Home Physical Sciences Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2
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Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2

  • Yang Liguo EMAIL logo , Liu Qingyun , Wang Xin , Gao Qianqian and Dai Yuqiang
Published/Copyright: January 15, 2018
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 233 Issue 2

Abstract

C14H38B10NiBr2P2, monoclinic, P21/c (no. 14), a = 10.1920(14) Å, b = 19.055(2) Å, c = 13.5243(17) Å, β = 103.394(2)°, V = 2555.1(6) Å3, Z = 4, Rgt(F) = 0.0461, wRref(F2) = 0.0869, T = 298 K.

CCDC no.:: 1810972

The crystal structure is shown in the figure. Hydrogen atoms are omitted for clarity. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Red blocks
Size:0.48 × 0.43 × 0.40 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:4.01 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
2θmax, completeness:27.5°, >98%
N(hkl)measured, N(hkl)unique, Rint:14632, 5770, 0.074
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3486
N(param)refined:271
Programs:Bruker programs [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.55409(5)0.02644(2)0.25172(4)0.02018(15)
Br10.58007(5)−0.08574(2)0.19032(4)0.04528(17)
Br20.33882(5)0.00036(2)0.27564(4)0.04179(16)
P10.76257(11)0.04350(5)0.24828(8)0.0192(3)
P20.51873(10)0.13386(5)0.28887(8)0.0185(2)
B30.7245(5)0.2011(2)0.1929(4)0.0195(11)
H30.65870.18790.11860.023*
B40.6867(5)0.2710(2)0.2689(4)0.0268(12)
H40.59710.30440.24410.032*
B50.7454(5)0.2464(2)0.3976(4)0.0285(12)
H50.69450.26390.45670.034*
B60.8173(5)0.1611(2)0.3997(4)0.0239(11)
H60.81130.12260.45900.029*
B70.9009(5)0.1924(2)0.2158(4)0.0249(12)
H70.95040.17480.15600.030*
B80.8277(5)0.2765(2)0.2133(4)0.0284(12)
H80.83000.31390.15190.034*
B90.8425(5)0.3043(2)0.3400(4)0.0330(13)
H90.85540.36000.36130.040*
B100.9233(5)0.2357(2)0.4232(4)0.0329(13)
H100.98780.24600.49900.040*
B110.9602(5)0.1677(2)0.3441(4)0.0272(12)
H111.04940.13390.36790.033*
B120.9753(5)0.2557(2)0.3089(4)0.0293(12)
H121.07400.27970.31070.035*
C10.8087(4)0.13843(18)0.2755(3)0.0163(9)
C20.6798(4)0.18602(18)0.3049(3)0.0180(9)
C30.8717(5)−0.0059(2)0.3569(4)0.0380(12)
H3A0.94330.02620.39080.046*
C40.7911(5)−0.0266(2)0.4355(4)0.0538(15)
H4A0.7275−0.06270.40770.081*
H4B0.74360.01370.45200.081*
H4C0.8517−0.04370.49590.081*
C50.9402(5)−0.0708(2)0.3257(4)0.0676(18)
H5A0.9897−0.09450.38540.101*
H5B1.0010−0.05690.28460.101*
H5C0.8731−0.10190.28740.101*
C60.8207(5)0.0195(2)0.1331(3)0.0344(11)
H6A0.8083−0.03150.12720.041*
C70.9717(5)0.0313(3)0.1360(4)0.0557(15)
H7A1.0074−0.00950.10990.084*
H7B1.02020.03940.20480.084*
H7C0.98120.07130.09510.084*
C80.7313(5)0.0488(2)0.0365(3)0.0471(13)
H8A0.74230.09880.03510.071*
H8B0.63880.03780.03460.071*
H8C0.75630.0283−0.02140.071*
C90.4499(5)0.1511(2)0.4016(3)0.0335(11)
H9A0.36090.12870.38560.040*
C100.5276(5)0.1125(2)0.4966(3)0.0485(14)
H10A0.61820.13010.51550.073*
H10B0.52960.06320.48250.073*
H10C0.48380.11990.55140.073*
C110.4217(5)0.2264(2)0.4241(4)0.0586(15)
H11A0.33440.22960.43910.088*
H11B0.42380.25500.36610.088*
H11C0.48910.24250.48150.088*
C120.3994(4)0.1740(2)0.1773(3)0.0325(11)
H12A0.43910.21870.16340.039*
C130.3853(5)0.1290(2)0.0824(3)0.0442(13)
H13A0.34170.08560.09150.066*
H13B0.47300.11950.07100.066*
H13C0.33220.15360.02500.066*
C140.2607(5)0.1900(3)0.1925(5)0.0784(19)
H14A0.20450.20660.12970.118*
H14B0.26700.22550.24370.118*
H14C0.22220.14820.21350.118*

