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Each of the title compounds, 8-methoxy-7,7-bis­(tri­phenyl­phosphine-P)-8,9:10,11-di-μH-7-platina-nido-undecaborane di­chloro­methane hemisolvate, [Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2, (I), 8-isopropoxy-7,7-bis­(tri­phenyl­phosphine-P)-8,9:10,11-di-μH-7-platina-nido-undecaborane di­chloro­methane solvate, [Pt(C3H18B10O)(C18H15P)2]·CH2Cl2, (II), and 9-isopropoxy-7,7-bis­(tri­phenyl­phosphine-P)-8,9:10,11-di-μH-7-platina-nido-undecaborane di­chloro­methane solvate, [Pt(C3H18B10O)(C18H15P)2]·CH2Cl2, (III), has an 11-vertex nido polyhedral skeleton, with the 7-platinum centre ligating to two exo-polyhedral PPh3 groups and an alkoxy-substituted polyhedral borane ligand. Compounds (II) and (III) are isomers. The Pt—B distances are in the range 2.214 (7)–2.303 (7) Å for (I), 2.178 (16)–2.326 (16) Å for (II) and 2.205 (6)–2.327 (6) Å for (III).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101007788/gd1151sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151IIIsup4.hkl
Contains datablock III

CCDC references: 170165; 170166; 170167

Comment top

The polyhedral borane dianion, B10H102-, has been extensively studied due to its extreme thermal, hydrolytic, and oxidative stability (Mutterties & Knoth, 1968; Kennedy, 1986; Barton & Srivastava, 1995). Although a number of metal derivatives have been prepared, little work has been reported on the cage-opening mechanism. Marshall et al. (1967) postulated the cage opening of B10H102- in the anhydrous HCl/diethyl sulfide system as occurring via a two-proton attack process on two pairs of apex-to-equatorial B atoms. Paxson & Hawthorne (1975) studied the reaction of PtCl2(PPh3)2 and K2B10H10 in alcoholic chloroform, and obtained the alkoxy-substituted nido-[(PPh3)2PtB10H11(OC2H5)]; spectroscopic studies showed that the ethoxy group could be at various positions (i.e. 2, 3, 8, 9, 10 or 11). Gaft et al. (1983) found that the hydrogen-bridged compound [(PPh3)2PtB10H10], derived from the reaction of PtI2(PPh3)2 and Ag2B10H10 in CH3CN/CH2Cl2, could also be transformed in C2H5OH into nido-[(PPh3)2PtB10H11(OC2H5)], so that [(PPh3)2PtB10H10] could be the intermediate of the reaction system containing B10H102- and a platinum halide. However, none of these intermediates or their ultimate products have been structurally characterized. To extend the study of the cage-opening mode and the substituent effect on the cluster geometry, we have carried out the same reaction in methanol and iso-propyl alcohol, and here we report the structures of the three title platinaboranes, (I), (II) and (III). \sch

As expected, in compounds (I)-(III) the 11-vertex nido clusters are produced, the methoxy group is found to be on atom B8 in (I), and the isopropoxy groups are on atom B8 in (II) and atom B9 in (III). The intramolecular distances and angles, and even the orientations of the PPh3 ligands, are essentially the same in (I)-(III). The Pt—B distances vary in the ranges 2.214 (7)–2.303 (7) Å in (I), 2.178 (16)–2.326 (16) Å in (II), and 2.205 (6)–2.327 (6) Å in (III), which are similar to but slightly longer than those of the unsubstituted cluster [(PMe2Ph)2PtB10H12] [2.214 (5)–2.301 (6) Å; Boocock et al., 1981], probably as another consequence of the presence of the alkoxy groups. With regard to the B—O bond lengths, the present values are both close to each other and in the range of those reported for cage-B—OR groups (1.371–1.409 Å; Kennedy, 1986).

The present three structures, along with the related examples described above, suggest that the reaction of PtX2(PR3)2 in alcohols is so complex that alcohols could attack on the (opened) cage intermediates from different positions. It should be noted that a number of the 1,2-bis(diphenylphosphinoethane) and PMe2Ph relatives of the title compounds have been prepared, namely, the mono-substituted 8-OR or 9-OR compounds (R is Me or Et), but these, unfortunately, have not been structurally characterized (Kennedy, 1986).

Related literature top

For related literature, see: Barton & Srivastava (1995); Boocock et al. (1981); Gaft et al. (1983); Kennedy (1986); Marshall et al. (1967); Mutterties & Knoth (1968); Paxson & Hawthorne (1975).

Experimental top

The synthesis of compound (I) was effected by the reaction of [RuCl2(PPh3)3] (0.38 g, 0.4 mmol), [PtCl2(PPh3)2] (0.32 g, 0.4 mmol) and (NEt4)2B10H10 (0.16 g, 0.4 mmol) in refluxing methanol (65 ml) for 68 h under dry nitrogen. The resulting mixture was filtered. The yellowish precipitate was dissolved in the minimum of dichloromethane and chromatographed using dichloromethane/light petroleum (b.p. 303–333 K) (4:1) as the eluting medium to give compound (I) (Rf = 0.72). Compounds (II) and (III) were synthesized by the reaction of [PtCl2(PPh3)2] (0.284 g, 0.35 mmol) and (NEt4)2B10H10 (0.265 g, 0.7 mmol) with i-PrOH under reflux for 132 h in an atmosphere of dry nitrogen. After filtration, the resulting solution was reduced in volume and chromatographed using dichloromethane/light petrolem (4:1) as the eluting medium to give the two compounds at Rf = 0.83 for (II) and Rf = 0.45 for (III). All three products were recrystallized from n-hexane-dichloromethane solution.

