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

Su, F.; Guo, Q.; Dou, J.; Li, D.; Wang, D.

doi:10.1107/S1600536807065130

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 1| January 2008| Page m134

https://doi.org/10.1107/S1600536807065130

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

Fangfang Su,^a Qingliang Guo,^b Jianmin Dou,^a ^* Dacheng Li ^a and Daqi Wang ^a

^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 Hg^II 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 ); Liu et al. (2004 ); Paavola, Kivekäs et al. (2002 ), Paavola, Teixidor et al. (2002a ,b ). For the synthesis and structure of the ligand, see: Kivekäs et al. (1995 ).

Experimental

Crystal data

[HgCl₂(C₁₄H₃₈B₁₀P₂)]
M_r = 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 ) T_min = 0.145, T_max = 0.167 (expected range = 0.053–0.062)
22446 measured reflections
4815 independent reflections
3491 reflections with I > 2σ(I)
R_int = 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
Δρ_max = 1.37 e Å⁻³
Δρ_min = −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); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536807065130/hb2648sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807065130/hb2648Isup2.hkl

checkCIF report

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 Hg^II and chloride ions as the title compound, (I).

As shown in Fig. 1, The Hg^II 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).

Structure description 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).

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

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)]	D_x = 1.571 Mg m⁻³
M_r = 647.97	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4₁/a	Cell parameters from 5681 reflections
Hall symbol: -I 4ad	θ = 2.3–25.3°
a = 21.110 (3) Å	µ = 5.93 mm⁻¹
c = 24.585 (6) Å	T = 298 K
V = 10956 (3) Å³	Block, colorless
Z = 16	0.53 × 0.49 × 0.47 mm
F(000) = 5056

Data collection top

Bruker SMART CCD diffractometer	4815 independent reflections
Radiation source: fine-focus sealed tube	3491 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.081
ω scans	θ_max = 25.0°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −25→23
T_min = 0.145, T_max = 0.167	k = −17→25
22446 measured reflections	l = −29→27

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.077	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.031P)²] where P = (F_o² + 2F_c²)/3
4815 reflections	(Δ/σ)_max = 0.002
270 parameters	Δρ_max = 1.37 e Å⁻³
290 restraints	Δρ_min = −1.23 e Å⁻³

Crystal data top

[HgCl₂(C₁₄H₃₈B₁₀P₂)]	Z = 16
M_r = 647.97	Mo Kα radiation
Tetragonal, I4₁/a	µ = 5.93 mm⁻¹
a = 21.110 (3) Å	T = 298 K
c = 24.585 (6) Å	0.53 × 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)
T_min = 0.145, T_max = 0.167	R_int = 0.081
22446 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	290 restraints
wR(F²) = 0.077	H-atom parameters constrained
S = 1.00	Δρ_max = 1.37 e Å⁻³
4815 reflections	Δρ_min = −1.23 e Å⁻³
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

