Literature DB >> 21581536

Tris(2,2'-bipyridine-κN,N')cadmium(II) bis-(perchlorate) hemihydrate.

Weiguang Zhang1, Zhengjing Jiang, Lude Lu.   

Abstract

The asymmetric unit of the title compound, [Cd(C(10)H(8)N(2))(3)](ClO(4))(2)·0.5H(2)O, consists of one complex [Cd(bpy)(3)](2+) cation (bpy = 2,2'-bipyridine), two perchlorate anions and one water molecule with half-occupancy. The central cadmium(II) ion is bound to six N atoms from three bpy ligands in a distorted octa-hedral coordination, with Cd-N bond distances ranging from 2.304 (3) to 2.395 (2) Å.

Entities:  

Year:  2008        PMID: 21581536      PMCID: PMC2967850          DOI: 10.1107/S1600536808036593

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For applications of metal complexes of 2,2′-bipyridine and its derivatives, see: Kuang et al. (2006 ▶). For cadmium complexes, see: Kundu et al. (2005 ▶); Ranjbar et al. (2007 ▶); Shi et al. (2006 ▶); Zheng et al. (2005 ▶).

Experimental

Crystal data

[Cd(C10H8N2)3](ClO4)2·0.5H2O M = 788.87 Triclinic, a = 8.1704 (3) Å b = 11.0282 (5) Å c = 18.3875 (7) Å α = 104.631 (1)° β = 92.652 (1)° γ = 100.520 (1)° V = 1568.68 (11) Å3 Z = 2 Mo Kα radiation μ = 0.93 mm−1 T = 173 (2) K 0.20 × 0.16 × 0.12 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.82, T max = 0.90 19563 measured reflections 6067 independent reflections 5114 reflections with I > 2σ(I) R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.034 wR(F 2) = 0.107 S = 1.01 6067 reflections 434 parameters H-atom parameters constrained Δρmax = 0.44 e Å−3 Δρmin = −0.54 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808036593/hg2440sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808036593/hg2440Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(C10H8N2)3](ClO4)2·0.5H2OZ = 2
Mr = 788.87F(000) = 794
Triclinic, P1Dx = 1.670 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.1704 (3) ÅCell parameters from 5350 reflections
b = 11.0282 (5) Åθ = 2.3–24.2°
c = 18.3875 (7) ŵ = 0.93 mm1
α = 104.631 (1)°T = 173 K
β = 92.652 (1)°Block, light red
γ = 100.520 (1)°0.20 × 0.16 × 0.12 mm
V = 1568.68 (11) Å3
Bruker SMART CCD area-detector diffractometer6067 independent reflections
Radiation source: fine-focus sealed tube5114 reflections with I > 2σ(I)
graphiteRint = 0.037
φ and ω scansθmax = 26.0°, θmin = 1.2°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −9→10
Tmin = 0.82, Tmax = 0.90k = −13→13
19563 measured reflectionsl = −22→22
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0692P)2] where P = (Fo2 + 2Fc2)/3
6067 reflections(Δ/σ)max = 0.001
434 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = −0.54 e Å3
