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Acta Cryst. (2010). B66, 503-514
https://doi.org/10.1107/S0108768110031496
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Bond catastrophes in rhodium complexes: experimental charge-density studies of [Rh(C7H8)(PtBu3)Cl] and [Rh(C7H8)(PCy3)Cl]

H. A. Sparkes, A. B. Chaplin, A. S. Weller and J. A. K. Howard
Rhodium complexes have potential uses in both catalysis and promoting the cleavage of C—C bonds. In order to further our understanding of these species and their potential applications, it is vital to obtain insight into the bonding within the species, particularly the Rh—C interactions, and to this end experimental charge-density studies have been undertaken on the title complexes. High-resolution single-crystal datasets to sin θ/λ = 1.06 Å−1 were obtained at 100 K and analysed using Bader's `Atoms in Molecules' (AIM) approach. The results of the studies have provided unique insights into the bonding involving rhodium and highlight the importance of undertaking such investigations for transition metal compounds.
Keywords: charge density; X-ray diffraction; organometallic; bonding; rhodium complexes.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768110031496/so5039sup1.cif
Contains datablocks publication_text, RhC7H8PtBu3Cl, RhC7H8PCy3Cl

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110031496/so5039RhC7H8PtBu3Clsup2.hkl
Contains datablock RhC7H8PtBu3Cl

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110031496/so5039RhC7H8PCy3Clsup3.hkl
Contains datablock RhC7H8PCy3Cl

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768110031496/so5039sup4.pdf
Extra figures and tables

CCDC references: 798607; 798608

Computing details top

For both structures, data collection: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET) (compiled Apr 18 2008,18:17:43); cell refinement: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET) (compiled Apr 18 2008,18:17:43); data reduction: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET) (compiled Apr 18 2008,18:17:43); program(s) used to solve structure: SHELXS97 (Sheldrick, 1998); program(s) used to refine structure: Volkov et al., (2006); molecular graphics: Volkov et al., (2006); software used to prepare material for publication: Volkov et al., (2006).

(RhC7H8PtBu3Cl) top
Crystal data top
C19H35ClPRhF(000) = 904
Mr = 432.80Dx = 1.505 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 123970 reflections
a = 8.43502 (5) Åθ = 2.9–50.4°
b = 13.97075 (6) ŵ = 1.11 mm−1
c = 16.67516 (7) ÅT = 100 K
β = 103.5630 (5)°Block, red
V = 1910.26 (2) Å30.40 × 0.36 × 0.26 mm
Z = 4
Data collection top
Xcalibur, Sapphire3, Gemini ultra
diffractometer		19057 independent reflections
Radiation source: Enhance (Mo) X-ray Source17131 reflections with I > 3 σ(I)
Graphite monochromatorRint = 0.029
Detector resolution: 16.1511 pixels mm-1θmax = 48.9°, θmin = 2.9°
CCD scansh = −17→17
Absorption correction: analytical
CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)		k = −29→29
Tmin = 0.717, Tmax = 0.799l = −35→35
198001 measured reflections
Refinement top
Refinement on F430 parameters
Least-squares matrix: full0 restraints
R[F2 > 2σ(F2)] = 0.012 w1 = 1/[s2(Fo)]