	x	y	z	U_iso*/U_eq
P1	0.88138 (6)	0.58515 (7)	0.21383 (4)	0.0258 (3)
Hg1	0.906748 (11)	0.554286 (12)	0.117243 (8)	0.03997 (11)
P2	1.02256 (7)	0.53987 (8)	0.13960 (5)	0.0344 (4)
Cl1	0.87446 (8)	0.63978 (9)	0.05593 (7)	0.0653 (5)
Cl2	0.85996 (8)	0.45816 (8)	0.07802 (7)	0.0598 (5)
B3	1.0185 (3)	0.6349 (3)	0.2328 (2)	0.0303 (16)
H3	1.0115	0.6728	0.2028	0.036*
B4	0.9818 (3)	0.6364 (4)	0.2987 (2)	0.0391 (19)
H4	0.9519	0.6761	0.3122	0.047*
B5	0.9646 (3)	0.5571 (3)	0.3155 (2)	0.0401 (19)
H5	0.9232	0.5447	0.3406	0.048*
B6	0.9896 (3)	0.5093 (3)	0.2589 (2)	0.0319 (16)
H6	0.9638	0.4667	0.2457	0.038*
B7	1.0743 (3)	0.5145 (4)	0.2565 (3)	0.0413 (19)
H7	1.1044	0.4750	0.2430	0.050*
B8	1.0922 (3)	0.5945 (3)	0.2405 (3)	0.0379 (18)
H8	1.1341	0.6074	0.2164	0.046*
B9	1.0649 (3)	0.6428 (4)	0.2937 (3)	0.046 (2)
H9	1.0894	0.6872	0.3041	0.056*
B10	1.0309 (3)	0.5941 (4)	0.3432 (3)	0.050 (2)
H10	1.0334	0.6065	0.3866	0.060*
B11	1.0350 (3)	0.5142 (4)	0.3206 (3)	0.047 (2)
H11	1.0393	0.4738	0.3486	0.057*
B12	1.0978 (3)	0.5680 (4)	0.3086 (3)	0.050 (2)
H12	1.1436	0.5629	0.3294	0.060*
C1	0.9610 (2)	0.5824 (3)	0.24933 (18)	0.0280 (12)
C2	1.0262 (2)	0.5577 (3)	0.21524 (19)	0.0301 (12)
C3	0.8303 (3)	0.5299 (3)	0.2536 (2)	0.0326 (13)
H3A	0.8588	0.4975	0.2683	0.039*
C4	0.7960 (3)	0.5584 (3)	0.3027 (2)	0.0508 (17)
H4A	0.7646	0.5880	0.2903	0.076*
H4B	0.8260	0.5799	0.3255	0.076*
H4C	0.7758	0.5252	0.3230	0.076*
C5	0.7850 (3)	0.4955 (3)	0.2166 (2)	0.0515 (18)
H5A	0.7646	0.4620	0.2364	0.077*
H5B	0.8079	0.4778	0.1864	0.077*
H5C	0.7537	0.5246	0.2034	0.077*
C6	0.8465 (3)	0.6652 (3)	0.2224 (2)	0.0380 (14)
H6A	0.8417	0.6741	0.2613	0.046*
C7	0.8844 (3)	0.7185 (3)	0.1962 (3)	0.0577 (18)
H7A	0.8959	0.7066	0.1598	0.087*
H7B	0.9220	0.7263	0.2171	0.087*
H7C	0.8590	0.7563	0.1951	0.087*
C8	0.7808 (3)	0.6633 (3)	0.1959 (3)	0.0584 (18)
H8A	0.7606	0.7037	0.2001	0.088*
H8B	0.7556	0.6312	0.2131	0.088*
H8C	0.7851	0.6537	0.1579	0.088*
C9	1.0537 (3)	0.4602 (3)	0.1261 (3)	0.0523 (16)
H9A	1.0981	0.4580	0.1375	0.063*
C10	1.0167 (4)	0.4082 (3)	0.1536 (3)	0.078 (2)
H10A	0.9722	0.4173	0.1511	0.116*
H10B	1.0288	0.4057	0.1912	0.116*
H10C	1.0255	0.3686	0.1360	0.116*
C11	1.0495 (4)	0.4506 (4)	0.0638 (3)	0.085 (2)
H11A	1.0616	0.4080	0.0549	0.128*
H11B	1.0774	0.4798	0.0459	0.128*
H11C	1.0068	0.4580	0.0519	0.128*
C12	1.0783 (3)	0.5968 (3)	0.1081 (2)	0.0502 (16)