Refinement top

H atoms, other than the B—H—B bridging atoms, were treated as riding, with B—H(general), CH(phenyl), C—H(—CH), C—H(—CH2) and C—H(—CH3) distances of 1.10, 0.93, 0.98, 0.97 and 0.96 Å, respectively. In all three compounds, the bridging H atoms were refined isotropically.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992) for (I), (III); CAD-4 Manual (Enraf-Nonius, 1988) for (II). Cell refinement: MSC/AFC Diffractometer Control Software for (I), (III); CAD-4 Manual for (II). Data reduction: TEXSAN (Molecular Structure Corporation, 1985) for (I), (III); SDP-Plus (Frenz, 1985) for (II). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ZORTEP (Zsolnai, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) with the atom-numbering scheme and 30% probability displacement ellipsoids. Borane H atoms are shown as small spheres of arbitrary radii; the remainder have been omitted for clarity.
[Figure 2] Fig. 2. The molecular structure of (II) with the atom-numbering scheme and 30% probability displacement ellipsoids. Borane H atoms are shown as small spheres of arbitrary radii; the remainder have been omitted for clarity.
[Figure 3] Fig. 3. The molecular structure of (III) with the atom-numbering scheme and 30% probability displacement ellipsoids. Borane H atoms are shown as small spheres of arbitrary radii; the remainder have been omitted for clarity.
(I) 8-methoxy-7,7-bis(triphenylphosphorine-P)- 8,9:10,11-di-µ-H-7-platina-nido-undecaborane dichloromethane hemisolvate top
Crystal data top
[Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2F(000) = 1812
Mr = 912.32Dx = 1.426 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
a = 12.850 (2) ÅCell parameters from 25 reflections
b = 25.824 (7) Åθ = 6.8–10.8°
c = 13.308 (2) ŵ = 3.47 mm1
β = 105.77 (1)°T = 293 K
V = 4249.9 (15) Å3Prism, yellow
Z = 40.3 × 0.2 × 0.2 mm
Data collection top
Rigaku AFC-7R
diffractometer
5607 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.048
Graphite monochromatorθmax = 25°, θmin = 2.3°
θ/2θ scansh = 013
Absorption correction: ψ scans
(North et al., 1968)
k = 030
Tmin = 0.423, Tmax = 0.544l = 1515
7336 measured reflections3 standard reflections every 200 reflections
6984 independent reflections intensity decay: 1.3
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0601P)2 + 4.5436P]
where P = (Fo2 + 2Fc2)/3
6984 reflections(Δ/σ)max = 0.030
495 parametersΔρmax = 1.98 e Å3
2 restraintsΔρmin = 1.71 e Å3
Crystal data top
[Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2V = 4249.9 (15) Å3
Mr = 912.32Z = 4
Monoclinic, P21/nMo Kα radiation
a = 12.850 (2) ŵ = 3.47 mm1
b = 25.824 (7) ÅT = 293 K
c = 13.308 (2) Å0.3 × 0.2 × 0.2 mm
β = 105.77 (1)°
Data collection top
Rigaku AFC-7R
diffractometer
5607 reflections with I > 2σ(I)
Absorption correction: ψ scans
(North et al., 1968)
Rint = 0.048
Tmin = 0.423, Tmax = 0.5443 standard reflections every 200 reflections
7336 measured reflections intensity decay: 1.3
6984 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0372 restraints
wR(F2) = 0.105H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 1.98 e Å3
6984 reflectionsΔρmin = 1.71 e Å3
495 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*/UeqOcc. (<1)
Pt70.699111 (18)0.192397 (8)0.859548 (16)0.02893 (10)
P10.77647 (13)0.14883 (6)0.73977 (12)0.0335 (3)
P20.61525 (14)0.12207 (6)0.91964 (13)0.0369 (4)
O10.4562 (4)0.21328 (18)0.8252 (3)0.0437 (11)
C10.3641 (6)0.2219 (3)0.7389 (6)0.059 (2)
H1A0.30930.19680.74010.089*
H1B0.38450.21870.67500.089*
H1C0.33640.25610.74360.089*
C110.7424 (5)0.1844 (2)0.6165 (5)0.0354 (14)
C120.6346 (6)0.1948 (2)0.5681 (6)0.0462 (16)
H120.58260.18680.60250.055*
C130.6030 (6)0.2167 (3)0.4704 (6)0.0541 (18)
H130.53000.22230.43850.065*
C140.6789 (7)0.2303 (3)0.4199 (6)0.061 (2)
H140.65750.24410.35290.073*
C150.7870 (6)0.2234 (3)0.4692 (6)0.060 (2)
H150.83890.23410.43670.072*
C160.8187 (6)0.2007 (3)0.5662 (6)0.0495 (17)
H160.89190.19620.59870.059*
C210.7404 (5)0.0820 (2)0.6954 (5)0.0386 (14)
C220.6695 (6)0.0703 (3)0.5996 (6)0.0526 (18)
H220.63720.09710.55540.063*
C230.6456 (7)0.0199 (3)0.5683 (7)0.069 (2)
H230.59570.01260.50490.082*
C240.6967 (8)0.0194 (3)0.6322 (8)0.080 (3)
H240.68180.05350.61130.096*
C250.7696 (8)0.0091 (3)0.7265 (7)0.069 (2)
H250.80420.03600.76920.083*
C260.7905 (6)0.0415 (3)0.7568 (6)0.0519 (18)
H260.84000.04860.82060.062*
C310.9225 (5)0.1433 (2)0.7838 (5)0.0394 (14)
C320.9807 (6)0.1205 (3)0.7199 (6)0.0540 (18)
H320.94440.10940.65310.065*
C331.0912 (6)0.1147 (3)0.7553 (7)0.065 (2)
H331.12900.10030.71160.079*
C341.1455 (6)0.1296 (3)0.8532 (8)0.066 (2)
H341.22020.12550.87600.079*
C351.0910 (6)0.1506 (3)0.9189 (7)0.060 (2)
H351.12820.15980.98670.072*
C360.9799 (6)0.1580 (3)0.8836 (5)0.0477 (17)
H360.94350.17320.92770.057*
C410.5037 (5)0.0890 (2)0.8277 (5)0.0394 (15)
C420.4790 (6)0.1019 (3)0.7232 (5)0.0468 (16)
H420.51980.12690.70110.056*
C430.3953 (6)0.0784 (3)0.6515 (6)0.061 (2)
H430.37930.08750.58140.073*
C440.3350 (7)0.0410 (4)0.6842 (8)0.075 (3)
H440.27910.02450.63550.090*
C450.3568 (8)0.0280 (3)0.7882 (8)0.078 (3)
H450.31570.00290.80980.094*
C460.4394 (7)0.0523 (3)0.8594 (6)0.062 (2)
H460.45300.04420.92980.075*
C510.7207 (6)0.0737 (3)0.9696 (6)0.0510 (18)
C520.7031 (7)0.0204 (3)0.9567 (7)0.066 (2)
H520.63520.00840.92000.079*
C530.7825 (10)0.0139 (4)0.9965 (9)0.092 (3)
H530.76960.04920.98620.110*
C540.8817 (10)0.0032 (5)1.0516 (9)0.104 (4)
H540.93610.02061.07940.124*
C550.9033 (8)0.0565 (4)1.0673 (8)0.090 (3)
H550.97140.06781.10490.108*
C560.8218 (6)0.0915 (3)1.0259 (6)0.063 (2)
H560.83440.12691.03570.075*
C610.5635 (5)0.1319 (2)1.0338 (5)0.0403 (15)
C620.6251 (8)0.1209 (4)1.1329 (6)0.089 (3)
H620.69540.10871.14370.106*
C630.5821 (10)0.1280 (5)1.2176 (7)0.114 (5)
H630.62440.12111.28490.137*
C640.4778 (9)0.1452 (4)1.2023 (7)0.095 (3)
H640.44880.14841.25880.114*
C650.4182 (8)0.1571 (4)1.1066 (7)0.077 (3)
H650.34830.16971.09660.093*
C660.4603 (6)0.1508 (3)1.0220 (6)0.058 (2)
H660.41800.15940.95560.070*
B10.7087 (7)0.3118 (3)0.9745 (7)0.0449 (18)
H10.73210.33221.04990.054*
B20.7851 (6)0.2598 (3)0.9467 (6)0.0383 (16)
H20.85780.24651.00580.046*
B30.6514 (6)0.2491 (3)0.9658 (5)0.0374 (16)
H30.64010.22951.03550.045*
B40.5714 (7)0.3031 (3)0.9086 (6)0.0429 (18)
H40.50790.31860.94130.052*
B50.6523 (7)0.3427 (3)0.8528 (6)0.0454 (19)
H50.63690.38460.84710.054*
B60.7867 (7)0.3196 (3)0.8829 (6)0.0417 (17)
H60.85790.34510.90030.050*
B80.5483 (6)0.2432 (3)0.8437 (5)0.0368 (16)
B90.5557 (7)0.3046 (3)0.7697 (6)0.0434 (18)
H90.49190.30720.69560.052*
B100.6993 (7)0.3158 (3)0.7552 (6)0.0434 (18)
H100.70100.32420.67460.052*
B110.7897 (6)0.2613 (3)0.8132 (6)0.0369 (16)
H110.83600.24560.76180.044*
H1U0.569 (5)0.261 (3)0.750 (5)0.053 (19)*
H2U0.718 (4)0.266 (2)0.741 (4)0.029 (15)*
Cl20.8352 (7)0.0758 (3)0.4255 (8)0.175 (4)0.50
Cl10.9635 (8)0.0140 (3)0.3448 (8)0.167 (4)0.50
C1S0.9467 (17)0.0601 (9)0.411 (3)0.170 (16)0.50
H1S0.97410.09030.38300.204*0.50
H2S0.99420.05460.48040.204*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt70.03273 (16)0.02862 (13)0.02808 (13)0.00030 (10)0.01277 (9)0.00093 (9)
P10.0356 (9)0.0338 (8)0.0339 (8)0.0007 (7)0.0142 (7)0.0043 (6)
P20.0452 (10)0.0334 (8)0.0369 (8)0.0015 (7)0.0193 (7)0.0039 (6)
O10.039 (3)0.050 (3)0.044 (3)0.009 (2)0.016 (2)0.003 (2)
C10.046 (5)0.082 (6)0.048 (4)0.009 (4)0.010 (3)0.003 (4)
C110.040 (4)0.036 (3)0.035 (3)0.001 (3)0.018 (3)0.000 (2)
C120.041 (4)0.050 (4)0.053 (4)0.003 (3)0.024 (3)0.007 (3)
C130.049 (4)0.058 (4)0.055 (4)0.006 (4)0.012 (3)0.009 (4)
C140.072 (6)0.065 (5)0.049 (4)0.009 (4)0.023 (4)0.015 (4)
C150.058 (5)0.071 (5)0.061 (5)0.004 (4)0.035 (4)0.020 (4)
C160.043 (4)0.061 (4)0.050 (4)0.002 (3)0.021 (3)0.004 (3)
C210.041 (4)0.035 (3)0.044 (3)0.004 (3)0.019 (3)0.012 (3)
C220.054 (5)0.041 (4)0.057 (4)0.002 (3)0.006 (3)0.009 (3)
C230.064 (5)0.061 (5)0.073 (6)0.009 (4)0.007 (4)0.025 (4)
C240.106 (8)0.046 (5)0.095 (7)0.008 (5)0.039 (6)0.027 (5)
C250.093 (7)0.047 (4)0.073 (6)0.008 (4)0.031 (5)0.005 (4)
