supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers buy article online

ng2366 scheme

Acta Cryst. (2007). E63, m3072    [ doi:10.1107/S1600536807057947 ]

([mu]-4,4'-Bipyridyl-[kappa]2N:N')bis[bis(tri-tert-butoxysilanethiolato-[kappa]2S,O)cadmium(II)] toluene disolvate

A. Dolega, K. Baranowska and A. Pladzyk

Abstract top

The structure of the title compound, [Cd2(C12H27O3SSi)4(C10H8N2)]·2C7H8, consists of discrete molecules, with the two halves of the complex molecule related to each other by inversion symmetry. Two (tri-tert-butoxysilanothiolato)cadmium units are bridged through the 4,4'-bipyridyl ligand. The geometry of the CdII atoms is intermediate between square-pyramidal and trigonal-bipyramidal. The solvent toluene molecules pack in the voids between the mid-point of the 4,4'-bipyridine and the tert-butyl groups of an adjacent complex. There is disorder in the 4,4'-bipyridine molecule, with site occupancies of 0.506 (7):0.494 (7).

Comment top

The asymmetric unit of (I) consists of one half-molecule of the complex and one toluene molecule. An inversion centre is located at the mid-point of the bridging C—C bond of the 4,4'-bipyridine, at Wyckoff position c (0,1/2,0). The 4,4'-bipy rings in compound (I) exhibit deviation from planarity, which is most probably "artificial" effect resulting from the disorder of the bipyridine moiety. The environment of the Cd can be approximated either to trigonal–bipyramidal or square pyramidal, but distortions are found for both approximations. Molecules of (I) pack in the crystal structure as discrete entities with no interactions other than van der Waals. Also position of solvating toluene is such that no pi-pi stacking can be considered.

Related literature top

For an analogous compound as the THF solvate, see: Pladzyk et al. (2007). For the synthetic procedure, see: Wojnowski et al. (1992).

Experimental top

Compound (I) was synthesized from dimeric cadmium bis(tri-tert-butoxysilanethiolate) (Wojnowski et al. 1992). Cadmium bis(tri-tert-butoxysilanethiolate) (1.00 g; 0.75 mmol) was suspended in ethanol (40 ml). 4,4'-bipyridine (0.23 g, 1,5 mmol) and toluene (8 ml) were added to the suspension and the reaction mixture was heated for 1 h. The solution, kept at 269 K, yielded colourless needles suitable for X-ray analysis after approx. one month.

Refinement top

All C—H hydrogen atoms were refined as riding on carbon atoms with methyl C—H = 0.98 Å, aromatic C—H = 0.95 Å and Uiso(H) = 1.2Ueq(C) for aromatic CH and 1.5Ueq(C) for methyl groups. Atoms C25–C26, and C28–C29 in the 4,4'-bipyridine molecule is disordered (0.506 (7)/0.494 (7)).

