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A modified Laue method is shown to produce excited-state structures at atomic resolution of a quality competitive with those from monochromatic experiments. The much faster data collection allows the use of only one or a few X-ray pulses per data frame, which minimizes crystal damage caused by laser exposure of the samples and optimizes the attainable time resolution. The method has been applied to crystals of the α-modification of Rh2(μ-PNP)2(PNP)2 (BPh4)2 [PNP = CH3N(P(OCH3)2)2, Ph = phenyl]. The experimental results show a shortening of the Rh—Rh distance in the organometallic complex of 0.136 (8) Å on excitation and are quantitatively supported by quantum-mechanical (QM)/molecular-mechanics (MM) theoretical calculations which take into account the confining effect of the crystal environment, but not by theoretical results on the isolated complex, demonstrating the defining effect of the crystal matrix.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108767311011883/sh5129sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108767311011883/sh5129Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108767311011883/sh5129sup3.pdf
Details of the six data sets

CCDC reference: 841921

Computing details top

Data collection: Bruker APEX2; cell refinement: Bruker SAINT; data reduction: Bruker SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
C20H60N4O16P8Rh2·2(C24H20B)F(000) = 3536
Mr = 1704.72Dx = 1.425 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 13.9783 (3) ÅCell parameters from 14691 reflections
b = 20.2046 (5) Åθ = 1.2–27.0°
c = 28.1465 (7) ŵ = 0.64 mm1
β = 90.842 (1)°T = 225 K
V = 7948.4 (3) Å3Prismatic, red
Z = 40.31 × 0.18 × 0.10 mm
Data collection top
Bruker APEX-II CCD
diffractometer
17345 independent reflections
Radiation source: RIGAKU rotating anode14691 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
ϕ and ω scansθmax = 27.0°, θmin = 1.2°
Absorption correction: numerical
BRUKER SADABS
h = 1717
Tmin = 0.826, Tmax = 0.939k = 025
17345 measured reflectionsl = 035
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0311P)2 + 6.6036P]
where P = (Fo2 + 2Fc2)/3
17345 reflections(Δ/σ)max = 0.001
905 parametersΔρmax = 1.12 e Å3
0 restraintsΔρmin = 0.40 e Å3
Crystal data top
C20H60N4O16P8Rh2·2(C24H20B)V = 7948.4 (3) Å3
Mr = 1704.72Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.9783 (3) ŵ = 0.64 mm1
b = 20.2046 (5) ÅT = 225 K
c = 28.1465 (7) Å0.31 × 0.18 × 0.10 mm
β = 90.842 (1)°
Data collection top
Bruker APEX-II CCD
diffractometer
17345 independent reflections
Absorption correction: numerical
BRUKER SADABS
14691 reflections with I > 2σ(I)
Tmin = 0.826, Tmax = 0.939Rint = 0.000
17345 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.081H-atom parameters constrained
S = 1.03Δρmax = 1.12 e Å3
17345 reflectionsΔρmin = 0.40 e Å3
905 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
C10.40916 (18)0.35330 (16)0.13648 (12)0.0557 (8)