wR(F2) = 0.011(Δ/σ)max < 0.001
S = 1.30Δρmax = 0.32 e Å−3
16456 reflectionsΔρmin = −0.40 e Å−3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
RH(1)0.614419 (3)0.373422 (2)0.148656 (1)0.009
CL(1)0.356394 (13)0.296758 (8)0.100428 (6)0.018
P(1)0.584554 (9)0.424741 (5)0.283789 (4)0.008
C(1)0.69701 (5)0.30137 (3)0.04903 (2)0.013
C(2)0.63092 (5)0.38978 (3)0.02057 (2)0.013
C(3)0.77198 (5)0.46234 (3)0.03969 (2)0.013
C(4)0.80307 (4)0.46644 (2)0.13427 (2)0.011
C(5)0.86991 (4)0.37619 (3)0.163219 (19)0.011
C(6)0.87970 (5)0.31859 (3)0.08586 (2)0.013
C(7)0.91651 (5)0.39926 (3)0.02952 (2)0.014
C(8)0.78209 (4)0.45424 (2)0.364435 (18)0.011
C(9)0.90108 (4)0.51723 (2)0.32970 (2)0.014
C(10)0.87508 (4)0.36015 (2)0.39196 (2)0.016
C(11)0.75500 (4)0.50782 (3)0.440970 (19)0.016
C(12)0.47654 (4)0.32850 (2)0.333828 (19)0.012
C(13)0.48939 (5)0.33767 (3)0.42721 (2)0.017
C(14)0.54697 (5)0.23069 (2)0.31632 (2)0.017
C(15)0.29263 (4)0.32519 (3)0.29301 (2)0.017
C(16)0.45233 (4)0.53735 (2)0.268235 (18)0.011
C(17)0.55391 (4)0.62318 (2)0.25070 (2)0.016
C(18)0.31657 (4)0.52363 (3)0.18922 (2)0.017
C(19)0.37342 (4)0.56541 (2)0.33940 (2)0.015
H(1)0.6336550.2321920.0369030.028
H(2)0.5083840.402935−0.0184440.023
H(3)0.7525490.5307480.0061580.029
H(4)0.8172430.5349770.167670.021
H(5)0.9461750.3607240.2249660.024
H(6)0.9641080.25740.0968090.024
H(7A)0.9079190.376231−0.034440.023
H(7B)1.0361430.4328380.053690.03
H(9A)0.8488860.5833190.3018330.03
H(9B)0.999520.5356080.3815630.031
H(9C)0.9498330.4810630.2835060.027
H(10A)0.8864910.3163820.3402180.023
H(10B)0.997430.3781440.4251140.029
H(10C)0.8243170.317870.4340740.024
H(11A)0.7167130.5806740.4257350.028
H(11B)0.6682170.4738220.4702020.031
H(11C)0.868710.5049680.4870570.036
H(13A)0.4413670.404440.4440410.027
H(13B)0.611590.3257830.4637310.025
H(13C)0.4132410.2827250.4441340.031
H(14A)0.531560.2194760.2508610.037
H(14B)0.676020.2237510.3432010.031
H(14C)0.4861830.1739790.3414150.032
H(15A)0.2653440.3153740.2269480.029
H(15B)0.224080.3868440.3046340.027
H(15C)0.2415530.265220.3191890.031
H(17A)0.614770.6070320.2020970.031
H(17B)0.6412970.6492580.3043150.023
H(17C)0.4729230.6830960.2316620.032
H(18A)0.3670880.5120530.1361950.03
H(18B)0.2329270.4655050.1907910.033
H(18C)0.2445720.5883290.1790580.035
H(19A)0.3031320.6301510.3234610.034
H(19B)0.4598960.5788880.3971850.028
H(19C)0.2900560.5110670.3505270.03
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
RH(1)0.008908 (11)0.009296 (10)0.007749 (9)−0.000830 (7)0.002308 (6)−0.000872 (7)
CL(1)0.01389 (4)0.02263 (4)0.01613 (4)−0.00683 (3)0.00357 (3)−0.00589 (3)
P(1)0.00757 (3)0.00781 (3)0.00760 (2)−0.000207 (19)0.001901 (19)−0.000300 (18)
C(1)0.01645 (15)0.01240 (12)0.01183 (11)−0.00021 (10)0.00445 (10)−0.00246 (9)
C(2)0.01345 (14)0.01630 (13)0.00962 (10)0.00152 (10)0.00237 (9)0.00018 (9)
C(3)0.01478 (14)0.01277 (12)0.01168 (11)0.00224 (10)0.00557 (10)0.00283 (9)
C(4)0.01227 (13)0.01041 (11)0.01166 (11)−0.00036 (9)0.00404 (9)−0.00026 (8)
C(5)0.01097 (12)0.01262 (11)0.01029 (10)0.00114 (10)0.00272 (8)0.00086 (9)
C(6)0.01468 (14)0.01214 (12)0.01254 (11)0.00306 (10)0.00563 (10)0.00087 (9)
C(7)0.01537 (15)0.01610 (13)0.01376 (12)0.00246 (11)0.00784 (11)0.00226 (10)
C(8)0.01001 (11)0.01332 (10)0.00938 (9)−0.00005 (8)0.00078 (8)−0.00129 (8)