Source of material

The ligand 1,2-(PiPr2)2-1,2-C2B10H10, was synthesized according to the literature method [4]. To a suspension of 1,2-(PiPr2)2-1,2-C2B10H10 (1 mmol) in chloromethane (10 mL) was added NiCl2 (1 mmol). The mixture was refluxed for 4 h with protection of dry N2, then a colourless solution formed. Single crystals suitable were obtained by slow evaporation of a dichloromethane-n-hexane solution (35.6%, m.p. 323–325 K). FTIR (KBr) v (cm−1): 2985, 2964, 2928, 2870 (C—H); 2612, 2600, 2583, 2554 (B—H); 1072 (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

Organic or organo-element derivatives of dicarba-closo-dodecaborane have been given much attention due to their interesting chemical and physical properties. These compounds can be used as catalysts, precursors for ceramic materials and in medical field [5, 6] . The 1,2-dicarba-closo-dodecaborane is an icosahedral cluster with the two carbon atoms in adjacent positions, whose tertiary phosphine derivatives were first reported in 1963 [7]. Since then, these types of compounds have been employed as ligands in transition metal chemistry and starting materials for the preparation of other 1,2–dicarba-closo-dodecaborane-containing organophosphorus compounds [8], [9], [10]. A great deal of complexes of 1,2-(PiPr2)2-1,2-C2B10H10 with transition metals such as cobalt, gold, platium, palladium, chromium, molybdenum, tungsten, iron, manganese, copper and silver have been reported. Although metal complexes of the above ligand have been synthesized, there has been no reported example of a nickel(II) complex of 1,2-(PiPr2)2-1,2-C2B10H10 characterized by X-ray diffraction. With this and the point that nickel complexes can exhibit both biological and catalytic activity in mind, our interests concentrated on the synthesis of Ni(II) complex of 1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane.

The figure depicts a perspective of the structure unit of the complex showing the atom numbering. The environment of the Ni atom is four coordinated, in which two positions are occupied by the chelating closo diphosphine ligand 1,2-(PiPr2)2-1,2-C2B10H10, and the other two come from the bromido ligands at cis position. The mean deviation 0.493 Å from the plane P1P2NiO1O2 and the dihedral angle 9.98° between the two planes P1NiP2 and Br1NiBr2 show that the coordination sphere of the Ni atom is slightly distorted square-planar. The structure of the compound is similar with the reported structure of [NiBr2{1,2-(PPh2)2-1,2-C2B10H10}]⋅CH2Cl2 [11]. The distances of the Ni—Br (2.337(7) Å) and P—Ni (2.159(11) Å) are very close to the corresponding distances 2.328(2) and 2.148(5) Å in the complex dibromo[1,2-bis(diphenylphosphino)ethane]nickel(II). The angles of Br(1)—Ni(1)—Br(2) (92.42(2)°) and P(1)—Ni(1)—P(2) (94.60(4)°) are also comparable to values in the same complex. The P1—C1—C2—P2 torsion angle is 6.3(3)°.

Acknowledgements

This work was supported by Henan science and technology project (nos. 172102210161, 172102210160) and the Research Fund of Anyang Institute of Technology (nos. YJJ2016014).