H1A0.36010.34960.11190.084*
H1B0.39590.39140.15630.084*
H1C0.40940.31350.15580.084*
C20.5349 (3)0.49389 (15)0.16084 (13)0.0688 (9)
H2A0.52910.52550.18660.103*
H2B0.47220.48540.14690.103*
H2C0.57660.51180.13680.103*
C30.93105 (18)0.38238 (14)0.06004 (10)0.0472 (6)
H3A0.94840.40290.03020.071*
H3B0.94580.33550.05890.071*
H3C0.96680.40290.08590.071*
C40.8219 (2)0.47746 (13)0.15501 (12)0.0582 (8)
H4A0.85320.49630.18290.087*
H4B0.75490.48990.15460.087*
H4C0.85220.49410.12660.087*
C50.6448 (2)0.43172 (16)0.06363 (10)0.0541 (8)
H5A0.66210.40930.03450.081*
H5B0.67800.47380.06560.081*
H5C0.57620.43930.06360.081*
C60.6049 (2)0.07544 (13)0.13756 (11)0.0522 (7)
H6A0.63720.03790.15210.078*
H6B0.62260.07850.10440.078*
H6C0.53620.06960.13970.078*
C70.42909 (19)0.17813 (17)0.18806 (10)0.0534 (7)
H7A0.36120.17390.18110.080*
H7B0.43920.21220.21190.080*
H7C0.45360.13630.20000.080*
C80.7020 (2)0.12052 (16)0.00387 (10)0.0565 (8)
H8A0.73880.08130.00370.085*
H8B0.69850.14920.02380.085*
H8C0.63790.10770.01290.085*
C90.7620 (2)0.28391 (17)0.01143 (9)0.0532 (7)
H9A0.73670.31270.03620.080*
H9B0.78420.24300.02550.080*
H9C0.81490.30570.00480.080*
C100.51781 (17)0.19984 (15)0.05363 (9)0.0435 (6)
H10A0.46590.22900.06240.065*
H10B0.49690.15420.05600.065*
H10C0.53650.20910.02130.065*
C110.9785 (2)0.24800 (19)0.27245 (9)0.0613 (9)
H11A0.94870.25890.30240.092*
H11B1.03740.27290.26940.092*
H11C0.99260.20100.27170.092*
C121.05222 (19)0.35787 (13)0.18527 (10)0.0477 (6)
H12A1.11750.37090.17880.071*
H12B1.03970.36380.21880.071*
H12C1.00840.38510.16670.071*
C130.8718 (4)0.02134 (18)0.1312 (2)0.141 (3)
H13A0.83010.01000.14680.212*
H13B0.93750.01350.14130.212*
H13C0.86630.01580.09700.212*
C140.99257 (19)0.17595 (14)0.05140 (9)0.0450 (6)
H14A1.02700.15290.02670.067*
H14B1.03640.20440.06900.067*
H14C0.94220.20260.03700.067*
C151.0544 (2)0.13666 (14)0.18628 (11)0.0518 (7)
H15A1.08060.11200.15990.078*
H15B1.03560.10620.21110.078*
H15C1.10260.16690.19870.078*
C160.4763 (2)0.3616 (2)0.27901 (13)0.0739 (10)
H16A0.43000.39100.29330.111*
H16B0.47570.31930.29520.111*
H16C0.45980.35520.24570.111*
C170.8294 (2)0.40082 (19)0.27488 (14)0.0723 (10)
H17A0.86130.44130.28460.108*
H17B0.84790.38940.24280.108*
H17C0.84760.36530.29640.108*
C180.5622 (3)0.1560 (2)0.32156 (12)0.0822 (12)
H18A0.50250.13150.32070.123*
H18B0.55710.19250.34380.123*
H18C0.61380.12690.33160.123*
C190.7742 (2)0.11632 (16)0.25468 (11)0.0598 (8)
H19A0.83010.09480.26840.090*
H19B0.78420.12380.22110.090*
H19C0.71860.08830.25880.090*
C200.6993 (3)0.29074 (16)0.35101 (9)0.0606 (8)
H20A0.72780.33300.35950.091*
H20B0.74190.25520.36080.091*
H20C0.63850.28590.36680.091*
C210.24434 (16)0.28299 (11)0.03113 (9)0.0333 (5)
C220.22048 (18)0.27995 (13)0.07908 (9)0.0405 (6)
H220.20280.31930.09450.049*
C230.2217 (2)0.22166 (15)0.10503 (11)0.0537 (7)
H230.20510.22230.13730.064*
C240.2464 (2)0.16394 (15)0.08434 (12)0.0559 (8)
H240.24860.12470.10220.067*
C250.2684 (2)0.16306 (14)0.03711 (13)0.0575 (8)
