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X-ray diffraction shows that the title cadmium(II) complex, [Cd2(C14H20O2)2(C5H5N)6]·2C5H5N, has a dimeric structure in which two (py)3Cd(3,5-di-tert-butylcatecholate) units (py is pyridine) are connected by two bridging O atoms, the coordination of the Cd atoms being distorted octahedral. There are two symmetrically independent dimers in the crystal structure; one is in a general position and the other lies about an inversion centre. In both cases, the bridging Cd—O distances between the Cd–catecholate units [2.224 (2)–2.237 (2) Å] are shorter than the bridging Cd—O distances within the catecholate cycle [2.273 (2)–2.281 (2) Å]. The Cd—Npy distances are 2.354 (2)–2.471 (2) Å. Besides the main mol­ecules, the crystal also contains pyridine solvate mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010100854X/av1076sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010100854X/av1076Isup2.hkl
Contains datablock I

CCDC reference: 173341

Comment top

The title compound, (I), was synthesized by the reaction of 3,5-di-tert-butyl-1,2-benzoquinone with cadmium in pyridine solution. The X-ray diffraction study shows that (I) is a dimeric complex of cadmium in which the two (py)3Cd(3,5-di-tert-butylcatecholato) units are connected by two bridging µ-O atoms, the environment of the Cd atoms being a distorted octahedron (Fig. 1). There are two symmetrically independent molecules of (I) in the crystal structure; one is in a general position, (Ia), and the other on an inversion centre, (Ib). Molecule (Ia) has an approximately centrosymmetric structure. \sch

The central Cd2O2 and the two chelate CdO2C2 fragments are planar within 0.004, 0.012 and 0.020 Å, respectively, for (Ia) and 0.007 and 0.007 Å, respectively, for (Ib). The dihedral angles between the Cd2O2 and the CdO2C2 fragments are 4.43 (14) and 6.15 (13)° for (Ia) and 6.93 (16)° for (Ib). The O—C and C—C distances in the chelate metallocycles in (I) [1.316 (3)–1.343 (3) and 1.381 (4)–1.441 (4) Å query, respectively] are typical for the catecholate ligand (Pierpont & Lange, 1994). The Cd—Npy distances in (I) are 2.373 (2)–2.440 (3) Å (Table 1) query.

In both (Ia) and (Ib), the bridging Cd—O distances between the Cd-catecholate units [2.224 (2)–2.237 (2) Å] are shorter than the bridging Cd—O distances within the catecholate cycles [2.278 (2)–2.281 (2) Å]. Similar features have been found in other dimeric and tetrameric catecholate complexes of different metals, e.g. Zn (Reynolds & Coucouvanis, 1998), Fe (Shoner & Power, 1992) and Co (Olmstead et al., 1988), as well as in the sulfur analogue on Zn, bis(µ-1,2-benzenedithiolato-S,S';S,S')bis[(2,2'-bipyrimidine-N,N')zinc(II)] (Gronlund et al., 1995). The non-bridging bonds Cd1—O1, Cd2—O3 and Cd3—O6 [2.206 (2), 2.209 (2) and 2.219 (2) Å, respectively] are shorter than the bridging Cd—O bonds.

Besides the main molecules (Ia) and (Ib), the crystal of (I) also contains solvating pyridine molecules. No shortened intermolecular contacts were found in the crystal structure of (I).

Experimental top

3,5-Di-tert-butyl-1,2-benzoquinone was prepared by the usual method of Muller et al. (1957). Pyridine was freshly distilled after drying by standard techniques (Gordon & Ford, 1976). The synthesis of cadmium catecholate was performed under an atmosphere of dry oxygen-free argon. To cadmium turnings (135 mg, 1.2 mmol) was added 3,5-di-tert-butyl-1,2-benzoquinone (66 mg, 0.3 mmol) in pyridine (5 ml). The mixture was stirred at 343 K for 48 h. Pyridine (20 ml) was then added under warming to dissolve the yellow precipiate. The resulting hot solution was filtered from the unreacted metal. Slow cooling of the solution gave 150 mg of crystals of (I) suitable for X-ray analysis. A second crop of the product (34 mg) was obtained after partial removal of the solvent (yield 92%). The product is air sensitive and decomposes without melting at 532 K.

Refinement top

The positions of the H atoms were calculated using Csp2—H and Csp3—H distances of 0.93 and 0.96 Å, respectively, and the H atoms were treated as riding in the refinement. In the final difference map, there are two relatively high peaks (4.88 and 4.87 e Å-3) at the Cd atoms (Q1—Cd2 and Q2—Cd1 0.71 and 0.72 Å, respectively) which cannot be interpretated as real atoms.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of (Ia) and the solvating pyridine molecules, with 50% probability displacement ellipsoids. H atoms are shown as small spheres of arbitrary radii.
bis(µ-3,5-di-tert-butylcatecholato-O1:O1,O2)bis[tripyridinecadmium(II)] dipyridine solvate top
Crystal data top
C58H70Cd2N6O4·2C5H5NZ = 3
Mr = 1298.22F(000) = 2016
Triclinic, P1Dx = 1.346 Mg m3
a = 15.743 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 17.549 (6) ÅCell parameters from 95 reflections
c = 19.945 (7) Åθ = 5–27°
α = 91.051 (7)°µ = 0.72 mm1
β = 108.916 (6)°T = 110 K
γ = 111.094 (6)°Plate, yellow
V = 4806 (3) Å30.5 × 0.4 × 0.1 mm
Data collection top
Bruker SMART-1000 CCD area-detector
diffractometer
27455 independent reflections
Radiation source: X-ray tube16608 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
θ/2θ scansθmax = 30.1°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2222
Tmin = 0.456, Tmax = 0.931k = 2424
55993 measured reflectionsl = 2728
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: block-diagonalSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0665P)2]
where P = (Fo2 + 2Fc2)/3
27455 reflections(Δ/σ)max = 0.045
1108 parametersΔρmax = 4.89 e Å3
0 restraintsΔρmin = 1.19 e Å3
Crystal data top
C58H70Cd2N6O4·2C5H5Nγ = 111.094 (6)°
Mr = 1298.22V = 4806 (3) Å3
Triclinic, P1Z = 3
a = 15.743 (5) ÅMo Kα radiation
b = 17.549 (6) ŵ = 0.72 mm1
c = 19.945 (7) ÅT = 110 K
α = 91.051 (7)°0.5 × 0.4 × 0.1 mm
β = 108.916 (6)°
Data collection top
Bruker SMART-1000 CCD area-detector
diffractometer
27455 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
16608 reflections with I > 2σ(I)
Tmin = 0.456, Tmax = 0.931Rint = 0.034
55993 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0500 restraints
wR(F2) = 0.133H-atom parameters constrained
S = 0.96Δρmax = 4.89 e Å3
27455 reflectionsΔρmin = 1.19 e Å3
1108 parameters
Special details top

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)

0.0223 (0.0151) x + 13.0613 (0.0092) y - 13.5435 (0.0110) z = 15.4526 (0.0204)

* 0.0122 (0.0009) C d1 * -0.0135 (0.0014) O1 * -0.0172 (0.0014) O2 * 0.0053 (0.0017) C1 * 0.0133 (0.0018) C6

Rms deviation of fitted atoms = 0.0129

-1.1844 (0.0112) x + 13.5988 (0.0133) y - 12.8877 (0.0177) z = 13.9979 (0.0114)

Angle to previous plane (with approximate e.s.d.) = 4.43 (0.14)

* 0.0038 (0.0007) C d1 * -0.0038 (0.0007) O2 * 0.0038 (0.0007) C d2 * -0.0038 (0.0007) O4

Rms deviation of fitted atoms = 0.0038

0.5039 (0.0150) x + 12.9333 (0.0093) y - 13.6376 (0.0108) z = 15.8015 (0.0166)

Angle to previous plane (with approximate e.s.d.) = 6.15 (0.13)

* -0.0196 (0.0009) C d2 * 0.0201 (0.0014) O3 * 0.0293 (0.0014) O4 * -0.0054 (0.0017) C15 * -0.0244 (0.0018) C20

Rms deviation of fitted atoms = 0.0213

-1.5426 (0.0140) x + 13.8513 (0.0165) y - 12.5274 (0.0233) z = 6.9256 (0.0083)

Angle to previous plane (with approximate e.s.d.) = 7.53 (0.16)

* 0.0000 (0.0000) C d3 * 0.0000 (0.0000) C d3_$1 * 0.0000 (0.0000) O5 * 0.0000 (0.0000) O5_$2