C(9)0.01113 (12)0.01740 (12)0.01450 (11)−0.00352 (9)0.00224 (9)−0.00257 (9)
C(10)0.01356 (13)0.01784 (12)0.01456 (11)0.00402 (9)0.00061 (9)0.00173 (9)
C(11)0.01497 (13)0.01961 (13)0.01126 (10)−0.00063 (10)0.00174 (9)−0.00461 (9)
C(12)0.01336 (12)0.01053 (10)0.01295 (10)−0.00141 (8)0.00587 (9)0.00015 (8)
C(13)0.02213 (15)0.01739 (13)0.01348 (11)−0.00106 (11)0.00873 (10)0.00204 (9)
C(14)0.02113 (15)0.00950 (10)0.02186 (13)−0.00025 (9)0.00905 (11)0.00045 (9)
C(15)0.01281 (13)0.01747 (12)0.02060 (13)−0.00472 (10)0.00656 (10)−0.00319 (10)
C(16)0.01119 (11)0.01008 (9)0.01194 (10)0.00180 (8)0.00217 (8)−0.00019 (7)
C(17)0.01772 (13)0.01032 (10)0.02013 (12)0.00110 (9)0.00506 (10)0.00209 (9)
C(18)0.01474 (13)0.01748 (12)0.01494 (11)0.00391 (10)−0.00172 (9)−0.00003 (9)
C(19)0.01457 (13)0.01550 (11)0.01699 (12)0.00288 (9)0.00565 (10)−0.00313 (9)
Geometric parameters (Å, º) top
RH(1)—CL(1)2.3895 (1)C(10)—H(10A)1.0800
RH(1)—P(1)2.4334 (1)C(10)—H(10B)1.0800
RH(1)—C(1)2.1911 (3)C(10)—H(10C)1.0800
RH(1)—C(2)2.1846 (3)C(11)—H(11A)1.0800
RH(1)—C(4)2.1113 (3)C(11)—H(11B)1.0800
RH(1)—C(5)2.1117 (3)C(11)—H(11C)1.0800
P(1)—C(8)1.9245 (3)C(12)—C(13)1.5407 (4)
P(1)—C(12)1.9211 (3)C(12)—C(14)1.5449 (5)
P(1)—C(16)1.9107 (3)C(12)—C(15)1.5416 (5)
C(1)—C(2)1.3919 (5)C(13)—H(13A)1.0800
C(1)—C(6)1.5381 (6)C(13)—H(13B)1.0800
C(1)—H(1)1.1000C(13)—H(13C)1.0800
C(2)—C(3)1.5386 (5)C(14)—H(14A)1.0800
C(2)—H(2)1.1000C(14)—H(14B)1.0800
C(3)—C(4)1.5379 (5)C(14)—H(14C)1.0800
C(3)—C(7)1.5455 (5)C(15)—H(15A)1.0800
C(3)—H(3)1.1000C(15)—H(15B)1.0800
C(4)—C(5)1.4188 (5)C(15)—H(15C)1.0800
C(4)—H(4)1.1000C(16)—C(17)1.5411 (5)
C(5)—C(6)1.5390 (5)C(16)—C(18)1.5415 (4)
C(5)—H(5)1.1000C(16)—C(19)1.5412 (5)
C(6)—C(7)1.5447 (5)C(17)—H(17A)1.0800
C(6)—H(6)1.1000C(17)—H(17B)1.0800
C(7)—H(7A)1.1000C(17)—H(17C)1.0800
C(7)—H(7B)1.1000C(18)—H(18A)1.0800
C(8)—C(9)1.5460 (5)C(18)—H(18B)1.0800
C(8)—C(10)1.5444 (4)C(18)—H(18C)1.0800
C(8)—C(11)1.5421 (4)C(19)—H(19A)1.0800
C(9)—H(9A)1.0800C(19)—H(19B)1.0800
C(9)—H(9B)1.0800C(19)—H(19C)1.0800
C(9)—H(9C)1.0800
CL(1)—RH(1)—P(1)99.195 (3)C(10)—C(8)—C(11)109.31 (3)
CL(1)—RH(1)—C(1)88.016 (11)C(8)—C(9)—H(9A)114.39
CL(1)—RH(1)—C(2)88.835 (11)C(8)—C(9)—H(9B)106.27
CL(1)—RH(1)—C(4)152.738 (10)C(8)—C(9)—H(9C)112.96
CL(1)—RH(1)—C(5)150.614 (10)H(9A)—C(9)—H(9B)107.49
P(1)—RH(1)—C(1)163.294 (10)H(9A)—C(9)—H(9C)106.14
P(1)—RH(1)—C(2)156.732 (10)H(9B)—C(9)—H(9C)109.42
P(1)—RH(1)—C(4)99.690 (9)C(8)—C(10)—H(10A)112.25
P(1)—RH(1)—C(5)102.274 (9)C(8)—C(10)—H(10B)108.16
C(1)—RH(1)—C(2)37.094 (14)C(8)—C(10)—H(10C)114.05
C(1)—RH(1)—C(4)79.309 (14)H(10A)—C(10)—H(10B)106.69
C(1)—RH(1)—C(5)66.312 (14)H(10A)—C(10)—H(10C)109.46
C(2)—RH(1)—C(4)66.548 (14)H(10B)—C(10)—H(10C)105.75
C(2)—RH(1)—C(5)79.236 (14)C(8)—C(11)—H(11A)110.91
C(4)—RH(1)—C(5)39.263 (13)C(8)—C(11)—H(11B)114.06
RH(1)—P(1)—C(8)116.711 (10)C(8)—C(11)—H(11C)106.96
RH(1)—P(1)—C(12)111.016 (10)H(11A)—C(11)—H(11B)108.89
RH(1)—P(1)—C(16)107.506 (10)H(11A)—C(11)—H(11C)111.64
C(8)—P(1)—C(12)105.512 (14)H(11B)—C(11)—H(11C)104.21
C(8)—P(1)—C(16)107.500 (14)P(1)—C(12)—C(13)116.92 (2)
C(12)—P(1)—C(16)108.303 (15)P(1)—C(12)—C(14)107.12 (2)
RH(1)—C(1)—C(2)71.20 (2)P(1)—C(12)—C(15)111.09 (2)
RH(1)—C(1)—C(6)95.30 (2)C(13)—C(12)—C(14)108.99 (3)
