metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

[1,2-Bis(diiso­propyl­phosphino)-1,2-dicarba-closo-dodeca­borane-κ2P,P′]di­chloridomercury(II)

aSchool of Chemistry and Chemical Engineering, Liaocheng University, Shandong 252059, People's Republic of China, and bDepartment of Chemistry, Taishan University, Shandong 271021, People's Republic of China
*Correspondence e-mail: jmdou@lcu.edu.cn

(Received 8 November 2007; accepted 2 December 2007; online 6 December 2007)

In the title complex, [HgCl2(C14H38B10P2)], the HgII atom is in a distorted HgCl2P2 tetra­hedral coordination environment. The chelation of the Hg atom by two P atoms and two C atoms from the carborane skeleton results in a nearly planar five-membered ring.

Related literature

For related structures see: Mariyatra et al. (2005[Mariyatra, M. B., Panchanatheswaran, K., Low, J. N. & Glidewell, C. (2005). Acta Cryst. C61, m211-m214.]); Liu et al. (2004[Liu, L., Zhang, Q.-F. & Leung, W.-H. (2004). Acta Cryst. E60, m394-m395.]); Paavola, Kivekäs et al. (2002[Paavola, S., Kivekäs, R., Teixidor, F. & Viñas, C. (2002). J. Organomet. Chem. 606, 183-187.]), Paavola, Teixidor et al. (2002a[Paavola, S., Teixidor, F., Viñas, C. & Kivekäs, R. (2002a). Acta Cryst. C58, m237-m239.],b[Paavola, S., Teixidor, F., Viñas, C. & Kivekäs, R. (2002b). J. Organomet. Chem. 645, 39-46.]). For the synthesis and structure of the ligand, see: Kivekäs et al. (1995[Kivekäs, R., Sillanpää, R., Teixidor, F., Viñas, C., Nuñez, R. & Abad, M. (1995). Acta Cryst. C51, 1864-1868.]).

[Scheme 1]

Experimental

Crystal data
  • [HgCl2(C14H38B10P2)]

  • Mr = 647.97

  • Tetragonal, I 41 /a

  • a = 21.110 (3) Å

  • c = 24.585 (6) Å

  • V = 10956 (3) Å3

  • Z = 16

  • Mo Kα radiation

  • μ = 5.93 mm−1

  • T = 298 (2) K

  • 0.53 × 0.49 × 0.47 mm

Data collection
  • Bruker SMART CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SMART, SAINT, SADABS and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.145, Tmax = 0.167 (expected range = 0.053–0.062)

  • 22446 measured reflections

  • 4815 independent reflections

  • 3491 reflections with I > 2σ(I)

  • Rint = 0.081

Refinement
  • R[F2 > 2σ(F2)] = 0.038

  • wR(F2) = 0.077

  • S = 1.00

  • 4815 reflections

  • 270 parameters

  • 290 restraints

  • H-atom parameters constrained

  • Δρmax = 1.37 e Å−3

  • Δρmin = −1.23 e Å−3

Table 1
Selected bond lengths (Å)

Hg1—Cl1 2.4482 (17)
Hg1—Cl2 2.4542 (17)
Hg1—P1 2.5200 (10)
Hg1—P2 2.5242 (16)

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART, SAINT, SADABS and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART, SAINT, SADABS and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.]); molecular graphics: SHELXTL (Bruker, 2001[Bruker (2001). SMART, SAINT, SADABS and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The synthesis and structure of 1,2-(PiPr2)2-1,2-C2B10H10 was reported by Kivekäs et al. (1995). Since then, only a few complexes containing this ligand have been described, containing Pt(II) and Pd(II) (Paavola et al. (2002,2002a,b). We now report the structure of this ligand combined with HgII and chloride ions as the title compound, (I).

As shown in Fig. 1, The HgII atom in (I) is in a distorted HgCl2P2 tetrahedral coordination environment (Table 1). The Hg—P distances in (I) are longer than those of 2.3991Å in [Ph3PHgCl(µ-Cl)2ClHgPPh3] (Mariyatra et al., 2005). The Hg—Cl distances in (I) are also longer than the corresponding distance of 2.4015 (8)Å for in the Mariyatra et al. (2005) phase. The Cl—Hg—Cl angle in (I) of 104.81 (6) Å, is slight bigger than that of 101.19 (4)° in [(HgCl2)2((C6H11)3P)2] (Liu et al., 2004).