Rms deviation of fitted atoms = 0.0000

0.3065 (0.0149) x + 12.9114 (0.0093) y - 13.7021 (0.0108) z = 6.8969 (0.0150)

Angle to previous plane (with approximate e.s.d.) = 6.93 (0.16)

* 0.0030 (0.0009) C d3 * -0.0083 (0.0014) O5 * 0.0009 (0.0014) O6 * 0.0110 (0.0017) C59 * -0.0066 (0.0017) C64

Rms deviation of fitted atoms = 0.0070

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd11.446996 (15)0.880466 (13)0.290369 (11)0.02054 (5)
O11.53049 (14)0.83112 (13)0.33592 (10)0.0230 (4)
N11.60369 (19)0.98051 (16)0.21004 (14)0.0296 (6)
C11.47777 (19)0.77347 (17)0.39300 (14)0.0183 (6)
Cd21.190615 (15)0.773414 (13)0.379765 (11)0.02007 (5)
O21.33373 (14)0.78123 (13)0.38408 (10)0.0231 (4)
N21.45877 (19)0.99711 (17)0.35347 (15)0.0315 (6)
C21.51968 (19)0.73554 (17)0.42925 (15)0.0193 (6)
O31.10853 (13)0.82628 (12)0.33557 (10)0.0227 (4)
N31.46498 (18)0.80299 (16)0.19363 (14)0.0280 (6)
C31.4584 (2)0.67601 (17)0.49069 (15)0.0212 (6)
H3A1.48680.65230.51470.025*
O41.30470 (13)0.87202 (13)0.28562 (11)0.0238 (4)
N41.17746 (18)0.65418 (16)0.32197 (13)0.0253 (5)
C41.3571 (2)0.65074 (18)0.51745 (15)0.0211 (6)
N51.02971 (17)0.67626 (15)0.46187 (13)0.0244 (5)
C51.3167 (2)0.68781 (18)0.48044 (15)0.0209 (6)
H5A1.24950.67250.49720.025*
N61.17639 (17)0.85074 (16)0.47627 (13)0.0237 (5)
C61.37329 (19)0.74669 (17)0.41959 (14)0.0184 (6)
C71.6302 (2)0.75928 (18)0.40031 (16)0.0225 (6)
C81.6639 (2)0.7128 (2)0.44508 (19)0.0373 (8)
H8A1.64570.72440.49340.056*
H8B1.63390.65450.44520.056*
H8C1.73340.73030.42480.056*
C91.6611 (2)0.7387 (2)0.32327 (17)0.0305 (7)
H9A1.73020.75350.30470.046*
H9B1.62840.68060.32400.046*
H9C1.64370.76940.29330.046*
C101.6833 (2)0.85149 (19)0.39874 (18)0.0295 (7)
H10A1.66440.86460.44650.044*
H10B1.75230.86550.38030.044*
H10C1.66650.88240.36850.044*
C111.2969 (2)0.58670 (19)0.58502 (16)0.0259 (7)
C121.3206 (2)0.6226 (2)0.64970 (17)0.0365 (8)
H12A1.30640.67130.65590.055*
H12B1.28190.58230.69210.055*
H12C1.38840.63650.64130.055*
C131.3197 (2)0.5082 (2)0.57502 (18)0.0350 (8)
H13A1.30480.48590.53470.053*
H13B1.38740.52200.56670.053*
H13C1.28090.46790.61750.053*
C141.1869 (2)0.5613 (2)0.60304 (18)0.0351 (8)
H14A1.17100.60930.60950.053*
H14B1.16900.53680.56450.053*
H14C1.15190.52210.64640.053*
C151.16164 (19)0.88272 (17)0.27821 (14)0.0176 (5)
C161.12073 (19)0.92176 (17)0.24185 (15)0.0191 (6)
C171.1814 (2)0.97857 (17)0.17902 (15)0.0209 (6)
H17A1.15331.00280.15530.025*
C181.2819 (2)1.00035 (18)0.15056 (15)0.0215 (6)
C191.3222 (2)0.96394 (18)0.18818 (15)0.0207 (6)
H19A1.38920.97850.17110.025*
C201.2657 (2)0.90709 (17)0.24987 (15)0.0195 (6)
C211.0103 (2)0.90013 (18)0.27210 (16)0.0218 (6)
C220.9780 (2)0.9498 (2)0.22870 (19)0.0356 (8)
H22A0.90880.93410.24970.053*
H22B1.01021.00770.22900.053*
H22C0.99460.93860.18020.053*
C230.9807 (2)0.9192 (2)0.34925 (17)0.0291 (7)
H23A0.91180.90560.36810.044*
H23B0.99730.88690.37850.044*
H23C1.01470.97690.34930.044*
C240.9567 (2)0.80840 (18)0.27094 (17)0.0273 (7)
H24A0.88770.79460.28980.041*
H24B0.97530.79730.22250.041*
H24C0.97330.77570.29980.041*
C251.3427 (2)1.0609 (2)0.08049 (16)0.0296 (7)
C261.3142 (3)1.0221 (2)0.01856 (18)0.0491 (10)
H26A1.32520.97170.01440.074*
H26B1.24661.01040.02800.074*
H26C1.35301.05990.02540.074*
C271.3246 (3)1.1415 (2)0.0868 (2)0.0418 (9)
H27A1.34231.16620.12540.063*
H27B1.36321.17920.04280.063*
H27C1.25691.12950.09630.063*
C281.4521 (2)1.0819 (2)0.06166 (18)0.0396 (9)
H28A1.46421.03200.05760.059*
H28B1.48801.11860.01690.059*
H28C1.47251.10810.09870.059*
C291.6862 (2)0.9699 (2)0.20532 (18)0.0346 (8)
H29A1.67980.92470.23440.041*
C301.7768 (3)1.0190 (2)0.1624 (2)0.0514 (11)
H30A1.82991.00600.15990.062*
C311.7884 (3)1.0886 (2)0.1223 (2)0.0407 (9)
H31A1.85031.12530.09370.049*
C321.7086 (3)1.1034 (2)0.12484 (19)0.0415 (9)
H32A1.71481.14950.09700.050*
C331.6175 (2)1.0483 (2)0.16984 (18)0.0366 (8)
H33A1.56331.05940.17200.044*
C341.5242 (4)1.0192 (3)0.3851 (3)0.092 (2)
H34A1.56120.98780.38380.110*
C351.5392 (4)1.0874 (4)0.4200 (3)0.111 (3)
H35A1.58521.10040.44220.134*
C361.4883 (3)1.1355 (2)0.4225 (2)0.0507 (11)
H36A1.49881.18190.44540.061*
C371.4210 (3)1.1130 (2)0.3902 (2)0.0429 (9)
H37A1.38371.14390.39080.052*
C381.4083 (2)1.0436 (2)0.35618 (18)0.0339 (8)
H38A1.36201.02920.33430.041*
C391.5295 (3)0.7675 (3)0.1815 (2)0.0504 (11)
H39A1.56560.77460.21140.060*
C401.5457 (3)0.7212 (3)0.1277 (2)0.0540 (11)
H40A1.59210.69830.12120.065*
C411.4925 (2)0.7093 (2)0.08388 (17)0.0332 (8)
H41A1.50180.67800.04700.040*
C421.4249 (2)0.7446 (2)0.09561 (17)0.0335 (8)
H42A1.38760.73780.06670.040*
C431.4133 (2)0.7905 (2)0.15097 (17)0.0291 (7)
H43A1.36700.81370.15870.035*
C441.0973 (2)0.6132 (2)0.30708 (17)0.0328 (8)
H44A1.04490.62950.32330.039*
C451.0889 (2)0.5478 (2)0.26862 (18)0.0355 (8)
H45A1.03170.52040.26000.043*
C461.1656 (3)0.5237 (2)0.24345 (18)0.0354 (8)
H46A1.16230.48080.21640.042*
C471.2487 (2)0.5651 (2)0.25941 (19)0.0375 (8)
H47A1.30180.54970.24360.045*
C481.2518 (2)0.6290 (2)0.29880 (17)0.0302 (7)
H48A1.30730.65570.30980.036*
C491.0179 (2)0.6153 (2)0.50901 (17)0.0325 (8)
H49A1.07270.60730.51010.039*
C500.9274 (2)0.5632 (2)0.55662 (18)0.0375 (8)
H50A0.92170.52070.58840.045*