H12A	1.0793	0.6333	0.1326	0.060*
C13	1.1470 (3)	0.5732 (4)	0.1045 (3)	0.069 (2)
H13A	1.1509	0.5437	0.0750	0.104*
H13B	1.1584	0.5527	0.1380	0.104*
H13C	1.1748	0.6086	0.0983	0.104*
C14	1.0553 (4)	0.6221 (4)	0.0543 (3)	0.093 (3)
H14A	1.0866	0.6501	0.0393	0.140*
H14B	1.0164	0.6448	0.0596	0.140*
H14C	1.0483	0.5875	0.0297	0.140*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
P1	0.0229 (8)	0.0301 (9)	0.0245 (7)	−0.0001 (7)	−0.0025 (6)	−0.0018 (6)
Hg1	0.03668 (17)	0.05346 (19)	0.02979 (13)	0.00074 (13)	−0.00920 (11)	−0.00648 (11)
P2	0.0269 (9)	0.0513 (10)	0.0249 (7)	0.0046 (8)	−0.0005 (7)	−0.0113 (7)
Cl1	0.0625 (12)	0.0856 (14)	0.0479 (9)	0.0170 (11)	−0.0108 (9)	0.0162 (10)
Cl2	0.0628 (12)	0.0618 (12)	0.0547 (10)	−0.0097 (10)	−0.0096 (9)	−0.0179 (9)
B3	0.030 (4)	0.032 (4)	0.030 (3)	−0.008 (3)	−0.001 (3)	−0.006 (3)
B4	0.037 (4)	0.052 (5)	0.029 (3)	0.002 (4)	0.000 (3)	−0.018 (3)
B5	0.035 (4)	0.062 (5)	0.023 (3)	−0.005 (4)	0.002 (3)	0.009 (3)
B6	0.026 (4)	0.033 (4)	0.036 (3)	0.001 (3)	0.002 (3)	0.011 (3)
B7	0.029 (4)	0.056 (5)	0.038 (4)	0.006 (4)	−0.007 (3)	0.009 (4)
B8	0.022 (4)	0.060 (5)	0.032 (3)	−0.008 (4)	−0.001 (3)	−0.005 (4)
B9	0.033 (4)	0.061 (6)	0.045 (4)	−0.005 (4)	−0.008 (4)	−0.020 (4)
B10	0.036 (5)	0.093 (7)	0.020 (3)	0.003 (5)	−0.011 (3)	−0.012 (4)
B11	0.033 (4)	0.075 (6)	0.034 (4)	0.006 (4)	−0.004 (3)	0.028 (4)
B12	0.031 (4)	0.089 (7)	0.031 (4)	0.003 (5)	−0.008 (3)	−0.008 (4)
C1	0.023 (3)	0.038 (3)	0.023 (2)	−0.001 (2)	0.001 (2)	−0.002 (2)
C2	0.026 (3)	0.037 (3)	0.027 (2)	0.004 (2)	0.002 (2)	−0.003 (2)
C3	0.027 (3)	0.040 (3)	0.030 (3)	−0.008 (3)	0.001 (2)	−0.002 (2)
C4	0.038 (4)	0.068 (4)	0.046 (3)	−0.004 (3)	0.009 (3)	−0.001 (3)
C5	0.041 (4)	0.066 (4)	0.047 (3)	−0.018 (4)	0.003 (3)	−0.005 (3)
C6	0.033 (3)	0.045 (3)	0.037 (3)	0.005 (3)	−0.003 (3)	−0.004 (3)
C7	0.063 (4)	0.039 (4)	0.071 (4)	0.007 (4)	−0.009 (4)	−0.002 (3)
C8	0.047 (4)	0.064 (4)	0.064 (4)	0.017 (4)	−0.011 (3)	0.002 (4)
C9	0.042 (3)	0.060 (4)	0.055 (3)	0.010 (3)	−0.004 (3)	−0.021 (3)
C10	0.083 (5)	0.054 (5)	0.096 (5)	0.018 (4)	−0.004 (5)	−0.028 (4)
C11	0.073 (5)	0.109 (5)	0.075 (4)	0.014 (4)	0.001 (4)	−0.052 (4)
C12	0.038 (3)	0.073 (4)	0.039 (3)	−0.003 (3)	0.006 (3)	0.000 (3)
C13	0.041 (4)	0.105 (5)	0.062 (4)	−0.007 (4)	0.016 (3)	−0.015 (4)
C14	0.081 (5)	0.142 (7)	0.057 (4)	−0.012 (5)	0.005 (4)	0.029 (5)