C260.070 (5)0.041 (4)0.049 (4)0.003 (3)0.023 (4)0.009 (3)
C310.042 (4)0.034 (3)0.045 (4)0.004 (3)0.016 (3)0.001 (3)
C320.046 (4)0.058 (4)0.059 (5)0.001 (3)0.015 (3)0.016 (4)
C330.044 (5)0.065 (5)0.097 (7)0.011 (4)0.034 (5)0.002 (5)
C340.034 (4)0.058 (5)0.102 (7)0.002 (4)0.014 (4)0.008 (5)
C350.045 (5)0.053 (4)0.071 (5)0.003 (4)0.005 (4)0.004 (4)
C360.052 (5)0.042 (4)0.047 (4)0.000 (3)0.010 (3)0.001 (3)
C410.044 (4)0.033 (3)0.049 (4)0.005 (3)0.024 (3)0.003 (3)
C420.051 (4)0.046 (4)0.046 (4)0.009 (3)0.018 (3)0.002 (3)
C430.067 (5)0.060 (5)0.057 (5)0.008 (4)0.020 (4)0.013 (4)
C440.066 (6)0.074 (6)0.084 (6)0.018 (5)0.017 (5)0.031 (5)
C450.076 (6)0.067 (6)0.098 (7)0.037 (5)0.034 (5)0.012 (5)
C460.076 (6)0.057 (5)0.062 (5)0.022 (4)0.032 (4)0.003 (4)
C510.062 (5)0.053 (4)0.050 (4)0.018 (4)0.035 (4)0.017 (3)
C520.077 (6)0.045 (4)0.091 (6)0.020 (4)0.048 (5)0.018 (4)
C530.110 (9)0.068 (6)0.121 (9)0.040 (6)0.071 (8)0.038 (6)
C540.108 (9)0.102 (8)0.119 (9)0.065 (8)0.062 (8)0.073 (7)
C550.062 (6)0.128 (9)0.088 (7)0.044 (6)0.032 (5)0.048 (6)
C560.061 (5)0.073 (5)0.058 (5)0.018 (4)0.023 (4)0.019 (4)
C610.054 (4)0.033 (3)0.040 (3)0.004 (3)0.023 (3)0.002 (3)
C620.090 (7)0.136 (9)0.044 (5)0.055 (6)0.024 (5)0.014 (5)
C630.135 (10)0.176 (12)0.039 (5)0.070 (9)0.039 (6)0.011 (6)
C640.113 (9)0.127 (9)0.064 (6)0.042 (7)0.057 (6)0.022 (6)
C650.075 (6)0.101 (7)0.074 (6)0.016 (5)0.049 (5)0.021 (5)
C660.054 (5)0.077 (5)0.051 (4)0.009 (4)0.029 (4)0.013 (4)
B10.045 (5)0.038 (4)0.054 (5)0.001 (3)0.016 (4)0.012 (3)
B20.043 (4)0.035 (4)0.040 (4)0.004 (3)0.016 (3)0.005 (3)
B30.046 (5)0.035 (4)0.035 (4)0.003 (3)0.017 (3)0.002 (3)
B40.045 (5)0.039 (4)0.048 (4)0.001 (3)0.020 (4)0.009 (3)
B50.058 (5)0.030 (4)0.055 (5)0.001 (3)0.026 (4)0.000 (3)
B60.044 (5)0.037 (4)0.047 (4)0.004 (3)0.017 (4)0.002 (3)
B80.040 (4)0.041 (4)0.032 (3)0.004 (3)0.013 (3)0.004 (3)
B90.049 (5)0.037 (4)0.047 (4)0.003 (3)0.016 (4)0.007 (3)
B100.051 (5)0.040 (4)0.042 (4)0.001 (3)0.016 (4)0.006 (3)
B110.041 (4)0.036 (4)0.035 (4)0.007 (3)0.013 (3)0.003 (3)
Cl20.141 (7)0.136 (6)0.242 (11)0.038 (5)0.041 (7)0.085 (7)
Cl10.183 (9)0.137 (7)0.213 (10)0.006 (6)0.107 (8)0.025 (6)
C1S0.16 (3)0.12 (2)0.29 (4)0.089 (19)0.17 (3)0.12 (2)
Geometric parameters (Å, º) top
Pt7—B22.214 (7)C51—C561.390 (11)
Pt7—B32.234 (7)C51—C521.397 (11)
Pt7—B112.301 (7)C52—C531.346 (12)
Pt7—B82.303 (7)C52—H520.9300
Pt7—P22.3595 (16)C53—C541.360 (15)
Pt7—P12.3783 (15)C53—H530.9300
P1—C311.813 (7)C54—C551.407 (16)
P1—C111.827 (6)C54—H540.9300
P1—C211.842 (6)C55—C561.381 (11)
P2—C411.824 (7)C55—H550.9300
P2—C511.831 (7)C56—H560.9300
P2—C611.834 (6)C61—C621.371 (10)
O1—B81.379 (9)C61—C661.382 (10)
O1—C11.425 (8)C62—C631.396 (11)
C1—H1A0.9600C62—H620.9300
C1—H1B0.9600C63—C641.373 (14)
C1—H1C0.9600C63—H630.9300
C11—C121.386 (9)C64—C651.332 (12)
C11—C161.394 (9)C64—H640.9300
C12—C131.374 (10)C65—C661.385 (10)
C12—H120.9300C65—H650.9300
C13—C141.372 (10)C66—H660.9300
C13—H130.9300B1—B41.759 (12)
C14—C151.377 (10)B1—B21.760 (10)
C14—H140.9300B1—B31.769 (10)
C15—C161.374 (10)B1—B51.773 (12)
C15—H150.9300B1—B61.787 (11)
C16—H160.9300B1—H11.1000
C21—C261.374 (10)B2—B61.765 (10)
C21—C221.384 (9)B2—B111.793 (10)
C22—C231.375 (10)B2—B31.825 (10)
C22—H220.9300B2—H21.1000
C23—C241.372 (12)B3—B41.775 (10)
C23—H230.9300B3—B81.803 (10)
C24—C251.372 (12)B3—H31.1000
C24—H240.9300B4—B81.756 (10)
C25—C261.373 (10)B4—B51.760 (11)
C25—H250.9300B4—B91.804 (11)
C26—H260.9300B4—H41.1000
C31—C361.386 (9)B5—B101.720 (11)
C31—C321.405 (9)B5—B91.728 (11)
C32—C331.378 (10)B5—B61.766 (11)
C32—H320.9300B5—H51.1000
C33—C341.356 (12)B6—B101.766 (11)
C33—H330.9300B6—B111.774 (10)
C34—C351.373 (12)B6—H61.1000
C34—H340.9300B8—B91.882 (10)
C35—C361.389 (10)B8—H1U1.43 (7)
C35—H350.9300B9—B101.929 (12)
C36—H360.9300B9—H91.1000
C41—C421.380 (9)B9—H1U1.17 (7)
C41—C461.397 (9)B10—B111.854 (11)
C42—C431.370 (10)B10—H101.1000
C42—H420.9300B10—H2U1.33 (5)
C43—C441.380 (12)B11—H111.1000
C43—H430.9300B11—H2U1.15 (5)
C44—C451.377 (13)Cl2—C1S1.552 (16)
C44—H440.9300Cl1—C1S1.531 (15)
C45—C461.368 (11)C1S—H1S0.9700
C45—H450.9300C1S—H2S0.9700
C46—H460.9300
B2—Pt7—B348.5 (3)B2—B1—B659.7 (4)
B2—Pt7—B1146.8 (3)B3—B1—B6111.1 (5)
B3—Pt7—B1184.7 (3)B5—B1—B659.5 (5)
B2—Pt7—B883.5 (3)B4—B1—H1120.3
B3—Pt7—B846.8 (3)B2—B1—H1121.8
B11—Pt7—B890.5 (3)B3—B1—H1120.2
B2—Pt7—P2129.56 (19)B5—B1—H1124.1
B3—Pt7—P293.49 (19)B6—B1—H1120.2
B11—Pt7—P2175.72 (18)B1—B2—B660.9 (4)
B8—Pt7—P291.10 (18)B1—B2—B11111.2 (5)
B2—Pt7—P1118.88 (19)B6—B2—B1159.8 (4)
B3—Pt7—P1166.14 (19)B1—B2—B359.1 (4)
B11—Pt7—P181.51 (19)B6—B2—B3109.5 (5)
B8—Pt7—P1134.67 (18)B11—B2—B3115.2 (5)
P2—Pt7—P1100.12 (6)B1—B2—Pt7118.8 (5)
C31—P1—C11107.8 (3)B6—B2—Pt7120.4 (5)
C31—P1—C21100.2 (3)B11—B2—Pt769.2 (3)
C11—P1—C21101.9 (3)B3—B2—Pt766.3 (3)
C31—P1—Pt7113.9 (2)B1—B2—H2120.1
C11—P1—Pt7108.8 (2)B6—B2—H2120.0
C21—P1—Pt7122.9 (2)B11—B2—H2117.7
C41—P2—C51107.1 (3)B3—B2—H2120.1
C41—P2—C61103.0 (3)Pt7—B2—H2109.5
C51—P2—C61101.1 (3)B1—B3—B459.5 (4)
C41—P2—Pt7118.7 (2)B1—B3—B8109.1 (5)
C51—P2—Pt7106.7 (2)B4—B3—B858.8 (4)
C61—P2—Pt7118.4 (2)B1—B3—B258.6 (4)
B8—O1—C1122.7 (5)B4—B3—B2106.2 (5)
O1—C1—H1A109.5B8—B3—B2112.1 (5)
O1—C1—H1B109.5B1—B3—Pt7117.4 (4)
H1A—C1—H1B109.5B4—B3—Pt7118.0 (4)
O1—C1—H1C109.5B8—B3—Pt768.6 (3)
H1A—C1—H1C109.5B2—B3—Pt765.2 (3)
H1B—C1—H1C109.5B1—B3—H3120.9
C12—C11—C16117.6 (6)B4—B3—H3121.9
C12—C11—P1118.7 (5)B8—B3—H3119.2
C16—C11—P1123.7 (5)B2—B3—H3122.1
C13—C12—C11121.3 (6)Pt7—B3—H3110.7
C13—C12—H12119.3B8—B4—B1111.8 (5)
C11—C12—H12119.3B8—B4—B5110.1 (5)
C14—C13—C12120.1 (7)B1—B4—B560.5 (5)
C14—C13—H13119.9B8—B4—B361.4 (4)
C12—C13—H13119.9B1—B4—B360.1 (4)
C13—C14—C15119.5 (7)B5—B4—B3107.3 (6)
C13—C14—H14120.2B8—B4—B963.8 (4)
C15—C14—H14120.2B1—B4—B9109.0 (6)
C16—C15—C14120.3 (7)B5—B4—B958.0 (4)
C16—C15—H15119.8B3—B4—B9110.3 (5)
C14—C15—H15119.8B8—B4—H4118.2
C15—C16—C11120.8 (7)B1—B4—H4120.5
C15—C16—H16119.6B5—B4—H4122.8
C11—C16—H16119.6B3—B4—H4121.5
C26—C21—C22117.9 (6)B9—B4—H4120.6
C26—C21—P1119.0 (5)B10—B5—B968.0 (5)
C22—C21—P1123.0 (5)B10—B5—B4117.0 (5)
C23—C22—C21121.5 (7)B9—B5—B462.3 (4)
C23—C22—H22119.3B10—B5—B660.9 (5)
C21—C22—H22119.3B9—B5—B6116.2 (5)
C24—C23—C22118.8 (8)B4—B5—B6111.2 (5)
C24—C23—H23120.6B10—B5—B1111.6 (6)
C22—C23—H23120.6B9—B5—B1111.9 (5)
C23—C24—C25121.1 (8)B4—B5—B159.7 (5)
C23—C24—H24119.4B6—B5—B160.7 (5)
C25—C24—H24119.4B10—B5—H5116.0
C24—C25—C26118.9 (8)B9—B5—H5115.5
C24—C25—H25120.5B4—B5—H5119.1
C26—C25—H25120.5B6—B5—H5119.6
C25—C26—C21121.7 (7)B1—B5—H5121.8
C25—C26—H26119.1B2—B6—B5105.4 (5)
C21—C26—H26119.1B2—B6—B10109.1 (5)
C36—C31—C32117.6 (6)B5—B6—B1058.3 (4)
C36—C31—P1121.5 (5)B2—B6—B1160.9 (4)
C32—C31—P1120.8 (5)B5—B6—B11109.1 (5)
C33—C32—C31120.5 (7)B10—B6—B1163.2 (4)
C33—C32—H32119.7B2—B6—B159.4 (4)
C31—C32—H32119.7B5—B6—B159.9 (4)
C34—C33—C32120.7 (8)B10—B6—B1108.8 (6)
C34—C33—H33119.6B11—B6—B1110.9 (5)
C32—C33—H33119.6B2—B6—H6122.7
C33—C34—C35120.4 (7)B5—B6—H6123.5
C33—C34—H34119.8B10—B6—H6120.7
C35—C34—H34119.8B11—B6—H6118.9
C34—C35—C36119.7 (8)B1—B6—H6120.8
C34—C35—H35120.2O1—B8—B4127.2 (6)
C36—C35—H35120.2O1—B8—B3126.4 (5)
C31—C36—C35121.1 (7)B4—B8—B359.8 (4)
C31—C36—H36119.5O1—B8—B9122.8 (5)
C35—C36—H36119.5B4—B8—B959.4 (4)
C42—C41—C46118.3 (6)B3—B8—B9105.7 (5)
C42—C41—P2119.2 (5)O1—B8—Pt7110.9 (4)
C46—C41—P2122.5 (6)B4—B8—Pt7115.5 (5)
C43—C42—C41121.2 (7)B3—B8—Pt764.6 (3)
C43—C42—H42119.4B9—B8—Pt7111.5 (4)
C41—C42—H42119.4O1—B8—H1U112 (3)
C42—C43—C44119.5 (8)B4—B8—H1U95 (3)
C42—C43—H43120.3B3—B8—H1U120 (3)
C44—C43—H43120.3B9—B8—H1U38 (3)
C45—C44—C43120.6 (8)Pt7—B8—H1U85 (3)
C45—C44—H44119.7B5—B9—B459.7 (4)
C43—C44—H44119.7B5—B9—B8105.9 (5)
C46—C45—C44119.5 (8)B4—B9—B856.8 (4)
C46—C45—H45120.3B5—B9—B1055.8 (4)
C44—C45—H45120.3B4—B9—B10105.2 (5)
C45—C46—C41120.9 (8)B8—B9—B10111.4 (5)
C45—C46—H46119.5B5—B9—H9140.3
C41—C46—H46119.5B4—B9—H9140.2
C56—C51—C52119.3 (7)B8—B9—H9112.9
C56—C51—P2117.4 (6)B10—B9—H9113.7
C52—C51—P2123.3 (7)B5—B9—H1U125 (3)
C53—C52—C51121.3 (10)B4—B9—H1U103 (3)