C510.8463 (2)0.5754 (2)0.55621 (19)0.0392 (9)
H51A0.78490.54090.58750.047*
C520.8569 (2)0.6389 (2)0.50921 (19)0.0372 (8)
H52A0.80360.65020.50920.045*
C530.9464 (2)0.6839 (2)0.46352 (15)0.0230 (6)
H53A0.95210.72430.42960.028*
C541.2480 (2)0.8824 (2)0.50224 (17)0.0291 (7)
H54A1.30200.86820.48600.035*
C551.2444 (2)0.9356 (2)0.55250 (19)0.0355 (8)
H55A1.29580.95750.56900.043*
C561.1642 (2)0.95562 (19)0.57775 (17)0.0306 (7)
H56A1.16060.99120.61160.037*
C571.0891 (2)0.9222 (2)0.55212 (18)0.0330 (7)
H57A1.03340.93390.56880.040*
C581.0990 (2)0.8707 (2)0.50107 (18)0.0338 (8)
H58A1.04910.84890.48310.041*
Cd31.127226 (14)0.551792 (13)0.041596 (11)0.01880 (4)
O51.01179 (13)0.45424 (13)0.05209 (10)0.0235 (4)
O61.20838 (13)0.49986 (12)0.00538 (10)0.0221 (4)
N71.28652 (17)0.65429 (16)0.11787 (13)0.0258 (6)
N81.15553 (17)0.48167 (15)0.14082 (13)0.0228 (5)
N91.13295 (17)0.65917 (16)0.02982 (13)0.0255 (6)
C591.04928 (19)0.41738 (17)0.08740 (15)0.0182 (6)
C600.9903 (2)0.35848 (17)0.14830 (15)0.0212 (6)
H60A0.92350.34530.16500.025*
C611.0282 (2)0.31840 (18)0.18533 (15)0.0226 (6)
C621.1290 (2)0.33979 (18)0.15800 (16)0.0224 (6)
H62A1.15570.31340.18130.027*
C631.1916 (2)0.39916 (17)0.09712 (15)0.0196 (6)
C641.15344 (19)0.44130 (17)0.06123 (14)0.0183 (6)
C651.3016 (2)0.41812 (19)0.06809 (17)0.0242 (6)
C661.3308 (2)0.3661 (2)0.1116 (2)0.0388 (8)
H66A1.39980.38040.09120.058*
H66B1.31380.37660.16030.058*
H66C1.29730.30860.11070.058*
C671.3317 (2)0.4002 (2)0.00954 (17)0.0326 (7)
H67A1.40030.41210.02770.049*
H67B1.29630.34310.01050.049*
H67C1.31730.43440.03880.049*
C681.3594 (2)0.50955 (19)0.06921 (17)0.0280 (7)
H68A1.42780.52080.05100.042*
H68B1.34550.54390.03980.042*
H68C1.34100.52100.11750.042*
C690.9652 (2)0.25417 (19)0.25270 (16)0.0270 (7)
C700.9934 (3)0.2864 (2)0.31681 (17)0.0392 (8)
H70A1.06120.29840.30640.059*
H70B0.98110.33580.32540.059*
H70C0.95530.24510.35860.059*
C710.9795 (3)0.1732 (2)0.24074 (19)0.0409 (9)
H71A0.96180.15350.20060.061*
H71B1.04650.18240.23110.061*
H71C0.93910.13270.28290.061*
C720.8566 (2)0.2364 (2)0.27217 (19)0.0390 (9)
H72A0.83640.21600.23320.058*
H72B0.81960.19570.31450.058*
H72C0.84590.28640.28100.058*
C731.3633 (2)0.6610 (2)0.0999 (2)0.0498 (12)
H73A1.35200.62590.05970.060*
C741.4555 (3)0.7143 (2)0.1347 (2)0.0611 (13)
H74A1.50440.71900.11670.073*
C751.4754 (3)0.7616 (2)0.1979 (2)0.0477 (10)
H75A1.53860.79750.22470.057*
C761.3994 (3)0.7543 (2)0.2204 (2)0.0468 (10)
H76A1.41020.78520.26290.056*
C771.3076 (2)0.7006 (2)0.17905 (18)0.0408 (9)
H77A1.25670.69620.19480.049*
C781.2374 (2)0.4670 (2)0.16405 (17)0.0295 (7)
H78A1.28500.49120.14430.035*
C791.2548 (2)0.4174 (2)0.21604 (17)0.0309 (7)
H79A1.31300.40950.23160.037*
C801.1827 (2)0.38024 (19)0.24391 (17)0.0292 (7)
H80A1.19120.34580.27820.035*
C811.0973 (2)0.39484 (19)0.22004 (16)0.0281 (7)
H81A1.04780.37020.23790.034*
C821.0875 (2)0.44659 (18)0.16928 (15)0.0229 (6)
H82A1.03110.45740.15430.027*
C831.1709 (2)0.6594 (2)0.08132 (17)0.0317 (7)
H83A1.19140.61710.08780.038*
C841.1806 (2)0.7195 (2)0.12484 (18)0.0371 (8)
H84A1.20540.71690.16090.044*
C851.1530 (2)0.7843 (2)0.11413 (19)0.0414 (9)
H85A1.16210.82730.14100.050*
C861.1117 (3)0.7830 (2)0.06266 (19)0.0403 (9)
H86A1.09050.82440.05520.048*
C871.1022 (2)0.7195 (2)0.02228 (18)0.0331 (7)
H87A1.07310.71860.01170.040*
N1S1.4789 (4)0.5238 (5)0.2368 (3)0.117 (2)
C1S1.4740 (4)0.4494 (5)0.2499 (4)0.111 (3)
H1SB1.48630.42020.21180.134*
C2S1.4515 (4)0.4129 (4)0.3170 (5)0.111 (3)
H2SA1.44800.35940.32560.133*
C3S1.4339 (3)0.4581 (4)0.3729 (3)0.0799 (17)
H3SA1.41810.43610.42010.096*
C4S1.4408 (3)0.5344 (3)0.3555 (3)0.0680 (15)
H4SA1.43010.56680.39130.082*
C5S1.4624 (3)0.5646 (3)0.2884 (3)0.0692 (14)
H5SA1.46580.61780.27820.083*
N2S0.8581 (4)0.8703 (3)0.0895 (2)0.0920 (16)
C6S0.8521 (4)0.7954 (3)0.1016 (3)0.0711 (15)
H6SA0.82960.77110.14920.085*
C7S0.8765 (3)0.7498 (3)0.0498 (2)0.0525 (11)
H7SA0.87050.69620.06180.063*
C8S0.9099 (3)0.7845 (3)0.0204 (2)0.0484 (10)
H8SA0.92760.75500.05710.058*
C9S0.9168 (3)0.8634 (3)0.0359 (3)0.0627 (13)
H9SA0.93820.88840.08310.075*
C10S0.8911 (4)0.9049 (3)0.0208 (3)0.0879 (18)
H10D0.89690.95890.01080.105*
N3S1.1870 (3)0.1998 (3)0.5752 (2)0.0629 (10)
C11S1.2158 (4)0.2349 (3)0.6430 (3)0.0633 (13)
H11A1.22590.29020.65180.076*
C12S1.2315 (3)0.1920 (3)0.7014 (2)0.0545 (11)
H12D1.25080.21800.74800.065*
C13S1.2178 (3)0.1112 (2)0.6883 (2)0.0444 (9)
H13D1.22910.08130.72590.053*
C14S1.1868 (3)0.0743 (2)0.6182 (2)0.0458 (9)
H14D1.17590.01900.60770.055*
C15S1.1726 (3)0.1207 (3)0.5649 (2)0.0555 (11)
H15A1.15120.09500.51790.067*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01962 (10)0.02497 (12)0.01778 (11)0.01075 (8)0.00525 (8)0.00213 (9)
O10.0178 (10)0.0287 (11)0.0194 (10)0.0096 (8)0.0027 (8)0.0042 (9)
N10.0307 (15)0.0244 (14)0.0261 (14)0.0068 (11)0.0050 (12)0.0025 (11)
C10.0202 (14)0.0196 (14)0.0169 (14)0.0096 (11)0.0065 (11)0.0041 (11)
Cd20.01971 (10)0.02487 (12)0.01681 (10)0.01091 (8)0.00544 (8)0.00198 (8)
O20.0189 (10)0.0325 (12)0.0166 (10)0.0108 (9)0.0040 (8)0.0056 (9)
N20.0308 (15)0.0395 (17)0.0319 (15)0.0196 (13)0.0136 (12)0.0171 (13)
C20.0177 (13)0.0227 (15)0.0191 (14)0.0094 (11)0.0068 (11)0.0061 (11)
