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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2010 Dec 4;67(Pt 1):m2. doi: 10.1107/S1600536810049263

Di-μ-thio­cyanato-bis­{[1,2-bis­(diiso­propyl­phosphan­yl)-1,2-dicarba-closo-dodeca­borane]silver(I)}

Liguo Yang a, Chengchen Zhu a, Dacheng Li a,*
PMCID: PMC3050408  PMID: 21522546

Abstract

The title compound, [Ag2(NCS)2(C14H38B10P2)2], was synthesized by the reaction of 1,2-bis­(diiso­propyl­phos­phan­yl)-1,2-dicarba-closo-dodeca­borane with AgSCN. The diisopropyl­phosphanyl-closo-carborane ligand is coordinated in a bidentate manner to the AgI atom through the two P atoms. The coordination of the AgI atom is distorted tetra­hedral, in which two vertices are formed by the P atoms of the chelating diphosphine ligand, and the other two are occupied by the S and N atoms of the two bridging thio­cyanate anions, leading to a centrosymmetric binuclear complex. The distance between the two C atoms in the carborane skeleton is 1.851 (6) Å.

Related literature

For related structures, see: Zhang et al. (2006); Paavola et al. (2002, 2002a ,b ). For the synthesis and structure of 1,2-bis­(di­isopropyl­phosphan­yl)-1,2-dicarba-closo-dodeca­borane, see: Kivekäs et al. (1995).graphic file with name e-67-000m2-scheme1.jpg

Experimental

Crystal data

  • [Ag2(NCS)2(C14H38B10P2)2]

  • M r = 1084.87

  • Monoclinic, Inline graphic

  • a = 7.8075 (9) Å

  • b = 34.220 (3) Å

  • c = 10.6886 (12) Å

  • β = 110.074 (1)°

  • V = 2682.2 (5) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.95 mm−1

  • T = 298 K

  • 0.41 × 0.18 × 0.08 mm

Data collection

  • Bruker SMART 1000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T min = 0.696, T max = 0.928

  • 13386 measured reflections

  • 4714 independent reflections

  • 3238 reflections with I > 2σ(I)

  • R int = 0.050

Refinement

  • R[F 2 > 2σ(F 2)] = 0.052

  • wR(F 2) = 0.099

  • S = 1.06

  • 4714 reflections

  • 279 parameters

  • 2 restraints

  • H-atom parameters constrained

  • Δρmax = 0.82 e Å−3

  • Δρmin = −0.92 e Å−3

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810049263/gk2319sup1.cif

e-67-000m2-sup1.cif (27KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810049263/gk2319Isup2.hkl

e-67-000m2-Isup2.hkl (230.9KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected geometric parameters (Å, °).

Ag1—N1 2.251 (5)
Ag1—P1 2.4566 (14)
Ag1—P2 2.4981 (14)
Ag1—S1 2.5693 (17)
P1—Ag1—P2 90.97 (4)
N1—Ag1—S1 97.27 (14)

Acknowledgments

This work was supported by the National Natural Science Foundation of China (project No. 20971063), the Natural Science Foundation of Shandong Province (Y2007B01) and the Shandong Tai-Shan Scholar Research Fund.

supplementary crystallographic information

Comment

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 of this ligand with Pt(II) and Pd(II) have been described (Paavola et al., 2002, 2002a,b). Here we report the structure of this ligand combined with Ag and thiocyanate ion.

As shown in Fig. 1, the coordination of the Ag atom is distorted tetrahedral, formed by one S atom and one N atom of the two SCN anions and the P atoms of diisopropylphosphanyl-closo-carborane ligand (Table 1). The two P—Ag bond lengths are slightly shorter than the corresponding bond lengths in the complex [Ag2Cl2(C26H30B10P2)2].2CH2Cl2 [2.5052 (14) Å; Zhang et al., 2006]). The P—Ag—P angle is slightly larger than the corresponding value of 89.80 Å for the complex [Ag2Cl2(C26H30B10P2)2].2CH2Cl2 (Zhang et al., 2006). The five-memebered chelate ring fomed by the silver atom, two phosphorus atoms and two carbon atoms of the carborane skeleton is strongly flattened with a maximum deviation of 0.322 Å for C2. The torsion angle P1—C1—C2—P2 is -0.4 (5)°, viz. smaller than that of 12.1 (2)° in the free ligand (Kivekäs et al., 1995).