C53—C52—H52119.4B8—B9—H1U49 (3)
C51—C52—H52119.4B10—B9—H1U85 (3)
C52—C53—C54119.8 (10)H9—B9—H1U88.4
C52—C53—H53120.1B5—B10—B660.9 (5)
C54—C53—H53120.1B5—B10—B11107.5 (5)
C53—C54—C55121.1 (9)B6—B10—B1158.6 (4)
C53—C54—H54119.5B5—B10—B956.2 (4)
C55—C54—H54119.5B6—B10—B9106.7 (5)
C56—C55—C54119.0 (10)B11—B10—B9110.6 (5)
C56—C55—H55120.5B5—B10—H10139.6
C54—C55—H55120.5B6—B10—H10138.7
C55—C56—C51119.6 (9)B11—B10—H10112.3
C55—C56—H56120.2B9—B10—H10113.6
C51—C56—H56120.2B5—B10—H2U128 (2)
C62—C61—C66117.9 (7)B6—B10—H2U96 (2)
C62—C61—P2121.6 (6)B11—B10—H2U38 (2)
C66—C61—P2120.5 (5)B9—B10—H2U95 (2)
C61—C62—C63119.9 (8)H10—B10—H2U89.9
C61—C62—H62120.1B6—B11—B259.3 (4)
C63—C62—H62120.1B6—B11—B1058.2 (4)
C64—C63—C62120.5 (9)B2—B11—B10104.1 (5)
C64—C63—H63119.8B6—B11—Pt7115.6 (4)
C62—C63—H63119.8B2—B11—Pt764.1 (3)
C65—C64—C63120.1 (8)B10—B11—Pt7113.2 (4)
C65—C64—H64120.0B6—B11—H11137.0
C63—C64—H64120.0B2—B11—H11141.0
C64—C65—C66120.0 (9)B10—B11—H11113.9
C64—C65—H65120.0Pt7—B11—H11106.2
C66—C65—H65120.0B6—B11—H2U103 (3)
C61—C66—C65121.6 (7)B2—B11—H2U127 (3)
C61—C66—H66119.2B10—B11—H2U45 (3)
C65—C66—H66119.2Pt7—B11—H2U88 (3)
B4—B1—B2109.8 (5)H11—B11—H2U88.0
B4—B1—B360.4 (4)Cl1—C1S—Cl2123.6 (14)
B2—B1—B362.3 (4)Cl1—C1S—H1S106.4
B4—B1—B559.8 (5)Cl2—C1S—H1S106.4
B2—B1—B5105.3 (6)Cl1—C1S—H2S106.5
B3—B1—B5107.0 (5)Cl2—C1S—H2S106.5
B4—B1—B6110.3 (6)H1S—C1S—H2S106.5
(II) 8-isopropoxy-7,7-bis(triphenylphosphorine-P)- 8,9:10,11-di-µ-H-7-platina-nido-undecaborane dichloromethane solvate top
Crystal data top
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2F(000) = 1960
Mr = 982.83Dx = 1.472 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.114 (3) ÅCell parameters from 25 reflections
b = 21.634 (8) Åθ = 9–13.2°
c = 18.990 (8) ŵ = 3.39 mm1
β = 103.75 (3)°T = 293 K
V = 4435 (3) Å3Plate, yellow
Z = 40.42 × 0.27 × 0.07 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
4066 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.081
Graphite monochromatorθmax = 25.1°, θmin = 1.5°
θ/2θ scansh = 1312
Absorption correction: ψ scans
(North et al., 1968)
k = 025
Tmin = 0.330, Tmax = 0.797l = 022
8141 measured reflections3 standard reflections every 200 reflections
7894 independent reflections intensity decay: 5.4%
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)] = 0.069Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.238H atoms treated by a mixture of independent and constrained refinement
S = 1.38 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
7894 reflections(Δ/σ)max = 0.001
507 parametersΔρmax = 2.19 e Å3
0 restraintsΔρmin = 3.02 e Å3
Crystal data top
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2V = 4435 (3) Å3
Mr = 982.83Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.114 (3) ŵ = 3.39 mm1
b = 21.634 (8) ÅT = 293 K
c = 18.990 (8) Å0.42 × 0.27 × 0.07 mm
β = 103.75 (3)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
4066 reflections with I > 2σ(I)
Absorption correction: ψ scans
(North et al., 1968)
Rint = 0.081
Tmin = 0.330, Tmax = 0.7973 standard reflections every 200 reflections
8141 measured reflections intensity decay: 5.4%
7894 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0690 restraints
wR(F2) = 0.238H atoms treated by a mixture of independent and constrained refinement
S = 1.38Δρmax = 2.19 e Å3
7894 reflectionsΔρmin = 3.02 e Å3
507 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
Pt70.94224 (5)0.18408 (3)0.80843 (3)0.0411 (2)
P10.8422 (4)0.25483 (19)0.8715 (2)0.0430 (9)
P21.1265 (4)0.2400 (2)0.8119 (2)0.0454 (9)
C1S0.646 (4)0.4630 (12)1.0861 (17)0.174 (17)
H1S10.54850.44921.07820.209*
H1S20.69750.44161.13700.209*
Cl10.7014 (14)0.4321 (6)1.0158 (7)0.236 (6)
Cl20.6532 (15)0.5307 (6)1.0957 (10)0.279 (8)
C110.9236 (14)0.3199 (7)0.9208 (8)0.051 (4)
C120.9385 (15)0.3748 (7)0.8838 (10)0.057 (4)
H120.90600.37620.83400.069*
C130.997 (2)0.4247 (11)0.9161 (14)0.097 (8)
H130.99570.46160.89100.116*
C141.058 (2)0.4198 (11)0.9887 (17)0.109 (10)
H141.10690.45291.01030.130*
C151.0510 (16)0.3653 (11)1.0324 (11)0.079 (6)
H151.09030.36261.08140.094*
C160.9808 (14)0.3184 (8)0.9952 (8)0.056 (4)
H160.97020.28301.02090.067*
C210.7894 (13)0.2092 (9)0.9390 (8)0.053 (4)
C220.8729 (14)0.1699 (8)0.9851 (9)0.059 (5)
H220.95520.16990.98190.071*
C230.8391 (17)0.1307 (9)1.0355 (9)0.069 (5)
H230.89320.10171.06200.083*
C240.7185 (19)0.1382 (8)1.0434 (9)0.061 (5)
H240.69410.11441.07840.074*
C250.635 (2)0.1772 (11)1.0041 (15)0.106 (10)
H250.55640.18131.01260.127*
C260.6714 (18)0.2122 (9)0.9486 (11)0.069 (5)
H260.61360.23750.91850.083*
C310.7043 (13)0.2914 (7)0.8160 (8)0.044 (4)
C320.6571 (16)0.2767 (9)0.7432 (10)0.070 (5)
H320.69440.24610.72130.084*
C330.5536 (17)0.3082 (9)0.7035 (10)0.077 (6)
H330.52580.29970.65430.092*
C340.4908 (18)0.3518 (9)0.7346 (12)0.078 (6)
H340.41610.36850.70900.093*
C350.5410 (18)0.3683 (8)0.8015 (11)0.071 (5)
H350.50450.40100.82070.085*
C360.6479 (15)0.3400 (8)0.8473 (10)0.063 (5)
H360.67880.35260.89500.075*
C411.2332 (14)0.2579 (8)0.8983 (8)0.052 (4)
C421.3487 (14)0.2859 (9)0.9028 (8)0.063 (5)
H421.37790.29100.86110.075*
C431.4201 (17)0.3062 (9)0.9697 (11)0.073 (6)
H431.49060.33010.97250.088*
C441.3814 (19)0.2891 (9)1.0335 (10)0.075 (6)
H441.42530.30361.07840.090*
C451.2811 (15)0.2518 (11)1.0296 (9)0.077 (6)
H451.26500.23541.07170.093*
C461.2030 (15)0.2383 (9)0.9626 (9)0.066 (5)
H461.13040.21620.96020.080*
C511.2261 (17)0.2088 (9)0.7569 (11)0.070 (5)
C521.2156 (17)0.2249 (9)0.6870 (9)0.064 (5)
H521.15750.25490.66730.077*
C531.285 (3)0.1999 (14)0.6430 (12)0.119 (10)
H531.27190.20910.59390.143*
C541.380 (3)0.1583 (12)0.6804 (16)0.106 (8)
H541.43080.14030.65390.127*
C551.3987 (19)0.1439 (11)0.7501 (13)0.089 (7)
H551.46050.11590.77080.107*
C561.3251 (16)0.1710 (8)0.7922 (10)0.065 (5)
H561.34120.16430.84190.078*
C611.0802 (13)0.3109 (8)0.7662 (7)0.048 (4)
C621.1417 (18)0.3676 (11)0.7779 (12)0.089 (7)
H621.21440.36950.81420.107*
C631.104 (2)0.4192 (10)0.7410 (12)0.094 (7)
H631.15080.45520.75040.113*
C640.995 (3)0.4183 (12)0.6887 (12)0.107 (8)
H640.97180.45340.66050.128*
C650.920 (2)0.3694 (13)0.6768 (13)0.101 (8)
H650.84190.37130.64550.121*
C660.9646 (18)0.3153 (9)0.7133 (11)0.076 (6)
H660.91650.27980.70270.092*
B10.867 (2)0.0549 (13)0.7068 (16)0.093 (9)
H10.85650.03640.65170.112*
B20.8220 (19)0.1309 (10)0.7169 (9)0.060 (5)
H20.78550.16100.67000.072*
B30.9944 (18)0.1100 (10)0.7439 (12)0.069 (6)
H31.06280.12760.71540.082*
B40.994 (2)0.0284 (11)0.7733 (13)0.075 (7)
H41.05800.00640.76130.090*
B50.8409 (17)0.0082 (10)0.7744 (13)0.068 (6)
H50.81300.04060.76740.081*
B60.7301 (18)0.0702 (10)0.7331 (9)0.062 (6)
H60.63700.06240.69840.074*
B81.0450 (19)0.0912 (7)0.8356 (11)0.056 (5)
B90.950 (2)0.0303 (12)0.8594 (18)0.093 (9)
H90.98330.01510.91590.112*
B100.775 (2)0.0541 (11)0.8289 (12)0.072 (6)
H100.72850.04730.87350.087*
B110.7545 (17)0.1324 (10)0.7944 (10)0.060 (6)
H110.69650.16120.82100.072*
H1U0.965 (13)0.088 (6)0.876 (7)0.05 (4)*
H2U0.83 (3)0.091 (15)0.875 (17)0.22 (14)*
O11.1626 (10)0.0994 (6)0.8792 (7)0.075 (4)
C11.222 (2)0.0542 (9)0.9286 (13)0.092 (7)
H1A1.17810.00930.91200.110*
C21.359 (3)0.0482 (14)0.933 (2)0.182 (16)
H2A1.38080.06880.88450.219*
H2B1.38540.00090.93650.219*
H2C1.41200.07250.98160.219*
C31.203 (3)0.0700 (14)1.0026 (15)0.167 (15)
H3A1.26290.10921.02530.201*
H3B1.22670.02971.03850.201*
H3C1.10560.08270.99780.201*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt70.0344 (3)0.0528 (4)0.0365 (3)0.0006 (3)0.0093 (2)0.0030 (3)
P10.036 (2)0.053 (2)0.040 (2)0.0005 (17)0.0087 (16)0.0039 (18)
P20.038 (2)0.061 (3)0.040 (2)0.0033 (18)0.0133 (17)0.0033 (18)
C1S0.33 (5)0.083 (19)0.16 (3)0.09 (3)0.16 (3)0.057 (19)
Cl10.315 (17)0.222 (12)0.200 (11)0.009 (12)0.119 (11)0.081 (10)
Cl20.281 (16)0.181 (12)0.42 (2)0.024 (11)0.178 (16)0.140 (14)
C110.049 (9)0.052 (9)0.054 (9)0.017 (8)0.014 (7)0.019 (8)
C120.063 (11)0.034 (9)0.084 (12)0.001 (8)0.034 (9)0.001 (8)
C130.099 (18)0.091 (17)0.103 (18)0.047 (14)0.030 (14)0.032 (14)