O30.0187 (10)0.0292 (11)0.0177 (10)0.0098 (8)0.0033 (8)0.0042 (9)
N30.0288 (14)0.0350 (15)0.0247 (14)0.0166 (12)0.0101 (11)0.0087 (12)
C30.0232 (15)0.0238 (15)0.0230 (15)0.0131 (12)0.0117 (12)0.0043 (12)
O40.0162 (10)0.0314 (12)0.0223 (11)0.0108 (9)0.0039 (8)0.0059 (9)
N40.0256 (13)0.0274 (14)0.0240 (14)0.0116 (11)0.0088 (11)0.0066 (11)
C40.0211 (14)0.0232 (15)0.0202 (14)0.0096 (12)0.0076 (12)0.0019 (12)
N50.0225 (13)0.0268 (14)0.0196 (13)0.0081 (11)0.0039 (10)0.0005 (11)
C50.0165 (13)0.0273 (16)0.0179 (14)0.0098 (11)0.0036 (11)0.0016 (12)
N60.0254 (13)0.0294 (14)0.0189 (13)0.0139 (11)0.0073 (10)0.0044 (11)
C60.0191 (13)0.0239 (15)0.0164 (14)0.0124 (11)0.0068 (11)0.0045 (11)
C70.0171 (14)0.0257 (16)0.0267 (16)0.0096 (12)0.0088 (12)0.0028 (12)
C80.0273 (17)0.047 (2)0.043 (2)0.0194 (15)0.0145 (15)0.0054 (17)
C90.0226 (15)0.0406 (19)0.0337 (18)0.0176 (14)0.0104 (14)0.0123 (15)
C100.0217 (15)0.0323 (18)0.0350 (18)0.0091 (13)0.0124 (14)0.0070 (14)
C110.0236 (15)0.0316 (17)0.0200 (15)0.0104 (13)0.0054 (12)0.0031 (13)
C120.040 (2)0.046 (2)0.0217 (17)0.0172 (16)0.0092 (15)0.0000 (15)
C130.0362 (19)0.0296 (18)0.0320 (19)0.0115 (15)0.0049 (15)0.0053 (14)
C140.0254 (17)0.039 (2)0.0319 (18)0.0088 (14)0.0039 (14)0.0120 (15)
C150.0187 (13)0.0198 (14)0.0155 (13)0.0082 (11)0.0066 (11)0.0052 (11)
C160.0189 (13)0.0219 (14)0.0196 (14)0.0091 (11)0.0092 (11)0.0060 (11)
C170.0253 (15)0.0227 (15)0.0204 (15)0.0128 (12)0.0115 (12)0.0028 (12)
C180.0224 (14)0.0210 (15)0.0199 (15)0.0073 (12)0.0074 (12)0.0006 (12)
C190.0203 (14)0.0248 (15)0.0168 (14)0.0098 (12)0.0051 (11)0.0017 (12)
C200.0202 (14)0.0238 (15)0.0160 (14)0.0098 (11)0.0068 (11)0.0028 (11)
C210.0187 (14)0.0262 (16)0.0254 (16)0.0110 (12)0.0111 (12)0.0052 (13)
C220.0294 (17)0.041 (2)0.043 (2)0.0191 (15)0.0149 (15)0.0012 (16)
C230.0240 (16)0.0375 (19)0.0303 (17)0.0175 (14)0.0089 (13)0.0112 (14)
C240.0198 (15)0.0294 (17)0.0326 (17)0.0080 (12)0.0110 (13)0.0057 (14)
C250.0329 (17)0.0330 (18)0.0206 (16)0.0135 (14)0.0060 (13)0.0028 (13)
C260.060 (3)0.058 (3)0.0219 (18)0.016 (2)0.0134 (18)0.0022 (17)
C270.040 (2)0.035 (2)0.042 (2)0.0145 (16)0.0063 (17)0.0151 (16)
C280.0333 (19)0.043 (2)0.0294 (19)0.0139 (16)0.0028 (15)0.0152 (16)
C290.0322 (18)0.048 (2)0.0317 (18)0.0304 (16)0.0048 (15)0.0023 (16)
C300.0274 (19)0.052 (3)0.054 (3)0.0110 (17)0.0061 (18)0.014 (2)
C310.0300 (19)0.039 (2)0.037 (2)0.0039 (15)0.0031 (16)0.0026 (16)
C320.040 (2)0.037 (2)0.036 (2)0.0030 (16)0.0131 (17)0.0079 (16)
C330.0329 (18)0.037 (2)0.0347 (19)0.0080 (15)0.0130 (15)0.0059 (16)
C340.106 (4)0.127 (5)0.142 (5)0.096 (4)0.107 (4)0.108 (4)
C350.111 (4)0.153 (6)0.181 (6)0.105 (4)0.123 (5)0.142 (5)
C360.039 (2)0.049 (2)0.055 (3)0.0128 (18)0.0079 (19)0.029 (2)
C370.046 (2)0.033 (2)0.046 (2)0.0185 (17)0.0071 (18)0.0117 (17)
C380.0347 (18)0.0350 (19)0.0351 (19)0.0166 (15)0.0125 (15)0.0090 (15)
C390.063 (3)0.083 (3)0.045 (2)0.057 (2)0.035 (2)0.035 (2)
C400.075 (3)0.075 (3)0.048 (2)0.059 (3)0.032 (2)0.032 (2)
C410.042 (2)0.0281 (17)0.0207 (16)0.0120 (15)0.0021 (14)0.0079 (13)
C420.0268 (17)0.0380 (19)0.0297 (18)0.0059 (14)0.0099 (14)0.0080 (15)
C430.0217 (15)0.0345 (18)0.0300 (17)0.0104 (13)0.0079 (13)0.0092 (14)
C440.0291 (17)0.043 (2)0.0288 (18)0.0162 (15)0.0112 (14)0.0074 (15)
C450.0365 (19)0.037 (2)0.0330 (19)0.0106 (15)0.0162 (16)0.0090 (15)
C460.045 (2)0.0301 (18)0.0306 (18)0.0149 (15)0.0117 (16)0.0115 (15)
C470.0348 (19)0.043 (2)0.036 (2)0.0213 (16)0.0075 (16)0.0148 (17)
C480.0271 (16)0.0342 (18)0.0284 (17)0.0128 (14)0.0076 (14)0.0084 (14)
C490.0294 (17)0.0376 (19)0.0285 (18)0.0105 (15)0.0110 (14)0.0030 (15)
C500.0356 (19)0.038 (2)0.0292 (18)0.0050 (15)0.0097 (15)0.0099 (15)
C510.0266 (17)0.038 (2)0.036 (2)0.0026 (15)0.0014 (15)0.0074 (16)
C520.0231 (17)0.037 (2)0.043 (2)0.0077 (14)0.0069 (15)0.0005 (16)
C530.0188 (14)0.0381 (18)0.0211 (15)0.0201 (13)0.0081 (12)0.0072 (13)
C540.0234 (15)0.0340 (18)0.0310 (18)0.0121 (13)0.0096 (13)0.0097 (14)
C550.0314 (18)0.037 (2)0.041 (2)0.0117 (15)0.0182 (16)0.0168 (16)
C560.0399 (19)0.0245 (16)0.0274 (17)0.0128 (14)0.0112 (15)0.0074 (13)
C570.0345 (18)0.0378 (19)0.0336 (19)0.0227 (15)0.0105 (15)0.0113 (15)
C580.0332 (18)0.043 (2)0.0351 (19)0.0221 (16)0.0162 (15)0.0149 (16)
Cd30.01698 (9)0.02276 (10)0.01723 (10)0.00864 (8)0.00569 (8)0.00336 (8)
O50.0171 (10)0.0306 (12)0.0218 (11)0.0097 (8)0.0054 (8)0.0032 (9)
O60.0178 (10)0.0260 (11)0.0206 (10)0.0084 (8)0.0046 (8)0.0016 (8)
N70.0208 (12)0.0292 (14)0.0233 (13)0.0073 (11)0.0054 (10)0.0015 (11)
N80.0230 (12)0.0289 (14)0.0188 (12)0.0132 (10)0.0065 (10)0.0065 (10)
N90.0217 (13)0.0286 (14)0.0252 (14)0.0108 (11)0.0058 (11)0.0081 (11)
C590.0194 (13)0.0213 (14)0.0175 (14)0.0096 (11)0.0088 (11)0.0055 (11)
C600.0181 (13)0.0242 (15)0.0216 (15)0.0096 (11)0.0060 (11)0.0017 (12)
C610.0261 (15)0.0228 (15)0.0203 (15)0.0102 (12)0.0090 (12)0.0024 (12)
C620.0258 (15)0.0229 (15)0.0247 (15)0.0126 (12)0.0132 (12)0.0047 (12)
C630.0222 (14)0.0216 (14)0.0193 (14)0.0114 (11)0.0091 (11)0.0063 (11)
C640.0170 (13)0.0238 (15)0.0168 (13)0.0103 (11)0.0063 (11)0.0068 (11)
C650.0204 (14)0.0271 (16)0.0312 (17)0.0136 (12)0.0119 (13)0.0061 (13)