The chelation of the mercury(II) atom in (I) with phosphorus atoms and carbon atoms form a nearly planar five-membered ring with a maximum deviation of 0.033Å for C2. The torsion angle P1—C1—C2—P2 in (I) is 5.8 (6)°, which is smaller than that of 12.1 (2)° in the free ligand (Kivekas et al., 1995).

Related literature top

For related structures see: Mariyatra et al. (2005); Liu et al. (2004); Paavola et al. (2002,2002a,b). For the synthesis and structure of the ligand, see: Kivekäs et al., (1995).

Experimental top

The title compound was synthesizd by the reaction of 1 mmol HgCl2 and 1 mmol 1,2-(PiPr2)2-1,2-C2B10H10 in 10 ml dichloromethane under the protection of N2. The mixture was refluxed for 4 h, then a colourless solution formed, and colourless blocks of (I) were obtained from a dichloromethane/n-hexane solution (61.7%, m.p. 405–406 K). FTIR (KBr) \v (cm-l): 2990, 2968, 2932, 2875 (C—H); 2615, 2603, 2586, 2558 (B—H); 1072 (C—P).

Refinement top

All H atoms were placed geometrically (B—H = 1.10 Å, C—H = 0.96–0.98 Å) and refined as riding with Uiso(H) = 1.2Ueq(B) or 1.5Ueq(C).

Structure description top

The synthesis and structure of 1,2-(PiPr2)2-1,2-C2B10H10 was reported by Kivekäs et al. (1995). Since then, only a few complexes containing this ligand have been described, containing Pt(II) and Pd(II) (Paavola et al. (2002,2002a,b). We now report the structure of this ligand combined with HgII and chloride ions as the title compound, (I).

As shown in Fig. 1, The HgII atom in (I) is in a distorted HgCl2P2 tetrahedral coordination environment (Table 1). The Hg—P distances in (I) are longer than those of 2.3991Å in [Ph3PHgCl(µ-Cl)2ClHgPPh3] (Mariyatra et al., 2005). The Hg—Cl distances in (I) are also longer than the corresponding distance of 2.4015 (8)Å for in the Mariyatra et al. (2005) phase. The Cl—Hg—Cl angle in (I) of 104.81 (6) Å, is slight bigger than that of 101.19 (4)° in [(HgCl2)2((C6H11)3P)2] (Liu et al., 2004).

The chelation of the mercury(II) atom in (I) with phosphorus atoms and carbon atoms form a nearly planar five-membered ring with a maximum deviation of 0.033Å for C2. The torsion angle P1—C1—C2—P2 in (I) is 5.8 (6)°, which is smaller than that of 12.1 (2)° in the free ligand (Kivekas et al., 1995).