H250.28380.12290.02220.069*
C260.2678 (2)0.22213 (13)0.01092 (11)0.0475 (6)
H260.28390.22070.02140.057*
C270.32680 (16)0.34652 (11)0.04053 (8)0.0305 (5)
C280.42136 (17)0.33183 (13)0.02628 (9)0.0402 (5)
H280.43480.32540.00620.048*
C290.49542 (18)0.32654 (14)0.05820 (10)0.0459 (6)
H290.55760.31680.04720.055*
C300.47828 (19)0.33553 (14)0.10604 (10)0.0463 (6)
H300.52820.33180.12790.056*
C310.3868 (2)0.35014 (14)0.12139 (9)0.0447 (6)
H310.37400.35610.15400.054*
C320.31312 (17)0.35609 (12)0.08889 (8)0.0358 (5)
H320.25160.36700.10020.043*
C330.13700 (16)0.35945 (11)0.02663 (8)0.0308 (5)
C340.07937 (17)0.30510 (12)0.03877 (8)0.0345 (5)
H340.10130.26240.03120.041*
C350.00921 (18)0.31190 (13)0.06167 (9)0.0406 (6)
H350.04530.27400.06930.049*
C360.04423 (17)0.37350 (13)0.07314 (9)0.0406 (6)
H360.10410.37820.08840.049*
C370.01023 (18)0.42825 (13)0.06178 (9)0.0433 (6)
H370.01280.47080.06930.052*
C380.09878 (17)0.42115 (12)0.03940 (9)0.0380 (5)
H380.13470.45940.03250.046*
C390.26314 (17)0.41729 (11)0.03337 (8)0.0345 (5)
C400.1969 (2)0.43726 (14)0.06751 (10)0.0473 (6)
H400.13900.41390.06980.057*
C410.2135 (2)0.49018 (17)0.09802 (11)0.0632 (9)
H410.16820.50080.12120.076*
C420.2954 (3)0.52690 (15)0.09452 (12)0.0650 (10)
H420.30660.56270.11520.078*
C430.3609 (2)0.51095 (14)0.06049 (11)0.0562 (8)
H430.41650.53660.05720.067*
C440.3449 (2)0.45677 (12)0.03090 (9)0.0423 (6)
H440.39120.44630.00820.051*
C450.71480 (16)0.16948 (11)0.82290 (8)0.0329 (5)
C460.7147 (2)0.23092 (13)0.84617 (10)0.0468 (6)
H460.70230.23220.87890.056*
C470.7323 (2)0.29040 (13)0.82239 (12)0.0558 (8)
H470.73200.33050.83930.067*
C480.7499 (2)0.29067 (14)0.77458 (12)0.0530 (7)
H480.76220.33060.75870.064*
C490.7494 (2)0.23211 (14)0.75040 (11)0.0471 (6)
H490.76020.23170.71750.057*
C500.73303 (16)0.17329 (12)0.77430 (9)0.0362 (5)
H500.73420.13370.75680.043*
C510.79779 (18)0.08350 (11)0.88335 (9)0.0367 (5)
C520.86476 (18)0.13093 (13)0.89733 (9)0.0399 (5)
H520.85710.17440.88600.048*
C530.9421 (2)0.11722 (16)0.92709 (10)0.0518 (7)
H530.98520.15120.93530.062*
C540.9564 (2)0.05458 (16)0.94477 (11)0.0606 (8)
H541.00790.04550.96560.073*
C550.8939 (3)0.00584 (16)0.93134 (14)0.0714 (10)
H550.90280.03750.94260.086*
C560.8173 (2)0.02011 (14)0.90103 (13)0.0631 (9)
H560.77630.01470.89190.076*
C570.68558 (18)0.04139 (11)0.80956 (8)0.0356 (5)
C580.7615 (2)0.00950 (13)0.78717 (11)0.0500 (7)
H580.82380.01490.79960.060*
C590.7478 (2)0.02989 (14)0.74726 (11)0.0585 (8)
H590.80080.04970.73280.070*
C600.6570 (2)0.04029 (13)0.72854 (10)0.0539 (7)
H600.64780.06670.70140.065*
C610.5804 (2)0.01115 (13)0.75046 (10)0.0493 (7)
H610.51800.01830.73860.059*
C620.59503 (19)0.02883 (12)0.79021 (9)0.0395 (5)
H620.54160.04820.80460.047*
C630.60599 (18)0.09786 (12)0.88475 (8)0.0375 (5)
C640.5843 (2)0.04150 (15)0.91118 (10)0.0561 (8)
H640.62690.00550.91070.067*
C650.5022 (3)0.0365 (2)0.93823 (11)0.0778 (12)
H650.48970.00240.95530.093*
C660.4396 (3)0.0885 (3)0.93991 (14)0.0893 (14)
H660.38410.08530.95820.107*