C660.0318 (18)0.045 (2)0.049 (2)0.0230 (16)0.0176 (17)0.0003 (17)
C670.0258 (16)0.043 (2)0.0363 (19)0.0204 (14)0.0112 (14)0.0164 (16)
C680.0188 (14)0.0313 (17)0.0342 (18)0.0086 (12)0.0109 (13)0.0075 (14)
C690.0291 (16)0.0298 (17)0.0207 (15)0.0131 (13)0.0056 (13)0.0021 (13)
C700.048 (2)0.047 (2)0.0226 (17)0.0175 (17)0.0130 (16)0.0007 (15)
C710.047 (2)0.0283 (18)0.036 (2)0.0130 (16)0.0025 (17)0.0054 (15)
C720.0281 (18)0.044 (2)0.0342 (19)0.0097 (15)0.0035 (15)0.0123 (16)
C730.0317 (19)0.0236 (17)0.091 (3)0.0104 (14)0.043 (2)0.0247 (19)
C740.027 (2)0.051 (3)0.085 (3)0.0117 (17)0.027 (2)0.029 (2)
C750.0239 (18)0.047 (2)0.053 (3)0.0034 (16)0.0024 (17)0.0066 (19)
C760.034 (2)0.058 (3)0.030 (2)0.0043 (17)0.0046 (16)0.0101 (17)
C770.0302 (18)0.052 (2)0.0306 (19)0.0050 (16)0.0118 (15)0.0079 (16)
C780.0277 (16)0.0366 (18)0.0279 (17)0.0148 (14)0.0113 (13)0.0088 (14)
C790.0278 (16)0.0345 (18)0.0298 (18)0.0167 (14)0.0044 (14)0.0054 (14)
C800.0379 (18)0.0226 (16)0.0251 (16)0.0113 (14)0.0088 (14)0.0080 (13)
C810.0293 (16)0.0256 (16)0.0262 (16)0.0058 (13)0.0111 (13)0.0047 (13)
C820.0189 (14)0.0271 (16)0.0201 (15)0.0078 (12)0.0050 (11)0.0036 (12)
C830.0260 (16)0.0358 (19)0.0327 (18)0.0099 (14)0.0117 (14)0.0085 (15)
C840.0287 (17)0.042 (2)0.0316 (19)0.0041 (15)0.0105 (15)0.0123 (16)
C850.0348 (19)0.036 (2)0.038 (2)0.0044 (15)0.0039 (16)0.0199 (17)
C860.050 (2)0.0306 (19)0.037 (2)0.0188 (17)0.0065 (17)0.0070 (16)
C870.0402 (19)0.0313 (18)0.0267 (17)0.0172 (15)0.0067 (15)0.0031 (14)
N1S0.079 (4)0.217 (7)0.068 (3)0.059 (4)0.039 (3)0.029 (4)
C1S0.073 (4)0.172 (8)0.124 (6)0.066 (5)0.053 (4)0.117 (6)
C2S0.071 (4)0.063 (4)0.227 (9)0.036 (3)0.074 (5)0.037 (5)
C3S0.060 (3)0.097 (4)0.068 (3)0.007 (3)0.032 (3)0.017 (3)
C4S0.036 (2)0.080 (4)0.072 (3)0.006 (2)0.017 (2)0.041 (3)
C5S0.045 (3)0.065 (3)0.091 (4)0.016 (2)0.024 (3)0.008 (3)
N2S0.164 (5)0.116 (4)0.070 (3)0.106 (4)0.075 (3)0.055 (3)
C6S0.097 (4)0.105 (4)0.051 (3)0.069 (3)0.042 (3)0.027 (3)
C7S0.050 (2)0.053 (3)0.059 (3)0.021 (2)0.023 (2)0.014 (2)
C8S0.043 (2)0.051 (2)0.048 (2)0.0126 (18)0.0176 (19)0.021 (2)
C9S0.078 (3)0.070 (3)0.057 (3)0.033 (3)0.040 (3)0.018 (2)
C10S0.145 (5)0.073 (4)0.102 (5)0.071 (4)0.080 (4)0.036 (3)
N3S0.088 (3)0.073 (3)0.055 (2)0.050 (2)0.038 (2)0.029 (2)
C11S0.080 (3)0.049 (3)0.078 (3)0.032 (2)0.040 (3)0.019 (2)
C12S0.059 (3)0.055 (3)0.051 (3)0.019 (2)0.025 (2)0.005 (2)
C13S0.041 (2)0.050 (2)0.046 (2)0.0160 (18)0.0216 (18)0.0195 (19)
C14S0.043 (2)0.044 (2)0.051 (2)0.0177 (18)0.0176 (19)0.0055 (19)
C15S0.064 (3)0.080 (3)0.034 (2)0.040 (2)0.017 (2)0.012 (2)
Geometric parameters (Å, º) top
Cd1—O12.206 (2)C47—H47A0.9300
Cd1—O42.224 (2)C48—H48A0.9300
Cd1—O22.278 (2)C49—C501.386 (4)
Cd1—N32.381 (3)C49—H49A0.9300
Cd1—N22.404 (3)C50—C511.369 (5)
Cd1—N12.440 (3)C50—H50A0.9300
O1—C11.323 (3)C51—C521.369 (5)
N1—C331.331 (4)C51—H51A0.9300
N1—C291.352 (4)C52—C531.333 (4)
C1—C21.417 (4)C52—H52A0.9300
C1—C61.441 (4)C53—H53A0.9300
Cd2—O32.209 (2)C54—C551.384 (4)
Cd2—O22.237 (2)C54—H54A0.9300
Cd2—O42.281 (2)C55—C561.373 (5)
Cd2—N62.373 (2)C55—H55A0.9300
Cd2—N42.384 (3)C56—C571.382 (4)
Cd2—N52.471 (2)C56—H56A0.9300
O2—C61.341 (3)C57—C581.381 (4)
N2—C381.320 (4)C57—H57A0.9300
N2—C341.324 (4)C58—H58A0.9300
C2—C31.409 (4)Cd3—O62.219 (2)
C2—C71.534 (4)Cd3—O5i2.231 (2)
O3—C151.316 (3)Cd3—O52.273 (2)
N3—C431.327 (4)Cd3—N82.354 (2)
N3—C391.333 (4)Cd3—N92.376 (3)
C3—C41.399 (4)Cd3—N72.453 (2)
C3—H3A0.9300O5—C591.338 (3)
O4—C201.343 (3)O5—Cd3i2.231 (2)
N4—C441.340 (4)O6—C641.319 (3)
N4—C481.344 (4)N7—C771.329 (4)
C4—C51.399 (4)N7—C731.335 (4)
C4—C111.526 (4)N8—C821.334 (3)
N5—C491.330 (4)N8—C781.342 (4)
N5—C531.356 (3)N9—C871.337 (4)
C5—C61.387 (4)N9—C831.345 (4)
C5—H5A0.9300C59—C601.392 (4)
N6—C581.332 (4)C59—C641.442 (4)
N6—C541.337 (4)C60—C611.402 (4)
C7—C101.525 (4)C60—H60A0.9300
C7—C81.529 (4)C61—C621.400 (4)
C7—C91.546 (4)C61—C691.528 (4)
C8—H8A0.9600C62—C631.404 (4)
C8—H8B0.9600C62—H62A0.9300
C8—H8C0.9600C63—C641.414 (4)
C9—H9A0.9600C63—C651.541 (4)
C9—H9B0.9600C65—C661.526 (4)
C9—H9C0.9600C65—C681.538 (4)
C10—H10A0.9600C65—C671.539 (4)
C10—H10B0.9600C66—H66A0.9600
C10—H10C0.9600C66—H66B0.9600
C11—C141.537 (4)C66—H66C0.9600
C11—C121.541 (4)C67—H67A0.9600
C11—C131.545 (5)C67—H67B0.9600
C12—H12A0.9600C67—H67C0.9600
C12—H12B0.9600C68—H68A0.9600
C12—H12C0.9600C68—H68B0.9600
C13—H13A0.9600C68—H68C0.9600
C13—H13B0.9600C69—C711.528 (5)
C13—H13C0.9600C69—C721.533 (4)
C14—H14A0.9600C69—C701.538 (4)
C14—H14B0.9600C70—H70A0.9600
C14—H14C0.9600C70—H70B0.9600
C15—C161.419 (4)C70—H70C0.9600
C15—C201.440 (4)C71—H71A0.9600
C16—C171.403 (4)C71—H71B0.9600
C16—C211.539 (4)C71—H71C0.9600
C17—C181.396 (4)C72—H72A0.9600
C17—H17A0.9300C72—H72B0.9600
C18—C191.399 (4)C72—H72C0.9600
C18—C251.531 (4)C73—C741.346 (5)
C19—C201.381 (4)C73—H73A0.9300
C19—H19A0.9300C74—C751.376 (5)
C21—C241.530 (4)C74—H74A0.9300
C21—C221.531 (4)C75—C761.374 (5)
C21—C231.537 (4)C75—H75A0.9300
C22—H22A0.9600C76—C771.370 (5)
C22—H22B0.9600C76—H76A0.9300
C22—H22C0.9600C77—H77A0.9300
C23—H23A0.9600C78—C791.388 (4)
C23—H23B0.9600C78—H78A0.9300
C23—H23C0.9600C79—C801.383 (4)
C24—H24A0.9600C79—H79A0.9300