RH(1)—C(1)—H(1)108.41C(13)—C(12)—C(15)105.89 (3)
C(2)—C(1)—C(6)106.32 (3)C(14)—C(12)—C(15)106.37 (3)
C(2)—C(1)—H(1)125.34C(12)—C(13)—H(13A)113.12
C(6)—C(1)—H(1)127.51C(12)—C(13)—H(13B)112.88
RH(1)—C(2)—C(1)71.71 (2)C(12)—C(13)—H(13C)107.44
RH(1)—C(2)—C(3)95.15 (2)H(13A)—C(13)—H(13B)110.66
RH(1)—C(2)—H(2)109.23H(13A)—C(13)—H(13C)105.29
C(1)—C(2)—C(3)106.59 (3)H(13B)—C(13)—H(13C)106.91
C(1)—C(2)—H(2)126.56C(12)—C(14)—H(14A)111.03
C(3)—C(2)—H(2)125.89C(12)—C(14)—H(14B)113.32
C(2)—C(3)—C(4)100.06 (3)C(12)—C(14)—H(14C)109.70
C(2)—C(3)—C(7)101.14 (3)H(14A)—C(14)—H(14B)106.09
C(2)—C(3)—H(3)116.83H(14A)—C(14)—H(14C)109.24
C(4)—C(3)—C(7)100.64 (3)H(14B)—C(14)—H(14C)107.29
C(4)—C(3)—H(3)117.27C(12)—C(15)—H(15A)113.94
C(7)—C(3)—H(3)117.84C(12)—C(15)—H(15B)114.99
RH(1)—C(4)—C(3)98.15 (2)C(12)—C(15)—H(15C)107.48
RH(1)—C(4)—C(5)70.39 (2)H(15A)—C(15)—H(15B)106.82
RH(1)—C(4)—H(4)118.27H(15A)—C(15)—H(15C)107.70
C(3)—C(4)—C(5)105.92 (3)H(15B)—C(15)—H(15C)105.37
C(3)—C(4)—H(4)121.59P(1)—C(16)—C(17)109.49 (2)
C(5)—C(4)—H(4)127.87P(1)—C(16)—C(18)107.85 (2)
RH(1)—C(5)—C(4)70.35 (2)P(1)—C(16)—C(19)116.66 (2)
RH(1)—C(5)—C(6)98.51 (2)C(17)—C(16)—C(18)105.62 (3)
RH(1)—C(5)—H(5)117.45C(17)—C(16)—C(19)107.94 (3)
C(4)—C(5)—C(6)105.94 (3)C(18)—C(16)—C(19)108.74 (3)
C(4)—C(5)—H(5)126.27C(16)—C(17)—H(17A)111.30
C(6)—C(5)—H(5)123.18C(16)—C(17)—H(17B)114.04
C(1)—C(6)—C(5)99.83 (3)C(16)—C(17)—H(17C)108.50
C(1)—C(6)—C(7)101.34 (3)H(17A)—C(17)—H(17B)109.84
C(1)—C(6)—H(6)119.58H(17A)—C(17)—H(17C)108.70
C(5)—C(6)—C(7)100.73 (3)H(17B)—C(17)—H(17C)104.10
C(5)—C(6)—H(6)115.28C(16)—C(18)—H(18A)111.21
C(7)—C(6)—H(6)116.96C(16)—C(18)—H(18B)115.56
C(3)—C(7)—C(6)94.19 (3)C(16)—C(18)—H(18C)107.92
C(3)—C(7)—H(7A)113.51H(18A)—C(18)—H(18B)107.02
C(3)—C(7)—H(7B)113.33H(18A)—C(18)—H(18C)108.19
C(6)—C(7)—H(7A)113.53H(18B)—C(18)—H(18C)106.65
C(6)—C(7)—H(7B)112.72C(16)—C(19)—H(19A)109.56
H(7A)—C(7)—H(7B)109.04C(16)—C(19)—H(19B)114.08
P(1)—C(8)—C(9)113.07 (2)C(16)—C(19)—H(19C)111.70
P(1)—C(8)—C(10)108.76 (2)H(19A)—C(19)—H(19B)106.88
P(1)—C(8)—C(11)114.22 (2)H(19A)—C(19)—H(19C)106.80
C(9)—C(8)—C(10)105.47 (3)H(19B)—C(19)—H(19C)107.46
C(9)—C(8)—C(11)105.60 (3)
(RhC7H8PCy3Cl) top
Crystal data top
C25H41ClPRhZ = 4
Mr = 510.91F(000) = 1072
Monoclinic, P21/nDx = 1.448 Mg m−3
Hall symbol: -P 2ynMo Kα radiation, λ = 0.71073 Å
a = 10.21309 (7) ÅCell parameters from 46899 reflections
b = 15.82275 (8) Åθ = 2.6–50.4°
c = 14.64123 (8) ŵ = 0.92 mm−1
β = 97.7784 (6)°T = 100 K
V = 2344.24 (5) Å3Block, orange
Data collection top
Xcalibur, Sapphire3, Gemini ultra
diffractometer		24737 independent reflections
Radiation source: Enhance (Mo) X-ray Source21046 reflections with I > 3 σ(I)
Graphite monochromatorRint = 0.048
Detector resolution: 16.1511 pixels mm-1θmax = 48.9°, θmin = 2.6°
CCD scansh = −21→21
Absorption correction: analytical
CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)		k = −33→33
l = −31→31
297875 measured reflections
Refinement top
Refinement on F517 parameters
Least-squares matrix: full0 restraints
R[F2 > 2σ(F2)] = 0.016 w1 = 1/[s2(Fo)]
wR(F2) = 0.013(Δ/σ)max < 0.001
S = 1.23Δρmax = 0.41 e Å−3
18953 reflectionsΔρmin = −0.39 e Å−3
Special details top

Experimental. Absorption corrections were applied to the two datasets separately.