C670.4578 (3)0.1449 (2)0.91489 (14)0.0792 (11)
H670.41520.18090.91610.095*
C680.5396 (2)0.14901 (17)0.88768 (10)0.0545 (7)
H680.55070.18810.87050.065*
B10.24281 (18)0.35194 (13)0.00058 (9)0.0300 (5)
B20.7012 (2)0.09858 (12)0.85061 (9)0.0330 (5)
N10.67242 (13)0.38986 (10)0.10526 (7)0.0328 (4)
N20.60115 (13)0.21081 (10)0.08637 (6)0.0307 (4)
N30.97026 (14)0.17461 (10)0.16973 (7)0.0348 (4)
N40.68384 (16)0.28788 (10)0.29912 (7)0.0403 (5)
O10.50180 (11)0.36135 (9)0.11476 (6)0.0417 (4)
O20.57471 (12)0.43304 (8)0.17894 (6)0.0403 (4)
O30.82973 (12)0.39110 (9)0.06758 (6)0.0397 (4)
O40.82995 (12)0.40627 (8)0.15648 (6)0.0368 (4)
O50.63286 (12)0.13536 (8)0.16203 (6)0.0347 (3)
O60.47829 (11)0.19577 (9)0.14555 (6)0.0377 (4)
O70.74828 (12)0.15562 (9)0.04301 (6)0.0414 (4)
O80.68762 (12)0.26949 (9)0.02228 (5)0.0394 (4)
O90.91393 (12)0.26459 (9)0.23346 (6)0.0404 (4)
O101.03879 (11)0.28944 (8)0.17266 (6)0.0376 (4)
O110.84541 (14)0.08523 (8)0.14330 (7)0.0469 (4)
O120.95116 (12)0.12845 (8)0.08326 (6)0.0403 (4)
O130.57071 (16)0.39052 (10)0.28304 (7)0.0561 (5)
O140.73123 (15)0.40991 (10)0.27612 (8)0.0573 (5)
O150.58122 (13)0.18081 (10)0.27603 (6)0.0477 (4)
O160.75919 (13)0.17848 (9)0.27801 (6)0.0440 (4)
P10.59530 (4)0.36876 (3)0.14741 (2)0.02903 (12)
P20.78467 (4)0.36107 (3)0.11485 (2)0.02791 (11)
P30.59161 (4)0.20599 (3)0.146395 (19)0.02736 (11)
P40.71172 (4)0.22250 (3)0.066653 (19)0.02898 (12)
P50.93796 (4)0.25355 (3)0.17927 (2)0.02862 (12)
P60.89047 (4)0.15314 (3)0.12709 (2)0.03076 (12)
P70.66074 (5)0.35145 (3)0.26195 (2)0.03718 (14)
P80.67130 (4)0.22378 (3)0.26176 (2)0.03160 (12)
Rh10.646168 (12)0.286987 (8)0.195882 (6)0.02576 (5)
Rh20.814582 (11)0.251932 (8)0.125405 (5)0.02466 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0259 (12)0.0680 (19)0.073 (2)0.0019 (12)0.0066 (12)0.0170 (16)
C20.083 (2)0.0412 (16)0.082 (2)0.0253 (16)0.0134 (19)0.0030 (16)
C30.0388 (14)0.0533 (16)0.0498 (15)0.0079 (12)0.0135 (12)0.0038 (13)
C40.0637 (19)0.0350 (14)0.076 (2)0.0052 (13)0.0036 (16)0.0118 (14)
C50.0490 (16)0.0647 (19)0.0488 (16)0.0125 (14)0.0017 (12)0.0313 (14)
C60.0674 (19)0.0339 (13)0.0552 (17)0.0095 (13)0.0021 (14)0.0044 (12)
C70.0347 (14)0.084 (2)0.0417 (14)0.0072 (14)0.0085 (11)0.0113 (14)
C80.0599 (18)0.0671 (19)0.0423 (15)0.0076 (15)0.0033 (13)0.0272 (14)
C90.0455 (15)0.085 (2)0.0291 (12)0.0159 (15)0.0049 (11)0.0098 (13)
C100.0316 (12)0.0676 (18)0.0310 (12)0.0106 (12)0.0090 (10)0.0037 (11)
C110.0543 (18)0.100 (3)0.0291 (13)0.0045 (17)0.0113 (12)0.0064 (15)
C120.0404 (14)0.0451 (15)0.0571 (16)0.0107 (12)0.0102 (12)0.0011 (12)
C130.151 (5)0.0340 (19)0.242 (7)0.008 (2)0.117 (5)0.009 (3)
C140.0403 (14)0.0551 (16)0.0396 (13)0.0021 (12)0.0082 (11)0.0005 (12)
C150.0439 (15)0.0500 (16)0.0611 (18)0.0109 (12)0.0138 (13)0.0103 (13)
C160.0491 (19)0.099 (3)0.074 (2)0.0109 (18)0.0175 (16)0.010 (2)
C170.057 (2)0.079 (2)0.081 (2)0.0011 (18)0.0104 (18)0.004 (2)
C180.105 (3)0.096 (3)0.0458 (18)0.048 (2)0.0071 (18)0.0117 (18)
C190.072 (2)0.0608 (19)0.0468 (16)0.0240 (16)0.0057 (14)0.0008 (14)