For related structures see: Mariyatra et al. (2005); Liu et al. (2004); Paavola et al. (2002,2002a,b). For the synthesis and structure of the ligand, see: Kivekäs et al., (1995).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with 30% probability displacement ellipsoids (H atoms omitted for clarity).
[1,2-Bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-\k2P,P']dichloridomercury(II) top
Crystal data top
[HgCl2(C14H38B10P2)]Dx = 1.571 Mg m3
Mr = 647.97Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/aCell parameters from 5681 reflections
Hall symbol: -I 4adθ = 2.3–25.3°
a = 21.110 (3) ŵ = 5.93 mm1
c = 24.585 (6) ÅT = 298 K
V = 10956 (3) Å3Block, colorless
Z = 160.53 × 0.49 × 0.47 mm
F(000) = 5056
Data collection top
Bruker SMART CCD
diffractometer
4815 independent reflections
Radiation source: fine-focus sealed tube3491 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 2523
Tmin = 0.145, Tmax = 0.167k = 1725
22446 measured reflectionsl = 2927
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.031P)2]
where P = (Fo2 + 2Fc2)/3
4815 reflections(Δ/σ)max = 0.002
270 parametersΔρmax = 1.37 e Å3
290 restraintsΔρmin = 1.23 e Å3
Crystal data top
[HgCl2(C14H38B10P2)]Z = 16
Mr = 647.97Mo Kα radiation
Tetragonal, I41/aµ = 5.93 mm1
a = 21.110 (3) ÅT = 298 K
c = 24.585 (6) Å0.53 × 0.49 × 0.47 mm
V = 10956 (3) Å3
Data collection top
Bruker SMART CCD
diffractometer
4815 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
3491 reflections with I > 2σ(I)
Tmin = 0.145, Tmax = 0.167Rint = 0.081
22446 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.038290 restraints
wR(F2) = 0.077H-atom parameters constrained
S = 1.00Δρmax = 1.37 e Å3
4815 reflectionsΔρmin = 1.23 e Å3
270 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
P10.88138 (6)0.58515 (7)0.21383 (4)0.0258 (3)
Hg10.906748 (11)0.554286 (12)0.117243 (8)0.03997 (11)
P21.02256 (7)0.53987 (8)0.13960 (5)0.0344 (4)
Cl10.87446 (8)0.63978 (9)0.05593 (7)0.0653 (5)
Cl20.85996 (8)0.45816 (8)0.07802 (7)0.0598 (5)
B31.0185 (3)0.6349 (3)0.2328 (2)0.0303 (16)
H31.01150.67280.20280.036*
B40.9818 (3)0.6364 (4)0.2987 (2)0.0391 (19)
H40.95190.67610.31220.047*
B50.9646 (3)0.5571 (3)0.3155 (2)0.0401 (19)
H50.92320.54470.34060.048*
B60.9896 (3)0.5093 (3)0.2589 (2)0.0319 (16)
H60.96380.46670.24570.038*
B71.0743 (3)0.5145 (4)0.2565 (3)0.0413 (19)
H71.10440.47500.24300.050*
B81.0922 (3)0.5945 (3)0.2405 (3)0.0379 (18)
H81.13410.60740.21640.046*
B91.0649 (3)0.6428 (4)0.2937 (3)0.046 (2)
H91.08940.68720.30410.056*
B101.0309 (3)0.5941 (4)0.3432 (3)0.050 (2)
H101.03340.60650.38660.060*
B111.0350 (3)0.5142 (4)0.3206 (3)0.047 (2)
H111.03930.47380.34860.057*
B121.0978 (3)0.5680 (4)0.3086 (3)0.050 (2)
H121.14360.56290.32940.060*
C10.9610 (2)0.5824 (3)0.24933 (18)0.0280 (12)
C21.0262 (2)0.5577 (3)0.21524 (19)0.0301 (12)
C30.8303 (3)0.5299 (3)0.2536 (2)0.0326 (13)
H3A0.85880.49750.26830.039*
C40.7960 (3)0.5584 (3)0.3027 (2)0.0508 (17)
