Home Crystal structure of di-μ-chlorido-bis[1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]zinc(II), C52H108B20Cl2P4Zn2
Article Open Access

Crystal structure of di-μ-chlorido-bis[1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]zinc(II), C52H108B20Cl2P4Zn2

  • Wang Xin , Yang Liguo EMAIL logo , Gao Qianqian and Dai Yuqiang
Published/Copyright: October 8, 2016

Abstract

C52H108B20Cl2P4Zn2, monoclinic, C2/c (no. 15), a = 31.783(3) Å, b = 10.0780(10) Å, c = 24.9326(19) Å, β = 109.901(2)°, V = 7509.2(11) Å3, Z = 4, Rgt(F) = 0.0569, wRref(F2) = 0.0972, T = 298 K.

CCDC no.:: 1504437

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 0.18 × 0.08 × 0.06 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:8.3 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:18590, 6558, 0.132
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2649
N(param)refined:362
Programs:SHELX [7], Bruker programs [8]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.30463(2)0.76624(7)0.53116(3)0.0388(2)
Cl10.25360(4)0.59301(14)0.52602(5)0.0376(4)
P10.34466(5)0.85758(15)0.61647(6)0.0319(4)
P20.36191(5)0.73367(16)0.49798(5)0.0309(4)
B10.4322(2)0.7336(8)0.6165(2)0.0389(18)
H10.41930.63640.62360.047*
B20.4501(2)0.8572(7)0.6712(3)0.042(2)
H20.45030.83920.71480.051*
B30.4356(2)1.0162(8)0.6366(3)0.044(2)
H30.42651.10200.65760.053*
B40.4094(2)0.9821(7)0.5629(3)0.0368(19)
H40.38181.04360.53570.044*
B50.4500(2)0.9091(7)0.5364(3)0.042(2)
H50.45010.92550.49280.050*
B60.4646(2)0.7524(8)0.5713(3)0.0431(19)
H60.47420.66710.55050.052*
B70.4898(2)0.7796(8)0.6463(3)0.048(2)
H70.51520.71160.67360.058*
B80.4919(2)0.9561(8)0.6568(3)0.051(2)
H80.51951.00290.69110.061*
B90.4655(2)1.0377(8)0.5893(3)0.049(2)
H90.47501.13720.57930.059*
B100.5013(2)0.8937(8)0.5969(3)0.051(2)
H100.53450.90070.59270.061*
C10.40250(18)0.8793(6)0.6143(2)0.0371(16)
C20.41169(18)0.8138(5)0.5516(2)0.0362(16)
C30.32592(19)1.0220(6)0.6342(2)0.0404(16)
H3A0.34611.04940.67190.049*
C40.32459(19)1.1325(6)0.5909(2)0.0434(16)
H4A0.35471.15000.59100.052*
H4B0.30661.10390.55280.052*
C50.3049(2)1.2589(7)0.6061(2)0.0554(17)
H5A0.32441.29090.64280.066*
H5B0.30361.32650.57790.066*
C60.2587(2)1.2383(7)0.6087(2)0.0576(18)
H6A0.23821.21460.57120.069*
H6B0.24821.31990.62040.069*
C70.2598(2)1.1282(6)0.6510(2)0.0558(19)
H7A0.27751.15700.68920.067*
H7B0.22961.11110.65040.067*
C80.27955(18)1.0006(6)0.6372(2)0.0418(17)
H8A0.28120.93490.66630.050*
H8B0.26000.96640.60090.050*
C90.35583(18)0.7548(6)0.68182(19)0.0389(15)
H9A0.38240.70240.68460.047*
C100.36732(19)0.8267(6)0.7399(2)0.0429(17)
H10A0.39140.88960.74430.052*
H10B0.34140.87550.74120.052*
C110.3814(2)0.7268(6)0.7880(2)0.0465(17)
H11A0.40830.68150.78780.056*
H11B0.38830.77250.82420.056*
C120.3449(2)0.6262(6)0.7820(2)0.0576(19)
H12A0.35510.56160.81250.069*
H12B0.31890.67070.78540.069*
C130.3319(2)0.5559(6)0.7252(2)0.0528(19)
H13A0.30710.49660.72170.063*
H13B0.35690.50260.72380.063*
C140.3186(2)0.6530(6)0.6753(2)0.0486(17)
H14A0.29130.69870.67380.058*
H14B0.31270.60470.63990.058*
C150.35554(19)0.8075(5)0.4272(2)0.0358(16)
H150.38250.78890.41780.043*
C160.34621(19)0.9577(6)0.4221(2)0.0416(16)
H16A0.32040.97730.43320.050*
H16B0.37181.00500.44760.050*
C170.3373(2)1.0041(6)0.3611(2)0.0542(18)
H17A0.33091.09840.35850.065*
H17B0.36380.98950.35090.065*
C180.2981(2)0.9297(7)0.3198(2)0.062(2)
H18A0.29350.95930.28120.075*
H18B0.27110.94970.32830.075*
C190.3061(2)0.7800(7)0.3237(2)0.0584(19)
H19A0.27980.73450.29870.070*
H19B0.33120.75850.31160.070*
C200.31566(18)0.7349(6)0.3845(2)0.0440(16)
H20A0.32170.64030.38700.053*
H20B0.28930.74970.39500.053*
C210.38465(19)0.5631(5)0.4955(2)0.0349(15)
H210.40620.54640.53370.042*
C220.41062(19)0.5435(6)0.4540(2)0.0444(17)
H22A0.39040.55250.41510.053*
H22B0.43360.61110.46080.053*
C230.4321(2)0.4070(6)0.4623(3)0.0569(19)
H23A0.45450.40170.50010.068*
H23B0.44710.39420.43470.068*
C240.3975(2)0.2966(6)0.4555(2)0.0568(19)
H24A0.37770.29350.41610.068*
H24B0.41280.21180.46450.068*
C250.3703(2)0.3189(5)0.4940(2)0.0478(18)
H25A0.38940.30860.53340.057*
H25B0.34690.25230.48590.057*
C260.34870(19)0.4585(6)0.4858(2)0.0411(16)
H26A0.32720.46660.44750.049*
H26B0.33290.47110.51260.049*