C140.093 (18)0.089 (18)0.17 (3)0.039 (14)0.085 (19)0.068 (18)
C150.042 (10)0.117 (18)0.070 (13)0.007 (11)0.001 (9)0.034 (13)
C160.043 (8)0.080 (12)0.049 (9)0.022 (9)0.022 (7)0.003 (9)
C210.032 (8)0.084 (12)0.045 (9)0.003 (8)0.011 (7)0.015 (8)
C220.037 (8)0.082 (13)0.059 (10)0.006 (8)0.014 (7)0.026 (9)
C230.063 (12)0.084 (14)0.055 (10)0.022 (10)0.000 (9)0.010 (10)
C240.078 (13)0.054 (11)0.050 (10)0.004 (10)0.010 (9)0.009 (8)
C250.090 (17)0.108 (19)0.15 (2)0.053 (15)0.093 (18)0.048 (18)
C260.066 (12)0.059 (11)0.088 (14)0.008 (9)0.032 (11)0.002 (10)
C310.036 (8)0.056 (9)0.044 (8)0.012 (7)0.018 (7)0.006 (7)
C320.053 (11)0.083 (14)0.068 (12)0.007 (10)0.003 (9)0.011 (10)
C330.071 (13)0.087 (15)0.060 (12)0.026 (11)0.007 (10)0.005 (10)
C340.066 (13)0.072 (13)0.085 (14)0.024 (11)0.001 (11)0.003 (11)
C350.073 (13)0.052 (11)0.094 (15)0.006 (10)0.034 (11)0.013 (10)
C360.053 (10)0.064 (11)0.078 (12)0.001 (8)0.027 (9)0.038 (9)
C410.040 (8)0.081 (12)0.046 (9)0.001 (8)0.027 (7)0.020 (8)
C420.032 (8)0.117 (15)0.038 (8)0.010 (9)0.006 (7)0.004 (9)
C430.053 (10)0.091 (15)0.076 (13)0.029 (10)0.015 (9)0.022 (11)
C440.078 (14)0.076 (13)0.056 (11)0.020 (11)0.016 (10)0.025 (10)
C450.039 (10)0.14 (2)0.045 (10)0.014 (11)0.004 (8)0.003 (11)
C460.041 (9)0.103 (15)0.050 (10)0.005 (9)0.001 (8)0.028 (10)
C510.055 (11)0.073 (12)0.088 (14)0.001 (9)0.029 (10)0.031 (11)
C520.066 (12)0.087 (14)0.041 (9)0.002 (10)0.019 (8)0.006 (9)
C530.14 (2)0.18 (3)0.054 (13)0.03 (2)0.047 (15)0.006 (15)
C540.12 (2)0.111 (19)0.11 (2)0.004 (16)0.074 (18)0.040 (17)
C550.073 (14)0.111 (18)0.094 (16)0.035 (13)0.041 (12)0.016 (14)
C560.056 (11)0.070 (13)0.070 (11)0.000 (9)0.017 (9)0.020 (9)
C610.033 (7)0.075 (11)0.034 (7)0.014 (8)0.007 (6)0.001 (8)
C620.052 (11)0.095 (16)0.109 (17)0.014 (11)0.003 (11)0.048 (14)
C630.106 (18)0.069 (14)0.090 (16)0.011 (13)0.009 (13)0.015 (12)
C640.13 (2)0.091 (18)0.087 (17)0.010 (17)0.001 (16)0.034 (14)
C650.081 (16)0.13 (2)0.086 (16)0.007 (16)0.008 (13)0.017 (16)
C660.074 (13)0.073 (13)0.086 (14)0.028 (11)0.025 (11)0.033 (11)
B10.061 (14)0.11 (2)0.11 (2)0.000 (14)0.019 (14)0.049 (18)
B20.062 (12)0.086 (15)0.032 (9)0.013 (11)0.010 (8)0.000 (9)
B30.047 (11)0.068 (13)0.098 (16)0.016 (10)0.031 (11)0.048 (12)
B40.061 (13)0.072 (15)0.096 (17)0.008 (12)0.024 (12)0.035 (13)
B50.038 (10)0.051 (12)0.112 (18)0.012 (9)0.015 (11)0.014 (12)
B60.051 (12)0.084 (15)0.040 (10)0.005 (11)0.008 (9)0.031 (10)
B80.067 (13)0.012 (7)0.074 (13)0.004 (8)0.014 (10)0.013 (8)
B90.046 (13)0.087 (19)0.14 (2)0.007 (12)0.011 (14)0.038 (18)
B100.070 (15)0.072 (15)0.072 (14)0.001 (12)0.015 (12)0.007 (12)
B110.045 (10)0.080 (15)0.058 (11)0.039 (10)0.022 (9)0.017 (10)
O10.044 (7)0.076 (9)0.105 (10)0.021 (6)0.020 (7)0.034 (8)
C10.097 (17)0.048 (12)0.111 (18)0.013 (11)0.013 (14)0.017 (12)
C20.11 (2)0.14 (3)0.27 (4)0.09 (2)0.00 (3)0.08 (3)
C30.24 (4)0.15 (3)0.10 (2)0.08 (3)0.02 (2)0.09 (2)
Geometric parameters (Å, º) top
Pt7—B32.178 (16)C51—C521.35 (2)
Pt7—B22.24 (2)C51—C561.41 (2)
Pt7—B82.308 (16)C52—C531.37 (3)
Pt7—B112.326 (16)C53—C541.44 (4)
Pt7—P22.366 (4)C54—C551.33 (3)
Pt7—P12.376 (4)C55—C561.40 (2)
P1—C111.810 (16)C61—C621.40 (3)
P1—C311.821 (15)C61—C661.43 (2)
P1—C211.821 (17)C62—C631.33 (3)
P2—C611.776 (17)C63—C641.37 (3)
P2—C411.823 (16)C64—C651.33 (3)
P2—C511.822 (19)C65—C661.39 (3)
C1S—Cl21.48 (3)B1—B51.71 (4)
C1S—Cl11.73 (3)B1—B61.74 (3)
C11—C161.40 (2)B1—B21.74 (3)
C11—C121.41 (2)B1—B41.75 (4)
C12—C131.33 (2)B1—B31.86 (3)
C13—C141.39 (3)B2—B61.74 (3)
C14—C151.46 (3)B2—B111.80 (3)
C15—C161.37 (2)B2—B31.92 (3)
C21—C261.37 (2)B3—B81.75 (3)
C21—C221.40 (2)B3—B41.85 (3)
C22—C231.40 (2)B4—B51.76 (3)
C23—C241.39 (3)B4—B81.80 (3)
C24—C251.34 (3)B4—B91.81 (4)
C25—C261.43 (3)B5—B101.72 (3)
C31—C321.39 (2)B5—B91.84 (4)
C31—C361.42 (2)B5—B61.86 (3)
C32—C331.39 (2)B6—B111.76 (3)
C33—C341.38 (3)B6—B101.80 (3)
C34—C351.31 (3)B8—O11.38 (2)
C35—C361.43 (2)B8—B91.81 (3)
C41—C421.40 (2)B9—B101.96 (3)
C41—C461.41 (2)B10—B111.81 (3)
C42—C431.40 (2)O1—C11.41 (2)
C43—C441.43 (3)C1—C21.51 (3)
C44—C451.37 (3)C1—C31.51 (3)
C45—C461.39 (2)
B3—Pt7—B251.4 (7)B2—B1—B364.2 (13)
B3—Pt7—B845.7 (8)B4—B1—B361.7 (13)
B2—Pt7—B884.2 (7)B6—B2—B160.0 (13)
B3—Pt7—B1186.2 (8)B6—B2—B1159.5 (10)
B2—Pt7—B1146.5 (7)B1—B2—B11106.9 (16)
B8—Pt7—B1189.4 (8)B6—B2—B3111.6 (15)
B3—Pt7—P292.7 (6)B1—B2—B360.9 (12)
B2—Pt7—P2129.5 (5)B11—B2—B3111.7 (13)
B8—Pt7—P293.5 (5)B6—B2—Pt7121.2 (11)
B11—Pt7—P2174.8 (5)B1—B2—Pt7115.9 (13)
B3—Pt7—P1167.6 (5)B11—B2—Pt769.2 (8)
B2—Pt7—P1117.2 (5)B3—B2—Pt762.6 (8)
B8—Pt7—P1135.6 (6)B8—B3—B460.0 (12)
B11—Pt7—P181.5 (6)B8—B3—B1105.3 (17)
P2—Pt7—P199.33 (14)B4—B3—B156.3 (13)
C11—P1—C31102.1 (7)B8—B3—B2112.7 (14)
C11—P1—C21105.2 (7)B4—B3—B2103.3 (15)
C31—P1—C21105.9 (7)B1—B3—B254.9 (12)
C11—P1—Pt7121.7 (5)B8—B3—Pt771.1 (9)
C31—P1—Pt7114.8 (5)B4—B3—Pt7120.7 (14)
C21—P1—Pt7105.9 (6)B1—B3—Pt7113.8 (12)
C61—P2—C41107.9 (8)B2—B3—Pt766.0 (8)
C61—P2—C51100.6 (7)B1—B4—B558.3 (14)
C41—P2—C51103.9 (8)B1—B4—B8107.6 (16)
C61—P2—Pt7106.3 (5)B5—B4—B8109.6 (15)
C41—P2—Pt7120.5 (5)B1—B4—B9107.5 (17)
C51—P2—Pt7115.7 (6)B5—B4—B961.9 (13)
Cl2—C1S—Cl1117.3 (18)B8—B4—B960.1 (12)
C16—C11—C12116.3 (15)B1—B4—B362.1 (14)
C16—C11—P1123.6 (13)B5—B4—B3108.3 (16)
C12—C11—P1120.0 (13)B8—B4—B357.1 (11)
C13—C12—C11123.7 (19)B9—B4—B3105.8 (14)
C12—C13—C14118 (2)B1—B5—B10106.5 (17)
C13—C14—C15123 (2)B1—B5—B460.7 (14)
C16—C15—C14114.1 (19)B10—B5—B4114.6 (15)
C15—C16—C11124.6 (18)B1—B5—B9108.3 (15)
C26—C21—C22117.3 (16)B10—B5—B966.9 (14)
C26—C21—P1123.2 (14)B4—B5—B960.6 (13)
C22—C21—P1119.5 (11)B1—B5—B658.1 (13)
C23—C22—C21123.4 (16)B10—B5—B660.3 (11)
C22—C23—C24115.3 (17)B4—B5—B6111.1 (16)
C25—C24—C23124.7 (18)B9—B5—B6114.5 (15)
C24—C25—C26117.6 (18)B2—B6—B160.2 (13)
C21—C26—C25121 (2)B2—B6—B1162.2 (11)
C32—C31—C36118.9 (15)B1—B6—B11109.2 (15)
C32—C31—P1122.7 (12)B2—B6—B10107.0 (13)
C36—C31—P1118.2 (12)B1—B6—B10101.7 (16)
C31—C32—C33119.5 (18)B11—B6—B1061.2 (11)
C34—C33—C32122.4 (18)B2—B6—B5105.1 (13)
C35—C34—C33117.2 (18)B1—B6—B556.5 (14)
C34—C35—C36124.9 (19)B11—B6—B5106.9 (13)
C31—C36—C35116.5 (18)B10—B6—B556.0 (12)
C42—C41—C46118.8 (15)O1—B8—B3126.9 (17)
C42—C41—P2122.4 (11)O1—B8—B4126.6 (16)
C46—C41—P2118.6 (12)B3—B8—B462.9 (12)
C43—C42—C41120.2 (15)O1—B8—B9118.0 (15)
C42—C43—C44118.0 (16)B3—B8—B9110.5 (15)
C45—C44—C43121.0 (16)B4—B8—B960.2 (14)
C44—C45—C46119.8 (18)O1—B8—Pt7111.7 (11)
C45—C46—C41120.4 (17)B3—B8—Pt763.2 (7)
C52—C51—C56119.5 (18)B4—B8—Pt7116.5 (12)
C52—C51—P2123.1 (15)B9—B8—Pt7113.7 (13)
C56—C51—P2117.1 (14)B8—B9—B459.7 (12)
C51—C52—C53125 (2)B8—B9—B5105.8 (18)
C52—C53—C54113 (2)B4—B9—B557.6 (14)
C55—C54—C53124 (2)B8—B9—B10109.4 (15)
C54—C55—C56120 (2)B4—B9—B10101.5 (17)
C55—C56—C51117.9 (19)B5—B9—B1053.7 (11)
C62—C61—C66112.1 (16)B5—B10—B663.8 (13)
C62—C61—P2127.4 (12)B5—B10—B11110.8 (17)
C66—C61—P2120.4 (14)B6—B10—B1158.2 (11)
C63—C62—C61124.9 (19)B5—B10—B959.3 (14)
C62—C63—C64119 (2)B6—B10—B9111.3 (16)
C65—C64—C63123 (2)B11—B10—B9112.4 (15)
C64—C65—C66117 (2)B6—B11—B258.3 (12)
C65—C66—C61124 (2)B6—B11—B1060.6 (12)
B5—B1—B665.4 (14)B2—B11—B10103.8 (15)
B5—B1—B2111.9 (17)B6—B11—Pt7115.9 (12)
B6—B1—B259.8 (13)B2—B11—Pt764.3 (8)
B5—B1—B461.0 (15)B10—B11—Pt7112.2 (13)
B6—B1—B4118 (2)B8—O1—C1122.5 (14)
B2—B1—B4115.6 (17)O1—C1—C2114 (2)
B5—B1—B3110.1 (18)O1—C1—C3108.4 (19)
B6—B1—B3114.2 (16)C2—C1—C3109 (2)
(III) 9-isopropoxy-7,7-bis(triphenylphosphorine-P)- 8,9:10,11-di-µ-H-7-platina-nido-undecaborane dichloromethane solvate top
Crystal data top
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2F(000) = 1960
Mr = 982.83Dx = 1.459 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
a = 13.435 (3) ÅCell parameters from 22 reflections
b = 17.864 (4) Åθ = 9.1–10.8°
c = 19.383 (4) ŵ = 3.36 mm1
β = 105.94 (2)°T = 293 K
V = 4473.1 (17) Å3Square prism, red
Z = 40.44 × 0.34 × 0.32 mm
Data collection top
Rigaku AFC-7R
diffractometer
6198 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.048
Graphite monochromatorθmax = 25°, θmin = 2.3°
θ/2θ scansh = 015
Absorption correction: ψ scans