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, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); 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 molecule of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted.
(µ-4,4'-Bipyridyl-κ2N:N')bis[bis(tri-tert- butoxysilanethiolato-κ2S,O)cadmium(II)] toluene disolvate top
Crystal data top
[Cd2(C12H27O3SSi)4(C10H8N2)]·2C7H8F000 = 1780
Mr = 1683.2Dx = 1.269 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 27489 reflections
a = 9.8095 (2) Åθ = 2.1–32.5º
b = 19.4290 (5) ŵ = 0.68 mm−1
c = 23.1842 (6) ÅT = 120 (2) K
β = 94.355 (2)ºPrism, colourless
V = 4405.89 (18) Å30.14 × 0.10 × 0.08 mm
Z = 2
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		7785 independent reflections
Monochromator: graphite6924 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm-1Rint = 0.021
T = 120(2) Kθmax = 25.1º
ω scans, 0.70 deg widthθmin = 2.1º
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2006)		h = −11→11
Tmin = 0.962, Tmax = 1.056k = −23→23
27639 measured reflectionsl = −15→27
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.082  w = 1/[σ2(Fo2) + (0.0492P)2 + 1.2954P]
where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max = 0.002
7785 reflectionsΔρmax = 0.88 e Å−3
453 parametersΔρmin = −0.4 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Cd2(C12H27O3SSi)4(C10H8N2)]·2C7H8V = 4405.89 (18) Å3
Mr = 1683.2Z = 2
Monoclinic, P21/cMo Kα
a = 9.8095 (2) ŵ = 0.68 mm−1
b = 19.4290 (5) ÅT = 120 (2) K
c = 23.1842 (6) Å0.14 × 0.10 × 0.08 mm
β = 94.355 (2)º
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		7785 independent reflections
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2006)		6924 reflections with I > 2σ(I)
Tmin = 0.962, Tmax = 1.056Rint = 0.021
27639 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.027453 parameters
wR(F2) = 0.082H-atom parameters constrained
S = 1.17Δρmax = 0.88 e Å−3
7785 reflectionsΔρmin = −0.4 e Å−3
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 F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > σ(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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)
C10.7392 (2)0.39873 (11)0.24469 (9)0.0274 (5)
C20.8606 (3)0.43098 (18)0.21823 (12)0.0552 (8)
H2A0.90380.39680.19440.083*
H2B0.9270.44690.24910.083*
H2C0.82960.47020.1940.083*
C30.7834 (3)0.33610 (14)0.27929 (11)0.0495 (7)
H3A0.70380.31520.29550.074*
H3B0.85040.34950.31080.074*
H3C0.8250.30280.25410.074*
C40.6690 (3)0.44959 (17)0.28178 (13)0.0575 (9)