Source of material

The ligand 1,2-(PCy2)2-1,2-C2B10H10, was synthesized according to the literature method [1]. By the reaction of ZnCl2 (1 mmol) and 1,2-(PCy2)2-1,2-C2B10H10 in chloromethane (10 mL) under N2 atmosphere. The mixture was refluxed for 4 h, then a colourless solution formed. Single crystals were obtained by slow evaporation of a dichloromethane/n-hexane solution. Yield: (48.9%, m.p. 463–472 K). FTIR (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 complex shows a crystallographically imposed inversion symmetry (A = −x, y, 1/2−z. Comparison of the configuration of the free ligand 1,2-(PCy2)2-1,2-(C2B10H10): the P1—C1—C2—P2 torsion angle is 10.9(4)° in the free ligand [2, 3], whereas coordinated to Zn, this torsion angle is largely altered with the value 0.0(2) in the title complex. The two Cc—Cc—P angles in the free ligand is 113.48(5)° for C(2)—C(1)—P(1) and C(1)—C(2)—P(2), while these two angles in the title complex tend to become equivalent to each other (115.38 and 115.56°) [4, 5]. These data show that the symmetry of the moiety 1,2-(PCy2)2-1,2-(C2B10H10) in the three complexes has a tendency to approach C2v symmetry. The average bond lengths of C—P in the complexes (1.872(3) Å) are similar with the corresponding distance 1.894(3) Å in 1,2-(PCy2)2-1,2-(C2B10H10), indicating that the coordinating to the metal atom has no 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. Su, F. F.; Dou, J. M.; Li, D. C.; Wang, D. Q.: 1,2-Bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane. Acta Crystallogr. E63 (2007) o3335.10.1107/S1600536807030553Search in Google Scholar

2. Dou, D. M.; Zhang, D. P.; Li, D. C.; Wang, D. Q.: Two type skeleton heterobimetallic trinuclear Cu-Mo-S clusters containing closo carborane diphosphine ligand 1,2-bis(diphenylphosphino)-1,2-dicarba-closo-dodecaborane. Inorg. Chem. Comm. 9 (2006) 1109–1102.10.1016/j.inoche.2006.07.006Search in Google Scholar

3. Dou, D. M.; Zhang, D. P.; Zhu, Y. H.; Li, D. C.; Wang, D. Q.: Synthesis and characterization of two types of skeleton heterobimetallictrinuclear Mo(W)-C-S clusters containing 1,2-bis(diphenylphosphino)-1,2-dicarba-closo-dodecaborane. Polyhedron 26 (2007) 4216–4222.10.1016/j.poly.2007.05.030Search in Google Scholar

4. Dou, D. M.; Su, F. F.; Nie, Y.; Li, D. C.; Wang, D. Q.: Self-assembled 2D supramolecular networks of copper(I) carborane complexes through C—H⋯H—B dihydrogen bonding interactions. Dalton. Trans. 31 (2008) 4152–4156.10.1039/b801339jSearch in Google Scholar PubMed

5. Dou, D. M.; Zhang, D. P.; Gong, S. W.; Li, D. C.; Wang, D. Q.: Synthesis and characterization of three dinuclear copper(I) complexes of 1,2-bis(diphenylphosphino)-1,2-dicarba-closo-dodecaborane. Appl. Organometal. Chem. 20 (2006) 632–637.10.1002/aoc.1119Search in Google Scholar