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.
xyzUiso*/UeqOcc. (<1)
Cd10.49907 (3)0.73554 (2)0.243298 (12)0.03097 (10)
N10.6598 (3)0.6830 (2)0.33902 (14)0.0294 (6)
N20.6508 (3)0.5860 (2)0.18631 (14)0.0301 (6)
N30.3534 (3)0.7832 (3)0.14562 (14)0.0322 (6)
N40.6676 (3)0.8972 (3)0.20701 (14)0.0317 (6)
N50.2893 (3)0.5889 (3)0.28060 (15)0.0343 (6)
N60.3367 (3)0.8481 (3)0.32562 (14)0.0336 (6)
C10.7042 (3)0.5700 (3)0.31281 (16)0.0275 (6)
C20.7179 (4)0.4891 (3)0.35877 (18)0.0348 (7)
H20.74760.40860.33900.042*
C30.6876 (4)0.5275 (3)0.43375 (19)0.0402 (8)
H30.69490.47330.46610.048*
C40.6469 (4)0.6444 (4)0.46057 (19)0.0399 (8)
H40.62840.67350.51220.048*
C50.6330 (4)0.7198 (3)0.41210 (17)0.0336 (7)
H50.60340.80060.43100.040*
C60.7320 (4)0.5340 (3)0.23180 (17)0.0280 (6)
C70.8391 (4)0.4527 (3)0.20353 (19)0.0373 (8)
H70.89510.41540.23600.045*
C80.8633 (4)0.4266 (3)0.1278 (2)0.0411 (8)
H80.93690.37180.10770.049*
C90.7789 (4)0.4813 (3)0.08131 (19)0.0398 (8)
H90.79340.46510.02900.048*
C100.6737 (4)0.5596 (3)0.11315 (18)0.0352 (7)
H100.61460.59650.08150.042*
C110.4207 (4)0.8910 (3)0.12777 (17)0.0312 (7)
C120.3271 (5)0.9441 (4)0.0842 (2)0.0444 (9)
H120.37541.02100.07230.053*
C130.1647 (5)0.8857 (4)0.0582 (2)0.0491 (9)
H130.09980.92170.02820.059*
C140.0970 (4)0.7748 (4)0.07580 (19)0.0447 (9)
H14−0.01490.73200.05800.054*
C150.1953 (4)0.7269 (3)0.12003 (19)0.0414 (8)
H150.14850.65050.13290.050*
C160.5991 (4)0.9476 (3)0.15684 (17)0.0330 (7)
C170.6922 (5)1.0456 (4)0.1331 (2)0.0464 (9)
H170.64151.08390.09960.056*
C180.8591 (5)1.0872 (4)0.1585 (2)0.0555 (11)
H180.92491.15410.14230.067*
C190.9301 (4)1.0308 (4)0.2077 (2)0.0468 (9)
H191.04601.05560.22440.056*
C200.8297 (4)0.9392 (3)0.23142 (19)0.0409 (8)
H200.87690.90300.26710.049*
C210.2114 (4)0.6420 (3)0.34008 (17)0.0365 (8)
C220.1362 (4)0.5700 (4)0.3857 (2)0.0515 (11)
H220.08520.60960.42830.062*
C230.1353 (5)0.4418 (5)0.3693 (2)0.0656 (14)
H230.08320.39160.40010.079*
C240.2102 (5)0.3873 (4)0.3083 (3)0.0612 (13)
H240.20920.29810.29500.073*
C250.2881 (4)0.4648 (3)0.2658 (2)0.0450 (9)
H250.34320.42700.22410.054*
C260.2157 (4)0.7800 (3)0.35443 (17)0.0357 (8)
C270.0983 (4)0.8389 (5)0.3950 (2)0.0543 (11)
H270.01240.79010.41490.065*
C280.1078 (5)0.9681 (5)0.4058 (2)0.0625 (13)
H280.02981.00980.43390.075*
C290.2321 (6)1.0361 (4)0.3754 (2)0.0587 (12)
H290.23981.12510.38140.070*
C300.3449 (5)0.9735 (4)0.3362 (2)0.0434 (9)
H300.43171.02090.31590.052*
Cl10.30915 (10)0.28250 (8)0.06302 (4)0.03444 (19)
O10.2886 (4)0.4107 (3)0.07130 (16)0.0558 (7)
O20.4439 (3)0.2792 (3)0.11403 (16)0.0599 (8)
O30.3387 (6)0.2297 (4)−0.01150 (18)0.1051 (14)