H4A0.64570.49120.25920.086*
H4B0.73030.46170.31560.086*
H4C0.58530.42890.29460.086*
C50.3733 (2)0.51955 (11)0.14177 (9)0.0290 (5)
C60.3849 (3)0.58743 (12)0.17434 (11)0.0370 (6)
H6A0.36790.57970.2150.056*
H6B0.31730.620.1570.056*
H6C0.47690.60640.17210.056*
C70.2310 (2)0.48915 (13)0.14482 (12)0.0404 (6)
H7A0.22470.44570.12330.061*
H7B0.16270.52150.12780.061*
H7C0.2140.48070.18530.061*
C80.4073 (3)0.52946 (13)0.07947 (10)0.0453 (7)
H8A0.5010.54670.07880.068*
H8B0.34370.56280.06050.068*
H8C0.3990.48530.0590.068*
C90.3271 (2)0.31123 (11)0.25002 (10)0.0308 (5)
C100.4065 (3)0.24675 (12)0.23669 (12)0.0410 (6)
H10A0.40610.2410.19470.062*
H10B0.36370.20660.25350.062*
H10C0.5010.25110.25330.062*
C110.1852 (3)0.30822 (15)0.22104 (16)0.0566 (8)
H11A0.13490.34980.23050.085*
H11B0.13790.26760.23460.085*
H11C0.19010.30540.1790.085*
C120.3263 (4)0.32048 (14)0.31497 (12)0.0596 (9)
H12A0.42060.3240.3320.089*
H12B0.28150.28080.33160.089*
H12C0.27640.36260.32320.089*
C130.6504 (2)0.19441 (11)−0.02055 (8)0.0220 (4)
C140.5048 (2)0.17276 (12)−0.01138 (9)0.0278 (5)
H14A0.50550.12690.00630.042*
H14B0.45090.1715−0.04870.042*
H14C0.46410.20590.01420.042*
C150.6525 (3)0.26376 (13)−0.05094 (10)0.0355 (5)
H15A0.60780.2983−0.0280.053*
H15B0.60370.2601−0.08930.053*
H15C0.74740.2775−0.05510.053*
C160.7220 (2)0.13953 (12)−0.05393 (9)0.0312 (5)
H16A0.81650.1537−0.05840.047*
H16B0.67370.1336−0.09220.047*
H16C0.7220.0959−0.03270.047*
C171.0884 (2)0.11565 (12)0.06581 (10)0.0307 (5)
C181.1722 (3)0.17525 (16)0.09261 (13)0.0487 (7)
H18A1.17420.21290.06450.073*
H18B1.26570.15960.10330.073*
H18C1.13050.19150.12720.073*
C191.0757 (3)0.05792 (16)0.10891 (13)0.0529 (8)
H19A1.03530.07580.14330.079*
H19B1.16650.0390.12010.079*
H19C1.0170.02160.09130.079*
C201.1515 (3)0.08867 (14)0.01263 (11)0.0402 (6)
H20A1.09580.0507−0.00410.06*
H20B1.24420.07210.02350.06*
H20C1.15530.1257−0.01590.06*
C210.6584 (2)0.04645 (11)0.12376 (9)0.0244 (4)
C220.5906 (3)−0.01292 (12)0.08980 (10)0.0355 (5)
H22A0.53580.00520.05610.053*
H22B0.5313−0.03820.11450.053*
H22C0.661−0.04390.07690.053*
C230.7478 (2)0.02003 (12)0.17520 (9)0.0318 (5)
H23A0.8164−0.01170.16180.048*
H23B0.6911−0.00420.20170.048*
H23C0.79390.05890.19540.048*
C240.5507 (2)0.09622 (12)0.14296 (10)0.0333 (5)
H24A0.59570.13440.16440.05*
H24B0.49010.0720.16790.05*
H24C0.4970.11420.10890.05*
C250.7600 (6)0.4345 (3)0.0605 (2)0.0221 (14)*0.506 (7)
H250.67190.44490.07240.046 (15)*0.506 (7)
C260.8326 (6)0.4849 (3)0.0335 (3)0.0240 (15)*0.506 (7)
H260.79230.52910.02770.021 (11)*0.506 (7)