H4A0.76460.58800.29030.076*
H4B0.82600.57990.32550.076*
H4C0.77580.52520.32300.076*
C50.7850 (3)0.4955 (3)0.2166 (2)0.0515 (18)
H5A0.76460.46200.23640.077*
H5B0.80790.47780.18640.077*
H5C0.75370.52460.20340.077*
C60.8465 (3)0.6652 (3)0.2224 (2)0.0380 (14)
H6A0.84170.67410.26130.046*
C70.8844 (3)0.7185 (3)0.1962 (3)0.0577 (18)
H7A0.89590.70660.15980.087*
H7B0.92200.72630.21710.087*
H7C0.85900.75630.19510.087*
C80.7808 (3)0.6633 (3)0.1959 (3)0.0584 (18)
H8A0.76060.70370.20010.088*
H8B0.75560.63120.21310.088*
H8C0.78510.65370.15790.088*
C91.0537 (3)0.4602 (3)0.1261 (3)0.0523 (16)
H9A1.09810.45800.13750.063*
C101.0167 (4)0.4082 (3)0.1536 (3)0.078 (2)
H10A0.97220.41730.15110.116*
H10B1.02880.40570.19120.116*
H10C1.02550.36860.13600.116*
C111.0495 (4)0.4506 (4)0.0638 (3)0.085 (2)
H11A1.06160.40800.05490.128*
H11B1.07740.47980.04590.128*
H11C1.00680.45800.05190.128*
C121.0783 (3)0.5968 (3)0.1081 (2)0.0502 (16)
H12A1.07930.63330.13260.060*
C131.1470 (3)0.5732 (4)0.1045 (3)0.069 (2)
H13A1.15090.54370.07500.104*
H13B1.15840.55270.13800.104*
H13C1.17480.60860.09830.104*
C141.0553 (4)0.6221 (4)0.0543 (3)0.093 (3)
H14A1.08660.65010.03930.140*
H14B1.01640.64480.05960.140*
H14C1.04830.58750.02970.140*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0229 (8)0.0301 (9)0.0245 (7)0.0001 (7)0.0025 (6)0.0018 (6)
Hg10.03668 (17)0.05346 (19)0.02979 (13)0.00074 (13)0.00920 (11)0.00648 (11)
P20.0269 (9)0.0513 (10)0.0249 (7)0.0046 (8)0.0005 (7)0.0113 (7)
Cl10.0625 (12)0.0856 (14)0.0479 (9)0.0170 (11)0.0108 (9)0.0162 (10)
Cl20.0628 (12)0.0618 (12)0.0547 (10)0.0097 (10)0.0096 (9)0.0179 (9)
B30.030 (4)0.032 (4)0.030 (3)0.008 (3)0.001 (3)0.006 (3)
B40.037 (4)0.052 (5)0.029 (3)0.002 (4)0.000 (3)0.018 (3)
B50.035 (4)0.062 (5)0.023 (3)0.005 (4)0.002 (3)0.009 (3)
B60.026 (4)0.033 (4)0.036 (3)0.001 (3)0.002 (3)0.011 (3)
B70.029 (4)0.056 (5)0.038 (4)0.006 (4)0.007 (3)0.009 (4)
B80.022 (4)0.060 (5)0.032 (3)0.008 (4)0.001 (3)0.005 (4)
B90.033 (4)0.061 (6)0.045 (4)0.005 (4)0.008 (4)0.020 (4)
B100.036 (5)0.093 (7)0.020 (3)0.003 (5)0.011 (3)0.012 (4)
B110.033 (4)0.075 (6)0.034 (4)0.006 (4)0.004 (3)0.028 (4)
B120.031 (4)0.089 (7)0.031 (4)0.003 (5)0.008 (3)0.008 (4)
C10.023 (3)0.038 (3)0.023 (2)0.001 (2)0.001 (2)0.002 (2)
C20.026 (3)0.037 (3)0.027 (2)0.004 (2)0.002 (2)0.003 (2)
C30.027 (3)0.040 (3)0.030 (3)0.008 (3)0.001 (2)0.002 (2)
C40.038 (4)0.068 (4)0.046 (3)0.004 (3)0.009 (3)0.001 (3)
C50.041 (4)0.066 (4)0.047 (3)0.018 (4)0.003 (3)0.005 (3)
C60.033 (3)0.045 (3)0.037 (3)0.005 (3)0.003 (3)0.004 (3)
C70.063 (4)0.039 (4)0.071 (4)0.007 (4)0.009 (4)0.002 (3)
C80.047 (4)0.064 (4)0.064 (4)0.017 (4)0.011 (3)0.002 (4)
C90.042 (3)0.060 (4)0.055 (3)0.010 (3)0.004 (3)0.021 (3)
C100.083 (5)0.054 (5)0.096 (5)0.018 (4)0.004 (5)0.028 (4)
C110.073 (5)0.109 (5)0.075 (4)0.014 (4)0.001 (4)0.052 (4)
C120.038 (3)0.073 (4)0.039 (3)0.003 (3)0.006 (3)0.000 (3)
C130.041 (4)0.105 (5)0.062 (4)0.007 (4)0.016 (3)0.015 (4)
C140.081 (5)0.142 (7)0.057 (4)0.012 (5)0.005 (4)0.029 (5)