(North et al., 1968)
k = 021
Tmin = 0.320, Tmax = 0.413l = 2322
8222 measured reflections3 standard reflections every 200 reflections
7865 independent reflections intensity decay: 0.3%
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0575P)2 + 0.5166P]
where P = (Fo2 + 2Fc2)/3
7865 reflections(Δ/σ)max = 0.002
549 parametersΔρmax = 2.30 e Å3
0 restraintsΔρmin = 0.99 e Å3
Crystal data top
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2V = 4473.1 (17) Å3
Mr = 982.83Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.435 (3) ŵ = 3.36 mm1
b = 17.864 (4) ÅT = 293 K
c = 19.383 (4) Å0.44 × 0.34 × 0.32 mm
β = 105.94 (2)°
Data collection top
Rigaku AFC-7R
diffractometer
6198 reflections with I > 2σ(I)
Absorption correction: ψ scans
(North et al., 1968)
Rint = 0.048
Tmin = 0.320, Tmax = 0.4133 standard reflections every 200 reflections
8222 measured reflections intensity decay: 0.3%
7865 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 2.30 e Å3
7865 reflectionsΔρmin = 0.99 e Å3
549 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
Pt70.201146 (14)0.819610 (10)0.119982 (10)0.02727 (8)
P10.19465 (10)0.73495 (7)0.02513 (7)0.0310 (3)
P20.35817 (10)0.87605 (7)0.12119 (7)0.0303 (3)
O10.1650 (3)0.8291 (2)0.0655 (2)0.0497 (11)
C10.1979 (5)0.7704 (3)0.0141 (3)0.0497 (15)
H1F0.14080.75680.00590.060*
C20.2870 (6)0.8008 (5)0.0450 (4)0.075 (2)
H2A0.26410.84360.06650.112*
H2B0.34240.81530.02530.112*
H2C0.31110.76290.08080.112*
C30.2298 (6)0.7022 (4)0.0496 (5)0.076 (2)
H3A0.17150.68440.08670.114*
H3B0.25320.66360.01450.114*
H3C0.28470.71560.07020.114*
C110.2903 (4)0.7349 (3)0.0265 (3)0.0350 (11)
C120.3851 (4)0.6994 (3)0.0026 (3)0.0450 (14)
H120.39980.67860.04820.054*
C130.4571 (5)0.6951 (4)0.0362 (4)0.0598 (18)
H130.52030.67160.01650.072*
C140.4359 (5)0.7252 (5)0.1035 (4)0.066 (2)
H140.48470.72230.12940.079*
C150.3430 (5)0.7598 (4)0.1329 (3)0.0595 (17)
H150.32880.78020.17870.071*
C160.2699 (5)0.7646 (4)0.0946 (3)0.0482 (14)
H160.20670.78790.11500.058*
C210.0730 (4)0.7540 (3)0.0436 (3)0.0347 (11)
C220.0041 (5)0.6991 (3)0.0763 (3)0.0471 (15)
H220.01760.64920.06310.057*
C230.0861 (5)0.7180 (4)0.1295 (4)0.0608 (19)
H230.13210.68070.15170.073*
C240.1070 (5)0.7915 (5)0.1490 (3)0.0596 (18)
H240.16690.80400.18430.072*
C250.0389 (5)0.8462 (4)0.1159 (3)0.0545 (16)
H250.05330.89610.12850.065*
C260.0509 (4)0.8277 (3)0.0641 (3)0.0425 (13)
H260.09700.86520.04260.051*
C310.1982 (4)0.6356 (3)0.0475 (3)0.0401 (13)
C320.2066 (4)0.6118 (3)0.1176 (3)0.0452 (14)
H320.20460.64690.15270.054*
C330.2178 (5)0.5363 (4)0.1353 (4)0.066 (2)
H330.22450.52090.18220.079*
C340.2190 (7)0.4844 (4)0.0830 (5)0.083 (3)
H340.22580.43380.09460.100*
C350.2101 (7)0.5073 (4)0.0132 (5)0.078 (2)
H350.21050.47190.02190.093*
C360.2006 (5)0.5825 (3)0.0043 (4)0.0573 (17)
H360.19570.59750.05110.069*
C410.4049 (4)0.9536 (3)0.1838 (3)0.0337 (11)
C420.4613 (4)0.9378 (3)0.2541 (3)0.0476 (14)
H420.47440.88840.26890.057*
C430.4978 (5)0.9961 (4)0.3019 (4)0.0593 (18)
H430.53480.98530.34880.071*
C440.4800 (5)1.0693 (4)0.2808 (4)0.0579 (17)
H440.50551.10770.31320.069*
C450.4251 (5)1.0853 (3)0.2126 (4)0.0529 (16)
H450.41371.13500.19840.064*
C460.3853 (4)1.0282 (3)0.1634 (3)0.0404 (13)
H460.34591.04000.11720.048*
C510.4633 (4)0.8089 (3)0.1546 (3)0.0361 (12)
C520.5657 (5)0.8276 (4)0.1608 (4)0.0533 (16)
H520.58200.87470.14660.064*
C530.6439 (5)0.7758 (5)0.1882 (4)0.070 (2)
H530.71220.78790.19100.084*
C540.6203 (6)0.7066 (5)0.2113 (4)0.074 (2)
H540.67290.67210.22930.089*
C550.5199 (6)0.6886 (4)0.2078 (4)0.0569 (17)
H550.50430.64220.22410.068*
C560.4405 (5)0.7406 (3)0.1794 (3)0.0459 (14)
H560.37230.72880.17740.055*
C610.3659 (4)0.9116 (3)0.0348 (3)0.0342 (11)
C620.2874 (4)0.9593 (3)0.0039 (3)0.0462 (14)
H620.23300.97200.01500.055*
C630.2900 (5)0.9874 (4)0.0693 (3)0.0511 (15)
H630.23861.02030.09370.061*
C640.3670 (5)0.9677 (4)0.0988 (3)0.0546 (16)
H640.36780.98630.14340.065*
C650.4446 (5)0.9195 (4)0.0619 (4)0.0545 (16)
H650.49740.90590.08200.065*
C660.4436 (4)0.8919 (3)0.0039 (3)0.0434 (14)
H660.49580.85960.02810.052*
B10.0782 (5)0.8534 (4)0.2506 (4)0.0423 (15)
B20.1833 (5)0.8786 (3)0.2181 (3)0.0342 (13)
B30.1302 (5)0.7853 (4)0.2050 (3)0.0356 (13)
B40.0048 (5)0.7896 (4)0.1932 (4)0.0393 (14)
B50.0362 (5)0.8876 (4)0.1868 (4)0.0413 (15)
B60.0789 (5)0.9425 (4)0.2083 (4)0.0403 (15)
B80.0435 (5)0.7653 (3)0.1194 (3)0.0331 (13)
B90.0643 (5)0.8337 (3)0.1087 (4)0.0381 (14)
B100.0023 (5)0.9379 (3)0.1208 (4)0.0389 (15)
B110.1378 (5)0.9345 (3)0.1397 (3)0.0348 (13)
H10.087 (4)0.849 (3)0.309 (3)0.025 (12)*
H20.256 (4)0.891 (3)0.251 (3)0.032 (13)*
H30.174 (4)0.738 (3)0.226 (3)0.040 (15)*
H40.050 (5)0.749 (4)0.210 (3)0.059 (18)*
H50.104 (4)0.911 (3)0.202 (3)0.037 (14)*
H60.086 (4)0.998 (3)0.244 (3)0.046 (16)*
H80.034 (4)0.709 (3)0.098 (3)0.028 (13)*
H100.047 (4)0.985 (3)0.089 (3)0.031 (13)*
H110.175 (4)0.976 (3)0.118 (3)0.039 (15)*
H1U0.003 (5)0.810 (3)0.068 (4)0.07 (2)*
H2U0.055 (4)0.925 (3)0.094 (3)0.037 (14)*
Cl10.5410 (5)0.5221 (3)0.0903 (2)0.237 (3)
Cl20.7355 (3)0.4928 (4)0.1878 (3)0.226 (3)
C1S0.6056 (10)0.4766 (7)0.1599 (7)0.148 (5)
H1S0.59500.42350.14990.178*
H2S0.57660.48820.19930.178*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt70.02531 (11)0.02416 (11)0.03163 (12)0.00079 (8)0.00662 (8)0.00101 (8)
P10.0315 (7)0.0252 (6)0.0357 (7)0.0001 (5)0.0080 (5)0.0005 (5)
P20.0273 (6)0.0279 (6)0.0350 (7)0.0002 (5)0.0074 (5)0.0001 (5)
O10.0267 (19)0.047 (2)0.069 (3)0.0046 (17)0.0014 (19)0.010 (2)
C10.037 (3)0.050 (4)0.059 (4)0.002 (3)0.007 (3)0.011 (3)
C20.048 (4)0.083 (6)0.080 (5)0.004 (4)0.004 (4)0.000 (4)
C30.064 (5)0.046 (4)0.112 (7)0.012 (4)0.015 (5)0.004 (4)
C110.034 (3)0.032 (3)0.039 (3)0.001 (2)0.010 (2)0.008 (2)
C120.041 (3)0.045 (3)0.048 (3)0.004 (3)0.010 (3)0.007 (3)
C130.041 (4)0.061 (4)0.080 (5)0.006 (3)0.019 (3)0.014 (4)
C140.051 (4)0.092 (6)0.065 (5)0.011 (4)0.033 (4)0.022 (4)
C150.055 (4)0.082 (5)0.043 (4)0.006 (4)0.015 (3)0.007 (3)
C160.043 (3)0.058 (4)0.043 (3)0.000 (3)0.009 (3)0.000 (3)
C210.035 (3)0.033 (3)0.036 (3)0.004 (2)0.009 (2)0.006 (2)
C220.046 (3)0.039 (3)0.054 (4)0.009 (3)0.010 (3)0.012 (3)
C230.041 (3)0.079 (5)0.056 (4)0.016 (4)0.001 (3)0.028 (4)
C240.045 (4)0.082 (5)0.042 (4)0.003 (4)0.004 (3)0.004 (3)
C250.051 (4)0.056 (4)0.046 (4)0.011 (3)0.004 (3)0.010 (3)
C260.041 (3)0.041 (3)0.041 (3)0.002 (3)0.004 (3)0.004 (2)
C310.042 (3)0.026 (3)0.055 (4)0.002 (2)0.018 (3)0.001 (2)
C320.047 (3)0.039 (3)0.053 (4)0.007 (3)0.020 (3)0.007 (3)
C330.067 (5)0.058 (4)0.077 (5)0.016 (4)0.025 (4)0.029 (4)
C340.115 (7)0.029 (3)0.119 (7)0.013 (4)0.052 (6)0.018 (4)
C350.116 (7)0.031 (3)0.097 (6)0.005 (4)0.048 (5)0.009 (4)
C360.079 (5)0.033 (3)0.063 (4)0.001 (3)0.027 (4)0.006 (3)
C410.030 (3)0.032 (3)0.038 (3)0.005 (2)0.009 (2)0.007 (2)
C420.049 (3)0.043 (3)0.046 (3)0.002 (3)0.004 (3)0.006 (3)
C430.062 (4)0.061 (4)0.044 (4)0.004 (3)0.002 (3)0.010 (3)
C440.064 (4)0.048 (4)0.061 (4)0.011 (3)0.016 (3)0.025 (3)
C450.061 (4)0.032 (3)0.067 (4)0.005 (3)0.020 (3)0.007 (3)
C460.043 (3)0.032 (3)0.046 (3)0.001 (2)0.013 (3)0.003 (2)
C510.032 (3)0.036 (3)0.035 (3)0.010 (2)0.000 (2)0.002 (2)
C520.039 (3)0.052 (4)0.065 (4)0.002 (3)0.007 (3)0.005 (3)
C530.033 (3)0.085 (6)0.081 (5)0.013 (4)0.004 (3)0.011 (4)
C540.059 (5)0.072 (5)0.073 (5)0.030 (4)0.012 (4)0.012 (4)
C550.069 (5)0.044 (4)0.049 (4)0.014 (3)0.001 (3)0.006 (3)
C560.045 (3)0.043 (3)0.044 (3)0.006 (3)0.002 (3)0.001 (3)
C610.036 (3)0.030 (3)0.036 (3)0.006 (2)0.008 (2)0.000 (2)
C620.041 (3)0.046 (3)0.051 (3)0.003 (3)0.012 (3)0.007 (3)
C630.049 (4)0.055 (4)0.046 (3)0.003 (3)0.007 (3)0.012 (3)
C640.065 (4)0.057 (4)0.044 (3)0.010 (3)0.021 (3)0.009 (3)
C650.057 (4)0.054 (4)0.062 (4)0.001 (3)0.032 (3)0.003 (3)
C660.040 (3)0.042 (3)0.054 (4)0.002 (3)0.022 (3)0.007 (3)
B10.046 (4)0.041 (4)0.041 (4)0.002 (3)0.012 (3)0.001 (3)
B20.035 (3)0.033 (3)0.036 (3)0.002 (3)0.010 (3)0.004 (3)
B30.032 (3)0.037 (3)0.039 (3)0.004 (3)0.012 (3)0.008 (3)
B40.037 (3)0.033 (3)0.054 (4)0.000 (3)0.021 (3)0.009 (3)