Geometric parameters (Å, º) top

P1—C6	1.856 (6)	B10—B12	1.739 (10)
P1—C3	1.865 (5)	B10—B11	1.778 (11)
P1—C1	1.896 (5)	B10—H10	1.1000
Hg1—Cl1	2.4482 (17)	B11—B12	1.769 (10)
Hg1—Cl2	2.4542 (17)	B11—H11	1.1000
Hg1—P1	2.5200 (10)	B12—H12	1.1000
Hg1—P2	2.5242 (16)	C1—C2	1.694 (6)
P2—C9	1.836 (7)	C3—C5	1.507 (7)
P2—C12	1.851 (6)	C3—C4	1.531 (7)
P2—C2	1.899 (5)	C3—H3A	0.9800
B3—C1	1.691 (8)	C4—H4A	0.9600
B3—C2	1.693 (8)	C4—H4B	0.9600
B3—B8	1.783 (9)	C4—H4C	0.9600
B3—B4	1.795 (8)	C5—H5A	0.9600
B3—B9	1.798 (9)	C5—H5B	0.9600
B3—H3	1.1000	C5—H5C	0.9600
B4—C1	1.722 (8)	C6—C7	1.523 (8)
B4—B10	1.752 (10)	C6—C8	1.532 (7)
B4—B5	1.763 (10)	C6—H6A	0.9800
B4—B9	1.764 (10)	C7—H7A	0.9600
B4—H4	1.1000	C7—H7B	0.9600
B5—C1	1.713 (7)	C7—H7C	0.9600
B5—B10	1.743 (10)	C8—H8A	0.9600
B5—B11	1.745 (10)	C8—H8B	0.9600
B5—B6	1.797 (9)	C8—H8C	0.9600
B5—H5	1.1000	C9—C10	1.507 (9)
B6—C2	1.673 (8)	C9—C11	1.548 (9)
B6—C1	1.674 (8)	C9—H9A	0.9800
B6—B7	1.793 (9)	C10—H10A	0.9600
B6—B11	1.797 (9)	C10—H10B	0.9600
B6—H6	1.1000	C10—H10C	0.9600
B7—C2	1.701 (8)	C11—H11A	0.9600
B7—B8	1.775 (10)	C11—H11B	0.9600
B7—B12	1.778 (10)	C11—H11C	0.9600
B7—B11	1.781 (9)	C12—C14	1.507 (8)
B7—H7	1.1000	C12—C13	1.537 (8)
B8—C2	1.711 (8)	C12—H12A	0.9800
B8—B9	1.756 (9)	C13—H13A	0.9600
B8—B12	1.770 (9)	C13—H13B	0.9600
B8—H8	1.1000	C13—H13C	0.9600
B9—B10	1.748 (11)	C14—H14A	0.9600
B9—B12	1.765 (11)	C14—H14B	0.9600
B9—H9	1.1000	C14—H14C	0.9600