C281.0182 (5)0.4047 (2)0.0324 (2)0.0236 (12)*0.506 (7)
H281.10980.39380.02520.028*0.506 (7)
C290.9401 (5)0.3570 (2)0.0589 (2)0.0230 (11)*0.506 (7)
H290.97620.31310.06960.028*0.506 (7)
C25A0.7814 (6)0.4448 (3)0.0718 (3)0.0251 (15)*0.494 (7)
H25A0.70820.4590.09360.038 (14)*0.494 (7)
C26A0.8515 (6)0.4949 (3)0.0451 (3)0.0227 (15)*0.494 (7)
H26A0.82670.5420.04720.033 (13)*0.494 (7)
C28A0.9814 (5)0.4081 (2)0.0044 (2)0.0229 (12)*0.494 (7)
H28A1.04570.394−0.02190.027*0.494 (7)
C29A0.9070 (5)0.3604 (2)0.0330 (2)0.0231 (11)*0.494 (7)
H29A0.92630.31320.02650.028*0.494 (7)
C270.9606 (2)0.47356 (11)0.01469 (10)0.0292 (5)
C300.0194 (3)0.20285 (15)0.37305 (14)0.0499 (7)
H30−0.06960.21670.35850.06*
C310.0754 (3)0.23122 (17)0.42372 (13)0.0514 (7)
H310.0250.26390.44390.062*
C320.2049 (3)0.21219 (13)0.44523 (13)0.0435 (6)
H320.24460.2320.480.052*
C330.2757 (3)0.16450 (13)0.41587 (13)0.0457 (7)
H330.36450.15090.43070.055*
C340.2196 (3)0.13602 (13)0.36497 (12)0.0419 (6)
H340.27070.10340.34510.05*
C350.0899 (3)0.15424 (12)0.34249 (11)0.0388 (6)
C360.0282 (4)0.12362 (16)0.28714 (12)0.0587 (8)
H36A0.09960.11720.26030.088*
H36B−0.04220.15470.26980.088*
H36C−0.01310.0790.29520.088*
Cd10.681416 (15)0.293346 (7)0.114331 (6)0.02303 (7)
N10.80907 (19)0.37450 (9)0.06946 (8)0.0289 (4)
O10.64763 (14)0.37525 (8)0.19596 (6)0.0254 (3)
O20.47662 (15)0.47464 (7)0.16934 (6)0.0251 (3)
O30.39076 (15)0.37287 (7)0.22922 (6)0.0257 (3)
O40.72132 (15)0.20541 (6)0.03641 (6)0.0209 (3)
O50.95533 (14)0.14222 (7)0.04608 (6)0.0232 (3)
O60.74521 (15)0.07929 (7)0.08393 (6)0.0239 (3)
S10.44513 (5)0.33544 (3)0.10046 (2)0.02512 (12)
S20.84466 (6)0.20885 (3)0.15666 (2)0.02556 (13)
Si10.48493 (5)0.39138 (3)0.17697 (2)0.01919 (12)
Si20.81719 (5)0.15393 (3)0.07939 (2)0.01791 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0249 (11)0.0306 (11)0.0255 (11)0.0020 (9)−0.0051 (9)−0.0093 (9)
C20.0426 (16)0.078 (2)0.0428 (16)−0.0268 (15)−0.0084 (12)−0.0029 (14)
C30.078 (2)0.0430 (15)0.0250 (13)0.0088 (14)−0.0131 (13)−0.0032 (11)
C40.0446 (16)0.070 (2)0.0550 (18)0.0200 (14)−0.0185 (13)−0.0426 (16)
C50.0336 (12)0.0243 (11)0.0287 (11)0.0039 (9)−0.0008 (9)0.0041 (9)
C60.0467 (15)0.0263 (12)0.0387 (13)0.0047 (10)0.0072 (11)0.0014 (10)
C70.0303 (13)0.0367 (14)0.0525 (15)0.0050 (10)−0.0079 (11)0.0028 (11)
C80.0710 (19)0.0338 (13)0.0310 (13)0.0082 (13)0.0041 (12)0.0064 (10)
C90.0374 (13)0.0212 (10)0.0358 (12)−0.0076 (9)0.0160 (10)−0.0020 (9)
C100.0484 (15)0.0264 (12)0.0499 (15)0.0004 (11)0.0147 (12)0.0062 (11)
C110.0326 (15)0.0422 (15)0.096 (2)−0.0107 (12)0.0097 (15)0.0036 (16)
