Startseite Crystal structure of bis(μ-nitrato-κ2O:O)-bis[1,2-bis(diphenylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]disilver(I) dicloromethane monosolvate, C54H64B20Cl4O6P4Ag2
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Crystal structure of bis(μ-nitrato-κ2O:O)-bis[1,2-bis(diphenylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]disilver(I) dicloromethane monosolvate, C54H64B20Cl4O6P4Ag2

  • Wang Yanfei , Wang Xin , Gao Qianqian und Yang Liguo EMAIL logo
Veröffentlicht/Copyright: 29. Oktober 2016

Abstract

C54H64B20Cl4O6P4Ag2, triclinic, P1̅ (no. 2), a = 10.1200(10) Å, b = 11.9101(11) Å, c = 14.4999(15) Å, α = 86.432(2)°, β = 80.670(1)°, γ = 84.031(2)°, V = 1713.4(3)Å3, Z = 1, Rgt(F) = 0.0535, wRref(F2) = 0.1544, T = 298 K.

CCDC no.:: 768110

The crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Yellow blocks
Size:0.80 × 0.43 × 0.18 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:8.7 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:50°, >98%
N(hkl)measured, N(hkl)unique, Rint:8733, 5920, 0.038
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4341
N(param)refined:415
Programs:SHELX [7], Bruker programs [8]
Table 2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Ag10.09951(4)0.09046(3)0.39690(3)0.04984(17)
P10.32796(12)0.10265(10)0.31109(8)0.0384(3)
P20.00759(12)0.23383(10)0.28739(8)0.0395(3)
Cl10.3154(5)0.2567(5)0.7494(3)0.265(3)
Cl20.0975(6)0.3305(5)0.8800(2)0.268(3)
N10.0408(5)0.1597(4)0.6003(3)0.0534(11)
O10.0043(4)0.0854(3)0.5541(2)0.0534(9)
O20.1177(5)0.2259(4)0.5602(3)0.0727(12)
O30.0018(6)0.1602(5)0.6841(3)0.1086(19)
B10.2590(6)0.2522(5)0.1386(4)0.0437(13)
H10.23460.17780.10550.052*
B20.4277(6)0.2775(5)0.1463(4)0.0507(14)
H20.51480.22130.11570.061*
B30.4231(6)0.3413(5)0.2540(4)0.0481(14)
H30.50650.32720.29470.058*
B40.2524(6)0.3536(4)0.3088(4)0.0422(13)
H40.22350.34400.38520.051*
B50.1611(6)0.4511(5)0.2388(4)0.0495(14)
H50.07490.50840.26920.059*
B60.1652(7)0.3869(5)0.1314(4)0.0494(14)
H60.08150.40190.09100.059*
B70.3340(7)0.3690(5)0.0748(4)0.0547(16)
H70.35930.3717−0.00190.066*
B80.4349(7)0.4253(5)0.1480(5)0.0609(17)
H80.52610.46610.11860.073*
B90.3280(7)0.4726(5)0.2506(5)0.0545(15)
H90.34970.54340.28920.065*
B100.2748(7)0.4916(5)0.1392(5)0.0579(16)
H100.26270.57570.10400.070*
C10.3193(5)0.2406(4)0.2423(3)0.0395(11)
C20.1565(5)0.3096(4)0.2334(3)0.0399(10)
C30.4704(5)0.1114(4)0.3718(3)0.0436(11)
C40.4411(6)0.1590(5)0.4574(4)0.0563(14)
H4A0.35270.18410.48090.068*
C50.5429(7)0.1697(6)0.5093(4)0.0718(17)
H5A0.52340.20400.56640.086*
C60.6726(7)0.1292(6)0.4753(5)0.078(2)
H6A0.74170.13710.50890.094*
C70.6997(6)0.0771(6)0.3920(5)0.0733(18)
H7A0.78690.04680.37050.088*
C80.6001(5)0.0691(5)0.3398(4)0.0579(14)
H8A0.62020.03500.28260.069*
C90.3729(5)−0.0076(4)0.2272(3)0.0440(11)
C100.4781(6)−0.0159(5)0.1540(4)0.0621(15)
H10A0.53490.04160.14090.074*
C110.4996(7)−0.1096(5)0.0997(4)0.0727(18)
H110.5715−0.11530.05080.087*
C120.4157(7)−0.1942(5)0.1175(5)0.0709(17)
H120.4298−0.25630.08010.085*
C130.3130(7)−0.1875(5)0.1891(5)0.0758(18)
H130.2575−0.24590.20170.091*
C140.2891(6)−0.0954(4)0.2436(4)0.0564(14)
H140.2165−0.09120.29200.068*
C15−0.1099(5)0.3413(4)0.3477(4)0.0469(12)
C16−0.2313(6)0.3816(5)0.3217(5)0.0676(17)
H16−0.25440.36020.26630.081*
C17−0.3193(6)0.4546(6)0.3792(6)0.085(2)
H17−0.40200.48150.36230.102*
C18−0.2856(7)0.4868(6)0.4597(6)0.088(2)
H18−0.34440.53730.49670.105*
C19−0.1694(7)0.4471(7)0.4861(5)0.090(2)
H19−0.14700.46960.54140.108*
C20−0.0823(6)0.3729(6)0.4319(4)0.0699(17)
H20−0.00290.34320.45230.084*
C21−0.0618(5)0.1887(4)0.1895(3)0.0477(12)
C22−0.0559(5)0.0728(4)0.1814(4)0.0528(13)
H22−0.01590.02400.22360.063*
C23−0.1093(7)0.0296(6)0.1105(5)0.0738(18)
H23−0.1033−0.04820.10470.089*
C24−0.1695(7)0.0988(8)0.0504(5)0.084(2)
H24−0.20580.06830.00370.100*
C25−0.1786(7)0.2121(7)0.0563(4)0.0785(19)
H25−0.22090.25870.01380.094*
C26−0.1245(6)0.2596(5)0.1263(4)0.0627(15)
H26−0.13050.33760.13050.075*
C270.1641(10)0.3281(8)0.7698(6)0.115(3)
H27A0.17120.40530.74530.139*
H27B0.10400.29480.73580.139*