C6—P1—C3	106.3 (3)	B9—B10—H10	121.1
C6—P1—C1	109.1 (2)	B4—B10—H10	120.9
C3—P1—C1	104.6 (2)	B11—B10—H10	121.8
C6—P1—Hg1	115.26 (18)	B5—B11—B12	107.1 (5)
C3—P1—Hg1	117.07 (17)	B5—B11—B10	59.3 (4)
C1—P1—Hg1	103.73 (13)	B12—B11—B10	58.7 (4)
Cl1—Hg1—Cl2	104.81 (6)	B5—B11—B7	109.3 (5)
Cl1—Hg1—P1	109.29 (6)	B12—B11—B7	60.1 (4)
Cl2—Hg1—P1	119.90 (5)	B10—B11—B7	107.3 (5)
Cl1—Hg1—P2	119.51 (6)	B5—B11—B6	60.9 (4)
Cl2—Hg1—P2	112.06 (6)	B12—B11—B6	107.3 (4)
P1—Hg1—P2	91.82 (4)	B10—B11—B6	107.0 (5)
C9—P2—C12	107.0 (3)	B7—B11—B6	60.1 (4)
C9—P2—C2	110.2 (3)	B5—B11—H11	121.2
C12—P2—C2	104.8 (3)	B12—B11—H11	122.6
C9—P2—Hg1	114.7 (2)	B10—B11—H11	123.0
C12—P2—Hg1	116.5 (2)	B7—B11—H11	121.1
C2—P2—Hg1	103.19 (15)	B6—B11—H11	121.8
C1—B3—C2	60.0 (3)	B10—B12—B9	59.8 (4)
C1—B3—B8	106.7 (5)	B10—B12—B11	60.9 (4)
C2—B3—B8	58.9 (4)	B9—B12—B11	108.3 (5)
C1—B3—B4	59.1 (3)	B10—B12—B8	107.9 (5)
C2—B3—B4	106.8 (5)	B9—B12—B8	59.6 (4)
B8—B3—B4	106.8 (5)	B11—B12—B8	108.1 (5)
C1—B3—B9	104.6 (5)	B10—B12—B7	109.1 (5)
C2—B3—B9	104.5 (5)	B9—B12—B7	108.0 (5)
B8—B3—B9	58.7 (4)	B11—B12—B7	60.3 (4)
B4—B3—B9	58.8 (4)	B8—B12—B7	60.0 (4)
C1—B3—H3	122.8	B10—B12—H12	121.2
C2—B3—H3	122.9	B9—B12—H12	122.0
B8—B3—H3	122.5	B11—B12—H12	121.3
B4—B3—H3	122.3	B8—B12—H12	122.0
B9—B3—H3	124.4	B7—B12—H12	121.3
C1—B4—B10	104.7 (5)	B6—C1—B3	112.3 (4)
C1—B4—B5	58.9 (3)	B6—C1—C2	59.6 (3)
B10—B4—B5	59.4 (4)	B3—C1—C2	60.0 (3)
C1—B4—B9	104.8 (4)	B6—C1—B5	64.1 (4)
B10—B4—B9	59.6 (4)	B3—C1—B5	113.7 (4)
B5—B4—B9	107.1 (5)	C2—C1—B5	109.8 (4)
C1—B4—B3	57.5 (3)	B6—C1—B4	114.8 (4)
B10—B4—B3	107.4 (5)	B3—C1—B4	63.5 (4)
B5—B4—B3	106.4 (5)	C2—C1—B4	110.2 (4)
B9—B4—B3	60.7 (4)	B5—C1—B4	61.8 (4)
C1—B4—H4	124.8	B6—C1—P1	114.3 (4)
B10—B4—H4	122.6	B3—C1—P1	120.3 (4)
B5—B4—H4	122.3	C2—C1—P1	120.1 (3)
B9—B4—H4	122.2	B5—C1—P1	119.0 (3)
B3—B4—H4	122.2	B4—C1—P1	122.0 (3)
C1—B5—B10	105.4 (5)	B6—C2—C1	59.6 (3)
C1—B5—B11	105.5 (4)	B6—C2—B3	112.3 (4)
B10—B5—B11	61.3 (4)	C1—C2—B3	60.0 (3)
C1—B5—B4	59.4 (3)	B6—C2—B7	64.2 (4)
B10—B5—B4	60.0 (4)	C1—C2—B7	110.8 (4)
B11—B5—B4	109.5 (5)	B3—C2—B7	114.9 (5)
C1—B5—B6	56.9 (3)	B6—C2—B8	114.9 (4)
B10—B5—B6	108.6 (5)	C1—C2—B8	110.0 (4)
B11—B5—B6	61.0 (4)	B3—C2—B8	63.2 (4)
B4—B5—B6	107.0 (4)	B7—C2—B8	62.7 (4)
C1—B5—H5	124.9	B6—C2—P2	119.3 (4)
B10—B5—H5	121.6	C1—C2—P2	120.9 (3)
B11—B5—H5	120.9	B3—C2—P2	115.9 (4)
B4—B5—H5	121.4	B7—C2—P2	120.1 (3)
B6—B5—H5	122.3	B8—C2—P2	118.6 (3)
C2—B6—C1	60.8 (3)	C5—C3—C4	111.4 (5)
C2—B6—B7	58.7 (3)	C5—C3—P1	110.6 (4)
C1—B6—B7	107.3 (5)	C4—C3—P1	116.1 (4)
C2—B6—B5	106.8 (5)	C5—C3—H3A	106.0
C1—B6—B5	59.0 (3)	C4—C3—H3A	106.0
B7—B6—B5	106.5 (5)	P1—C3—H3A	106.0
C2—B6—B11	105.0 (5)	C3—C4—H4A	109.5
C1—B6—B11	104.9 (5)	C3—C4—H4B	109.5
B7—B6—B11	59.5 (4)	H4A—C4—H4B	109.5
B5—B6—B11	58.1 (4)	C3—C4—H4C	109.5
C2—B6—H6	122.6	H4A—C4—H4C	109.5
C1—B6—H6	122.3	H4B—C4—H4C	109.5
B7—B6—H6	122.3	C3—C5—H5A	109.5
B5—B6—H6	122.8	C3—C5—H5B	109.5
B11—B6—H6	124.1	H5A—C5—H5B	109.5
C2—B7—B8	58.9 (4)	C3—C5—H5C	109.5
C2—B7—B12	104.8 (5)	H5A—C5—H5C	109.5