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Received: 2017-8-23
Accepted: 2017-12-13
Published Online: 2018-1-15
Published in Print: 2018-3-28

©2018 Yang Liguo et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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https://doi.org/10.1515/ncrs-2017-0200
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Articles in the same Issue

  1. Cover and Frontmatter
  2. Crystal structure and optical properties of diaqua-tris(nitrato-κ2O,O′)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl 3-oxide-κN)praseodymium(III), C24H36N9O15Pr
  3. Crystal structure of dimethanol-bis(μ2-methanol-κ2O:O)-bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}dimanganese(II), C38H38Mn2N2O14
  4. Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12
  5. Crystal structure of catena-poly[triaqua-(isophthalato-κO)-(μ2-1,6-di(1H-imidazol-1-yl)hexane-κ2N:N′)]nickel(II), C20H28N4NiO7
  6. Crystal structure of cyclo[hexaqua-bis[1-[(2-ethyl-1H-imidazol-1-yl) methyl]-1H-benzotriazole-κ2N:N′]-bis(sulfato-κ1O)dicadmium(II)] monohydrate, C24H42Cd2N10O16S2
  7. Crystal Structure of bis(2-fluorbenzoato-κO)-bis(1,10-phenanthroline-κ2N,N′)manganese(II) dihydrate, C38H28F2MnN4O6
  8. Crystal structure of tetrapropylammonium 5-hydroxyisophthalate tetrahydrate, C20H41NO9
  9. Crystal structural of 2-amino-4-(3-bromophenyl)-3-cyano-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydrobenzo[b]pyran, C18H17BrN2O2
  10. Crystal structural of 2-amino-4-(4-methoxyphenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C17H16N2O3
  11. Crystal structure of catena-poly[aqua(μ2-1,3-bis(1H-benzo[d]imidazol-1-yl)propane-κ2N:N′)-(μ2-5-(tert-butyl)isophthalate-κ3O,O′:O′′)nickel(II)], C29H30N4NiO5
  12. Crystal structure of catena-poly[(μ2-dicyanamido-κ2N:N′)-(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O′)copper(II)], C9H8CuN4O
  13. Crystal structure of bis(5,5′-((butane-1,4-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido-k4N,N′,N′′,N′′′)copper(II), C24H32CuN4O4
  14. The crystal structure of the formamide solvate of (17b)-estra-1,3,5(10)-triene-3,17diol, C19H27NO3
  15. Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8
  16. Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2
  17. The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7
  18. The crystal structure of N′-(2-nitrobenzylidene)-2-phenylacetohydrazide, C15H13N3O3
  19. Crystal structure of dichlorido bis[1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κ1N]cadmium(II), C30H26CdCl2N10
  20. Crystal structure of aqua-bis(3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole-κ2N,N′)copper(II) sulfate tetrahydrate, C24H28CuN10O9S
  21. Crystal structure of dibromido-carbonyl-(η6-p-cymene)osmium(II), C11H14Br2OOs
  22. Crystal structure of catena-poly[chlorido-(μ2-chlorido)-bis(imidazole-κN)copper(II)] C6H8Cl2CuN4
  23. Crystal structure of [(1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]dibromidonickel(II)), C26H54B10NiBr2P2
  24. Crystal structure of dichlorido[1,1′-bis(diphenylphosphanyl)ferrocene-κ2P,P′]zinc(II), C34H28FeCl2P2Zn
  25. Crystal structure of tris(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O)-trithiocyanato-κN-dicobalt(III), C24H24Co2N6O3S3
  26. The crystal structure of diaqua-2,2′-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))diphenolato-κ4N,N′,O,O′)manganese(III) perchlorate, C20H24MnClN2O4
  27. Crystal structure of bis(μ3-chlorido)-bis(μ2-chlorido)-tetrakis(μ2-2,6-bis (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene solvate, C75.5H70Cl2CoLi2O2
  28. The crystal structure of hexaaqua-bis(μ2-3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κ2O:O′)-tetrakis(3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κO)dierbium(III) octahydrate, C60H76N18O32Er2