O40.1617 (4)0.2129 (3)0.0806 (2)0.0909 (13)
Cl20.75289 (11)0.16580 (8)0.41261 (5)0.0389 (2)
O50.7279 (3)0.0316 (2)0.40528 (15)0.0488 (6)
O60.6449 (3)0.2223 (3)0.46332 (17)0.0605 (8)
O70.9241 (3)0.2243 (3)0.44150 (15)0.0558 (7)
O80.7206 (4)0.1863 (2)0.34000 (15)0.0639 (8)
O90.4144 (9)0.1855 (6)0.2510 (3)0.0752 (19)0.50
H9A0.43230.21350.21250.090*0.50
H9B0.50800.18810.27410.090*0.50
U11U22U33U12U13U23
Cd10.03118 (15)0.03525 (17)0.03679 (15)0.01384 (10)0.01081 (10)0.02177 (11)
N10.0266 (13)0.0319 (15)0.0321 (13)0.0070 (11)0.0015 (10)0.0123 (11)
N20.0314 (14)0.0286 (14)0.0346 (14)0.0091 (11)0.0050 (11)0.0136 (11)
N30.0347 (14)0.0329 (15)0.0339 (14)0.0088 (12)0.0074 (11)0.0158 (12)
N40.0332 (14)0.0316 (15)0.0331 (14)0.0070 (11)0.0079 (11)0.0123 (12)
N50.0298 (14)0.0376 (17)0.0343 (14)−0.0015 (12)−0.0016 (11)0.0144 (12)
N60.0276 (13)0.0422 (17)0.0334 (14)0.0115 (12)0.0054 (11)0.0108 (12)
C10.0245 (15)0.0268 (16)0.0332 (15)0.0059 (12)0.0013 (12)0.0115 (13)
C20.0365 (17)0.0321 (18)0.0413 (18)0.0124 (14)0.0049 (14)0.0155 (15)
C30.044 (2)0.044 (2)0.0403 (18)0.0098 (16)0.0021 (15)0.0245 (16)
C40.0398 (19)0.052 (2)0.0304 (16)0.0107 (16)0.0043 (14)0.0142 (16)
C50.0330 (17)0.0354 (19)0.0342 (16)0.0093 (14)0.0040 (13)0.0104 (14)
C60.0260 (15)0.0258 (16)0.0349 (16)0.0062 (12)0.0033 (12)0.0120 (13)
C70.0389 (18)0.0336 (18)0.0431 (18)0.0155 (15)0.0008 (14)0.0117 (15)
C80.0415 (19)0.0353 (19)0.048 (2)0.0167 (15)0.0110 (15)0.0067 (16)
C90.048 (2)0.038 (2)0.0345 (17)0.0082 (16)0.0124 (15)0.0109 (15)
C100.0399 (18)0.0368 (19)0.0338 (17)0.0095 (15)0.0081 (14)0.0163 (14)
C110.0402 (18)0.0288 (17)0.0295 (15)0.0120 (14)0.0088 (13)0.0123 (13)
C120.053 (2)0.042 (2)0.047 (2)0.0158 (17)0.0025 (17)0.0229 (17)
C130.055 (2)0.054 (2)0.049 (2)0.0261 (19)−0.0013 (17)0.0233 (19)
C140.0367 (19)0.056 (2)0.0426 (19)0.0150 (17)−0.0029 (15)0.0124 (17)
C150.0425 (19)0.039 (2)0.0441 (19)0.0038 (15)0.0016 (15)0.0179 (16)
C160.0432 (18)0.0288 (17)0.0329 (16)0.0102 (14)0.0127 (14)0.0153 (14)
C170.054 (2)0.044 (2)0.048 (2)0.0061 (17)0.0139 (17)0.0257 (17)
C180.059 (3)0.042 (2)0.065 (3)−0.0041 (19)0.023 (2)0.020 (2)
C190.0372 (19)0.045 (2)0.053 (2)0.0009 (16)0.0099 (16)0.0086 (18)
C200.041 (2)0.038 (2)0.0427 (19)0.0066 (16)0.0029 (15)0.0106 (16)
C210.0248 (16)0.053 (2)0.0295 (16)−0.0026 (14)−0.0019 (12)0.0162 (15)
C220.0375 (19)0.074 (3)0.0388 (19)−0.0165 (19)−0.0037 (15)0.0289 (19)
C230.050 (2)0.088 (4)0.054 (3)−0.028 (2)−0.015 (2)0.044 (3)
C240.061 (3)0.047 (2)0.071 (3)−0.018 (2)−0.025 (2)0.035 (2)
C250.043 (2)0.039 (2)0.051 (2)−0.0024 (16)−0.0087 (16)0.0181 (17)
C260.0251 (16)0.056 (2)0.0271 (15)0.0074 (15)0.0023 (12)0.0129 (15)