C24—H24B0.9600C80—C811.393 (4)
C24—H24C0.9600C80—H80A0.9300
C25—C281.538 (4)C81—C821.381 (4)
C25—C261.537 (4)C81—H81A0.9300
C25—C271.540 (5)C82—H82A0.9300
C26—H26A0.9600C83—C841.377 (4)
C26—H26B0.9600C83—H83A0.9300
C26—H26C0.9600C84—C851.390 (5)
C27—H27A0.9600C84—H84A0.9300
C27—H27B0.9600C85—C861.379 (5)
C27—H27C0.9600C85—H85A0.9300
C28—H28A0.9600C86—C871.380 (4)
C28—H28B0.9600C86—H86A0.9300
C28—H28C0.9600C87—H87A0.9300
C29—C301.343 (5)N1S—C5S1.275 (7)
C29—H29A0.9300N1S—C1S1.295 (9)
C30—C311.368 (5)C1S—C2S1.353 (10)
C30—H30A0.9300C1S—H1SB0.9300
C31—C321.358 (5)C2S—C3S1.391 (8)
C31—H31A0.9300C2S—H2SA0.9300
C32—C331.390 (5)C3S—C4S1.335 (7)
C32—H32A0.9300C3S—H3SA0.9300
C33—H33A0.9300C4S—C5S1.317 (7)
C34—C351.381 (6)C4S—H4SA0.9300
C34—H34A0.9300C5S—H5SA0.9300
C35—C361.349 (6)N2S—C6S1.296 (6)
C35—H35A0.9300N2S—C10S1.339 (7)
C36—C371.358 (5)C6S—C7S1.359 (6)
C36—H36A0.9300C6S—H6SA0.9300
C37—C381.387 (5)C7S—C8S1.367 (6)
C37—H37A0.9300C7S—H7SA0.9300
C38—H38A0.9300C8S—C9S1.370 (6)
C39—C401.373 (5)C8S—H8SA0.9300
C39—H39A0.9300C9S—C10S1.385 (6)
C40—C411.365 (5)C9S—H9SA0.9300
C40—H40A0.9300C10S—H10D0.9300
C41—C421.376 (5)N3S—C15S1.324 (6)
C41—H41A0.9300N3S—C11S1.336 (6)
C42—C431.381 (4)C11S—C12S1.402 (6)
C42—H42A0.9300C11S—H11A0.9300
C43—H43A0.9300C12S—C13S1.361 (6)
C44—C451.383 (4)C12S—H12D0.9300
C44—H44A0.9300C13S—C14S1.382 (5)
C45—C461.368 (5)C13S—H13D0.9300
C45—H45A0.9300C14S—C15S1.360 (5)
C46—C471.391 (5)C14S—H14D0.9300
C46—H46A0.9300C15S—H15A0.9300
C47—C481.377 (4)
O1—Cd1—O4149.56 (7)N4—C44—C45122.9 (3)
O1—Cd1—O274.50 (7)N4—C44—H44A118.6
O4—Cd1—O275.46 (7)C45—C44—H44A118.6
O1—Cd1—N392.21 (8)C46—C45—C44119.4 (3)
O4—Cd1—N389.25 (8)C46—C45—H45A120.3
O2—Cd1—N3102.09 (9)C44—C45—H45A120.3
O1—Cd1—N297.49 (9)C45—C46—C47118.2 (3)
O4—Cd1—N291.12 (8)C45—C46—H46A120.9
O2—Cd1—N297.33 (9)C47—C46—H46A120.9
N3—Cd1—N2160.02 (10)C48—C47—C46119.5 (3)
O1—Cd1—N186.77 (9)C48—C47—H47A120.3
O4—Cd1—N1123.54 (8)C46—C47—H47A120.3
O2—Cd1—N1160.71 (8)N4—C48—C47122.4 (3)
N3—Cd1—N182.90 (9)N4—C48—H48A118.8
N2—Cd1—N180.27 (9)C47—C48—H48A118.8
C1—O1—Cd1115.26 (16)N5—C49—C50122.8 (3)
C33—N1—C29114.6 (3)N5—C49—H49A118.6
C33—N1—Cd1125.9 (2)C50—C49—H49A118.6
C29—N1—Cd1119.6 (2)C51—C50—C49119.0 (3)
O1—C1—C2122.7 (2)C51—C50—H50A120.5
O1—C1—C6119.4 (2)C49—C50—H50A120.5
C2—C1—C6117.9 (2)C50—C51—C52119.2 (3)
O3—Cd2—O2148.84 (7)C50—C51—H51A120.4
O3—Cd2—O474.36 (7)C52—C51—H51A120.4
O2—Cd2—O475.16 (7)C53—C52—C51117.7 (3)
O3—Cd2—N691.90 (8)C53—C52—H52A121.2
O2—Cd2—N688.22 (8)C51—C52—H52A121.2
O4—Cd2—N6102.10 (8)C52—C53—N5126.1 (3)
O3—Cd2—N4101.01 (8)C52—C53—H53A117.0
O2—Cd2—N490.00 (8)N5—C53—H53A116.9
O4—Cd2—N499.06 (8)N6—C54—C55122.1 (3)
N6—Cd2—N4157.55 (9)N6—C54—H54A119.0
O3—Cd2—N585.86 (8)C55—C54—H54A119.0
O2—Cd2—N5124.93 (8)C56—C55—C54119.4 (3)
O4—Cd2—N5159.80 (8)C56—C55—H55A120.3
N6—Cd2—N582.29 (8)C54—C55—H55A120.3
N4—Cd2—N580.42 (9)C55—C56—C57119.0 (3)
C6—O2—Cd2142.39 (17)C55—C56—H56A120.5
C6—O2—Cd1113.01 (16)C57—C56—H56A120.5
Cd2—O2—Cd1104.52 (8)C58—C57—C56118.0 (3)
C38—N2—C34117.1 (3)C58—C57—H57A121.0
C38—N2—Cd1125.1 (2)C56—C57—H57A121.0
C34—N2—Cd1117.8 (3)N6—C58—C57123.5 (3)
C3—C2—C1119.0 (2)N6—C58—H58A118.3
C3—C2—C7121.5 (2)C57—C58—H58A118.3
C1—C2—C7119.4 (2)O6—Cd3—O5i150.66 (7)
C15—O3—Cd2115.11 (16)O6—Cd3—O574.58 (7)
C43—N3—C39116.6 (3)O5i—Cd3—O576.89 (8)
C43—N3—Cd1124.6 (2)O6—Cd3—N891.36 (8)
C39—N3—Cd1118.8 (2)O5i—Cd3—N890.01 (8)
C4—C3—C2123.3 (3)O5—Cd3—N8106.00 (8)
C4—C3—H3A118.4O6—Cd3—N995.21 (8)
C2—C3—H3A118.4O5i—Cd3—N992.53 (8)
C20—O4—Cd1141.93 (17)O5—Cd3—N992.18 (8)
C20—O4—Cd2113.09 (16)N8—Cd3—N9161.74 (9)
Cd1—O4—Cd2104.86 (8)O6—Cd3—N786.60 (8)
C44—N4—C48117.6 (3)O5i—Cd3—N7122.53 (8)
C44—N4—Cd2120.5 (2)O5—Cd3—N7159.80 (8)
C48—N4—Cd2121.7 (2)N8—Cd3—N781.27 (9)
C5—C4—C3117.0 (3)N9—Cd3—N782.13 (9)
C5—C4—C11123.5 (3)C59—O5—Cd3i143.40 (17)
C3—C4—C11119.5 (3)C59—O5—Cd3113.02 (16)
C49—N5—C53115.1 (3)Cd3i—O5—Cd3103.11 (8)
C49—N5—Cd2123.5 (2)C64—O6—Cd3114.78 (16)
C53—N5—Cd2121.4 (2)C77—N7—C73114.8 (3)
C6—C5—C4122.3 (3)C77—N7—Cd3127.4 (2)
C6—C5—H5A118.8C73—N7—Cd3117.5 (2)
C4—C5—H5A118.9C82—N8—C78118.0 (3)
C58—N6—C54118.0 (3)C82—N8—Cd3122.08 (19)
C58—N6—Cd2119.4 (2)C78—N8—Cd3119.33 (19)
C54—N6—Cd2122.2 (2)C87—N9—C83117.8 (3)
O2—C6—C5121.8 (2)C87—N9—Cd3125.1 (2)
O2—C6—C1117.8 (2)C83—N9—Cd3117.2 (2)
C5—C6—C1120.4 (2)O5—C59—C60121.4 (2)
C10—C7—C8107.6 (2)O5—C59—C64118.1 (2)
C10—C7—C2110.4 (2)C60—C59—C64120.5 (2)
C8—C7—C2113.1 (2)C59—C60—C61122.2 (3)
C10—C7—C9109.1 (3)C59—C60—H60A118.9
C8—C7—C9107.6 (3)C61—C60—H60A118.9
C2—C7—C9108.9 (2)C62—C61—C60116.9 (3)
C7—C8—H8A109.5C62—C61—C69119.8 (3)
C7—C8—H8B109.5C60—C61—C69123.3 (3)
H8A—C8—H8B109.5C61—C62—C63123.1 (3)
C7—C8—H8C109.5C61—C62—H62A118.5
H8A—C8—H8C109.5C63—C62—H62A118.5
H8B—C8—H8C109.5C62—C63—C64119.8 (3)
C7—C9—H9A109.5C62—C63—C65120.7 (3)
C7—C9—H9B109.5C64—C63—C65119.4 (2)
H9A—C9—H9B109.5O6—C64—C63123.1 (2)
C7—C9—H9C109.5O6—C64—C59119.5 (2)
H9A—C9—H9C109.5C63—C64—C59117.4 (2)
H9B—C9—H9C109.5C66—C65—C68107.6 (2)
C7—C10—H10A109.5C66—C65—C63113.0 (3)
C7—C10—H10B109.5C68—C65—C63110.0 (2)
H10A—C10—H10B109.5C66—C65—C67107.6 (3)
C7—C10—H10C109.5C68—C65—C67109.1 (3)
H10A—C10—H10C109.5C63—C65—C67109.4 (2)
