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In the title complex, [K(C12H24)]2[Rh(CN)3(CO)]·C2H3N, the Rh atom is coordinated by three cyanide ligands and one carbonyl ligand in a square-planar geometry. The K atom in each cation is coordinated by six O atoms from the crown ether and one N atom from a cyanide ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805027297/bt6720sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805027297/bt6720Isup2.hkl
Contains datablock I

CCDC reference: 287461

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.036
  • wR factor = 0.081
  • Data-to-parameter ratio = 21.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.44 PLAT230_ALERT_2_C Hirshfeld Test Diff for C11 - C12 .. 5.87 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - C1 .. 5.13 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - C2 .. 7.39 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - C3 .. 5.76 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - C4 .. 8.51 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C29
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The carbonyltricyanorhodate(I) dianion was first proposed by Jewsbury & Maher (1971) as an intermediate in the preparation of K3[HRh(CN)5] on the basis of visible and IR spectroscopic evidence. The complex, however, was never isolated. We report here the synthesis and structure of the title acetonitrile solvate, (I).

In the title complex, the RhI atom is coordinated in a square-planar geometry by three C atoms of cyanide ligands and one C atom from a carbonyl ligand. Each N atom of two trans cyanide ligands is in close contact [2.741 (2) and 2.747 (2) Å] with a K atom from the cations. The carbonyl ligand was identified on the basis of its shorter Rh1—C1 bond length [1.828 (3) versus 2.051 (3) Å for Rh1—C3]. One of the trans cyanide ligands is slightly bent, having an Rh1—C2N2 bond angle of 174.2 (3)°. The other trans cyanide ligand is more linear, with an Rh1—C4N4 bond angle of 177.2 (2)°. The K atom of each cation is pulled toward the cyanide N atom and out of the plane of the crown ether.

Experimental top

A flask charged with [RhCl(cod)]2 (702 mg, 1.42 mmol) in MeCN (25 ml) was purged with CO for approximately 20 min. The resulting orange solution was treated with a solution of [K(18-crown-6)]CN (3.14 g, 9.54 mmol). During addition, the color of the solution changes from clear orange to clear yellow to cloudy blue to cloudy yellow. Addition of diethyl ether (100 ml) resulted in the precipitation of a yellow solid. The solid was isolated by filtration, washed with more diethyl ether and dried under vacuum to yield 2.124 g (92%) of [K(18-crown-6)]2[Rh(CN)3(CO)]. X-ray quality crystals were formed at room temperature by vapor diffusion of diethyl ether into an acetonitrile solution of the product. ν(CO), acetonitrile: 1959 and 2084 cm-1, consistent with the published IR data.

Refinement top

Methyl H-atom positions, R—CH3, were optimized by rotation about R—C bonds with idealized C—H, R—H and H—H distances. The remaining H atoms were included as riding idealized contributors. Methyl Uiso(H) values were assigned as 1.5 times Ueq of the adjacent atom; the remaining Uiso(H) values were assigned as 1.2 times the adjacent Ueq. A final analysis of variance between observed and calculated structure factors showed little dependence on amplitude or resolution.

Structure description top

The carbonyltricyanorhodate(I) dianion was first proposed by Jewsbury & Maher (1971) as an intermediate in the preparation of K3[HRh(CN)5] on the basis of visible and IR spectroscopic evidence. The complex, however, was never isolated. We report here the synthesis and structure of the title acetonitrile solvate, (I).

In the title complex, the RhI atom is coordinated in a square-planar geometry by three C atoms of cyanide ligands and one C atom from a carbonyl ligand. Each N atom of two trans cyanide ligands is in close contact [2.741 (2) and 2.747 (2) Å] with a K atom from the cations. The carbonyl ligand was identified on the basis of its shorter Rh1—C1 bond length [1.828 (3) versus 2.051 (3) Å for Rh1—C3]. One of the trans cyanide ligands is slightly bent, having an Rh1—C2N2 bond angle of 174.2 (3)°. The other trans cyanide ligand is more linear, with an Rh1—C4N4 bond angle of 177.2 (2)°. The K atom of each cation is pulled toward the cyanide N atom and out of the plane of the crown ether.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: CIFTAB in SHELXTL.