C270.0343 (19)0.097 (4)0.0361 (19)0.026 (2)0.0081 (15)0.016 (2)
C280.053 (3)0.103 (4)0.041 (2)0.050 (3)0.0073 (18)0.011 (2)
C290.075 (3)0.057 (3)0.047 (2)0.041 (2)−0.010 (2)0.003 (2)
C300.043 (2)0.040 (2)0.048 (2)0.0144 (16)−0.0003 (16)0.0095 (17)
Cl10.0324 (4)0.0375 (5)0.0363 (4)0.0062 (3)0.0032 (3)0.0155 (3)
O10.0639 (18)0.0448 (16)0.0671 (18)0.0208 (14)0.0003 (14)0.0238 (14)
O20.0509 (16)0.0511 (17)0.080 (2)0.0109 (13)−0.0190 (14)0.0257 (15)
O30.184 (4)0.103 (3)0.0511 (19)0.082 (3)0.038 (2)0.0193 (19)
O40.0405 (16)0.090 (3)0.167 (4)0.0002 (16)0.0150 (19)0.087 (3)
Cl20.0446 (5)0.0342 (5)0.0418 (4)0.0122 (4)0.0064 (4)0.0137 (4)
O50.0504 (15)0.0356 (14)0.0681 (17)0.0119 (11)0.0114 (13)0.0242 (13)
O60.0511 (16)0.0616 (18)0.0702 (19)0.0283 (14)0.0178 (14)0.0060 (15)
O70.0423 (14)0.0619 (18)0.0617 (17)−0.0040 (13)0.0091 (12)0.0235 (14)
O80.109 (2)0.0407 (16)0.0478 (15)0.0232 (16)−0.0063 (15)0.0195 (13)
O90.105 (5)0.075 (4)0.066 (4)0.045 (4)0.018 (3)0.036 (3)
Cd1—N42.304 (3)C13—H130.9500
Cd1—N22.312 (3)C14—C151.377 (5)
Cd1—N62.330 (3)C14—H140.9500
Cd1—N32.329 (3)C15—H150.9500
Cd1—N52.383 (3)C16—C171.380 (5)
Cd1—N12.395 (2)C17—C181.375 (5)
N1—C11.340 (4)C17—H170.9500
N1—C51.343 (4)C18—C191.382 (6)
N2—C101.332 (4)C18—H180.9500
N2—C61.341 (4)C19—C201.356 (5)
N3—C151.334 (4)C19—H190.9500
N3—C111.341 (4)C20—H200.9500
N4—C201.337 (4)C21—C221.384 (5)
N4—C161.341 (4)C21—C261.471 (5)
N5—C251.325 (4)C22—C231.368 (6)
N5—C211.349 (4)C22—H220.9500
N6—C301.336 (4)C23—C241.362 (7)
N6—C261.342 (4)C23—H230.9500
C1—C21.390 (4)C24—C251.389 (5)
C1—C61.481 (4)C24—H240.9500
C2—C31.384 (5)C25—H250.9500
C2—H20.9500C26—C271.395 (5)
C3—C41.367 (5)C27—C281.375 (6)
C3—H30.9500C27—H270.9500
C4—C51.378 (5)C28—C291.376 (6)
C4—H40.9500C28—H280.9500
C5—H50.9500C29—C301.374 (5)
C6—C71.391 (4)C29—H290.9500
C7—C81.380 (5)C30—H300.9500
C7—H70.9500Cl1—O31.398 (3)
C8—C91.389 (5)Cl1—O41.404 (3)
C8—H80.9500Cl1—O21.425 (2)
C9—C101.374 (5)Cl1—O11.425 (3)
C9—H90.9500Cl2—O61.422 (3)
C10—H100.9500Cl2—O51.427 (3)
C11—C121.384 (4)Cl2—O81.430 (3)
C11—C161.492 (4)Cl2—O71.444 (3)
C12—C131.370 (5)O9—H9A0.8500
C12—H120.9500O9—H9B0.8500
C13—C141.370 (5)
N4—Cd1—N292.41 (9)C11—C12—H12120.0
N4—Cd1—N6101.98 (10)C12—C13—C14119.3 (3)
N2—Cd1—N6162.88 (10)C12—C13—H13120.4
N4—Cd1—N371.23 (9)C14—C13—H13120.4
N2—Cd1—N3106.18 (9)C13—C14—C15118.3 (3)
N6—Cd1—N387.41 (9)C13—C14—H14120.8
N4—Cd1—N5170.37 (9)C15—C14—H14120.8
N2—Cd1—N596.17 (10)N3—C15—C14122.8 (3)
N6—Cd1—N570.34 (10)N3—C15—H15118.6
N3—Cd1—N5102.03 (9)C14—C15—H15118.6
N4—Cd1—N1107.32 (9)N4—C16—C17120.7 (3)
N2—Cd1—N170.96 (9)N4—C16—C11116.7 (3)
N6—Cd1—N195.64 (9)C17—C16—C11122.6 (3)