Experimental

The title compound was synthesizd by the reaction of 1 mmol AgSCN and 1 mmol 1,2-(PiPr2)2-1,2-C2B10H10 in 10 ml dichloromethane under the protection of N2, refluxed for 4 h, then a colorless solution formed, and crystals suitable for X-ray diffraction were obtained from a dichloromethane- n-hexane solution.(61.7%, m.p. 553–558 K). FTIR (KBr) v (cm-l): 2989, 2966, 2930, 2872 (C—H); 2614, 2602, 2585, 2556 (B—H); 1071 (C—P).

Refinement

All H atoms were placed geometrically and treated as riding on their parent atoms, with B—H 1.10, C—H 0.96 (methyl), C—H 0.98 Å (isopropyl), with Uiso(H) = 1.2Ueq(B), Uiso(H) = 1.5Ueq(C). A rigid bond restraints were applied to the Uij values of Ag1,P1 and Ag1,P2 atoms via DELU instruction of SHELXL97 (Sheldrick, 2008).

Figures

Fig. 1.

Fig. 1.

The molecular structure of the title compound with atom labels and 40% probability displacement ellipsoids for non-H atoms. Symmetry code for atoms with the A label: -x + 1,-y,-z + 2. H atoms have been omitted for clarity.

Crystal data

[Ag2(NCS)2(C14H38B10P2)2] F(000) = 1112
Mr = 1084.87 Dx = 1.343 Mg m3
Monoclinic, P21/n Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn Cell parameters from 3831 reflections
a = 7.8075 (9) Å θ = 2.4–25.8°
b = 34.220 (3) Å µ = 0.95 mm1
c = 10.6886 (12) Å T = 298 K
β = 110.074 (1)° Block, yellow
V = 2682.2 (5) Å3 0.41 × 0.18 × 0.08 mm
Z = 2

Data collection

Bruker SMART 1000 CCD diffractometer 4714 independent reflections
Radiation source: fine-focus sealed tube 3238 reflections with I > 2σ(I)
graphite Rint = 0.050
φ and ω scans θmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) h = −8→9
Tmin = 0.696, Tmax = 0.928 k = −36→40
13386 measured reflections l = −12→10

Refinement

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)] = 0.052 Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099 H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0185P)2 + 6.4963P] where P = (Fo2 + 2Fc2)/3
4714 reflections (Δ/σ)max = 0.001
279 parameters Δρmax = 0.82 e Å3
2 restraints Δρmin = −0.92 e Å3