C200.092 (2)0.0608 (19)0.0288 (13)0.0076 (17)0.0108 (14)0.0013 (12)
C210.0246 (10)0.0341 (12)0.0412 (12)0.0003 (9)0.0042 (9)0.0048 (10)
C220.0395 (13)0.0431 (14)0.0389 (13)0.0069 (11)0.0046 (10)0.0042 (11)
C230.0549 (17)0.0593 (18)0.0467 (16)0.0146 (14)0.0065 (13)0.0151 (14)
C240.0441 (15)0.0505 (17)0.073 (2)0.0062 (13)0.0041 (14)0.0268 (15)
C250.0458 (16)0.0352 (14)0.092 (2)0.0077 (12)0.0135 (15)0.0051 (15)
C260.0462 (15)0.0381 (14)0.0585 (17)0.0048 (11)0.0147 (13)0.0035 (12)
C270.0299 (11)0.0258 (10)0.0358 (11)0.0026 (8)0.0024 (9)0.0010 (9)
C280.0353 (13)0.0453 (14)0.0398 (13)0.0014 (11)0.0026 (10)0.0079 (11)
C290.0296 (12)0.0478 (15)0.0601 (17)0.0012 (11)0.0014 (11)0.0055 (13)
C300.0403 (14)0.0476 (15)0.0512 (15)0.0062 (12)0.0127 (12)0.0029 (12)
C310.0496 (15)0.0522 (15)0.0324 (12)0.0077 (12)0.0012 (11)0.0032 (11)
C320.0320 (12)0.0405 (13)0.0348 (12)0.0031 (10)0.0046 (9)0.0027 (10)
C330.0286 (11)0.0332 (11)0.0305 (11)0.0010 (9)0.0013 (9)0.0012 (9)
C340.0349 (12)0.0324 (12)0.0364 (12)0.0008 (9)0.0000 (9)0.0023 (9)
C350.0362 (13)0.0464 (14)0.0391 (13)0.0080 (11)0.0001 (10)0.0065 (11)
C360.0293 (12)0.0553 (15)0.0370 (13)0.0005 (11)0.0038 (10)0.0004 (11)
C370.0378 (13)0.0420 (14)0.0498 (15)0.0054 (11)0.0064 (11)0.0094 (11)
C380.0338 (12)0.0338 (12)0.0461 (14)0.0014 (10)0.0077 (10)0.0061 (10)
C390.0377 (12)0.0323 (12)0.0330 (11)0.0067 (10)0.0092 (9)0.0032 (9)
C400.0405 (14)0.0522 (16)0.0491 (15)0.0160 (12)0.0088 (12)0.0099 (12)
C410.065 (2)0.067 (2)0.0574 (18)0.0340 (17)0.0161 (15)0.0254 (16)
C420.083 (2)0.0417 (16)0.069 (2)0.0198 (16)0.0374 (18)0.0208 (15)
C430.073 (2)0.0353 (14)0.0591 (18)0.0048 (14)0.0277 (16)0.0028 (13)
C440.0540 (16)0.0341 (12)0.0386 (13)0.0014 (11)0.0111 (11)0.0063 (10)
C450.0294 (11)0.0274 (11)0.0417 (12)0.0024 (9)0.0067 (9)0.0040 (9)
C460.0575 (17)0.0339 (13)0.0489 (15)0.0022 (12)0.0023 (13)0.0071 (11)
C470.0590 (18)0.0275 (13)0.081 (2)0.0017 (12)0.0040 (16)0.0117 (13)
C480.0515 (17)0.0390 (15)0.068 (2)0.0033 (12)0.0002 (14)0.0109 (13)
C490.0430 (15)0.0476 (15)0.0507 (15)0.0021 (12)0.0000 (12)0.0082 (12)
C500.0312 (12)0.0355 (12)0.0416 (13)0.0003 (10)0.0046 (10)0.0004 (10)
C510.0404 (13)0.0301 (11)0.0395 (13)0.0066 (10)0.0026 (10)0.0047 (10)
C520.0461 (14)0.0384 (13)0.0350 (12)0.0028 (11)0.0054 (10)0.0028 (10)
C530.0478 (16)0.0603 (18)0.0469 (15)0.0001 (13)0.0120 (12)0.0069 (13)
C540.0567 (18)0.065 (2)0.0595 (18)0.0208 (16)0.0207 (15)0.0059 (15)
C550.080 (2)0.0418 (16)0.092 (3)0.0226 (16)0.030 (2)0.0047 (16)
C560.067 (2)0.0310 (14)0.091 (2)0.0065 (13)0.0281 (18)0.0005 (14)
C570.0452 (13)0.0230 (10)0.0385 (12)0.0018 (9)0.0003 (10)0.0013 (9)
C580.0469 (15)0.0370 (14)0.0661 (18)0.0038 (12)0.0057 (13)0.0166 (13)
C590.070 (2)0.0399 (15)0.0664 (19)0.0002 (14)0.0145 (16)0.0204 (14)
C600.085 (2)0.0347 (14)0.0423 (15)0.0024 (14)0.0027 (14)0.0098 (11)
C610.0627 (18)0.0404 (14)0.0444 (15)0.0030 (13)0.0155 (13)0.0044 (12)
C620.0482 (14)0.0328 (12)0.0375 (13)0.0007 (10)0.0048 (11)0.0025 (10)