C120.107 (3)0.0355 (15)0.0413 (16)−0.0214 (16)0.0364 (16)−0.0031 (12)
C130.0222 (10)0.0257 (10)0.0173 (10)−0.0011 (8)−0.0030 (8)0.0005 (8)
C140.0223 (11)0.0341 (12)0.0264 (11)−0.0023 (9)−0.0023 (8)−0.0029 (9)
C150.0357 (13)0.0368 (13)0.0330 (13)−0.0037 (10)−0.0045 (10)0.0125 (10)
C160.0306 (12)0.0419 (13)0.0211 (11)0.0032 (10)0.0018 (9)−0.0071 (9)
C170.0181 (10)0.0386 (13)0.0355 (12)0.0064 (9)0.0028 (9)0.0029 (10)
C180.0224 (13)0.0686 (19)0.0546 (17)−0.0019 (12)−0.0005 (11)−0.0181 (15)
C190.0419 (16)0.0657 (19)0.0515 (17)0.0263 (14)0.0066 (13)0.0242 (14)
C200.0296 (13)0.0443 (14)0.0480 (15)0.0058 (11)0.0120 (11)−0.0040 (12)
C210.0285 (11)0.0243 (11)0.0212 (10)−0.0066 (9)0.0072 (8)0.0016 (8)
C220.0439 (14)0.0343 (13)0.0293 (12)−0.0179 (11)0.0085 (10)−0.0021 (10)
C230.0388 (13)0.0288 (12)0.0280 (11)−0.0030 (10)0.0047 (10)0.0060 (9)
C240.0311 (12)0.0361 (13)0.0342 (12)−0.0011 (10)0.0124 (10)0.0045 (10)
C270.0262 (11)0.0274 (11)0.0353 (12)−0.0081 (9)0.0109 (9)−0.0119 (9)
C300.0332 (15)0.0565 (18)0.0591 (18)0.0040 (12)−0.0027 (13)0.0149 (14)
C310.0401 (16)0.0587 (18)0.0571 (18)0.0004 (14)0.0147 (13)0.0002 (15)
C320.0398 (15)0.0449 (15)0.0459 (15)−0.0157 (12)0.0029 (12)0.0059 (12)
C330.0316 (14)0.0360 (14)0.0674 (18)−0.0092 (11)−0.0092 (13)0.0115 (13)
C340.0356 (14)0.0314 (13)0.0584 (17)−0.0046 (10)0.0024 (12)0.0056 (12)
C350.0425 (14)0.0324 (13)0.0404 (14)−0.0095 (11)−0.0032 (11)0.0179 (11)
C360.073 (2)0.0538 (18)0.0471 (17)−0.0127 (16)−0.0137 (15)0.0145 (14)
Cd10.02256 (10)0.02152 (10)0.02558 (10)−0.00129 (6)0.00542 (6)−0.00431 (6)
N10.0275 (10)0.0277 (10)0.0328 (10)−0.0055 (8)0.0099 (8)−0.0082 (8)
O10.0209 (7)0.0301 (8)0.0250 (7)0.0021 (6)−0.0007 (6)−0.0111 (6)
O20.0268 (8)0.0209 (7)0.0275 (8)−0.0012 (6)0.0000 (6)0.0018 (6)
O30.0312 (8)0.0197 (7)0.0275 (8)−0.0043 (6)0.0112 (6)−0.0011 (6)
O40.0217 (8)0.0205 (7)0.0200 (7)0.0010 (5)−0.0019 (6)−0.0024 (5)
O50.0174 (7)0.0289 (8)0.0234 (7)0.0009 (6)0.0025 (6)0.0026 (6)
O60.0295 (8)0.0218 (7)0.0214 (7)−0.0046 (6)0.0087 (6)−0.0004 (6)
S10.0229 (3)0.0292 (3)0.0232 (3)−0.0020 (2)0.0007 (2)−0.0060 (2)
S20.0284 (3)0.0266 (3)0.0210 (3)−0.0005 (2)−0.0026 (2)−0.00446 (19)
Si10.0188 (3)0.0192 (3)0.0198 (3)−0.0014 (2)0.0034 (2)−0.0011 (2)
Si20.0174 (3)0.0184 (3)0.0180 (3)−0.0008 (2)0.0017 (2)0.0000 (2)
Geometric parameters (Å, °) top
C1—O11.462 (2)C21—O61.451 (2)
C1—C31.503 (3)C21—C231.515 (3)
C1—C41.510 (3)C21—C221.521 (3)
C1—C21.516 (4)C21—C241.523 (3)
C2—H2A0.98C22—H22A0.98
C2—H2B0.98C22—H22B0.98
C2—H2C0.98C22—H22C0.98