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

x y z Uiso*/Ueq
Ag1 0.61123 (6) 0.074944 (11) 0.96399 (4) 0.04357 (15)
P1 0.77035 (19) 0.13609 (4) 1.05474 (12) 0.0319 (3)
P2 0.62319 (19) 0.09058 (4) 0.73885 (13) 0.0335 (3)
S1 0.2929 (2) 0.06561 (4) 0.9800 (2) 0.0638 (5)
C2 0.7012 (7) 0.14225 (13) 0.7460 (4) 0.0309 (12)
N1 0.7232 (7) 0.01564 (15) 1.0410 (5) 0.0634 (16)
C1 0.7792 (7) 0.16616 (13) 0.9114 (5) 0.0311 (12)
C3 0.4009 (7) 0.08761 (15) 0.6024 (5) 0.0443 (14)
H3A 0.4158 0.0956 0.5187 0.053*
C9 1.0151 (7) 0.13069 (15) 1.1608 (5) 0.0398 (13)
H9A 1.0841 0.1309 1.0995 0.048*
B1 0.5741 (8) 0.17712 (16) 0.7899 (5) 0.0327 (14)
H1 0.4439 0.1695 0.8022 0.039*
B2 0.9279 (8) 0.15162 (17) 0.8327 (6) 0.0342 (14)
H2 1.0248 0.1276 0.8725 0.041*
C4 0.7877 (8) 0.06395 (14) 0.6774 (5) 0.0423 (14)
H4A 0.9030 0.0783 0.7119 0.051*
B3 0.9813 (9) 0.19488 (18) 0.7612 (6) 0.0420 (16)
H3 1.1164 0.1997 0.7530 0.050*
B4 0.8264 (9) 0.16041 (18) 0.6591 (6) 0.0401 (16)
H4 0.8620 0.1431 0.5848 0.048*
B5 0.7755 (9) 0.21104 (18) 0.6369 (6) 0.0469 (18)
H5 0.7765 0.2270 0.5478 0.056*
C10 0.6616 (8) 0.16743 (16) 1.1476 (5) 0.0459 (15)
H10A 0.7314 0.1917 1.1744 0.055*
B6 0.6018 (9) 0.17690 (17) 0.6309 (6) 0.0371 (15)
H6 0.4882 0.1708 0.5381 0.044*
B7 0.7247 (9) 0.21373 (16) 0.8895 (6) 0.0379 (16)
H7 0.6898 0.2313 0.9636 0.045*
B8 0.9487 (9) 0.19743 (16) 0.9160 (6) 0.0370 (15)
H8 1.0633 0.2041 1.0077 0.044*
B9 0.6147 (10) 0.22145 (17) 0.7165 (6) 0.0440 (17)
H9 0.5083 0.2439 0.6792 0.053*
C11 0.4625 (8) 0.17704 (17) 1.0711 (6) 0.0542 (16)
H11A 0.3993 0.1537 1.0310 0.081*
H11B 0.4556 0.1958 1.0029 0.081*
H11C 0.4072 0.1877 1.1312 0.081*
C5 0.8260 (9) 0.02295 (16) 0.7408 (6) 0.0586 (18)
H5A 0.7171 0.0074 0.7089 0.088*
H5B 0.8637 0.0253 0.8359 0.088*
H5C 0.9209 0.0106 0.7169 0.088*
B10 0.8498 (9) 0.23347 (17) 0.7945 (6) 0.0426 (17)
H10 0.8978 0.2639 0.8068 0.051*
C12 0.6691 (9) 0.1440 (2) 1.2724 (5) 0.069 (2)
H12A 0.6220 0.1596 1.3277 0.104*
H12B 0.7932 0.1369 1.3213 0.104*
H12C 0.5968 0.1207 1.2460 0.104*
C6 0.2489 (8) 0.11169 (17) 0.6243 (6) 0.0529 (16)
H6A 0.1335 0.1040 0.5607 0.079*
H6B 0.2694 0.1389 0.6131 0.079*
H6C 0.2481 0.1073 0.7128 0.079*
C7 0.3449 (9) 0.04416 (17) 0.5935 (6) 0.0640 (19)
H7A 0.3260 0.0366 0.6742 0.096*
H7B 0.4397 0.0284 0.5813 0.096*
H7C 0.2340 0.0405 0.5193 0.096*
C8 0.7401 (9) 0.06209 (17) 0.5261 (6) 0.0611 (18)
H8A 0.8417 0.0517 0.5059 0.092*
H8B 0.7129 0.0879 0.4894 0.092*
H8C 0.6357 0.0455 0.4883 0.092*
C13 1.0984 (8) 0.16309 (17) 1.2634 (5) 0.0591 (18)
H13A 1.0457 0.1620 1.3324 0.089*
H13B 1.0736 0.1881 1.2202 0.089*
H13C 1.2278 0.1593 1.3018 0.089*
C15 0.7150 (8) −0.01747 (17) 1.0327 (6) 0.0467 (15)
C14 1.0478 (8) 0.09062 (17) 1.2272 (6) 0.0565 (17)
H14A 1.1762 0.0867 1.2715 0.085*
H14B 1.0012 0.0707 1.1608 0.085*
H14C 0.9864 0.0892 1.2910 0.085*