C630.0410 (13)0.0413 (13)0.0300 (11)0.0041 (10)0.0050 (10)0.0069 (10)
C640.075 (2)0.0494 (16)0.0439 (15)0.0173 (15)0.0050 (14)0.0066 (13)
C650.111 (3)0.079 (2)0.0432 (17)0.050 (2)0.0201 (19)0.0165 (17)
C660.076 (3)0.123 (4)0.070 (2)0.040 (3)0.039 (2)0.044 (2)
C670.057 (2)0.103 (3)0.078 (2)0.002 (2)0.0220 (18)0.023 (2)
C680.0489 (16)0.0652 (19)0.0495 (16)0.0090 (14)0.0070 (13)0.0050 (14)
B10.0272 (12)0.0305 (12)0.0322 (12)0.0015 (10)0.0023 (10)0.0025 (10)
B20.0392 (14)0.0245 (12)0.0353 (13)0.0009 (10)0.0031 (11)0.0042 (10)
N10.0300 (10)0.0368 (10)0.0317 (10)0.0046 (8)0.0008 (8)0.0115 (8)
N20.0252 (9)0.0425 (11)0.0242 (9)0.0060 (8)0.0041 (7)0.0021 (8)
N30.0341 (10)0.0339 (10)0.0362 (10)0.0048 (8)0.0068 (8)0.0033 (8)
N40.0523 (13)0.0426 (12)0.0258 (10)0.0027 (10)0.0052 (9)0.0012 (8)
O10.0283 (8)0.0526 (11)0.0440 (10)0.0002 (7)0.0097 (7)0.0091 (8)
O20.0409 (9)0.0358 (9)0.0442 (10)0.0107 (7)0.0008 (7)0.0015 (7)
O30.0378 (9)0.0430 (9)0.0385 (9)0.0017 (7)0.0091 (7)0.0099 (7)
O40.0368 (9)0.0319 (8)0.0416 (9)0.0025 (7)0.0035 (7)0.0037 (7)
O50.0415 (9)0.0281 (8)0.0343 (8)0.0012 (7)0.0034 (7)0.0022 (6)
O60.0264 (8)0.0526 (10)0.0339 (8)0.0064 (7)0.0006 (6)0.0073 (7)
O70.0408 (9)0.0499 (10)0.0332 (9)0.0004 (8)0.0045 (7)0.0155 (8)
O80.0335 (9)0.0595 (11)0.0252 (8)0.0064 (8)0.0018 (6)0.0103 (7)
O90.0372 (9)0.0585 (11)0.0256 (8)0.0021 (8)0.0029 (7)0.0023 (7)
O100.0292 (8)0.0429 (9)0.0406 (9)0.0055 (7)0.0008 (7)0.0015 (7)
O110.0582 (12)0.0283 (9)0.0544 (11)0.0049 (8)0.0111 (9)0.0007 (8)
O120.0431 (10)0.0369 (9)0.0409 (9)0.0072 (7)0.0061 (7)0.0041 (7)
O130.0759 (14)0.0476 (11)0.0449 (11)0.0093 (10)0.0038 (10)0.0114 (9)
O140.0572 (13)0.0532 (12)0.0613 (13)0.0093 (10)0.0086 (10)0.0068 (10)
O150.0507 (11)0.0552 (11)0.0374 (9)0.0162 (9)0.0042 (8)0.0054 (8)
O160.0466 (10)0.0440 (10)0.0412 (9)0.0066 (8)0.0095 (8)0.0080 (8)
P10.0242 (3)0.0319 (3)0.0309 (3)0.0019 (2)0.0022 (2)0.0055 (2)
P20.0263 (3)0.0294 (3)0.0280 (3)0.0007 (2)0.0003 (2)0.0037 (2)
P30.0255 (3)0.0318 (3)0.0248 (3)0.0023 (2)0.0012 (2)0.0031 (2)
P40.0265 (3)0.0383 (3)0.0221 (3)0.0034 (2)0.0018 (2)0.0008 (2)
P50.0267 (3)0.0336 (3)0.0255 (3)0.0011 (2)0.0032 (2)0.0003 (2)
P60.0321 (3)0.0280 (3)0.0321 (3)0.0009 (2)0.0001 (2)0.0010 (2)
P70.0462 (4)0.0346 (3)0.0306 (3)0.0046 (3)0.0035 (3)0.0023 (2)
P80.0356 (3)0.0351 (3)0.0241 (3)0.0014 (2)0.0025 (2)0.0041 (2)
Rh10.02586 (8)0.02892 (9)0.02246 (8)0.00076 (6)0.00106 (6)0.00267 (6)
Rh20.02377 (8)0.02735 (9)0.02277 (8)0.00055 (6)0.00253 (6)0.00053 (6)
Geometric parameters (Å, º) top
C1—O11.449 (3)C51—C561.399 (4)
C2—O21.439 (3)C51—B21.652 (4)
C3—O31.446 (3)C52—C531.385 (4)
C4—O41.443 (3)C53—C541.374 (4)
C5—N11.491 (3)C54—C551.366 (5)
C6—O51.444 (3)C55—C561.390 (4)
C7—O61.434 (3)C57—C621.394 (3)
C8—O71.454 (3)C57—C581.400 (4)
C9—O81.447 (3)C57—B21.646 (3)
C10—N21.491 (3)C58—C591.388 (4)
C11—O91.450 (3)C59—C601.384 (4)
C12—O101.439 (3)C60—C611.376 (4)
C13—O111.387 (4)C61—C621.393 (3)
C14—O121.441 (3)C63—C681.392 (4)