B8—B7—B12	59.8 (4)	H5B—C5—H5C	109.5
C2—B7—B11	104.6 (5)	C7—C6—C8	108.3 (5)
B8—B7—B11	107.3 (5)	C7—C6—P1	114.6 (4)
B12—B7—B11	59.6 (4)	C8—C6—P1	106.7 (4)
C2—B7—B6	57.1 (3)	C7—C6—H6A	109.0
B8—B7—B6	106.1 (5)	C8—C6—H6A	109.0
B12—B7—B6	107.1 (5)	P1—C6—H6A	109.0
B11—B7—B6	60.4 (4)	C6—C7—H7A	109.5
C2—B7—H7	124.8	C6—C7—H7B	109.5
B8—B7—H7	122.1	H7A—C7—H7B	109.5
B12—B7—H7	122.5	C6—C7—H7C	109.5
B11—B7—H7	122.3	H7A—C7—H7C	109.5
B6—B7—H7	122.7	H7B—C7—H7C	109.5
C2—B8—B9	105.5 (5)	C6—C8—H8A	109.5
C2—B8—B12	104.7 (5)	C6—C8—H8B	109.5
B9—B8—B12	60.1 (4)	H8A—C8—H8B	109.5
C2—B8—B7	58.4 (3)	C6—C8—H8C	109.5
B9—B8—B7	108.5 (5)	H8A—C8—H8C	109.5
B12—B8—B7	60.2 (4)	H8B—C8—H8C	109.5
C2—B8—B3	57.9 (3)	C10—C9—C11	108.6 (6)
B9—B8—B3	61.1 (4)	C10—C9—P2	113.6 (5)
B12—B8—B3	108.1 (5)	C11—C9—P2	106.2 (5)
B7—B8—B3	107.0 (5)	C10—C9—H9A	109.4
C2—B8—H8	124.9	C11—C9—H9A	109.4
B9—B8—H8	121.4	P2—C9—H9A	109.4
B12—B8—H8	122.3	C9—C10—H10A	109.5
B7—B8—H8	121.7	C9—C10—H10B	109.5
B3—B8—H8	121.8	H10A—C10—H10B	109.5
B10—B9—B8	108.2 (6)	C9—C10—H10C	109.5
B10—B9—B4	59.9 (4)	H10A—C10—H10C	109.5
B8—B9—B4	109.4 (5)	H10B—C10—H10C	109.5
B10—B9—B12	59.4 (4)	C9—C11—H11A	109.5
B8—B9—B12	60.4 (4)	C9—C11—H11B	109.5
B4—B9—B12	108.0 (6)	H11A—C11—H11B	109.5
B10—B9—B3	107.5 (5)	C9—C11—H11C	109.5
B8—B9—B3	60.2 (4)	H11A—C11—H11C	109.5
B4—B9—B3	60.5 (3)	H11B—C11—H11C	109.5
B12—B9—B3	107.7 (5)	C14—C12—C13	111.6 (5)
B10—B9—H9	122.2	C14—C12—P2	113.2 (5)
B8—B9—H9	120.9	C13—C12—P2	114.5 (5)
B4—B9—H9	121.1	C14—C12—H12A	105.6
B12—B9—H9	122.1	C13—C12—H12A	105.6
B3—B9—H9	121.9	P2—C12—H12A	105.6
B12—B10—B5	108.6 (5)	C12—C13—H13A	109.5
B12—B10—B9	60.8 (4)	C12—C13—H13B	109.5
B5—B10—B9	108.7 (5)	H13A—C13—H13B	109.5
B12—B10—B4	109.6 (5)	C12—C13—H13C	109.5
B5—B10—B4	60.6 (4)	H13A—C13—H13C	109.5
B9—B10—B4	60.5 (4)	H13B—C13—H13C	109.5
B12—B10—B11	60.4 (4)	C12—C14—H14A	109.5
B5—B10—B11	59.4 (4)	C12—C14—H14B	109.5
B9—B10—B11	108.7 (5)	H14A—C14—H14B	109.5
B4—B10—B11	108.5 (5)	C12—C14—H14C	109.5
B12—B10—H10	120.8	H14A—C14—H14C	109.5
B5—B10—H10	121.6	H14B—C14—H14C	109.5

Experimental details

Crystal data
Chemical formula	[HgCl₂(C₁₄H₃₈B₁₀P₂)]
M_r	647.97
Crystal system, space group	Tetragonal, I4₁/a
Temperature (K)	298
a, c (Å)	21.110 (3), 24.585 (6)
V (Å³)	10956 (3)
Z	16
Radiation type	Mo Kα
µ (mm⁻¹)	5.93
Crystal size (mm)	0.53 × 0.49 × 0.47

Data collection
Diffractometer	Bruker SMART CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.145, 0.167
No. of measured, independent and observed [I > 2σ(I)] reflections	22446, 4815, 3491
R_int	0.081
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.077, 1.00
No. of reflections	4815
No. of parameters	270
No. of restraints	290
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	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—Cl1	2.4482 (17)	Hg1—P1	2.5200 (10)
Hg1—Cl2	2.4542 (17)	Hg1—P2	2.5242 (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

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