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Ag1 0.0537 (3) 0.0293 (2) 0.0454 (2) −0.0062 (2) 0.0139 (2) 0.0046 (2)
P1 0.0414 (9) 0.0266 (7) 0.0250 (7) −0.0005 (6) 0.0079 (6) 0.0023 (5)
P2 0.0384 (9) 0.0254 (7) 0.0320 (6) −0.0020 (6) 0.0060 (6) −0.0047 (6)
S1 0.0635 (12) 0.0317 (9) 0.1096 (14) 0.0047 (7) 0.0469 (11) 0.0074 (8)
C2 0.040 (3) 0.023 (3) 0.025 (3) 0.001 (2) 0.005 (2) 0.000 (2)
N1 0.051 (4) 0.039 (3) 0.093 (4) 0.003 (3) 0.015 (3) 0.023 (3)
C1 0.035 (3) 0.021 (3) 0.032 (3) −0.002 (2) 0.005 (2) 0.001 (2)
C3 0.044 (4) 0.039 (3) 0.042 (3) −0.006 (3) 0.005 (3) −0.009 (3)
C9 0.039 (3) 0.042 (3) 0.032 (3) −0.001 (3) 0.004 (3) 0.007 (2)
B1 0.037 (4) 0.032 (3) 0.025 (3) 0.005 (3) 0.006 (3) 0.002 (2)
B2 0.038 (4) 0.029 (3) 0.034 (3) 0.000 (3) 0.011 (3) −0.001 (3)
C4 0.050 (4) 0.030 (3) 0.045 (3) −0.001 (3) 0.014 (3) −0.010 (2)
B3 0.049 (4) 0.035 (4) 0.045 (4) 0.000 (3) 0.021 (3) 0.006 (3)
B4 0.047 (4) 0.043 (4) 0.030 (3) 0.002 (3) 0.012 (3) 0.005 (3)
B5 0.057 (5) 0.039 (4) 0.043 (4) −0.002 (3) 0.015 (3) 0.017 (3)
C10 0.060 (4) 0.039 (3) 0.036 (3) −0.002 (3) 0.014 (3) −0.004 (3)
B6 0.046 (4) 0.035 (3) 0.027 (3) 0.005 (3) 0.008 (3) 0.010 (3)
B7 0.054 (4) 0.016 (3) 0.034 (3) 0.007 (3) 0.003 (3) −0.001 (2)
B8 0.043 (4) 0.025 (3) 0.039 (4) −0.010 (3) 0.009 (3) 0.001 (3)
B9 0.056 (5) 0.026 (3) 0.044 (4) 0.004 (3) 0.011 (3) 0.009 (3)
C11 0.064 (4) 0.058 (4) 0.047 (4) 0.007 (3) 0.028 (3) −0.009 (3)
C5 0.064 (5) 0.038 (4) 0.069 (4) 0.010 (3) 0.017 (4) −0.006 (3)
B10 0.056 (5) 0.022 (3) 0.050 (4) −0.003 (3) 0.019 (4) 0.004 (3)
C12 0.088 (5) 0.088 (5) 0.034 (4) 0.016 (4) 0.025 (4) 0.006 (3)
C6 0.039 (4) 0.060 (4) 0.053 (4) −0.006 (3) 0.006 (3) −0.005 (3)
C7 0.056 (5) 0.058 (4) 0.066 (4) −0.017 (3) 0.006 (3) −0.021 (3)
C8 0.081 (5) 0.053 (4) 0.056 (4) −0.006 (3) 0.032 (4) −0.015 (3)
C13 0.057 (4) 0.058 (4) 0.045 (4) −0.017 (3) −0.005 (3) 0.001 (3)
C15 0.039 (4) 0.046 (4) 0.058 (4) 0.006 (3) 0.020 (3) 0.026 (3)
C14 0.059 (4) 0.055 (4) 0.044 (4) 0.006 (3) 0.004 (3) 0.017 (3)

Geometric parameters (Å, °)