B50.034 (3)0.041 (4)0.055 (4)0.003 (3)0.022 (3)0.004 (3)
B60.038 (3)0.035 (3)0.044 (4)0.004 (3)0.006 (3)0.006 (3)
B80.033 (3)0.023 (3)0.043 (3)0.002 (2)0.011 (3)0.006 (3)
B90.028 (3)0.032 (3)0.055 (4)0.002 (2)0.013 (3)0.004 (3)
B100.029 (3)0.027 (3)0.060 (4)0.005 (2)0.012 (3)0.000 (3)
B110.031 (3)0.029 (3)0.044 (3)0.000 (2)0.011 (3)0.005 (3)
Cl10.348 (7)0.163 (4)0.142 (4)0.063 (4)0.032 (4)0.008 (3)
Cl20.124 (3)0.379 (8)0.176 (4)0.042 (4)0.042 (3)0.059 (5)
C1S0.185 (14)0.122 (10)0.127 (10)0.019 (9)0.025 (9)0.033 (8)
Geometric parameters (Å, º) top
Pt7—B32.205 (6)C45—C461.398 (8)
Pt7—B22.243 (6)C45—H450.9300
Pt7—B112.294 (6)C46—H460.9300
Pt7—B82.327 (6)C51—C561.377 (8)
Pt7—P22.3325 (14)C51—C521.388 (8)
Pt7—P12.3636 (14)C52—C531.391 (9)
P1—C311.825 (5)C52—H520.9300
P1—C111.834 (5)C53—C541.381 (11)
P1—C211.834 (5)C53—H530.9300
P2—C611.821 (5)C54—C551.371 (11)
P2—C511.830 (5)C54—H540.9300
P2—C411.835 (5)C55—C561.409 (8)
O1—B91.384 (7)C55—H550.9300
O1—C11.431 (7)C56—H560.9300
C1—C21.514 (9)C61—C661.383 (7)
C1—C31.517 (9)C61—C621.403 (7)
C1—H1F0.9800C62—C631.375 (8)
C2—H2A0.9600C62—H620.9300
C2—H2B0.9600C63—C641.359 (9)
C2—H2C0.9600C63—H630.9300
C3—H3A0.9600C64—C651.388 (9)
C3—H3B0.9600C64—H640.9300
C3—H3C0.9600C65—C661.371 (8)
C11—C161.378 (8)C65—H650.9300
C11—C121.395 (8)C66—H660.9300
C12—C131.381 (9)B1—B21.756 (9)
C12—H120.9300B1—B31.757 (9)
C13—C141.367 (10)B1—B41.761 (10)
C13—H130.9300B1—B61.792 (9)
C14—C151.368 (10)B1—B51.796 (10)
C14—H140.9300B1—H11.10 (5)
C15—C161.387 (9)B2—B61.778 (9)
C15—H150.9300B2—B111.780 (9)
C16—H160.9300B2—B31.803 (9)
C21—C221.378 (7)B2—H21.04 (5)
C21—C261.384 (7)B3—B41.766 (9)
C22—C231.400 (9)B3—B81.781 (9)
C22—H220.9300B3—H31.05 (6)
C23—C241.373 (10)B4—B81.779 (9)
C23—H230.9300B4—B91.796 (10)
C24—C251.371 (10)B4—B51.797 (9)
C24—H240.9300B4—H41.06 (6)
C25—C261.382 (8)B5—B101.724 (9)
C25—H250.9300B5—B91.746 (9)
C26—H260.9300B5—B61.782 (9)
C31—C361.389 (8)B5—H51.11 (5)
C31—C321.398 (8)B6—B111.730 (9)
C32—C331.390 (9)B6—B101.748 (9)
C32—H320.9300B6—H61.20 (6)
C33—C341.377 (11)B8—B91.862 (8)
C33—H330.9300B8—H81.08 (5)
C34—C351.387 (11)B8—H1U1.28 (7)
C34—H340.9300B9—B102.025 (9)
C35—C361.382 (9)B9—H1U1.42 (7)
C35—H350.9300B10—B111.818 (9)
C36—H360.9300B10—H101.11 (5)
C41—C421.393 (8)B10—H2U1.07 (5)
C41—C461.395 (7)B11—H111.04 (5)
C42—C431.391 (8)B11—H2U1.23 (5)
C42—H420.9300Cl1—C1S1.609 (12)
C43—C441.370 (9)Cl2—C1S1.704 (13)
C43—H430.9300C1S—H1S0.9700
C44—C451.356 (9)C1S—H2S0.9700
C44—H440.9300
B3—Pt7—B247.8 (2)B2—B1—B4111.8 (5)
B3—Pt7—B1182.4 (2)B3—B1—B460.3 (4)
B2—Pt7—B1146.2 (2)B2—B1—B660.1 (4)
B3—Pt7—B846.2 (2)B3—B1—B6109.3 (5)
B2—Pt7—B883.7 (2)B4—B1—B6111.5 (5)
B11—Pt7—B889.7 (2)B2—B1—B5106.6 (5)
B3—Pt7—P2133.49 (17)B3—B1—B5105.8 (5)
B2—Pt7—P295.47 (16)B4—B1—B560.7 (4)
B11—Pt7—P289.28 (16)B6—B1—B559.6 (4)
B8—Pt7—P2178.97 (15)B2—B1—H1121 (2)
B3—Pt7—P1118.17 (18)B3—B1—H1121 (3)
B2—Pt7—P1165.92 (16)B4—B1—H1118 (3)
B11—Pt7—P1140.00 (16)B6—B1—H1122 (3)
B8—Pt7—P183.72 (16)B5—B1—H1124 (2)
P2—Pt7—P197.15 (5)B1—B2—B660.9 (4)
C31—P1—C1198.8 (2)B1—B2—B11109.2 (4)
C31—P1—C21108.2 (3)B6—B2—B1158.2 (3)
C11—P1—C21102.8 (2)B1—B2—B359.2 (4)
C31—P1—Pt7116.38 (19)B6—B2—B3107.9 (4)
C11—P1—Pt7122.91 (17)B11—B2—B3111.6 (4)
C21—P1—Pt7106.36 (17)B1—B2—Pt7117.9 (4)
C61—P2—C51108.7 (3)B6—B2—Pt7118.4 (4)
C61—P2—C41104.5 (2)B11—B2—Pt768.4 (3)
C51—P2—C4199.8 (2)B3—B2—Pt765.0 (3)
C61—P2—Pt7114.92 (17)B1—B2—H2123 (3)
C51—P2—Pt7109.18 (19)B6—B2—H2121 (3)
C41—P2—Pt7118.51 (16)B11—B2—H2117 (3)
B9—O1—C1121.9 (4)B3—B2—H2124 (3)
O1—C1—C2107.0 (5)Pt7—B2—H2109 (3)
O1—C1—C3110.2 (6)B1—B3—B460.0 (4)
C2—C1—C3111.7 (6)B1—B3—B8111.0 (4)
O1—C1—H1F109.3B4—B3—B860.2 (4)
C2—C1—H1F109.3B1—B3—B259.1 (4)
C3—C1—H1F109.3B4—B3—B2109.3 (4)
C1—C2—H2A109.5B8—B3—B2116.7 (4)
C1—C2—H2B109.5B1—B3—Pt7119.8 (4)
H2A—C2—H2B109.5B4—B3—Pt7122.1 (4)
C1—C2—H2C109.5B8—B3—Pt770.5 (3)
H2A—C2—H2C109.5B2—B3—Pt767.2 (3)
H2B—C2—H2C109.5B1—B3—H3128 (3)
C1—C3—H3A109.5B4—B3—H3122 (3)
C1—C3—H3B109.5B8—B3—H3111 (3)
H3A—C3—H3B109.5B2—B3—H3122 (3)
C1—C3—H3C109.5Pt7—B3—H3102 (3)
H3A—C3—H3C109.5B1—B4—B359.8 (4)
H3B—C3—H3C109.5B1—B4—B8111.0 (4)
C16—C11—C12118.8 (5)B3—B4—B860.3 (3)
C16—C11—P1122.5 (4)B1—B4—B9109.8 (5)
C12—C11—P1118.6 (4)B3—B4—B9108.7 (4)
C13—C12—C11120.2 (6)B8—B4—B962.8 (4)
C13—C12—H12119.9B1—B4—B560.6 (4)
C11—C12—H12119.9B3—B4—B5105.3 (4)
C14—C13—C12120.2 (6)B8—B4—B5108.2 (4)
C14—C13—H13119.9B9—B4—B558.1 (4)
C12—C13—H13119.9B1—B4—H4125 (3)
C13—C14—C15120.2 (6)B3—B4—H4126 (3)
C13—C14—H14119.9B8—B4—H4117 (3)
C15—C14—H14119.9B9—B4—H4116 (3)
C14—C15—C16120.3 (7)B5—B4—H4123 (3)
C14—C15—H15119.9B10—B5—B971.4 (4)
C16—C15—H15119.9B10—B5—B659.8 (4)
C11—C16—C15120.3 (6)B9—B5—B6118.2 (5)
C11—C16—H16119.8B10—B5—B1109.7 (4)
C15—C16—H16119.8B9—B5—B1110.5 (5)
C22—C21—C26118.7 (5)B6—B5—B160.1 (4)
C22—C21—P1123.7 (4)B10—B5—B4117.0 (5)
C26—C21—P1117.6 (4)B9—B5—B460.9 (4)
C21—C22—C23120.2 (6)B6—B5—B4110.3 (4)
C21—C22—H22119.9B1—B5—B458.7 (4)
C23—C22—H22119.9B10—B5—H5114 (3)
C24—C23—C22120.3 (6)B9—B5—H5116 (3)
C24—C23—H23119.9B6—B5—H5117 (3)
C22—C23—H23119.9B1—B5—H5123 (3)
C25—C24—C23119.5 (6)B4—B5—H5122 (3)
C25—C24—H24120.2B11—B6—B1063.0 (4)
C23—C24—H24120.2B11—B6—B261.0 (4)
C24—C25—C26120.4 (6)B10—B6—B2109.7 (4)
C24—C25—H25119.8B11—B6—B5109.1 (4)
C26—C25—H25119.8B10—B6—B558.5 (4)
C25—C26—C21120.8 (6)B2—B6—B5106.3 (4)
C25—C26—H26119.6B11—B6—B1109.9 (5)
C21—C26—H26119.6B10—B6—B1108.8 (4)
C36—C31—C32119.0 (5)B2—B6—B158.9 (4)
C36—C31—P1119.8 (5)B5—B6—B160.3 (4)
C32—C31—P1121.1 (4)B11—B6—H6122 (3)
C33—C32—C31120.6 (6)B10—B6—H6122 (3)
C33—C32—H32119.7B2—B6—H6122 (3)
C31—C32—H32119.7B5—B6—H6121 (3)
C34—C33—C32119.6 (7)B1—B6—H6119 (3)
C34—C33—H33120.2B4—B8—B359.5 (4)
C32—C33—H33120.2B4—B8—B959.1 (4)
C33—C34—C35120.3 (6)B3—B8—B9105.2 (4)
C33—C34—H34119.8B4—B8—Pt7115.3 (4)
C35—C34—H34119.8B3—B8—Pt763.3 (3)
C36—C35—C34120.2 (7)B9—B8—Pt7114.0 (3)
C36—C35—H35119.9B4—B8—H8121 (3)
C34—C35—H35119.9B3—B8—H8121 (3)
C35—C36—C31120.3 (7)B9—B8—H8124 (3)
C35—C36—H36119.8Pt7—B8—H8113 (3)
C31—C36—H36119.8B4—B8—H1U108 (3)
C42—C41—C46118.7 (5)B3—B8—H1U129 (3)
C42—C41—P2119.3 (4)B9—B8—H1U50 (3)
C46—C41—P2122.0 (4)Pt7—B8—H1U86 (3)
C43—C42—C41119.8 (6)H8—B8—H1U107 (4)
C43—C42—H42120.1O1—B9—B5120.0 (5)
C41—C42—H42120.1O1—B9—B4129.9 (5)
C44—C43—C42121.0 (6)B5—B9—B460.9 (4)
C44—C43—H43119.5O1—B9—B8129.0 (5)
C42—C43—H43119.5B5—B9—B8106.8 (4)
C45—C44—C43119.7 (6)B4—B9—B858.2 (3)
C45—C44—H44120.2O1—B9—B10115.3 (5)
C43—C44—H44120.2B5—B9—B1053.8 (3)
C44—C45—C46121.0 (6)B4—B9—B10103.4 (4)
C44—C45—H45119.5B8—B9—B10107.9 (4)
C46—C45—H45119.5O1—B9—H1U108 (3)
C41—C46—C45119.7 (5)B5—B9—H1U129 (3)
C41—C46—H46120.1B4—B9—H1U101 (3)
C45—C46—H46120.1B8—B9—H1U43 (3)
C56—C51—C52119.6 (5)B10—B9—H1U92 (3)
C56—C51—P2118.7 (4)B5—B10—B661.8 (4)
C52—C51—P2121.6 (4)B5—B10—B11107.7 (5)
C51—C52—C53120.0 (6)B6—B10—B1158.0 (4)
C51—C52—H52120.0B5—B10—B954.8 (3)
C53—C52—H52120.0B6—B10—B9106.5 (4)
C54—C53—C52120.2 (7)B11—B10—B9111.3 (4)
C54—C53—H53119.9B5—B10—H10126 (3)
C52—C53—H53119.9B6—B10—H10127 (3)
C55—C54—C53120.3 (6)B11—B10—H10121 (3)
C55—C54—H54119.8B9—B10—H10119 (3)
C53—C54—H54119.8B5—B10—H2U128 (3)
C54—C55—C56119.6 (7)B6—B10—H2U98 (3)
C54—C55—H55120.2B11—B10—H2U41 (3)
C56—C55—H55120.2B9—B10—H2U94 (3)
C51—C56—C55120.2 (6)H10—B10—H2U105 (4)
C51—C56—H56119.9B6—B11—B260.8 (4)
C55—C56—H56119.9B6—B11—B1059.0 (4)
C66—C61—C62118.0 (5)B2—B11—B10106.5 (4)
C66—C61—P2123.4 (4)B6—B11—Pt7118.1 (4)
C62—C61—P2118.6 (4)B2—B11—Pt765.4 (3)
C63—C62—C61120.6 (6)B10—B11—Pt7114.0 (3)
C63—C62—H62119.7B6—B11—H11129 (3)
C61—C62—H62119.7B2—B11—H11131 (3)
C64—C63—C62120.5 (6)B10—B11—H11119 (3)
C64—C63—H63119.7Pt7—B11—H11109 (3)
C62—C63—H63119.7B6—B11—H2U93 (2)
C63—C64—C65119.7 (6)B2—B11—H2U124 (3)
C63—C64—H64120.1B10—B11—H2U35 (2)
C65—C64—H64120.1Pt7—B11—H2U93 (3)
C66—C65—C64120.3 (6)H11—B11—H2U105 (4)
C66—C65—H65119.9Cl1—C1S—Cl2116.7 (8)
C64—C65—H65119.9Cl1—C1S—H1S108.1
C65—C66—C61120.8 (6)Cl2—C1S—H1S108.1
C65—C66—H66119.6Cl1—C1S—H2S108.1
C61—C66—H66119.6Cl2—C1S—H2S108.1
B2—B1—B361.7 (4)H1S—C1S—H2S107.3