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
RH(1)0.243360 (3)0.581601 (2)0.456144 (2)0.008
CL(1)0.306364 (11)0.685410 (6)0.567990 (7)0.016
P(1)0.194337 (9)0.678935 (5)0.338331 (6)0.008
C(1)0.34441 (5)0.47386 (3)0.53516 (3)0.013
C(2)0.21672 (5)0.47989 (3)0.55645 (3)0.013
C(3)0.12958 (4)0.42551 (3)0.48501 (3)0.012
C(4)0.13265 (4)0.47861 (3)0.39703 (3)0.011
C(5)0.26363 (5)0.47310 (3)0.37556 (3)0.012
C(6)0.33866 (4)0.41568 (3)0.45039 (3)0.013
C(7)0.22731 (5)0.35412 (3)0.46875 (3)0.014
C(8)0.09143 (4)0.62939 (2)0.23835 (3)0.011
C(9)−0.05388 (4)0.62125 (2)0.25449 (3)0.013
C(10)−0.12606 (4)0.55725 (3)0.18735 (3)0.017
C(11)−0.11880 (5)0.58339 (3)0.08753 (3)0.02
C(12)0.02483 (5)0.59788 (3)0.07137 (3)0.019
C(13)0.09579 (4)0.66209 (3)0.13988 (3)0.014
C(14)0.34204 (4)0.71671 (2)0.28971 (3)0.011
C(15)0.42039 (4)0.64327 (2)0.25542 (3)0.014
C(16)0.53376 (4)0.67671 (3)0.20700 (3)0.017
C(17)0.62675 (5)0.73288 (3)0.27111 (3)0.019
C(18)0.55030 (5)0.80435 (3)0.31031 (4)0.02
C(19)0.43443 (4)0.77161 (3)0.35664 (3)0.017
C(20)0.11715 (4)0.77916 (2)0.36938 (3)0.01
C(21)0.00330 (4)0.76821 (2)0.42709 (3)0.013
C(22)−0.04077 (5)0.85435 (3)0.45988 (3)0.016
C(23)−0.08022 (5)0.91456 (3)0.37914 (3)0.018
C(24)0.03186 (5)0.92464 (2)0.32070 (3)0.017
C(25)0.07690 (4)0.83886 (2)0.28764 (3)0.014
H(1)0.4346680.4977690.5766440.03
H(2)0.1855490.509610.6179120.028
H(3)0.0307050.4088210.5011520.022
H(4)0.0436010.4900310.3473260.022
H(5)0.2966990.4821580.3077870.027
H(6)0.4326390.3889660.4349380.022
H(7A)0.2540740.314170.5299170.033
H(7B)0.1904930.3149360.4086740.03
H(8)0.1323640.5650320.2396010.022
H(9A)−0.0615320.6028770.3260350.022
H(9B)−0.1046390.6821350.2405180.026
H(10A)−0.0797570.4948440.2002640.029
H(10B)−0.2288560.5497750.2006770.031
H(11A)−0.1647570.5339180.041030.035
H(11B)−0.1742250.6423680.0715430.032
H(12A)0.0785270.5375970.0813280.028
H(12B)0.0262760.6197470.0001970.033
H(13A)0.198220.6701960.1259780.026
H(13B)0.0474980.7240910.1289050.025
H(14)0.3029360.755570.229890.02
H(15A)0.3546010.6034140.207710.027
H(15B)0.4609970.6039580.3145010.029
H(16A)0.4939310.714260.1463150.029
H(16B)0.5892220.6236120.1825310.028
H(17A)0.703960.7594380.2339910.032
H(17B)0.6751340.6935230.3278090.029
H(18A)0.5114650.8464510.2532240.037
H(18B)0.6199990.8397480.3600350.042
H(19A)0.3795070.8258570.3791420.039
H(19B)0.4683290.7339850.4185210.028
H(20)0.1979280.808860.4157040.022
H(21A)0.033840.7275380.4871340.026
H(21B)−0.0825230.7381690.3862360.024
H(22A)0.0415240.8815430.5069720.029
H(22B)−0.1239910.8457510.4994410.034
H(23A)−0.108190.9762480.4052560.034
H(23B)−0.1680930.8896130.3357720.035
H(24A)0.1157160.9572010.3609920.032
H(24B)0.0004440.9652620.2607590.033
H(25A)0.1596550.8483590.2478420.029