C3—H3A0.98C23—H23A0.98
C3—H3B0.98C23—H23B0.98
C3—H3C0.98C23—H23C0.98
C4—H4A0.98C24—H24A0.98
C4—H4B0.98C24—H24B0.98
C4—H4C0.98C24—H24C0.98
C5—O21.449 (3)C25—N11.272 (5)
C5—C81.519 (3)C25—C261.388 (8)
C5—C61.520 (3)C25—H250.95
C5—C71.522 (3)C26—C271.378 (6)
C6—H6A0.98C26—H260.95
C6—H6B0.98C28—C291.377 (6)
C6—H6C0.98C28—C271.497 (5)
C7—H7A0.98C28—H280.95
C7—H7B0.98C29—N11.369 (5)
C7—H7C0.98C29—H290.95
C8—H8A0.98C25A—C26A1.365 (8)
C8—H8B0.98C25A—N11.395 (6)
C8—H8C0.98C25A—H25A0.95
C9—O31.450 (2)C26A—C271.389 (6)
C9—C111.501 (4)C26A—H26A0.95
C9—C121.517 (3)C28A—C271.313 (5)
C9—C101.519 (3)C28A—C29A1.380 (6)
C10—H10A0.98C28A—H28A0.95
C10—H10B0.98C29A—N11.355 (5)
C10—H10C0.98C29A—H29A0.95
C11—H11A0.98C27—C27i1.482 (4)
C11—H11B0.98C30—C311.374 (4)
C11—H11C0.98C30—C351.395 (4)
C12—H12A0.98C30—H300.95
C12—H12B0.98C31—C321.379 (4)
C12—H12C0.98C31—H310.95
C13—O41.461 (2)C32—C331.370 (4)
C13—C141.519 (3)C32—H320.95
C13—C161.520 (3)C33—C341.379 (4)
C13—C151.521 (3)C33—H330.95
C14—H14A0.98C34—C351.384 (4)
C14—H14B0.98C34—H340.95
C14—H14C0.98C35—C361.500 (4)
C15—H15A0.98C36—H36A0.98
C15—H15B0.98C36—H36B0.98
C15—H15C0.98C36—H36C0.98
C16—H16A0.98Cd1—N12.3097 (18)
C16—H16B0.98Cd1—S22.4462 (5)
C16—H16C0.98Cd1—S12.4560 (5)
C17—O51.445 (3)Cd1—O12.5137 (13)
C17—C191.514 (3)Cd1—O42.5384 (13)
C17—C201.515 (3)Cd1—Si13.1428 (5)
C17—C181.525 (4)Cd1—Si23.1514 (5)
C18—H18A0.98O1—Si11.6530 (15)
C18—H18B0.98O2—Si11.6286 (15)
C18—H18C0.98O3—Si11.6187 (14)
C19—H19A0.98O4—Si21.6538 (14)
C19—H19B0.98O5—Si21.6259 (14)
C19—H19C0.98O6—Si21.6198 (14)
C20—H20A0.98S1—Si12.0916 (7)
C20—H20B0.98S2—Si22.0851 (7)
C20—H20C0.98
O1—C1—C3107.18 (18)H22B—C22—H22C109.5
O1—C1—C4111.37 (18)C21—C23—H23A109.5
C3—C1—C4110.6 (2)C21—C23—H23B109.5
O1—C1—C2105.77 (18)H23A—C23—H23B109.5
C3—C1—C2110.3 (2)C21—C23—H23C109.5
C4—C1—C2111.5 (2)H23A—C23—H23C109.5
C1—C2—H2A109.5H23B—C23—H23C109.5
C1—C2—H2B109.5C21—C24—H24A109.5
H2A—C2—H2B109.5C21—C24—H24B109.5
C1—C2—H2C109.5H24A—C24—H24B109.5
H2A—C2—H2C109.5C21—C24—H24C109.5
H2B—C2—H2C109.5H24A—C24—H24C109.5
C1—C3—H3A109.5H24B—C24—H24C109.5
C1—C3—H3B109.5N1—C25—C26121.4 (5)
H3A—C3—H3B109.5N1—C25—H25119.3
C1—C3—H3C109.5C26—C25—H25119.3
H3A—C3—H3C109.5C27—C26—C25122.7 (5)
H3B—C3—H3C109.5C27—C26—H26118.6
C1—C4—H4A109.5C25—C26—H26118.6
C1—C4—H4B109.5C29—C28—C27120.8 (4)
H4A—C4—H4B109.5C29—C28—H28119.6
C1—C4—H4C109.5C27—C28—H28119.6
H4A—C4—H4C109.5N1—C29—C28118.4 (4)
H4B—C4—H4C109.5N1—C29—H29120.8
O2—C5—C8107.42 (18)C28—C29—H29120.8
O2—C5—C6106.28 (18)C26A—C25A—N1125.0 (5)
C8—C5—C6110.43 (19)C26A—C25A—H25A117.5