6. Yang, L. G.; Zhu, C. C.; Zhang, D. D.; Li, D. C.; Wang, D. Q.; Dou, D. M.: S1D 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.2011.02.052Search in Google Scholar

7. Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Search in Google Scholar PubMed

8. Bruker. APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, WI, USA, 2009.Search in Google Scholar

Received: 2016-5-18
Accepted: 2016-9-15
Published Online: 2016-10-8
Published in Print: 2017-1-1

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

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

Articles in the same Issue

  1. Cover and Frontmatter
  2. Editorial
  3. Twenty years of crystal structure publication and the road ahead
  4. Crystal Structures
  5. Crystal structure of poly-[triaqua-(μ4-5′-carboxy-[1,1′-biphenyl]-2,3,3′-tricarboxylate-κ6O1,O2:O3,O4:O5:O6)praseodymium(III), C16H13O11Pr
  6. Crystal structure of (R)-1-(2,3-dihydro-1H-pyrrolizin-5-yl)-2,3-dihydroxypropan-1-one, C10H13NO3
  7. Crystal structure of (E)-4-nitro-2-((2-phenoxyphenylimino)methyl)phenol, C19H14N2O4
  8. Crystal structure of 3,3′-di(furan-2-yl)-5,5′-bi-1,2,4-triazine
  9. Crystal structure of 11-(p-coumaroyloxy)-tremetone, C22H20O5
  10. The crystal structure of 1,3-bis(2,6-diiso-propylphenyl)imidazol-2-ylidene)-dibromido-(1-methyl-1H-imidazole-κ1N)palladium(II) – ethyl acetate – water (1/1/1), C31H42Br2N4Pd
  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
  13. Crystal structure of poly-[aqua-(μ7-benzene-1,3,5-tricarboxylato)-(μ3-1,2,4-triazol-1-ido)dicobalt(II)], C11H7Co2N3O7
  14. Crystal constructure of 16(S)-methyl-6α-carboxy-1, 15-dioxo-6, 7-seco-ent-kaur-2-en-7, 20-olide, C20H24O6
  15. Crystal structure of 1-(benzo[d]thiazol-2-yl)-3-phenylthiourea, C14H11N3S2
  16. Crystal structure of 3-(2-bromophenyl)-1,1-dimethylthiourea, C9H11BrN2S
  17. Crystal structure of 1-(adamantan-1-yl)-3-(3-chlorophenyl)thiourea, C17H21ClN2S
  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
  20. Crystal structure of methyl 2b-ethyl-1a,2a,2b,2b1,3,5,10,11-octahydro-1H-oxireno[2′,3′:6,7]indolizino[8,1-cd]carbazole-4-carboxylate, C21H24N2O3
  21. Crystal structure of 2-amino-5-oxo-4-(3,4,5-trimethoxy-phenyl)-4,5,6,7-tetrahydro-cyclopenta[b]pyran-3-carbonitrile, C18H18N2O5
  22. Crystal structure of 1,2,3-trimethyl-2,3-dihydro-1H-perimidine, C14H16N2
  23. Crystal structure of bis(2,6-dihydroxymethyl)pyridine-κ3N,O,O′)-bis(μ2-6-chloropyridin-2-olato-κ3N,O:O)-bis(6-chloropyridin-2-olato-κO)-bis(nitrato-κ2O,O′)digadolinium(III), C34H30Cl4Gd2N8O14
  24. Crystal structure of 8-isopropyl-8-aza-bicyclo[3.2.1]octan-3-yl 3-hydroxy-2-phenylpropanoate, C19H27NO3
  25. Crystal structure of 1-methyl-3-[((naphthalen-2-ylsulfonyl)oxy)imino]indolin-2-one, C19H14N2O4S
  26. Crystal structure (7,8-bis(diisopropylphosphino)-7,8-dicarba-nido-undecaborane-κ2P,P′)-(benzoato-κ2O,O′)nickel(II), C21H42B9NiO2P2
  27. Crystal structure of methyl-2-methyl-4-(2-oxo-2-phenylethyl)-5-phenyl-1H-pyrrole-3-carboxylate, C21H19NO3
  28. Crystal structure of 2-[(2-oxo-thiazolidine-3-carbonyl)sulfamoyl]-methy-benzoic acid methyl ester, C13H14N2O6S2
  29. Crystal structure of N′-(2-phenylacetyl)thiophene-2-carbohydrazide monohydrate, C13H14N2O3S
  30. Crystal structure of 1,1′-(hexane-1,6-diyl)bis(3-methyl-1H-imidazol-3-ium) bis(hexafluoro phosphate), C14H24F12N4P2