Ag1—N1 2.251 (5) B4—H4 1.1000
Ag1—P1 2.4566 (14) B5—B10 1.759 (9)
Ag1—P2 2.4981 (14) B5—B6 1.775 (9)
Ag1—S1 2.5693 (17) B5—B9 1.778 (10)
P1—C10 1.853 (6) B5—H5 1.1000
P1—C1 1.866 (5) C10—C11 1.524 (8)
P1—C9 1.867 (5) C10—C12 1.541 (7)
P2—C3 1.847 (5) C10—H10A 0.9800
P2—C2 1.863 (5) B6—B9 1.763 (8)
P2—C4 1.868 (5) B6—H6 1.1000
S1—C15i 1.652 (6) B7—B8 1.763 (9)
C2—B4 1.682 (8) B7—B10 1.767 (9)
C2—B6 1.693 (7) B7—B9 1.771 (8)
C2—B1 1.717 (7) B7—H7 1.1000
C2—B2 1.723 (8) B8—B10 1.765 (8)
C2—C1 1.851 (6) B8—H8 1.1000
N1—C15 1.137 (7) B9—B10 1.784 (9)
C1—B7 1.678 (7) B9—H9 1.1000
C1—B8 1.689 (7) C11—H11A 0.9600
C1—B1 1.722 (7) C11—H11B 0.9600
C1—B2 1.725 (8) C11—H11C 0.9600
C3—C6 1.527 (7) C5—H5A 0.9600
C3—C7 1.543 (7) C5—H5B 0.9600
C3—H3A 0.9800 C5—H5C 0.9600
C9—C14 1.525 (7) B10—H10 1.1000
C9—C13 1.538 (7) C12—H12A 0.9600
C9—H9A 0.9800 C12—H12B 0.9600
B1—B6 1.786 (8) C12—H12C 0.9600
B1—B9 1.786 (8) C6—H6A 0.9600
B1—B7 1.796 (8) C6—H6B 0.9600
B1—H1 1.1000 C6—H6C 0.9600
B2—B4 1.775 (8) C7—H7A 0.9600
B2—B3 1.780 (8) C7—H7B 0.9600
B2—B8 1.783 (8) C7—H7C 0.9600
B2—H2 1.1000 C8—H8A 0.9600
C4—C8 1.531 (7) C8—H8B 0.9600
C4—C5 1.542 (7) C8—H8C 0.9600
C4—H4A 0.9800 C13—H13A 0.9600
B3—B8 1.761 (9) C13—H13B 0.9600
B3—B4 1.772 (9) C13—H13C 0.9600
B3—B10 1.782 (9) C15—S1i 1.652 (6)
B3—B5 1.785 (9) C14—H14A 0.9600
B3—H3 1.1000 C14—H14B 0.9600
B4—B6 1.767 (9) C14—H14C 0.9600
B4—B5 1.775 (9)
N1—Ag1—P1 122.90 (14) B9—B5—B3 108.0 (4)
N1—Ag1—P2 114.03 (15) B10—B5—H5 121.0
P1—Ag1—P2 90.97 (4) B4—B5—H5 122.2
N1—Ag1—S1 97.27 (14) B6—B5—H5 121.9
P1—Ag1—S1 116.70 (5) B9—B5—H5 122.0
P2—Ag1—S1 116.60 (6) B3—B5—H5 121.8
C10—P1—C1 105.9 (2) C11—C10—C12 107.8 (5)
C10—P1—C9 107.1 (3) C11—C10—P1 114.1 (4)
C1—P1—C9 103.6 (2) C12—C10—P1 105.9 (4)
C10—P1—Ag1 116.2 (2) C11—C10—H10A 109.6
C1—P1—Ag1 107.57 (15) C12—C10—H10A 109.6
C9—P1—Ag1 115.41 (17) P1—C10—H10A 109.6
C3—P2—C2 106.9 (2) C2—B6—B9 107.3 (4)
C3—P2—C4 105.6 (2) C2—B6—B4 58.1 (3)
C2—P2—C4 102.9 (2) B9—B6—B4 108.1 (5)
C3—P2—Ag1 114.4 (2) C2—B6—B5 106.3 (4)
C2—P2—Ag1 106.46 (15) B9—B6—B5 60.4 (4)
C4—P2—Ag1 119.45 (17) B4—B6—B5 60.2 (4)
C15i—S1—Ag1 97.4 (2) C2—B6—B1 59.1 (3)
B4—C2—B6 63.1 (3) B9—B6—B1 60.4 (3)
B4—C2—B1 113.2 (4) B4—B6—B1 106.0 (4)
B6—C2—B1 63.1 (3) B5—B6—B1 107.7 (4)