O2—C5—C7111.03 (17)N1—C25A—H25A117.5
C8—C5—C7111.2 (2)C25A—C26A—C27116.9 (5)
C6—C5—C7110.3 (2)C25A—C26A—H26A121.6
C5—C6—H6A109.5C27—C26A—H26A121.6
C5—C6—H6B109.5C27—C28A—C29A117.9 (4)
H6A—C6—H6B109.5C27—C28A—H28A121
C5—C6—H6C109.5C29A—C28A—H28A121
H6A—C6—H6C109.5N1—C29A—C28A126.1 (4)
H6B—C6—H6C109.5N1—C29A—H29A116.9
C5—C7—H7A109.5C28A—C29A—H29A116.9
C5—C7—H7B109.5C28A—C27—C26111.7 (3)
H7A—C7—H7B109.5C28A—C27—C26A121.1 (3)
C5—C7—H7C109.5C28A—C27—C27i119.6 (3)
H7A—C7—H7C109.5C26—C27—C27i123.6 (3)
H7B—C7—H7C109.5C26A—C27—C27i118.4 (3)
C5—C8—H8A109.5C26—C27—C28113.0 (3)
C5—C8—H8B109.5C26A—C27—C28114.6 (3)
H8A—C8—H8B109.5C27i—C27—C28123.1 (3)
C5—C8—H8C109.5C31—C30—C35121.6 (3)
H8A—C8—H8C109.5C31—C30—H30119.2
H8B—C8—H8C109.5C35—C30—H30119.2
O3—C9—C11106.9 (2)C30—C31—C32120.0 (3)
O3—C9—C12105.50 (18)C30—C31—H31120
C11—C9—C12112.0 (2)C32—C31—H31120
O3—C9—C10111.91 (18)C33—C32—C31119.3 (3)
C11—C9—C10110.4 (2)C33—C32—H32120.4
C12—C9—C10109.9 (2)C31—C32—H32120.4
C9—C10—H10A109.5C32—C33—C34120.8 (3)
C9—C10—H10B109.5C32—C33—H33119.6
H10A—C10—H10B109.5C34—C33—H33119.6
C9—C10—H10C109.5C33—C34—C35121.0 (3)
H10A—C10—H10C109.5C33—C34—H34119.5
H10B—C10—H10C109.5C35—C34—H34119.5
C9—C11—H11A109.5C34—C35—C30117.3 (2)
C9—C11—H11B109.5C34—C35—C36121.4 (3)
H11A—C11—H11B109.5C30—C35—C36121.3 (3)
C9—C11—H11C109.5C35—C36—H36A109.5
H11A—C11—H11C109.5C35—C36—H36B109.5
H11B—C11—H11C109.5H36A—C36—H36B109.5
C9—C12—H12A109.5C35—C36—H36C109.5
C9—C12—H12B109.5H36A—C36—H36C109.5
H12A—C12—H12B109.5H36B—C36—H36C109.5
C9—C12—H12C109.5N1—Cd1—S2106.15 (5)
H12A—C12—H12C109.5N1—Cd1—S1104.61 (5)
H12B—C12—H12C109.5S2—Cd1—S1149.156 (19)
O4—C13—C14107.59 (16)N1—Cd1—O190.80 (6)
O4—C13—C16110.85 (16)S2—Cd1—O1104.03 (4)
C14—C13—C16110.64 (18)S1—Cd1—O173.18 (3)
O4—C13—C15105.48 (16)N1—Cd1—O491.19 (5)
C14—C13—C15110.86 (18)S2—Cd1—O472.67 (3)
C16—C13—C15111.24 (19)S1—Cd1—O4109.03 (3)
C13—C14—H14A109.5O1—Cd1—O4176.53 (5)
C13—C14—H14B109.5N1—Cd1—Si199.61 (5)
H14A—C14—H14B109.5S2—Cd1—Si1128.835 (17)
C13—C14—H14C109.5S1—Cd1—Si141.656 (15)
H14A—C14—H14C109.5O1—Cd1—Si131.56 (3)
H14B—C14—H14C109.5O4—Cd1—Si1150.45 (3)
C13—C15—H15A109.5N1—Cd1—Si2102.52 (5)
C13—C15—H15B109.5S2—Cd1—Si241.386 (15)
H15A—C15—H15B109.5S1—Cd1—Si2131.734 (16)
C13—C15—H15C109.5O1—Cd1—Si2145.10 (3)
H15A—C15—H15C109.5O4—Cd1—Si231.51 (3)
H15B—C15—H15C109.5Si1—Cd1—Si2157.776 (14)
C13—C16—H16A109.5C25—N1—C29A111.1 (3)
C13—C16—H16B109.5C25—N1—C29123.1 (3)
H16A—C16—H16B109.5C29A—N1—C25A111.8 (3)
C13—C16—H16C109.5C29—N1—C25A115.9 (3)
H16A—C16—H16C109.5C25—N1—Cd1119.2 (3)