C15—N31.474 (3)C63—C641.396 (4)
C16—O131.446 (4)C63—B21.653 (4)
C17—O141.385 (4)C64—C651.391 (5)
C18—O151.405 (3)C65—C661.368 (6)
C19—O161.434 (3)C66—C671.367 (6)
C20—N41.474 (3)C67—C681.388 (4)
C21—C261.396 (4)N1—P11.6700 (19)
C21—C221.396 (3)N1—P21.6914 (19)
C21—B11.654 (3)N2—P41.6665 (19)
C22—C231.386 (4)N2—P31.6995 (18)
C23—C241.351 (4)N3—P51.680 (2)
C24—C251.369 (5)N3—P61.683 (2)
C25—C261.403 (4)N4—P81.676 (2)
C27—C321.385 (3)N4—P71.685 (2)
C27—C281.407 (3)O1—P11.5938 (17)
C27—B11.641 (3)O2—P11.6014 (18)
C28—C291.385 (4)O3—P21.5999 (16)
C29—C301.376 (4)O4—P21.6082 (17)
C30—C311.375 (4)O5—P31.5985 (16)
C31—C321.393 (3)O6—P31.5972 (16)
C33—C381.401 (3)O7—P41.5937 (18)
C33—C341.401 (3)O8—P41.6007 (17)
C33—B11.648 (3)O9—P51.5825 (17)
C34—C351.394 (3)O10—P51.5984 (17)
C35—C361.374 (4)O11—P61.5799 (18)
C36—C371.378 (4)O12—P61.5877 (17)
C37—C381.388 (3)O13—P71.607 (2)
C39—C441.396 (4)O14—P71.586 (2)
C39—C401.403 (4)O15—P81.5860 (18)
C39—B11.652 (3)O16—P81.5935 (18)
C40—C411.389 (4)P1—Rh12.2512 (6)
C41—C421.369 (5)P2—Rh22.2631 (6)
C42—C431.374 (5)P3—Rh12.2736 (6)
C43—C441.392 (4)P4—Rh22.2552 (6)
C45—C501.397 (3)P5—Rh22.2796 (6)
C45—C461.404 (3)P5—P62.5853 (8)
C45—B21.643 (3)P6—Rh22.2606 (6)
C46—C471.399 (4)P7—Rh12.2769 (6)
C47—C481.372 (5)P7—P82.5837 (9)
C48—C491.365 (4)P8—Rh12.2746 (6)
C49—C501.386 (4)Rh1—Rh23.1805 (2)
C51—C521.392 (3)
C26—C21—C22114.6 (2)C6—O5—P3121.56 (16)
C26—C21—B1121.5 (2)C7—O6—P3120.49 (16)
C22—C21—B1123.9 (2)C8—O7—P4126.03 (18)
C23—C22—C21123.1 (3)C9—O8—P4119.08 (17)
C24—C23—C22120.5 (3)C11—O9—P5123.94 (18)
C23—C24—C25119.5 (3)C12—O10—P5121.29 (16)
C24—C25—C26120.0 (3)C13—O11—P6129.0 (2)
C21—C26—C25122.3 (3)C14—O12—P6119.90 (15)
C32—C27—C28115.1 (2)C16—O13—P7119.45 (19)
C32—C27—B1125.0 (2)C17—O14—P7120.5 (2)
C28—C27—B1119.8 (2)C18—O15—P8126.0 (2)
C29—C28—C27122.6 (2)C19—O16—P8119.29 (17)
C30—C29—C28120.2 (2)O1—P1—O2104.07 (10)
C31—C30—C29118.9 (2)O1—P1—N198.44 (9)
C30—C31—C32120.4 (2)O2—P1—N1108.05 (10)
C27—C32—C31122.7 (2)O1—P1—Rh1121.98 (7)
C38—C33—C34114.8 (2)O2—P1—Rh1108.49 (7)
C38—C33—B1122.2 (2)N1—P1—Rh1114.61 (7)
C34—C33—B1123.0 (2)O3—P2—O4103.59 (9)
C35—C34—C33122.6 (2)O3—P2—N196.46 (9)
C36—C35—C34120.6 (2)O4—P2—N1105.97 (10)
C35—C36—C37118.6 (2)O3—P2—Rh2113.86 (7)
C36—C37—C38120.6 (2)O4—P2—Rh2112.81 (7)
C37—C38—C33122.9 (2)N1—P2—Rh2121.69 (7)
C44—C39—C40114.7 (2)O6—P3—O5104.03 (9)
C44—C39—B1124.2 (2)O6—P3—N294.88 (9)
C40—C39—B1121.1 (2)O5—P3—N2106.95 (9)
C41—C40—C39122.6 (3)O6—P3—Rh1115.20 (7)
C42—C41—C40120.3 (3)O5—P3—Rh1110.95 (6)
C41—C42—C43119.4 (3)N2—P3—Rh1122.49 (7)
C42—C43—C44119.9 (3)O7—P4—O8104.03 (10)
C43—C44—C39123.0 (3)O7—P4—N2108.87 (10)
C50—C45—C46114.2 (2)O8—P4—N299.11 (9)
C50—C45—B2122.5 (2)O7—P4—Rh2108.95 (7)
C46—C45—B2123.3 (2)O8—P4—Rh2122.70 (7)
C47—C46—C45122.3 (3)N2—P4—Rh2112.18 (7)
C48—C47—C46120.5 (3)O9—P5—O10104.37 (9)
C49—C48—C47119.1 (3)O9—P5—N3110.44 (10)
C48—C49—C50120.1 (3)O10—P5—N399.95 (10)
C49—C50—C45123.8 (2)O9—P5—Rh2118.28 (7)