B4—C2—B2 62.9 (3) C2—B6—H6 123.3
B6—C2—B2 113.0 (4) B9—B6—H6 121.1
B1—C2—B2 107.9 (4) B4—B6—H6 122.6
B4—C2—C1 107.6 (4) B5—B6—H6 121.8
B6—C2—C1 107.6 (3) B1—B6—H6 122.4
B1—C2—C1 57.6 (3) C1—B7—B8 58.7 (3)
B2—C2—C1 57.6 (3) C1—B7—B10 106.7 (4)
B4—C2—P2 124.9 (4) B8—B7—B10 60.0 (4)
B6—C2—P2 124.9 (3) C1—B7—B9 107.4 (4)
B1—C2—P2 117.3 (4) B8—B7—B9 108.3 (5)
B2—C2—P2 117.4 (3) B10—B7—B9 60.5 (4)
C1—C2—P2 117.0 (3) C1—B7—B1 59.3 (3)
C15—N1—Ag1 150.0 (5) B8—B7—B1 106.6 (4)
B7—C1—B8 63.2 (3) B10—B7—B1 107.7 (4)
B7—C1—B1 63.8 (3) B9—B7—B1 60.1 (3)
B8—C1—B1 113.6 (4) C1—B7—H7 122.9
B7—C1—B2 113.1 (4) B8—B7—H7 122.3
B8—C1—B2 62.9 (3) B10—B7—H7 121.8
B1—C1—B2 107.6 (4) B9—B7—H7 121.2
B7—C1—C2 108.1 (3) B1—B7—H7 122.3
B8—C1—C2 107.8 (4) C1—B8—B7 58.1 (3)
B1—C1—C2 57.3 (3) C1—B8—B3 107.8 (4)
B2—C1—C2 57.5 (3) B7—B8—B3 108.7 (4)
B7—C1—P1 124.8 (4) C1—B8—B10 106.3 (4)
B8—C1—P1 125.1 (3) B7—B8—B10 60.1 (4)
B1—C1—P1 116.9 (3) B3—B8—B10 60.7 (3)
B2—C1—P1 117.5 (3) C1—B8—B2 59.5 (3)
C2—C1—P1 116.6 (3) B7—B8—B2 106.4 (4)
C6—C3—C7 108.1 (5) B3—B8—B2 60.3 (3)
C6—C3—P2 114.7 (4) B10—B8—B2 107.7 (4)
C7—C3—P2 105.8 (4) C1—B8—H8 123.1
C6—C3—H3A 109.4 B7—B8—H8 122.4
C7—C3—H3A 109.4 B3—B8—H8 120.8
P2—C3—H3A 109.4 B10—B8—H8 121.9
C14—C9—C13 110.7 (4) B2—B8—H8 122.2
C14—C9—P1 110.1 (4) B6—B9—B7 109.5 (4)
C13—C9—P1 117.1 (4) B6—B9—B5 60.1 (4)
C14—C9—H9A 106.0 B7—B9—B5 107.5 (5)
C13—C9—H9A 106.0 B6—B9—B10 108.0 (5)
P1—C9—H9A 106.0 B7—B9—B10 59.6 (4)
C2—B1—C1 65.1 (3) B5—B9—B10 59.2 (4)
C2—B1—B6 57.8 (3) B6—B9—B1 60.4 (3)
C1—B1—B6 109.4 (4) B7—B9—B1 60.7 (3)
C2—B1—B9 105.3 (4) B5—B9—B1 107.5 (4)
C1—B1—B9 104.9 (4) B10—B9—B1 107.5 (4)
B6—B1—B9 59.2 (3) B6—B9—H9 120.9
C2—B1—B7 108.9 (4) B7—B9—H9 121.2
C1—B1—B7 56.9 (3) B5—B9—H9 122.4
B6—B1—B7 107.4 (4) B10—B9—H9 122.4
B9—B1—B7 59.3 (3) B1—B9—H9 121.7
C2—B1—H1 120.8 C10—C11—H11A 109.5
C1—B1—H1 121.1 C10—C11—H11B 109.5
B6—B1—H1 122.1 H11A—C11—H11B 109.5
B9—B1—H1 124.3 C10—C11—H11C 109.5
B7—B1—H1 122.6 H11A—C11—H11C 109.5
C2—B2—C1 65.0 (3) H11B—C11—H11C 109.5
C2—B2—B4 57.4 (3) C4—C5—H5A 109.5
C1—B2—B4 109.1 (4) C4—C5—H5B 109.5
C2—B2—B3 105.8 (4) H5A—C5—H5B 109.5
C1—B2—B3 105.4 (4) C4—C5—H5C 109.5
B4—B2—B3 59.8 (3) H5A—C5—H5C 109.5
C2—B2—B8 109.4 (4) H5B—C5—H5C 109.5