H(25B)−0.0044360.8097640.2412670.025
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
RH(1)0.008823 (13)0.007688 (11)0.008502 (12)−0.000107 (10)0.001038 (7)0.000655 (9)
CL(1)0.01966 (5)0.01316 (4)0.01366 (4)−0.00116 (3)−0.00131 (3)−0.00297 (3)
P(1)0.00850 (4)0.00767 (3)0.00924 (3)0.00002 (2)0.00122 (3)0.00073 (2)
C(1)0.01246 (17)0.01237 (14)0.01447 (16)−0.00012 (13)−0.00078 (13)0.00288 (12)
C(2)0.01543 (18)0.01242 (14)0.01137 (15)−0.00102 (13)0.00285 (13)0.00154 (12)
C(3)0.01227 (15)0.01092 (14)0.01463 (15)−0.00137 (12)0.00306 (12)0.00196 (12)
C(4)0.01141 (15)0.01028 (13)0.01240 (15)−0.00088 (11)0.00052 (12)0.00068 (11)
C(5)0.01413 (16)0.00997 (13)0.01201 (15)0.00081 (12)0.00376 (13)0.00039 (11)
C(6)0.01225 (15)0.01035 (13)0.01715 (16)0.00186 (13)0.00289 (13)0.00192 (13)
C(7)0.01628 (18)0.00943 (13)0.01737 (18)−0.00022 (13)0.00249 (14)0.00223 (12)
C(8)0.01117 (13)0.01034 (11)0.01056 (12)0.00045 (10)0.00005 (10)0.00036 (9)
C(9)0.01060 (13)0.01187 (12)0.01558 (14)−0.00037 (10)0.00010 (11)−0.00103 (10)
C(10)0.01425 (16)0.01343 (13)0.02149 (18)−0.00174 (12)−0.00264 (13)−0.00259 (12)
C(11)0.02043 (18)0.01766 (16)0.01839 (17)0.00111 (15)−0.00679 (14)−0.00371 (14)
C(12)0.02352 (19)0.01890 (16)0.01246 (15)0.00161 (14)−0.00183 (13)−0.00234 (12)
C(13)0.01722 (16)0.01497 (13)0.01071 (13)−0.00003 (12)0.00006 (11)0.00152 (10)
C(14)0.01020 (13)0.01073 (12)0.01203 (13)−0.00011 (10)0.00271 (10)0.00052 (10)
C(15)0.01279 (14)0.01310 (13)0.01575 (15)0.00226 (11)0.00353 (11)0.00008 (11)
C(16)0.01438 (15)0.02170 (17)0.01539 (15)0.00320 (13)0.00571 (12)0.00051 (12)
C(17)0.01149 (15)0.0274 (2)0.01829 (18)−0.00029 (14)0.00450 (13)0.00183 (15)
C(18)0.01515 (17)0.02249 (18)0.0247 (2)−0.00741 (14)0.00787 (15)−0.00379 (15)
C(19)0.01361 (15)0.02105 (16)0.01826 (16)−0.00651 (13)0.00584 (13)−0.00611 (13)
C(20)0.01088 (13)0.00852 (11)0.01238 (13)0.00065 (9)0.00271 (10)0.00108 (9)
C(21)0.01359 (14)0.01081 (12)0.01506 (14)0.00108 (10)0.00536 (11)0.00163 (10)
C(22)0.01934 (17)0.01381 (14)0.01733 (16)0.00424 (12)0.00678 (13)0.00033 (11)
C(23)0.01879 (17)0.01439 (14)0.02220 (18)0.00651 (14)0.00597 (14)0.00271 (14)
C(24)0.02034 (17)0.01008 (13)0.02248 (17)0.00286 (12)0.00656 (14)0.00394 (12)
C(25)0.01691 (15)0.01106 (12)0.01514 (14)0.00284 (11)0.00463 (12)0.00358 (10)
Geometric parameters (Å, º) top
RH(1)—CL(1)2.3469 (1)C(12)—H(12A)1.1000
RH(1)—P(1)2.3160 (1)C(12)—H(12B)1.1000
RH(1)—C(1)2.2330 (4)C(13)—H(13A)1.1000
RH(1)—C(2)2.2201 (4)C(13)—H(13B)1.1000
RH(1)—C(4)2.1019 (4)C(14)—C(15)1.5334 (5)
RH(1)—C(5)2.1091 (4)C(14)—C(19)1.5346 (6)
P(1)—C(8)1.8561 (4)C(14)—H(14)1.1000
P(1)—C(14)1.8522 (4)C(15)—C(16)1.5315 (6)
P(1)—C(20)1.8547 (4)C(15)—H(15A)1.1000