  29. Crystal structure of dimethylammonium bis(naphthalene-2,3-diolato)borate, C22H20BNO4
  30. Crystal structure of 2-amino-4-(4-nitro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H17N3O4
  31. The crystal structure of (E)-4-chloro-2-(((5-methylpyridin-2-yl)imino)methyl)phenol, C13H11ClN2O
  32. Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3
  33. The crystal structure of N-((3,5-di-tert-butyl-4-hydroxyphenyl)(phenyl)methyl)-4-methylbenzenesulfonamide, C28H35N3S
  34. Crystal structure of 2-(4-chlorophenyl)-2,3-dihydro-1H-perimidine, C17H13Cl1N2
  35. The Crystal structure of 2-iodo-1-(p-tolyl)propan-1-one, C10H11IO
  36. Crystal structure of ethyl 1-(4-bromobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17BrN2O2
  37. Crystal structure of ethyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17FN2O2
  38. Crystal structure of catena-poly[diaqua-(μ2-2,5-dihydroxyterephthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C8H8O8Cd
  39. Crystal structure of tetraaqua-bis[6-(1H-imidazol-1-yl-κN)nicotinato]zinc(II), C18H20N6O8Zn
  40. Crystal structure of dichlorido-bis(N-phenyl-2-(quinolin-8-yloxy)acetamide-κ2N,O) – acetone (2/1), C35.5H31N4O4.5Cl2Cu
  41. Crystal Structure of ethyl (E)-3,4-dimethyl-5-((2-(4-methylbenzoyl)hydrazono)methyl)-1H-pyrrole-2-carboxylate — water — ethanol (1/1/1), C20H29N3O5
  42. Crystal structure of 5-((4-(1H-benzo[d]imidazol-2-yl)-2-methoxyphenoxy)methyl)-2-chlorothiazole - trichloromethane - methanol (1/1/1), C20H19Cl4N3O3S
  43. The crystal structure of a matrine derivative: 41S,7aS,12S,13aR,13bR)-12-(4-methylpiperazin-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one, C20H34N4O
  44. Crystal structure of cesium beryllophosphate, Be3Cs2P4O14
  45. Crystal Structure of 3-((3-hydroxybenzyl)ammonio)-3-phenylpropanoate, C16H17NO3
  46. Crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino[3,2-a]isoquinolin-7-ium chloride — 4-hydroxy-3-methoxybenzoic acid — water (2/1/5), C48H54N2Cl2O17
  47. The crystal structure of (1R, 2R)-N1,N2-diferrocenyl-1,2-cyclohexanedicarboxamide, C28H30Fe2N2O2
  48. Crystal structure of N-(2-methylphenyl)ethoxycarbothioamide, C10H13NOS
  49. Crystal Structure of ethyl (E)-2,4-dimethyl-5-((2-tosylhydrazono)methyl)-1H-pyrrole-3-carboxylate monohydrate, C17H23N3O5
  50. Crystal structure of Diiodo-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3N,N′,O)cadium(II) – dimethylformamide (1/1), C19H19N5O2CdI2
  51. Crystal structure of dinitrato-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3-N,N′,O)copper(II), C16H12N6O7Cu
  52. Crystal structure of benzoato-κO-bis(1,3,5-triaza-7-phosphaadamantane-κP)silver(I) monohydrate C19H31AgN6O3P2
  53. Crystal structure of (E)-2-(anthracen-9-ylmethylene)hydrazine-1-carbothioamide, C16H13N3S
  54. The crystal structure of 8-chloro-7-ethyl-1,3-dimethyl-1H-purine-2,6(3H,7H)-dione, C9H11ClN4O2
  55. Crystal structure of {5,5′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′}zinc(II), C23H30N4O4Cu
  56. Crystal structure of bis(4-dimethylamino-pyridin-1-ium)tetrafluorosuccinate, C18H22F4N4O4
  57. Crystal structure of dimethyl 3,9-dibenzyl-6,12-dicyclohexyl-3,9-diazahexacyclo [6.4.0.02,7.04,11.05,10]-dodecane-1,11-dicarboxylate, C40H50N2O4
  58. Crystal structure of diethyl 3,9-diphenyl-6,12-bis(3-methoxyphenyl)-3,9-diazahexacyclo[6.4.0.02,7.04,11.05,10]dodecane-1,11-dicarboxylate, C42H42N2O6
  59. Crystal structure of bis(acetato-κO)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)nickel(II), C18H22N4NiO6
  60. Crystal structure of (N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3N,O,O′)-diphenyltin(IV), C28H23FN2O3Sn
  61. Crystal structure of {N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3O,N,O′}dimethyltin(IV), C18H19FN2O3Sn
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