Source of material

The reaction was carried out under an atmosphere of dry nitrogen. Ethanol and dichloromethane were dried and distilled under nitrogen prior to use. 1,2-(PPh2)2-1,2-C2B10H10, was synthesized according to the literature [1]. All the other chemicals were purchased and used as received. AgNO3 (16.9 mg, 0.1 mmol) and 1,2-(PPh2)2-1,2-C2B10H10 (51.2 mg, 0.1 mmol) were mixed in chloromethane (10 mL). The mixture was stirred for 6 h under a dry N2 atmosphere, during which a yellow solution formed. After filtration, the solution was concentrated. The crystals were grown from a dichloromethane/n-hexane solution. (54.1%, m.p. 275–277 K). FT-IR (KBr) v (cm−l): 2989, 2966 2930, 2872 (C—H); 2614, 2602, 2585, 2556 (B—H); 1071 (C—P).

Experimental details

All H atoms were placed geometrically and treated as riding on their parent atoms, with B—H 1.10, C—H 0.96, with Uiso(H) = 1.2Ueq(B), Uiso(H) = 1.5Ueq(C).

Discussion

The title structure possesses a binuclear structure with two bidentate organic ligands and two bridiging nitrato ligands (cf. the figure). Both Ag atoms have the same coordination environment because the complex is located round an inversion center. The Ag atom is tetrahedrally surrounded by two P atoms and two oxygen atoms of two nitrato ligands. The Ag—O bond lengths are 2.326(3) and 2.455(3) Å, which is longer than the corresponding bond reported for the complex [(Ag2(μ-ONO2)2){1,2-(PCy)2-1,2-C2B10H10}2] [2]. The Ag—P bond lengths are 2.4554(13) and 2.4726(13) Å, which are similar with the corresponding bond length of 2.49(3) in the complex [(Ag2(μ-I)2){1,2-(PCy)2-1,2-C2B10H10}2] [2]. The P—Ag—P angle is 90.80(4)°, which is smaller than the corresponding value of [(Ag2(μ-ONO2)2){1,2-(PCy)2-1,2-C2B10H10}2]. A similar change of P—Ag—P angles has also been observed previously [3]. The P(1)—C(1)—C(2)—P(2) angle in the title structure is 0°, while the value of the free ligand is 10.9(4)° [4, 5], indicating that this fragment is planar. The average bond lengths of C—P in the complexes (1.872(3) Å) are in agreement with that of 1.894(3)Å in the free ligand, suggesting that the coordination with the metal atom has no obvious influence on this distance [6].