N3—Cd1—N1176.86 (8)C18—C17—C16119.4 (4)
N5—Cd1—N179.74 (9)C18—C17—H17120.3
C1—N1—C5118.7 (3)C16—C17—H17120.3
C1—N1—Cd1111.40 (18)C17—C18—C19119.4 (4)
C5—N1—Cd1121.4 (2)C17—C18—H18120.3
C10—N2—C6119.4 (3)C19—C18—H18120.3
C10—N2—Cd1123.3 (2)C20—C19—C18118.1 (3)
C6—N2—Cd1116.9 (2)C20—C19—H19120.9
C15—N3—C11119.1 (3)C18—C19—H19120.9
C15—N3—Cd1123.0 (2)N4—C20—C19123.1 (3)
C11—N3—Cd1116.1 (2)N4—C20—H20118.4
C20—N4—C16119.1 (3)C19—C20—H20118.4
C20—N4—Cd1123.3 (2)N5—C21—C22121.2 (4)
C16—N4—Cd1117.5 (2)N5—C21—C26116.2 (3)
C25—N5—C21118.0 (3)C22—C21—C26122.5 (3)
C25—N5—Cd1122.9 (2)C23—C22—C21120.0 (4)
C21—N5—Cd1114.7 (2)C23—C22—H22120.0
C30—N6—C26119.6 (3)C21—C22—H22120.0
C30—N6—Cd1122.2 (2)C24—C23—C22118.9 (4)
C26—N6—Cd1117.6 (2)C24—C23—H23120.5
N1—C1—C2121.6 (3)C22—C23—H23120.5
N1—C1—C6116.5 (3)C23—C24—C25118.6 (4)
C2—C1—C6121.8 (3)C23—C24—H24120.7
C3—C2—C1119.0 (3)C25—C24—H24120.7
C3—C2—H2120.5N5—C25—C24123.2 (4)
C1—C2—H2120.5N5—C25—H25118.4
C4—C3—C2119.0 (3)C24—C25—H25118.4
C4—C3—H3120.5N6—C26—C27120.6 (4)
C2—C3—H3120.5N6—C26—C21117.1 (3)
C3—C4—C5119.4 (3)C27—C26—C21122.2 (3)
C3—C4—H4120.3C28—C27—C26119.5 (4)
C5—C4—H4120.3C28—C27—H27120.2
N1—C5—C4122.2 (3)C26—C27—H27120.2
N1—C5—H5118.9C27—C28—C29119.0 (4)
C4—C5—H5118.9C27—C28—H28120.5
N2—C6—C7120.9 (3)C29—C28—H28120.5
N2—C6—C1116.6 (3)C30—C29—C28119.1 (4)
C7—C6—C1122.5 (3)C30—C29—H29120.4
C8—C7—C6119.4 (3)C28—C29—H29120.4
C8—C7—H7120.3N6—C30—C29122.2 (4)
C6—C7—H7120.3N6—C30—H30118.9
C7—C8—C9119.2 (3)C29—C30—H30118.9
C7—C8—H8120.4O3—Cl1—O4110.3 (3)
C9—C8—H8120.4O3—Cl1—O2110.4 (2)
C10—C9—C8118.1 (3)O4—Cl1—O2108.31 (19)
C10—C9—H9120.9O3—Cl1—O1109.2 (2)
C8—C9—H9120.9O4—Cl1—O1108.11 (19)
N2—C10—C9123.0 (3)O2—Cl1—O1110.55 (16)
N2—C10—H10118.5O6—Cl2—O5110.51 (17)
C9—C10—H10118.5O6—Cl2—O8109.87 (19)
N3—C11—C12120.6 (3)O5—Cl2—O8109.15 (16)
N3—C11—C16116.4 (3)O6—Cl2—O7108.97 (17)
C12—C11—C16123.0 (3)O5—Cl2—O7109.12 (16)
C13—C12—C11120.0 (3)O8—Cl2—O7109.20 (17)
C13—C12—H12120.0H9A—O9—H9B108.6
Table 1

Selected geometric parameters (Å, °)

Cd1—N42.304 (3)
Cd1—N22.312 (3)
Cd1—N62.330 (3)
Cd1—N32.329 (3)
Cd1—N52.383 (3)
Cd1—N12.395 (2)
  2 in total

1.  Ion coordinating sensitizer for high efficiency mesoscopic dye-sensitized solar cells: influence of lithium ions on the photovoltaic performance of liquid and solid-state cells.

Authors:  Daibin Kuang; Cedric Klein; Henry J Snaith; Jacques-E Moser; Robin Humphry-Baker; Pascal Comte; Shaik M Zakeeruddin; Michael Grätzel
Journal:  Nano Lett       Date:  2006-04       Impact factor: 11.189

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

  2 in total

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