C1—B2—B8 57.6 (3) B8—B10—B5 108.5 (4)
B4—B2—B8 107.7 (4) B8—B10—B7 59.9 (3)
B3—B2—B8 59.2 (3) B5—B10—B7 108.6 (4)
C2—B2—H2 120.8 B8—B10—B3 59.5 (3)
C1—B2—H2 121.1 B5—B10—B3 60.5 (4)
B4—B2—H2 122.1 B7—B10—B3 107.5 (4)
B3—B2—H2 123.9 B8—B10—B9 107.6 (4)
B8—B2—H2 122.2 B5—B10—B9 60.3 (4)
C8—C4—C5 111.5 (4) B7—B10—B9 59.8 (3)
C8—C4—P2 116.4 (4) B3—B10—B9 107.9 (4)
C5—C4—P2 110.0 (4) B8—B10—H10 121.9
C8—C4—H4A 106.1 B5—B10—H10 121.0
C5—C4—H4A 106.1 B7—B10—H10 121.8
P2—C4—H4A 106.1 B3—B10—H10 122.0
B8—B3—B4 108.9 (4) B9—B10—H10 121.9
B8—B3—B2 60.5 (3) C10—C12—H12A 109.5
B4—B3—B2 60.0 (3) C10—C12—H12B 109.5
B8—B3—B10 59.8 (3) H12A—C12—H12B 109.5
B4—B3—B10 107.3 (5) C10—C12—H12C 109.5
B2—B3—B10 107.1 (4) H12A—C12—H12C 109.5
B8—B3—B5 107.5 (5) H12B—C12—H12C 109.5
B4—B3—B5 59.9 (4) C3—C6—H6A 109.5
B2—B3—B5 107.1 (5) C3—C6—H6B 109.5
B10—B3—B5 59.1 (4) H6A—C6—H6B 109.5
B8—B3—H3 121.2 C3—C6—H6C 109.5
B4—B3—H3 121.4 H6A—C6—H6C 109.5
B2—B3—H3 122.1 H6B—C6—H6C 109.5
B10—B3—H3 122.6 C3—C7—H7A 109.5
B5—B3—H3 122.5 C3—C7—H7B 109.5
C2—B4—B6 58.8 (3) H7A—C7—H7B 109.5
C2—B4—B3 108.0 (4) C3—C7—H7C 109.5
B6—B4—B3 108.7 (5) H7A—C7—H7C 109.5
C2—B4—B5 106.8 (4) H7B—C7—H7C 109.5
B6—B4—B5 60.1 (4) C4—C8—H8A 109.5
B3—B4—B5 60.4 (4) C4—C8—H8B 109.5
C2—B4—B2 59.7 (3) H8A—C8—H8B 109.5
B6—B4—B2 107.1 (4) C4—C8—H8C 109.5
B3—B4—B2 60.2 (3) H8A—C8—H8C 109.5
B5—B4—B2 107.7 (4) H8B—C8—H8C 109.5
C2—B4—H4 122.6 C9—C13—H13A 109.5
B6—B4—H4 122.0 C9—C13—H13B 109.5
B3—B4—H4 121.0 H13A—C13—H13B 109.5
B5—B4—H4 121.9 C9—C13—H13C 109.5
B2—B4—H4 122.1 H13A—C13—H13C 109.5
B10—B5—B4 108.2 (4) H13B—C13—H13C 109.5
B10—B5—B6 108.6 (5) N1—C15—S1i 178.8 (6)
B4—B5—B6 59.7 (3) C9—C14—H14A 109.5
B10—B5—B9 60.6 (4) C9—C14—H14B 109.5
B4—B5—B9 107.1 (4) H14A—C14—H14B 109.5
B6—B5—B9 59.5 (4) C9—C14—H14C 109.5
B10—B5—B3 60.4 (4) H14A—C14—H14C 109.5
B4—B5—B3 59.7 (3) H14B—C14—H14C 109.5
B6—B5—B3 107.7 (4)
N1—Ag1—P1—C10 −111.6 (3) Ag1—P2—C2—C1 8.3 (3)
P2—Ag1—P1—C10 128.6 (2) P1—Ag1—N1—C15 −172.8 (9)
S1—Ag1—P1—C10 8.0 (2) P2—Ag1—N1—C15 −64.7 (10)
N1—Ag1—P1—C1 130.0 (2) S1—Ag1—N1—C15 58.7 (10)
P2—Ag1—P1—C1 10.24 (17) P2—C2—C1—P1 −0.4 (5)
S1—Ag1—P1—C1 −110.41 (18) C10—P1—C1—C2 −132.8 (3)
N1—Ag1—P1—C9 15.0 (3) C9—P1—C1—C2 114.7 (3)
P2—Ag1—P1—C9 −104.8 (2) Ag1—P1—C1—C2 −7.9 (4)