Acknowledgements

This work was supported by the Key Scientific Research Projects of Colleges and Universities, Henan Province (Nos. 16A150001, 16A430012) and the Research Fund of Anyang Institute of Technology (Nos. YJJ2015021, YJJ2015022).

References

1 Zhang, D. P.; Dou, J. M.; Li, D. C.; Wang, D. Q.: 1,2-Bis(diphenylphosphino) -1,2-dicarba-closo-dodecaborane. Acta Crystallogr. E62 (2006) o418.10.1107/S1600536805042510Suche in Google Scholar

2 Yang, L. G.; Zhu, C. C.; Zhang, D. D.; Li, D. C., Wang, D. Q.; Dou, D. M.: 1D and 2D supramolecular structures of silver carborane dicyclohexylphosphine complexes constructed by C-H⋯H-B dihydrogen bonding interactions. Polyhedron 30 (2011) 1469–1477.10.1016/j.poly.2011.02.052Suche in Google Scholar

3 Caruso, F.; Camalli, M.; Rimml, H.; Venanzi, L. M.: Coordination properties of silver diphosphine complexes. Crystal and molecular structures of Ag2X2(m-PP)2 (X = I, Cl, NO3; m-PP = 1,3-bis[(diphenylphosphino)methyl]benzene) and Ag2X2(o-PP)2 (X = I, Cl; o-PP = 1,2-bis[(diphenylphosphino)methyl]benzene). Synthesis and 1H- and 31P-NMR spectroscopy of silver diphosphine complexes. Inorg. Chem. 34 (1995) 673–679.10.1021/ic00107a022Suche in Google Scholar

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Received: 2016-7-20
Accepted: 2016-10-14
Published Online: 2016-10-29
Published in Print: 2017-1-1

©2016 Wang Yanfei et al., published by De Gruyter.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Editorial
  3. Twenty years of crystal structure publication and the road ahead
  4. Crystal Structures
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  11. Crystal structure of 2-((3-(5-methyl-1-phenyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazol-4-yl)methylene)-1H-indene-1,3(2H)-dione, C28H19N5O2
  12. Crystal structure of 2-(5-(4-fluorophenyl)-3-p-tolyl-4,5-dihydro-1H-pyrazol-1-yl)-4-(5-methyl-1-p-tolyl-1H-1,2,3-triazol-4-yl)thiazole, C29H25FN6S
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  18. Crystal structure of 3-(adamantan-1-yl)-1-(4-bromophenyl)urea, C17H21BrN2O
  19. Crystal structure of (Z)-Ethyl 2-cyano-2-(3-phenylthiazolidin-2-ylidene) acetate, C14H14N2O2S
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  59. Crystal structure of cis-bis(2,2′-bipyridine-κ2N,N′)bis(thiocyanato-κN)nickel(II), C22H16N6NiS2
  60. Crystal structure of trans-dibromido(1,4,8,11-tetraazacyclotetradecane)nickel(II), C10H24Br2N4Ni
  61. Crystal structure of cis-tetrabromidobis(pyridine-κN)platinum(IV), C10H10Br4N2Pt
  62. Crystal structure of (E)-5-((4-chlorophenyl)diazenyl)-2-(5-(4-fluorophenyl)-3-(thiophen-2-yl)-4,5-dihydro-1H-pyrazol-1-yl)-4-methylthiazole, C23H17ClFN5S2
  63. The crystal structure of 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium tetrachloridocobaltate(II) monohydrate, C10H18Cl4CoN2O
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