Experimental details

(I)(II)(III)
Crystal data
Chemical formula[Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2
Mr912.32982.83982.83
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)293293293
a, b, c (Å)12.850 (2), 25.824 (7), 13.308 (2)11.114 (3), 21.634 (8), 18.990 (8)13.435 (3), 17.864 (4), 19.383 (4)
α, β, γ (°)90, 105.77 (1), 9090, 103.75 (3), 9090, 105.94 (2), 90
V3)4249.9 (15)4435 (3)4473.1 (17)
Z444
Radiation typeMo KαMo KαMo Kα
µ (mm1)3.473.393.36
Crystal size (mm)0.3 × 0.2 × 0.20.42 × 0.27 × 0.070.44 × 0.34 × 0.32
Data collection
DiffractometerRigaku AFC-7R
diffractometer
Enraf-Nonius CAD-4
diffractometer
Rigaku AFC-7R
diffractometer
Absorption correctionψ scans
(North et al., 1968)
ψ scans
(North et al., 1968)
ψ scans
(North et al., 1968)
Tmin, Tmax0.423, 0.5440.330, 0.7970.320, 0.413
No. of measured, independent and
observed [I > 2σ(I)] reflections
7336, 6984, 5607 8141, 7894, 4066 8222, 7865, 6198
Rint0.0480.0810.048
(sin θ/λ)max1)0.5950.5970.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.105, 1.04 0.069, 0.238, 1.38 0.035, 0.096, 1.03
No. of reflections698478947865
No. of parameters495507549
No. of restraints200
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.98, 1.712.19, 3.022.30, 0.99

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992), CAD-4 Manual (Enraf-Nonius, 1988), MSC/AFC Diffractometer Control Software, CAD-4 Manual, TEXSAN (Molecular Structure Corporation, 1985), SDP-Plus (Frenz, 1985), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ZORTEP (Zsolnai, 1994), SHELXL97.

 

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