Geometric parameters (Å, º) top
P1—C61.856 (6)B10—B121.739 (10)
P1—C31.865 (5)B10—B111.778 (11)
P1—C11.896 (5)B10—H101.1000
Hg1—Cl12.4482 (17)B11—B121.769 (10)
Hg1—Cl22.4542 (17)B11—H111.1000
Hg1—P12.5200 (10)B12—H121.1000
Hg1—P22.5242 (16)C1—C21.694 (6)
P2—C91.836 (7)C3—C51.507 (7)
P2—C121.851 (6)C3—C41.531 (7)
P2—C21.899 (5)C3—H3A0.9800
B3—C11.691 (8)C4—H4A0.9600
B3—C21.693 (8)C4—H4B0.9600
B3—B81.783 (9)C4—H4C0.9600
B3—B41.795 (8)C5—H5A0.9600
B3—B91.798 (9)C5—H5B0.9600
B3—H31.1000C5—H5C0.9600
B4—C11.722 (8)C6—C71.523 (8)
B4—B101.752 (10)C6—C81.532 (7)
B4—B51.763 (10)C6—H6A0.9800
B4—B91.764 (10)C7—H7A0.9600
B4—H41.1000C7—H7B0.9600
B5—C11.713 (7)C7—H7C0.9600
B5—B101.743 (10)C8—H8A0.9600
B5—B111.745 (10)C8—H8B0.9600
B5—B61.797 (9)C8—H8C0.9600
B5—H51.1000C9—C101.507 (9)
B6—C21.673 (8)C9—C111.548 (9)
B6—C11.674 (8)C9—H9A0.9800
B6—B71.793 (9)C10—H10A0.9600
B6—B111.797 (9)C10—H10B0.9600
B6—H61.1000C10—H10C0.9600
B7—C21.701 (8)C11—H11A0.9600
B7—B81.775 (10)C11—H11B0.9600
B7—B121.778 (10)C11—H11C0.9600
B7—B111.781 (9)C12—C141.507 (8)
B7—H71.1000C12—C131.537 (8)
B8—C21.711 (8)C12—H12A0.9800
B8—B91.756 (9)C13—H13A0.9600
B8—B121.770 (9)C13—H13B0.9600
B8—H81.1000C13—H13C0.9600
B9—B101.748 (11)C14—H14A0.9600
B9—B121.765 (11)C14—H14B0.9600
B9—H91.1000C14—H14C0.9600
C6—P1—C3106.3 (3)B9—B10—H10121.1
C6—P1—C1109.1 (2)B4—B10—H10120.9
C3—P1—C1104.6 (2)B11—B10—H10121.8
C6—P1—Hg1115.26 (18)B5—B11—B12107.1 (5)
C3—P1—Hg1117.07 (17)B5—B11—B1059.3 (4)
C1—P1—Hg1103.73 (13)B12—B11—B1058.7 (4)
Cl1—Hg1—Cl2104.81 (6)B5—B11—B7109.3 (5)
Cl1—Hg1—P1109.29 (6)B12—B11—B760.1 (4)
Cl2—Hg1—P1119.90 (5)B10—B11—B7107.3 (5)
Cl1—Hg1—P2119.51 (6)B5—B11—B660.9 (4)
Cl2—Hg1—P2112.06 (6)B12—B11—B6107.3 (4)
P1—Hg1—P291.82 (4)B10—B11—B6107.0 (5)
C9—P2—C12107.0 (3)B7—B11—B660.1 (4)
C9—P2—C2110.2 (3)B5—B11—H11121.2
C12—P2—C2104.8 (3)B12—B11—H11122.6
C9—P2—Hg1114.7 (2)B10—B11—H11123.0
C12—P2—Hg1116.5 (2)B7—B11—H11121.1
C2—P2—Hg1103.19 (15)B6—B11—H11121.8
C1—B3—C260.0 (3)B10—B12—B959.8 (4)
C1—B3—B8106.7 (5)B10—B12—B1160.9 (4)
C2—B3—B858.9 (4)B9—B12—B11108.3 (5)
C1—B3—B459.1 (3)B10—B12—B8107.9 (5)
C2—B3—B4106.8 (5)B9—B12—B859.6 (4)
B8—B3—B4106.8 (5)B11—B12—B8108.1 (5)
C1—B3—B9104.6 (5)B10—B12—B7109.1 (5)
C2—B3—B9104.5 (5)B9—B12—B7108.0 (5)
B8—B3—B958.7 (4)B11—B12—B760.3 (4)
B4—B3—B958.8 (4)B8—B12—B760.0 (4)
C1—B3—H3122.8B10—B12—H12121.2
C2—B3—H3122.9B9—B12—H12122.0
B8—B3—H3122.5B11—B12—H12121.3
B4—B3—H3122.3B8—B12—H12122.0
B9—B3—H3124.4B7—B12—H12121.3
C1—B4—B10104.7 (5)B6—C1—B3112.3 (4)
C1—B4—B558.9 (3)B6—C1—C259.6 (3)
B10—B4—B559.4 (4)B3—C1—C260.0 (3)
C1—B4—B9104.8 (4)B6—C1—B564.1 (4)
B10—B4—B959.6 (4)B3—C1—B5113.7 (4)
B5—B4—B9107.1 (5)C2—C1—B5109.8 (4)
C1—B4—B357.5 (3)B6—C1—B4114.8 (4)
B10—B4—B3107.4 (5)B3—C1—B463.5 (4)
B5—B4—B3106.4 (5)C2—C1—B4110.2 (4)
B9—B4—B360.7 (4)B5—C1—B461.8 (4)
C1—B4—H4124.8B6—C1—P1114.3 (4)
B10—B4—H4122.6B3—C1—P1120.3 (4)
B5—B4—H4122.3C2—C1—P1120.1 (3)
B9—B4—H4122.2B5—C1—P1119.0 (3)