  31. Crystal structure of di-μ-chlorido-bis[1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]zinc(II), C52H108B20Cl2P4Zn2
  32. Crystal structure of dibromido-bis[μ-1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κN]mercury(II), C30H26Br2HgN10
  33. 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
  34. Crystal structure of dinuclear dichloridobis(dimethylformamide-kO)bis[μ2-3-(2-oxyphenyl)-5-(pyrazin-2-yl)-1,2,4-triazol-1ido-κ4-O,N:N′,N′′(2)]diiron(III) dimethylformamide (1/1), C36H42Cl2Fe2N14O6
  35. Crystal structure of diaqua-dinitrato-κO-bis(4-(1H-pyrazol-3-yl)pyridine-κN)manganese(II), C16H18MnN8O8
  36. Crystal structure of (Z)-6-methoxy-2-(2,2,2-trifluoro-1-hydroxyethylidene)-2,3-dihydro-1H-inden-1-one, C12H6F6O3
  37. Crystal Structure of 4-(2-chloroacetamido)pyridinium chloride monohydrate, C7H10Cl2N2O2
  38. Crystal structure of 2-amino-4-(4-chloro-phenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13ClN2O2
  39. Crystal structure of (E)-1-(2-(thiophen-2-ylmethylene)hydrazinyl)phthalazine hydrochloride–ethanol (1/1), C15H17ClN4OS
  40. Crystal structure of N,N-diethyl-5-bromo-3,4-dihydro-2,4-dioxopyrimidine-1(2H)-carboxamide, C9H12BrN3O3
  41. Crystal structure of 3-(2-(4-chlorophenyl)-3-hydroxy-3,3-diphenylpropyl)-1,1-dimethylurea, C24H25ClN2O2
  42. Crystal structure of 3-(4-chlorophenyl)-1,1-dimethylthiourea, C9H11ClN2S
  43. Crystal structure of 2-amino-4-(4-bromo-phenyl)-7-methyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-3-carbonitrile, C16H11BrN2O3
  44. Crystal structure of 4-(3,4-dimethyl-phenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydro-quinoline-3-carboxylic acid ethyl ester, C21H25NO3
  45. Crystal structure of (E)-2-({4-hydroxy-5-methoxy-3-[(4-methyl-1-piperazinyl)methyl]phenyl} methylidene)-1-indanone, C23H26N2O3
  46. Crystal structure of tripropylammonium 2′-carboxy-[1,1′-biphenyl]-2-carboxylate – [1,1′-biphenyl]-2,2′-dicarboxylic acid (2/1), C60H72N2O12
  47. Crystal structure of catena-poly-{aqua-[μ2-1,2-bis((1H-imidazol-1-yl)methyl)benzene-κ2N:N′]-[μ2-4,4′-(dimethylsilanediyl)dibenzato-κ3O,O′:O′]nickel(II)}, C30H30N4NiO5Si
  48. The crystal structure of 1-(4-bromophenyl)-2-(4-(4-fluorophenyl)piperazin-1-yl)ethanol, C18H20BrFN2O1
  49. Crystal structure of trimethylammonium 4-((4-carboxyphenyl)sulfonyl)benzoate, C17H19NO6S
  50. Crystal structure of syn-2,4-di-o-tolylpentane-2,4-diol, C19H24O2
  51. Crystal structure of 2-[3,5-bis(trifluoromethyl)benzylsulfanyl]-5-(5-bromothiophen-2-yl)-1,3,4-oxadiazole, C15H7BrF6N2OS2
  52. Crystal structure of (E)-3-((naphthalen-1-ylimino)methyl)-4-nitrophenol, C17H12N2O3
  53. Crystal structure of 2-dichloromethyl-2-p-nitrophenyl-1,3-dioxolane, C10H9Cl2NO4
  54. Crystal structure of (1,4,8,11-tetraazacyclotetradecane)palladium(II) tetracyanopalladate(II), C14H24N8Pd2
  55. Crystal structure of 2-(4-oxo-2-thioxothiazolidin-3-yl)acetic acid monohydrate, C5H7NO4S2
  56. Crystal structure of a P4-bridged (η5-pentamethyl-cyclopentadienyl)(η5-adamantylcyclopentadienyl) titanium(III)complex, C50H66P4Ti2
  57. Crystal structure of cis-bis(2,2′-bipyrimidine-κ2N,N′)bis(thiocyanato-κN)nickel(II), C18H12N10NiS2
  58. Crystal structure of cis-bis(2,2′-bipyridine-κ2N,N′)dibromidomanganese(II), C20H16Br2MnN4
  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
Downloaded on 5.10.2025 from https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2016-0155/html
Scroll to top button