H10B—C10—H10C109.5C65—C66—H66A109.5
C4—C11—C14112.3 (2)C65—C66—H66B109.5
C4—C11—C12109.9 (3)H66A—C66—H66B109.5
C14—C11—C12107.2 (3)C65—C66—H66C109.5
C4—C11—C13109.9 (3)H66A—C66—H66C109.5
C14—C11—C13108.0 (3)H66B—C66—H66C109.5
C12—C11—C13109.5 (3)C65—C67—H67A109.5
C11—C12—H12A109.5C65—C67—H67B109.5
C11—C12—H12B109.5H67A—C67—H67B109.5
H12A—C12—H12B109.5C65—C67—H67C109.5
C11—C12—H12C109.5H67A—C67—H67C109.5
H12A—C12—H12C109.5H67B—C67—H67C109.5
H12B—C12—H12C109.5C65—C68—H68A109.5
C11—C13—H13A109.5C65—C68—H68B109.5
C11—C13—H13B109.5H68A—C68—H68B109.5
H13A—C13—H13B109.5C65—C68—H68C109.5
C11—C13—H13C109.5H68A—C68—H68C109.5
H13A—C13—H13C109.5H68B—C68—H68C109.5
H13B—C13—H13C109.5C61—C69—C71109.7 (3)
C11—C14—H14A109.5C61—C69—C72112.0 (3)
C11—C14—H14B109.5C71—C69—C72108.2 (3)
H14A—C14—H14B109.5C61—C69—C70109.7 (3)
C11—C14—H14C109.5C71—C69—C70110.0 (3)
H14A—C14—H14C109.5C72—C69—C70107.2 (3)
H14B—C14—H14C109.5C69—C70—H70A109.5
O3—C15—C16122.7 (2)C69—C70—H70B109.5
O3—C15—C20120.0 (2)H70A—C70—H70B109.5
C16—C15—C20117.3 (2)C69—C70—H70C109.5
C17—C16—C15119.5 (2)H70A—C70—H70C109.5
C17—C16—C21121.5 (2)H70B—C70—H70C109.5
C15—C16—C21119.0 (2)C69—C71—H71A109.5
C18—C17—C16123.0 (3)C69—C71—H71B109.5
C18—C17—H17A118.5H71A—C71—H71B109.5
C16—C17—H17A118.5C69—C71—H71C109.5
C17—C18—C19117.1 (3)H71A—C71—H71C109.5
C17—C18—C25119.8 (3)H71B—C71—H71C109.5
C19—C18—C25123.0 (3)C69—C72—H72A109.5
C20—C19—C18122.2 (3)C69—C72—H72B109.5
C20—C19—H19A118.9H72A—C72—H72B109.5
C18—C19—H19A118.9C69—C72—H72C109.5
O4—C20—C19122.0 (2)H72A—C72—H72C109.5
O4—C20—C15117.3 (2)H72B—C72—H72C109.5
C19—C20—C15120.7 (3)N7—C73—C74125.7 (3)
C24—C21—C22107.8 (2)N7—C73—H73A117.1
C24—C21—C23110.2 (3)C74—C73—H73A117.1
C22—C21—C23107.3 (3)C73—C74—C75118.0 (4)
C24—C21—C16109.2 (2)C73—C74—H74A121.0
C22—C21—C16112.8 (2)C75—C74—H74A121.0
C23—C21—C16109.5 (2)C76—C75—C74118.3 (3)
C21—C22—H22A109.5C76—C75—H75A120.9
C21—C22—H22B109.5C74—C75—H75A120.9
H22A—C22—H22B109.5C77—C76—C75118.7 (4)
C21—C22—H22C109.5C77—C76—H76A120.6
H22A—C22—H22C109.5C75—C76—H76A120.6
H22B—C22—H22C109.5N7—C77—C76124.1 (3)
C21—C23—H23A109.5N7—C77—H77A117.9
C21—C23—H23B109.5C76—C77—H77A117.9
H23A—C23—H23B109.5N8—C78—C79123.4 (3)
C21—C23—H23C109.5N8—C78—H78A118.3
H23A—C23—H23C109.5C79—C78—H78A118.3
H23B—C23—H23C109.5C80—C79—C78117.8 (3)
C21—C24—H24A109.5C80—C79—H79A121.1
C21—C24—H24B109.5C78—C79—H79A121.1
H24A—C24—H24B109.5C79—C80—C81119.3 (3)
C21—C24—H24C109.5C79—C80—H80A120.4
H24A—C24—H24C109.5C81—C80—H80A120.4
H24B—C24—H24C109.5C82—C81—C80118.7 (3)
C18—C25—C28111.5 (3)C82—C81—H81A120.7
C18—C25—C26109.7 (3)C80—C81—H81A120.7
C28—C25—C26107.6 (3)N8—C82—C81122.8 (3)
C18—C25—C27110.1 (3)N8—C82—H82A118.6
C28—C25—C27108.8 (3)C81—C82—H82A118.6
C26—C25—C27109.1 (3)N9—C83—C84122.6 (3)
C25—C26—H26A109.5N9—C83—H83A118.7
C25—C26—H26B109.5C84—C83—H83A118.7
H26A—C26—H26B109.5C83—C84—C85119.1 (3)
C25—C26—H26C109.5C83—C84—H84A120.4
H26A—C26—H26C109.5C85—C84—H84A120.4
H26B—C26—H26C109.5C86—C85—C84118.3 (3)
C25—C27—H27A109.5C86—C85—H85A120.9
C25—C27—H27B109.5C84—C85—H85A120.9
H27A—C27—H27B109.5C85—C86—C87119.1 (4)
C25—C27—H27C109.5C85—C86—H86A120.4
H27A—C27—H27C109.5C87—C86—H86A120.4
H27B—C27—H27C109.5N9—C87—C86122.9 (3)
C25—C28—H28A109.5N9—C87—H87A118.5
C25—C28—H28B109.5C86—C87—H87A118.5
H28A—C28—H28B109.5C5S—N1S—C1S119.7 (6)
C25—C28—H28C109.5N1S—C1S—C2S122.0 (5)
H28A—C28—H28C109.5N1S—C1S—H1SB119.0
H28B—C28—H28C109.5C2S—C1S—H1SB119.0
C30—C29—N1125.8 (3)C1S—C2S—C3S117.8 (6)
C30—C29—H29A117.1C1S—C2S—H2SA121.1
N1—C29—H29A117.1C3S—C2S—H2SA121.1
C29—C30—C31118.0 (4)C4S—C3S—C2S117.0 (5)
C29—C30—H30A121.0C4S—C3S—H3SA121.5
C31—C30—H30A121.0C2S—C3S—H3SA121.5
C32—C31—C30119.2 (3)C5S—C4S—C3S120.9 (5)
C32—C31—H31A120.4C5S—C4S—H4SA119.5
C30—C31—H31A120.4C3S—C4S—H4SA119.5
C31—C32—C33118.8 (4)N1S—C5S—C4S122.6 (6)
C31—C32—H32A120.6N1S—C5S—H5SA118.7
C33—C32—H32A120.6C4S—C5S—H5SA118.7
N1—C33—C32123.5 (3)C6S—N2S—C10S117.3 (4)
N1—C33—H33A118.2N2S—C6S—C7S124.6 (5)
C32—C33—H33A118.2N2S—C6S—H6SA117.7
N2—C34—C35122.0 (4)C7S—C6S—H6SA117.7
N2—C34—H34A119.0C6S—C7S—C8S118.6 (4)
C35—C34—H34A119.0C6S—C7S—H7SA120.7
C36—C35—C34121.1 (4)C8S—C7S—H7SA120.7
C36—C35—H35A119.4C7S—C8S—C9S118.9 (4)
C34—C35—H35A119.4C7S—C8S—H8SA120.6
C35—C36—C37117.0 (4)C9S—C8S—H8SA120.6
C35—C36—H36A121.5C8S—C9S—C10S118.1 (5)
C37—C36—H36A121.5C8S—C9S—H9SA121.0
C36—C37—C38119.7 (4)C10S—C9S—H9SA121.0
C36—C37—H37A120.2N2S—C10S—C9S122.6 (5)
C38—C37—H37A120.2N2S—C10S—H10D118.7
N2—C38—C37123.1 (3)C9S—C10S—H10D118.7
N2—C38—H38A118.5C15S—N3S—C11S116.6 (4)
C37—C38—H38A118.5N3S—C11S—C12S123.0 (4)
N3—C39—C40123.9 (3)N3S—C11S—H11A118.5
N3—C39—H39A118.0C12S—C11S—H11A118.5
C40—C39—H39A118.0C13S—C12S—C11S118.3 (4)
C41—C40—C39118.9 (4)C13S—C12S—H12D120.9
C41—C40—H40A120.6C11S—C12S—H12D120.9
C39—C40—H40A120.6C12S—C13S—C14S119.0 (4)
C40—C41—C42118.3 (3)C12S—C13S—H13D120.5
C40—C41—H41A120.8C14S—C13S—H13D120.5
C42—C41—H41A120.8C15S—C14S—C13S118.6 (4)
C41—C42—C43119.0 (3)C15S—C14S—H14D120.7
C41—C42—H42A120.5C13S—C14S—H14D120.7
C43—C42—H42A120.5N3S—C15S—C14S124.6 (4)
N3—C43—C42123.2 (3)N3S—C15S—H15A117.7
N3—C43—H43A118.4C14S—C15S—H15A117.7
C42—C43—H43A118.4
Symmetry code: (i) x+2, y+1, z.