B3—B4—H4122.2B4—C1—P1122.0 (3)
C1—B5—B10105.4 (5)B6—C2—C159.6 (3)
C1—B5—B11105.5 (4)B6—C2—B3112.3 (4)
B10—B5—B1161.3 (4)C1—C2—B360.0 (3)
C1—B5—B459.4 (3)B6—C2—B764.2 (4)
B10—B5—B460.0 (4)C1—C2—B7110.8 (4)
B11—B5—B4109.5 (5)B3—C2—B7114.9 (5)
C1—B5—B656.9 (3)B6—C2—B8114.9 (4)
B10—B5—B6108.6 (5)C1—C2—B8110.0 (4)
B11—B5—B661.0 (4)B3—C2—B863.2 (4)
B4—B5—B6107.0 (4)B7—C2—B862.7 (4)
C1—B5—H5124.9B6—C2—P2119.3 (4)
B10—B5—H5121.6C1—C2—P2120.9 (3)
B11—B5—H5120.9B3—C2—P2115.9 (4)
B4—B5—H5121.4B7—C2—P2120.1 (3)
B6—B5—H5122.3B8—C2—P2118.6 (3)
C2—B6—C160.8 (3)C5—C3—C4111.4 (5)
C2—B6—B758.7 (3)C5—C3—P1110.6 (4)
C1—B6—B7107.3 (5)C4—C3—P1116.1 (4)
C2—B6—B5106.8 (5)C5—C3—H3A106.0
C1—B6—B559.0 (3)C4—C3—H3A106.0
B7—B6—B5106.5 (5)P1—C3—H3A106.0
C2—B6—B11105.0 (5)C3—C4—H4A109.5
C1—B6—B11104.9 (5)C3—C4—H4B109.5
B7—B6—B1159.5 (4)H4A—C4—H4B109.5
B5—B6—B1158.1 (4)C3—C4—H4C109.5
C2—B6—H6122.6H4A—C4—H4C109.5
C1—B6—H6122.3H4B—C4—H4C109.5
B7—B6—H6122.3C3—C5—H5A109.5
B5—B6—H6122.8C3—C5—H5B109.5
B11—B6—H6124.1H5A—C5—H5B109.5
C2—B7—B858.9 (4)C3—C5—H5C109.5
C2—B7—B12104.8 (5)H5A—C5—H5C109.5
B8—B7—B1259.8 (4)H5B—C5—H5C109.5
C2—B7—B11104.6 (5)C7—C6—C8108.3 (5)
B8—B7—B11107.3 (5)C7—C6—P1114.6 (4)
B12—B7—B1159.6 (4)C8—C6—P1106.7 (4)
C2—B7—B657.1 (3)C7—C6—H6A109.0
B8—B7—B6106.1 (5)C8—C6—H6A109.0
B12—B7—B6107.1 (5)P1—C6—H6A109.0
B11—B7—B660.4 (4)C6—C7—H7A109.5
C2—B7—H7124.8C6—C7—H7B109.5
B8—B7—H7122.1H7A—C7—H7B109.5
B12—B7—H7122.5C6—C7—H7C109.5
B11—B7—H7122.3H7A—C7—H7C109.5
B6—B7—H7122.7H7B—C7—H7C109.5
C2—B8—B9105.5 (5)C6—C8—H8A109.5
C2—B8—B12104.7 (5)C6—C8—H8B109.5
B9—B8—B1260.1 (4)H8A—C8—H8B109.5
C2—B8—B758.4 (3)C6—C8—H8C109.5
B9—B8—B7108.5 (5)H8A—C8—H8C109.5
B12—B8—B760.2 (4)H8B—C8—H8C109.5
C2—B8—B357.9 (3)C10—C9—C11108.6 (6)
B9—B8—B361.1 (4)C10—C9—P2113.6 (5)
B12—B8—B3108.1 (5)C11—C9—P2106.2 (5)
B7—B8—B3107.0 (5)C10—C9—H9A109.4
C2—B8—H8124.9C11—C9—H9A109.4
B9—B8—H8121.4P2—C9—H9A109.4
B12—B8—H8122.3C9—C10—H10A109.5
B7—B8—H8121.7C9—C10—H10B109.5
B3—B8—H8121.8H10A—C10—H10B109.5
B10—B9—B8108.2 (6)C9—C10—H10C109.5
B10—B9—B459.9 (4)H10A—C10—H10C109.5
B8—B9—B4109.4 (5)H10B—C10—H10C109.5
B10—B9—B1259.4 (4)C9—C11—H11A109.5
B8—B9—B1260.4 (4)C9—C11—H11B109.5
B4—B9—B12108.0 (6)H11A—C11—H11B109.5
B10—B9—B3107.5 (5)C9—C11—H11C109.5
B8—B9—B360.2 (4)H11A—C11—H11C109.5
B4—B9—B360.5 (3)H11B—C11—H11C109.5
B12—B9—B3107.7 (5)C14—C12—C13111.6 (5)
B10—B9—H9122.2C14—C12—P2113.2 (5)
B8—B9—H9120.9C13—C12—P2114.5 (5)
B4—B9—H9121.1C14—C12—H12A105.6
B12—B9—H9122.1C13—C12—H12A105.6
B3—B9—H9121.9P2—C12—H12A105.6
B12—B10—B5108.6 (5)C12—C13—H13A109.5
B12—B10—B960.8 (4)C12—C13—H13B109.5
B5—B10—B9108.7 (5)H13A—C13—H13B109.5
B12—B10—B4109.6 (5)C12—C13—H13C109.5
B5—B10—B460.6 (4)H13A—C13—H13C109.5
B9—B10—B460.5 (4)H13B—C13—H13C109.5
B12—B10—B1160.4 (4)C12—C14—H14A109.5
B5—B10—B1159.4 (4)C12—C14—H14B109.5
B9—B10—B11108.7 (5)H14A—C14—H14B109.5
B4—B10—B11108.5 (5)C12—C14—H14C109.5
B12—B10—H10120.8H14A—C14—H14C109.5
B5—B10—H10121.6H14B—C14—H14C109.5

