si2—O5—C17—C20−161.4 (6)
N1—Zn1—O1—C161.1 (5)Si2—O6—C21—C2240.5 (8)
S2—Zn1—O1—C1−52.5 (5)Si2—O6—C21—C23−82.7 (7)
S1—Zn1—O1—C1168.8 (5)Si2—O6—C21—C24159.3 (5)
N1—Zn1—O1—Si1−101.9 (2)Si3—O7—C25—C2833.0 (8)
S2—Zn1—O1—Si1144.49 (14)Si3—O7—C25—C27−89.5 (6)
S1—Zn1—O1—Si15.79 (15)Si3—O7—C25—C26152.3 (5)
O3—Si1—O2—C545.9 (6)Si3—O8—C29—C30−8.7 (14)
O1—Si1—O2—C5165.6 (6)Si3—O8—C29—C31−134.9 (7)
S1—Si1—O2—C5−83.4 (6)Si3—O8—C29—C32109.3 (8)
O2—Si1—O3—C9−163.3 (6)Si3—O9—C33—C35103.0 (10)
O1—Si1—O3—C983.5 (6)Si3—O9—C33—C36A29.3 (15)
S1—Si1—O3—C9−33.6 (6)Si3—O9—C33—C34A−102.3 (13)
O5—Si2—O4—C1370.5 (5)Si3—O9—C33—C34−131.5 (11)
O6—Si2—O4—C13−43.7 (5)Si3—O9—C33—C35A145.4 (9)
S2—Si2—O4—C13−164.9 (5)Si3—O9—C33—C36−16.0 (11)
O5—Si2—O4—Zn1−113.6 (2)Si4—O10—C37—C38−163.9 (5)
O6—Si2—O4—Zn1132.24 (19)Si4—O10—C37—C39−43.8 (8)
S2—Si2—O4—Zn110.98 (15)Si4—O10—C37—C4079.3 (8)
N1—Zn1—O4—C1353.2 (5)Si4—O11—C41—C42−84.6 (7)
S2—Zn1—O4—C13165.1 (5)Si4—O11—C41—C4437.3 (9)
S1—Zn1—O4—C13−54.9 (5)Si4—O11—C41—C43156.2 (6)
N1—Zn1—O4—Si2−122.2 (2)Si4—O12—C45—C4817.0 (14)
S2—Zn1—O4—Si2−10.24 (14)Si4—O12—C45—C46−104.8 (9)
S1—Zn1—O4—Si2129.79 (16)Si4—O12—C45—C47142.5 (7)
O6—Si2—O5—C17−170.3 (6)C59—N1—C49—C502.3 (9)
O4—Si2—O5—C1774.6 (7)Zn1—N1—C49—C50−171.9 (5)
S2—Si2—O5—C17−43.1 (7)N1—C49—C50—C510.3 (10)
O5—Si2—O6—C2138.7 (6)C49—C50—C51—C58−3.2 (9)
O4—Si2—O6—C21158.6 (5)C49—C50—C51—C52172.0 (6)
S2—Si2—O6—C21−88.4 (5)C58—C51—C52—C53146.2 (7)
O9—Si3—O7—C25−80.1 (6)C50—C51—C52—C53−28.8 (10)
O8—Si3—O7—C25166.6 (5)C58—C51—C52—C57−30.0 (9)
S3—Si3—O7—C2540.9 (6)C50—C51—C52—C57155.1 (6)
O9—Si3—O8—C29−177.0 (8)C57—C52—C53—C541.8 (10)
O7—Si3—O8—C29−58.6 (8)C51—C52—C53—C54−174.5 (6)
S3—Si3—O8—C2968.7 (8)C56—N2—C54—C53−2.4 (10)
O8—Si3—O9—C3359.0 (6)Zn2—N2—C54—C53−178.0 (5)
O7—Si3—O9—C33−55.1 (6)C52—C53—C54—N20.3 (10)
S3—Si3—O9—C33178.5 (5)C54—N2—C56—C572.3 (9)
O12—Si4—O10—C37−159.1 (5)Zn2—N2—C56—C57178.0 (5)
O11—Si4—O10—C37−38.6 (6)N2—C56—C57—C52−0.2 (10)
S4—Si4—O10—C3783.8 (5)C53—C52—C57—C56−1.8 (10)
O12—Si4—O11—C41−80.9 (6)C51—C52—C57—C56174.5 (6)
O10—Si4—O11—C41165.3 (6)C50—C51—C58—C593.6 (9)
S4—Si4—O11—C4142.4 (6)C52—C51—C58—C59−171.6 (6)
O11—Si4—O12—C45−62.1 (9)C49—N1—C59—C58−1.9 (9)
O10—Si4—O12—C4551.9 (9)Zn1—N1—C59—C58172.5 (5)
S4—Si4—O12—C45172.3 (8)C51—C58—C59—N1−1.1 (10)
S2—Zn1—N1—C59−176.4 (4)N2—Zn2—O13—C60−92.0 (5)
S1—Zn1—N1—C59−5.9 (5)S4—Zn2—O13—C60161.5 (5)
O1—Zn1—N1—C5972.3 (5)S3—Zn2—O13—C6018.4 (5)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O13—H13A···O100.99 (1)1.86 (4)2.771 (6)151 (6)
Table 1
Selected geometric parameters (Å, °) top
Zn1—N12.075 (5)Zn2—S42.2627 (16)
Zn1—S22.2664 (18)Zn2—S32.2704 (17)
Zn1—S12.2732 (16)S1—Si12.075 (2)
Zn1—O12.357 (4)S2—Si22.092 (2)
Zn1—O42.554 (4)S3—Si32.091 (2)
Zn2—N22.098 (5)S4—Si42.076 (2)
Zn2—O132.156 (5)
N1—Zn1—S2111.39 (14)N2—Zn2—O1393.72 (19)
N1—Zn1—S1107.81 (15)N2—Zn2—S4105.61 (15)
S2—Zn1—S1139.71 (7)O13—Zn2—S499.79 (13)
N1—Zn1—O192.46 (17)N2—Zn2—S3109.24 (15)
S2—Zn1—O1108.85 (12)O13—Zn2—S3100.81 (13)
S1—Zn1—O177.94 (11)S4—Zn2—S3137.87 (6)
N1—Zn1—O490.91 (17)Si1—S1—Zn185.98 (7)
S2—Zn1—O474.68 (10)Si2—S2—Zn189.35 (8)
S1—Zn1—O496.04 (11)Si3—S3—Zn293.88 (8)
O1—Zn1—O4173.77 (14)Si4—S4—Zn299.32 (8)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O13—H13A···O100.99 (1)1.86 (4)2.771 (6)151 (6)
Acknowledgements top

This work was undertaken with financial support from the Polish State Committee, grant No. 3 T09A 12028.

references
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