C52—C51—C56113.8 (2)O10—P5—Rh2126.08 (7)
C52—C51—B2124.9 (2)N3—P5—Rh294.74 (7)
C56—C51—B2121.4 (2)O9—P5—P6127.00 (7)
C53—C52—C51123.3 (3)O10—P5—P6120.63 (7)
C54—C53—C52120.8 (3)Rh2—P5—P654.942 (18)
C55—C54—C53118.4 (3)O11—P6—O1299.86 (10)
C54—C55—C56120.3 (3)O11—P6—N3106.30 (10)
C55—C56—C51123.5 (3)O12—P6—N3106.20 (10)
C62—C57—C58115.5 (2)O11—P6—Rh2125.73 (8)
C62—C57—B2120.8 (2)O12—P6—Rh2121.14 (7)
C58—C57—B2123.1 (2)N3—P6—Rh295.35 (7)
C59—C58—C57122.1 (3)O11—P6—P5128.14 (8)
C60—C59—C58120.7 (3)O12—P6—P5123.52 (7)
C61—C60—C59118.7 (3)Rh2—P6—P555.638 (18)
C60—C61—C62120.1 (3)O14—P7—O1391.62 (12)
C61—C62—C57122.8 (3)O14—P7—N4107.40 (11)
C68—C63—C64115.1 (3)O13—P7—N4106.80 (11)
C68—C63—B2124.8 (2)O14—P7—Rh1132.80 (9)
C64—C63—B2120.0 (2)O13—P7—Rh1121.45 (8)
C65—C64—C63122.5 (3)N4—P7—Rh194.88 (7)
C66—C65—C64119.8 (4)O14—P7—P8135.15 (9)
C67—C66—C65119.9 (3)O13—P7—P8122.44 (8)
C66—C67—C68119.7 (4)Rh1—P7—P855.370 (19)
C67—C68—C63122.9 (3)O15—P8—O16102.97 (10)
C27—B1—C33110.34 (18)O15—P8—N4109.89 (11)
C27—B1—C39109.32 (18)O16—P8—N4100.99 (10)
C33—B1—C39109.23 (18)O15—P8—Rh1113.58 (7)
C27—B1—C21108.05 (18)O16—P8—Rh1131.73 (7)
C33—B1—C21108.78 (18)N4—P8—Rh195.22 (7)
C39—B1—C21111.11 (18)O15—P8—P7120.02 (8)
C45—B2—C57107.09 (19)O16—P8—P7128.07 (8)
C45—B2—C51109.02 (19)Rh1—P8—P755.454 (19)
C57—B2—C51111.15 (19)P1—Rh1—P393.26 (2)
C45—B2—C63112.56 (19)P1—Rh1—P8161.76 (2)
C57—B2—C63107.61 (19)P3—Rh1—P898.15 (2)
C51—B2—C63109.42 (19)P1—Rh1—P795.67 (2)
C5—N1—P1122.72 (16)P3—Rh1—P7159.60 (2)
C5—N1—P2123.33 (16)P8—Rh1—P769.18 (2)
P1—N1—P2113.94 (10)P1—Rh1—Rh290.891 (16)
C10—N2—P4122.36 (15)P3—Rh1—Rh272.681 (15)
C10—N2—P3122.25 (15)P8—Rh1—Rh2106.054 (17)
P4—N2—P3115.21 (10)P7—Rh1—Rh2125.352 (19)
C15—N3—P5131.17 (18)P4—Rh2—P694.39 (2)
C15—N3—P6127.50 (18)P4—Rh2—P292.64 (2)
P5—N3—P6100.47 (10)P6—Rh2—P2161.59 (2)
C20—N4—P8131.63 (19)P4—Rh2—P5163.61 (2)
C20—N4—P7127.53 (19)P6—Rh2—P569.42 (2)
P8—N4—P7100.50 (11)P2—Rh2—P5102.12 (2)
C1—O1—P1119.84 (17)P4—Rh2—Rh192.651 (15)
C2—O2—P1124.63 (19)P6—Rh2—Rh1122.341 (16)
C3—O3—P2118.31 (16)P2—Rh2—Rh174.210 (15)
C4—O4—P2121.02 (17)P5—Rh2—Rh198.148 (16)

Experimental details

Crystal data
Chemical formulaC20H60N4O16P8Rh2·2(C24H20B)
Mr1704.72
Crystal system, space groupMonoclinic, P21/n
Temperature (K)225
a, b, c (Å)13.9783 (3), 20.2046 (5), 28.1465 (7)
β (°) 90.842 (1)
V3)7948.4 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.64
Crystal size (mm)0.31 × 0.18 × 0.10
Data collection
DiffractometerBruker APEX-II CCD
diffractometer
Absorption correctionNumerical
BRUKER SADABS
Tmin, Tmax0.826, 0.939
No. of measured, independent and
observed [I > 2σ(I)] reflections
17345, 17345, 14691
Rint0.000
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.081, 1.03
No. of reflections17345
No. of parameters905
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.12, 0.40

Computer programs: Bruker APEX2, Bruker SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL.

 

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