C(1)—C(2)1.3847 (7)C(15)—H(15B)1.1000
C(1)—C(6)1.5401 (7)C(16)—C(17)1.5269 (7)
C(1)—H(1)1.1000C(16)—H(16A)1.1000
C(2)—C(3)1.5408 (6)C(16)—H(16B)1.1000
C(2)—H(2)1.1000C(17)—C(18)1.5294 (7)
C(3)—C(4)1.5418 (6)C(17)—H(17A)1.1000
C(3)—C(7)1.5470 (6)C(17)—H(17B)1.1000
C(3)—H(3)1.1000C(18)—C(19)1.5318 (6)
C(4)—C(5)1.4177 (6)C(18)—H(18A)1.1000
C(4)—H(4)1.1000C(18)—H(18B)1.1000
C(5)—C(6)1.5445 (6)C(19)—H(19A)1.1000
C(5)—H(5)1.1000C(19)—H(19B)1.1000
C(6)—C(7)1.5483 (6)C(20)—C(21)1.5370 (5)
C(6)—H(6)1.1000C(20)—C(25)1.5363 (5)
C(7)—H(7A)1.1000C(20)—H(20)1.1000
C(7)—H(7B)1.1000C(21)—C(22)1.5327 (5)
C(8)—C(9)1.5396 (5)C(21)—H(21A)1.1000
C(8)—C(13)1.5380 (5)C(21)—H(21B)1.1000
C(8)—H(8)1.1000C(22)—C(23)1.5291 (6)
C(9)—C(10)1.5294 (6)C(22)—H(22A)1.1000
C(9)—H(9A)1.1000C(22)—H(22B)1.1000
C(9)—H(9B)1.1000C(23)—C(24)1.5276 (6)
C(10)—C(11)1.5303 (7)C(23)—H(23A)1.1000
C(10)—H(10A)1.1000C(23)—H(23B)1.1000
C(10)—H(10B)1.1000C(24)—C(25)1.5324 (6)
C(11)—C(12)1.5344 (7)C(24)—H(24A)1.1000
C(11)—H(11A)1.1000C(24)—H(24B)1.1000
C(11)—H(11B)1.1000C(25)—H(25A)1.1000
C(12)—C(13)1.5384 (6)C(25)—H(25B)1.1000
CL(1)—RH(1)—P(1)93.758 (3)C(12)—C(11)—H(11A)110.34
CL(1)—RH(1)—C(1)96.253 (13)C(12)—C(11)—H(11B)108.40
CL(1)—RH(1)—C(2)95.295 (12)H(11A)—C(11)—H(11B)107.93
CL(1)—RH(1)—C(4)155.679 (12)C(11)—C(12)—C(13)111.95 (4)
CL(1)—RH(1)—C(5)157.159 (13)C(11)—C(12)—H(12A)108.66
P(1)—RH(1)—C(1)158.692 (13)C(11)—C(12)—H(12B)109.20
P(1)—RH(1)—C(2)160.251 (13)C(13)—C(12)—H(12A)107.68
P(1)—RH(1)—C(4)99.139 (12)C(13)—C(12)—H(12B)110.15
P(1)—RH(1)—C(5)98.756 (12)H(12A)—C(12)—H(12B)109.14
C(1)—RH(1)—C(2)36.231 (17)C(8)—C(13)—C(12)108.56 (3)
C(1)—RH(1)—C(4)78.851 (17)C(8)—C(13)—H(13A)111.21
C(1)—RH(1)—C(5)66.110 (18)C(8)—C(13)—H(13B)111.57
C(2)—RH(1)—C(4)66.618 (17)C(12)—C(13)—H(13A)109.40
C(2)—RH(1)—C(5)79.060 (17)C(12)—C(13)—H(13B)109.35
C(4)—RH(1)—C(5)39.348 (17)P(1)—C(14)—C(15)111.70 (3)
RH(1)—P(1)—C(8)110.415 (12)P(1)—C(14)—C(19)113.55 (3)
RH(1)—P(1)—C(14)113.307 (13)P(1)—C(14)—H(14)105.05
RH(1)—P(1)—C(20)116.242 (12)C(15)—C(14)—C(19)109.57 (3)
C(8)—P(1)—C(14)103.694 (18)C(15)—C(14)—H(14)108.19
C(8)—P(1)—C(20)109.894 (19)C(19)—C(14)—H(14)108.52
C(14)—P(1)—C(20)102.341 (17)C(14)—C(15)—C(16)110.53 (3)
RH(1)—C(1)—C(2)71.38 (3)C(14)—C(15)—H(15A)109.96
RH(1)—C(1)—C(6)94.25 (3)C(14)—C(15)—H(15B)109.20
RH(1)—C(1)—H(1)108.51C(16)—C(15)—H(15A)109.83
C(2)—C(1)—C(6)106.76 (4)C(16)—C(15)—H(15B)109.35
C(2)—C(1)—H(1)126.62H(15A)—C(15)—H(15B)107.94
C(6)—C(1)—H(1)126.03C(15)—C(16)—C(17)111.27 (4)
RH(1)—C(2)—C(1)72.39 (3)C(15)—C(16)—H(16A)109.90
RH(1)—C(2)—C(3)93.84 (3)C(15)—C(16)—H(16B)109.99
RH(1)—C(2)—H(2)107.84C(17)—C(16)—H(16A)108.26
C(1)—C(2)—C(3)106.49 (4)C(17)—C(16)—H(16B)109.87
C(1)—C(2)—H(2)126.83H(16A)—C(16)—H(16B)107.45