Experimental details

Crystal data
Chemical formulaC58H70Cd2N6O4·2C5H5N
Mr1298.22
Crystal system, space groupTriclinic, P1
Temperature (K)110
a, b, c (Å)15.743 (5), 17.549 (6), 19.945 (7)
α, β, γ (°)91.051 (7), 108.916 (6), 111.094 (6)
V3)4806 (3)
Z3
Radiation typeMo Kα
µ (mm1)0.72
Crystal size (mm)0.5 × 0.4 × 0.1
Data collection
DiffractometerBruker SMART1000 CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.456, 0.931
No. of measured, independent and
observed [I > 2σ(I)] reflections
55993, 27455, 16608
Rint0.034
(sin θ/λ)max1)0.705
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.050, 0.133, 0.96
No. of reflections27455
No. of parameters1108
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)4.89, 1.19

Computer programs: SMART (Bruker, 2000), SMART, SHELXTL (Sheldrick, 1997), XP in SHELXTL.

Selected geometric parameters (Å, º) top
Cd1—O12.206 (2)O2—C61.341 (3)
Cd1—O42.224 (2)O3—C151.316 (3)
Cd1—O22.278 (2)O4—C201.343 (3)
Cd1—N32.381 (3)C15—C201.440 (4)
Cd1—N22.404 (3)Cd3—O62.219 (2)
Cd1—N12.440 (3)Cd3—O5i2.231 (2)
O1—C11.323 (3)Cd3—O52.273 (2)
C1—C61.441 (4)Cd3—N82.354 (2)
Cd2—O32.209 (2)Cd3—N92.376 (3)
Cd2—O22.237 (2)Cd3—N72.453 (2)
Cd2—O42.281 (2)O5—C591.338 (3)
Cd2—N62.373 (2)O6—C641.319 (3)
Cd2—N42.384 (3)C59—C641.442 (4)
Cd2—N52.471 (2)
O1—Cd1—O4149.56 (7)O2—Cd2—N5124.93 (8)
O1—Cd1—O274.50 (7)O4—Cd2—N5159.80 (8)
O4—Cd1—O275.46 (7)N6—Cd2—N582.29 (8)
O1—Cd1—N392.21 (8)N4—Cd2—N580.42 (9)
O4—Cd1—N389.25 (8)C6—O2—Cd2142.39 (17)
O2—Cd1—N3102.09 (9)C6—O2—Cd1113.01 (16)
O1—Cd1—N297.49 (9)Cd2—O2—Cd1104.52 (8)
O4—Cd1—N291.12 (8)O6—Cd3—O5i150.66 (7)
O2—Cd1—N297.33 (9)O6—Cd3—O574.58 (7)
N3—Cd1—N2160.02 (10)O5i—Cd3—O576.89 (8)
O1—Cd1—N186.77 (9)O6—Cd3—N891.36 (8)
O4—Cd1—N1123.54 (8)O5i—Cd3—N890.01 (8)
O2—Cd1—N1160.71 (8)O5—Cd3—N8106.00 (8)
N3—Cd1—N182.90 (9)O6—Cd3—N995.21 (8)
N2—Cd1—N180.27 (9)O5i—Cd3—N992.53 (8)
C1—O1—Cd1115.26 (16)O5—Cd3—N992.18 (8)
O3—Cd2—O2148.84 (7)N8—Cd3—N9161.74 (9)
O3—Cd2—O474.36 (7)O6—Cd3—N786.60 (8)
O2—Cd2—O475.16 (7)O5i—Cd3—N7122.53 (8)
O3—Cd2—N691.90 (8)O5—Cd3—N7159.80 (8)
O2—Cd2—N688.22 (8)N8—Cd3—N781.27 (9)
O4—Cd2—N6102.10 (8)N9—Cd3—N782.13 (9)
O3—Cd2—N4101.01 (8)C59—O5—Cd3i143.40 (17)
O2—Cd2—N490.00 (8)C59—O5—Cd3113.02 (16)
O4—Cd2—N499.06 (8)Cd3i—O5—Cd3103.11 (8)
N6—Cd2—N4157.55 (9)C64—O6—Cd3114.78 (16)
O3—Cd2—N585.86 (8)
Symmetry code: (i) x+2, y+1, z.
 

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