Experimental details

Crystal data
Chemical formula[HgCl2(C14H38B10P2)]
Mr647.97
Crystal system, space groupTetragonal, I41/a
Temperature (K)298
a, c (Å)21.110 (3), 24.585 (6)
V3)10956 (3)
Z16
Radiation typeMo Kα
µ (mm1)5.93
Crystal size (mm)0.53 × 0.49 × 0.47
Data collection
DiffractometerBruker SMART CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.145, 0.167
No. of measured, independent and
observed [I > 2σ(I)] reflections
22446, 4815, 3491
Rint0.081
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.077, 1.00
No. of reflections4815
No. of parameters270
No. of restraints290
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.37, 1.23

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).

Selected bond lengths (Å) top
Hg1—Cl12.4482 (17)Hg1—P12.5200 (10)
Hg1—Cl22.4542 (17)Hg1—P22.5242 (16)
 

Acknowledgements

This work was supported by the National Natural Science Foundation of China (Project No. 20371025), the Open Research Fund Program of the Key Laboratory of Marine Drugs (Ocean University of China), the Ministry of Education [Project No. KLMD (OUC) 2004] and the Postgraduate Foundation of Taishan University (No. Yo6-2-10).

References

First citationBruker (2001). SMART, SAINT, SADABS and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationKivekäs, R., Sillanpää, R., Teixidor, F., Viñas, C., Nuñez, R. & Abad, M. (1995). Acta Cryst. C51, 1864–1868.  CSD CrossRef Web of Science IUCr Journals Google Scholar
First citationLiu, L., Zhang, Q.-F. & Leung, W.-H. (2004). Acta Cryst. E60, m394–m395.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationMariyatra, M. B., Panchanatheswaran, K., Low, J. N. & Glidewell, C. (2005). Acta Cryst. C61, m211–m214.  Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
First citationPaavola, S., Kivekäs, R., Teixidor, F. & Viñas, C. (2002). J. Organomet. Chem. 606, 183–187.  Web of Science CrossRef Google Scholar
First citationPaavola, S., Teixidor, F., Viñas, C. & Kivekäs, R. (2002a). Acta Cryst. C58, m237–m239.  Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
First citationPaavola, S., Teixidor, F., Viñas, C. & Kivekäs, R. (2002b). J. Organomet. Chem. 645, 39–46.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.  Google Scholar

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