C(3)—C(2)—H(2)126.12C(16)—C(17)—C(18)110.76 (4)
C(2)—C(3)—C(4)100.82 (3)C(16)—C(17)—H(17A)110.27
C(2)—C(3)—C(7)100.76 (4)C(16)—C(17)—H(17B)108.23
C(2)—C(3)—H(3)116.80C(18)—C(17)—H(17A)109.86
C(4)—C(3)—C(7)100.52 (3)C(18)—C(17)—H(17B)109.59
C(4)—C(3)—H(3)115.69H(17A)—C(17)—H(17B)108.07
RH(1)—C(4)—C(3)98.57 (3)C(17)—C(18)—C(19)112.37 (4)
RH(1)—C(4)—C(5)70.60 (2)C(17)—C(18)—H(18A)108.20
RH(1)—C(4)—H(4)119.70C(17)—C(18)—H(18B)107.90
C(3)—C(4)—C(5)106.17 (4)C(19)—C(18)—H(18A)108.70
C(3)—C(4)—H(4)122.25C(19)—C(18)—H(18B)110.40
C(5)—C(4)—H(4)125.72H(18A)—C(18)—H(18B)109.20
RH(1)—C(5)—C(4)70.05 (2)C(14)—C(19)—C(18)110.72 (4)
RH(1)—C(5)—C(6)99.13 (3)C(14)—C(19)—H(19A)109.79
RH(1)—C(5)—H(5)117.65C(14)—C(19)—H(19B)108.50
C(4)—C(5)—C(6)105.74 (4)C(18)—C(19)—H(19A)108.95
C(4)—C(5)—H(5)127.32C(18)—C(19)—H(19B)111.83
C(6)—C(5)—H(5)122.21H(19A)—C(19)—H(19B)106.98
C(1)—C(6)—C(5)100.45 (3)P(1)—C(20)—C(21)114.63 (2)
C(1)—C(6)—C(7)100.64 (4)P(1)—C(20)—C(25)114.36 (3)
C(1)—C(6)—H(6)117.15P(1)—C(20)—H(20)102.02
C(5)—C(6)—C(7)100.82 (4)C(21)—C(20)—C(25)110.80 (3)
C(5)—C(6)—H(6)116.30C(21)—C(20)—H(20)105.62
C(7)—C(6)—H(6)118.42C(25)—C(20)—H(20)108.48
C(3)—C(7)—C(6)94.12 (3)C(20)—C(21)—C(22)110.37 (3)
C(3)—C(7)—H(7A)112.87C(20)—C(21)—H(21A)110.59
C(3)—C(7)—H(7B)112.13C(20)—C(21)—H(21B)110.87
C(6)—C(7)—H(7A)113.30C(22)—C(21)—H(21A)109.47
C(6)—C(7)—H(7B)113.28C(22)—C(21)—H(21B)107.96
H(3)—C(7)—H(7A)100.16H(21A)—C(21)—H(21B)107.49
H(3)—C(7)—H(7B)99.44C(21)—C(22)—C(23)111.69 (4)
H(7A)—C(7)—H(7B)110.33C(21)—C(22)—H(22A)108.19
P(1)—C(8)—C(9)111.64 (3)C(21)—C(22)—H(22B)109.61
P(1)—C(8)—C(13)120.80 (3)C(23)—C(22)—H(22A)109.87
P(1)—C(8)—H(8)101.80C(23)—C(22)—H(22B)110.04
C(9)—C(8)—C(13)108.85 (3)H(22A)—C(22)—H(22B)107.31
C(9)—C(8)—H(8)106.98C(22)—C(23)—C(24)111.04 (4)
C(13)—C(8)—H(8)105.54C(22)—C(23)—H(23A)109.74
C(8)—C(9)—C(10)110.33 (3)C(22)—C(23)—H(23B)109.37
C(8)—C(9)—H(9A)111.27C(24)—C(23)—H(23A)110.59
C(8)—C(9)—H(9B)109.75C(24)—C(23)—H(23B)109.20
C(10)—C(9)—H(9A)110.30H(23A)—C(23)—H(23B)106.80
C(10)—C(9)—H(9B)106.63C(23)—C(24)—C(25)111.36 (3)
H(8)—C(9)—H(9A)99.57C(23)—C(24)—H(24A)109.67
H(8)—C(9)—H(9B)138.50C(23)—C(24)—H(24B)110.38
H(9A)—C(9)—H(9B)108.42C(25)—C(24)—H(24A)109.82
C(9)—C(10)—C(11)110.70 (4)C(25)—C(24)—H(24B)109.45
C(9)—C(10)—H(10A)108.98H(24A)—C(24)—H(24B)106.02
C(9)—C(10)—H(10B)110.22C(20)—C(25)—C(24)111.01 (3)
C(11)—C(10)—H(10A)109.36C(20)—C(25)—H(25A)110.67
C(11)—C(10)—H(10B)111.68C(20)—C(25)—H(25B)108.88
H(10A)—C(10)—H(10B)105.75C(24)—C(25)—H(25A)109.35
C(10)—C(11)—C(12)111.02 (4)C(24)—C(25)—H(25B)109.37
C(10)—C(11)—H(11A)109.08H(25A)—C(25)—H(25B)107.49
C(10)—C(11)—H(11B)110.02
 

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