S1—Ag1—P1—C9 134.6 (2) C2—P2—C3—C6 −64.1 (5)
N1—Ag1—P2—C3 104.8 (2) C4—P2—C3—C6 −173.2 (4)
P1—Ag1—P2—C3 −128.15 (19) Ag1—P2—C3—C6 53.4 (5)
S1—Ag1—P2—C3 −7.42 (19) C2—P2—C3—C7 176.9 (4)
N1—Ag1—P2—C2 −137.4 (2) C4—P2—C3—C7 67.8 (4)
P1—Ag1—P2—C2 −10.35 (17) Ag1—P2—C3—C7 −65.6 (4)
S1—Ag1—P2—C2 110.38 (17) C10—P1—C9—C14 103.2 (4)
N1—Ag1—P2—C4 −21.7 (3) C1—P1—C9—C14 −145.2 (4)
P1—Ag1—P2—C4 105.3 (2) Ag1—P1—C9—C14 −28.0 (4)
S1—Ag1—P2—C4 −133.9 (2) C10—P1—C9—C13 −24.5 (5)
C3—P2—C2—B4 −88.9 (4) C1—P1—C9—C13 87.1 (4)
C4—P2—C2—B4 22.0 (5) Ag1—P1—C9—C13 −155.7 (4)
Ag1—P2—C2—B4 148.4 (4) C3—P2—C4—C8 25.7 (5)
C3—P2—C2—B6 −9.6 (5) C2—P2—C4—C8 −86.2 (4)
C4—P2—C2—B6 101.4 (4) Ag1—P2—C4—C8 156.3 (3)
Ag1—P2—C2—B6 −132.2 (4) C3—P2—C4—C5 −102.3 (4)
C3—P2—C2—B1 65.4 (4) C2—P2—C4—C5 145.8 (4)
C4—P2—C2—B1 176.3 (3) Ag1—P2—C4—C5 28.3 (4)
Ag1—P2—C2—B1 −57.3 (3) C1—P1—C10—C11 66.3 (5)
C3—P2—C2—B2 −163.5 (4) C9—P1—C10—C11 176.3 (4)
C4—P2—C2—B2 −52.6 (4) Ag1—P1—C10—C11 −53.0 (4)
Ag1—P2—C2—B2 73.8 (4) C1—P1—C10—C12 −175.3 (4)
C3—P2—C2—C1 130.9 (3) C9—P1—C10—C12 −65.3 (4)
C4—P2—C2—C1 −118.1 (3) Ag1—P1—C10—C12 65.4 (4)

Symmetry codes: (i) −x+1, −y, −z+2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: GK2319).

References

  1. Kivekäs, R., Sillanpää, R., Teixidor, F., Viñas, C., Nuñez, R. & Abad, M. (1995). Acta Cryst. C51, 1864–1868.
  2. Paavola, S., Kivekäs, R., Teixidor, F. & Vinas, C. (2002). J. Organomet. Chem. 606, 183–187.
  3. Paavola, S., Teixidor, F., Viñas, C. & Kivekäs, R. (2002a). Acta Cryst. C58, m237–m239. [DOI] [PubMed]
  4. Paavola, S., Teixidor, F., Vinas, C. & Kivekas, R. (2002b). J. Organomet. Chem. 645, 39–46.
  5. Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  6. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]
  7. Siemens (1996). SMART and SAINT Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
  8. Zhang, D.-P., Dou, J.-M., Li, D.-C. & Wang, D.-Q. (2006). Acta Cryst. E62, o418–o419.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810049263/gk2319sup1.cif

e-67-000m2-sup1.cif (27KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810049263/gk2319Isup2.hkl

e-67-000m2-Isup2.hkl (230.9KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


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