H16B—C16—H16C109.5C29A—N1—Cd1125.3 (2)
O5—C17—C19110.87 (18)C29—N1—Cd1117.4 (2)
O5—C17—C20106.33 (18)C25A—N1—Cd1122.5 (3)
C19—C17—C20109.9 (2)C1—O1—Si1132.12 (12)
O5—C17—C18107.68 (19)C1—O1—Cd1132.14 (11)
C19—C17—C18111.3 (2)Si1—O1—Cd195.70 (6)
C20—C17—C18110.7 (2)C5—O2—Si1132.37 (13)
C17—C18—H18A109.5C9—O3—Si1135.81 (13)
C17—C18—H18B109.5C13—O4—Si2131.77 (12)
H18A—C18—H18B109.5C13—O4—Cd1130.78 (11)
C17—C18—H18C109.5Si2—O4—Cd195.15 (6)
H18A—C18—H18C109.5C17—O5—Si2131.67 (13)
H18B—C18—H18C109.5C21—O6—Si2135.64 (13)
C17—C19—H19A109.5Si1—S1—Cd187.05 (2)
C17—C19—H19B109.5Si2—S2—Cd187.75 (2)
H19A—C19—H19B109.5O3—Si1—O2105.98 (8)
C17—C19—H19C109.5O3—Si1—O1110.67 (8)
H19A—C19—H19C109.5O2—Si1—O1104.87 (8)
H19B—C19—H19C109.5O3—Si1—S1116.03 (6)
C17—C20—H20A109.5O2—Si1—S1114.79 (6)
C17—C20—H20B109.5O1—Si1—S1103.98 (5)
H20A—C20—H20B109.5O3—Si1—Cd1128.03 (6)
C17—C20—H20C109.5O2—Si1—Cd1125.39 (6)
H20A—C20—H20C109.5O1—Si1—Cd152.74 (5)
H20B—C20—H20C109.5S1—Si1—Cd151.299 (18)
O6—C21—C23108.50 (17)O6—Si2—O5106.78 (8)
O6—C21—C22104.99 (16)O6—Si2—O4110.48 (8)
C23—C21—C22110.78 (19)O5—Si2—O4104.76 (7)
O6—C21—C24111.12 (17)O6—Si2—S2115.52 (6)
C23—C21—C24110.98 (18)O5—Si2—S2114.94 (6)
C22—C21—C24110.30 (19)O4—Si2—S2103.81 (5)
C21—C22—H22A109.5O6—Si2—Cd1123.92 (5)
C21—C22—H22B109.5O5—Si2—Cd1128.77 (6)
H22A—C22—H22B109.5O4—Si2—Cd153.34 (5)
C21—C22—H22C109.5S2—Si2—Cd150.863 (19)
H22A—C22—H22C109.5
Symmetry codes: (i) −x+2, −y+1, −z.
Table 1
Selected geometric parameters (Å, °) top
Cd1—N12.3097 (18)Cd1—O42.5384 (13)
Cd1—S22.4462 (5)S1—Si12.0916 (7)
Cd1—S12.4560 (5)S2—Si22.0851 (7)
Cd1—O12.5137 (13)
N1—Cd1—S2106.15 (5)S1—Cd1—O173.18 (3)
N1—Cd1—S1104.61 (5)N1—Cd1—O491.19 (5)
S2—Cd1—S1149.156 (19)S2—Cd1—O472.67 (3)
N1—Cd1—O190.80 (6)S1—Cd1—O4109.03 (3)
S2—Cd1—O1104.03 (4)O1—Cd1—O4176.53 (5)
Acknowledgements top

The work was undertaken with financial support from the Polish State Committee, grant No. 3 T09A 12028. The authors thank Dr Jarosław Chojnacki for common-sense remarks [helpful comments?].

references
References top

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565–?.

Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.

Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Versions 1.171.29.9. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.

Pladzyk, A., Dołęga, A. & Baranowska, K. (2007). Acta Cryst. E63, m1434–m1436.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Wojnowski, W., Becker, B., Walz, L., von Peters, E.-M. & Schnering, H. G. (1992). Polyhedron, 11, 607–612.