Figures top
[Figure 1] Fig. 1. SHELXTL (Bruker, 2001) plot showing 35% probability displacement ellipsoids for non-H atoms; H atoms have been omitted for clarity.
Bis[(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium] carbonyltricyanorhodate(I) acetonitrile solvate top
Crystal data top
[K(C12H24)]2[Rh(CN)3(CO)]·C2H3NF(000) = 1784
Mr = 856.86Dx = 1.441 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 949 reflections
a = 22.439 (6) Åθ = 2.2–26.1°
b = 8.553 (2) ŵ = 0.71 mm1
c = 20.576 (5) ÅT = 193 K
β = 90.178 (4)°Tabular, yellow
V = 3948.9 (17) Å30.40 × 0.18 × 0.10 mm
Z = 4
Data collection top
Siemens SMART CCD
diffractometer
9709 independent reflections
Radiation source: normal-focus sealed tube7084 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
ω scansθmax = 28.3°, θmin = 1.8°
Absorption correction: integration
[XPREP in SHELXTL (Bruker, 2001)]
h = 2929
Tmin = 0.775, Tmax = 0.935k = 1111
39007 measured reflectionsl = 2727
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters not refined
S = 1.02 w = 1/[σ2(Fo2) + (0.0376P)2 + 0.650P]
where P = (Fo2 + 2Fc2)/3
9709 reflections(Δ/σ)max = 0.001
452 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = 0.27 e Å3
Crystal data top
[K(C12H24)]2[Rh(CN)3(CO)]·C2H3NV = 3948.9 (17) Å3
Mr = 856.86Z = 4
Monoclinic, P21/cMo Kα radiation
a = 22.439 (6) ŵ = 0.71 mm1
b = 8.553 (2) ÅT = 193 K
c = 20.576 (5) Å0.40 × 0.18 × 0.10 mm
β = 90.178 (4)°
Data collection top
Siemens SMART CCD
diffractometer
9709 independent reflections
Absorption correction: integration
[XPREP in SHELXTL (Bruker, 2001)]
7084 reflections with I > 2σ(I)
Tmin = 0.775, Tmax = 0.935Rint = 0.039
39007 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0360 restraints
wR(F2) = 0.081H-atom parameters not refined
S = 1.02Δρmax = 0.65 e Å3
9709 reflectionsΔρmin = 0.27 e Å3
452 parameters
Special details top

Experimental. Four frame series were filtered for statistical outliers then corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001) before using SAINT/SADABS/TWINABS (Bruker, 2001) to sort, merge, and scale the combined data. A series of identical frames was collected twice during the experiment to monitor decay. No decay correction was applied.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.31857 (11)0.4631 (3)0.45378 (11)0.0374 (5)
C20.29937 (11)0.2486 (3)0.54646 (12)0.0436 (6)
C30.17146 (12)0.2831 (3)0.51821 (10)0.0372 (5)
C40.20208 (10)0.5043 (3)0.42098 (11)0.0332 (5)
C50.54676 (11)0.2815 (3)0.67632 (13)0.0467 (6)
H5A0.56630.22580.71280.056*
H5B0.56110.39100.67620.056*
C60.56204 (11)0.2047 (3)0.61387 (13)0.0475 (6)
H6A0.54130.25790.57750.057*
H6B0.60550.21150.60630.057*
C70.56500 (12)0.0415 (3)0.56224 (13)0.0517 (7)
H7A0.60890.03350.55940.062*
H7B0.54760.00170.52180.062*
C80.54711 (13)0.2083 (3)0.56989 (13)0.0562 (8)
H8A0.56120.26970.53220.067*
H8B0.56550.25220.60970.067*
C90.46425 (17)0.3753 (3)0.58089 (15)0.0693 (10)
H9A0.48260.42300.62000.083*
H9B0.47670.43680.54250.083*
C100.39816 (18)0.3782 (4)0.58675 (15)0.0727 (10)
H10A0.37980.31990.55030.087*
H10B0.38360.48740.58530.087*
C110.31963 (13)0.3122 (4)0.65649 (16)0.0648 (9)
H11A0.30540.42170.65530.078*
H11B0.29920.25340.62150.078*
C120.30564 (12)0.2413 (3)0.72043 (14)0.0554 (7)
H12A0.26250.25120.72950.067*
H12B0.32800.29580.75530.067*
C130.30712 (12)0.0012 (4)0.77658 (14)0.0551 (7)
H13A0.32990.04480.81370.066*
H13B0.26410.01320.78580.066*
C140.32187 (12)0.1655 (3)0.76785 (15)0.0563 (8)
H14A0.30120.20660.72890.068*
H14B0.30820.22590.80610.068*
C150.40007 (12)0.3432 (3)0.74927 (13)0.0492 (7)
H15A0.38630.40850.78600.059*
H15B0.38050.38100.70910.059*
C160.46622 (12)0.3553 (3)0.74277 (13)0.0473 (6)
H16A0.47830.46660.74130.057*
H16B0.48590.30580.78060.057*
C170.00508 (10)0.4871 (3)0.33507 (11)0.0360 (5)
H17A0.01760.37710.34110.043*
H17B0.03930.54670.31740.043*
C180.01399 (11)0.5552 (3)0.39893 (11)0.0364 (5)
H18A0.01820.54280.43140.044*
H18B0.04990.50030.41520.044*
C190.04607 (11)0.7895 (3)0.44790 (11)0.0393 (6)
H19A0.08540.74740.46110.047*
H19B0.01730.76860.48320.047*
C200.05061 (11)0.9617 (3)0.43606 (11)0.0410 (6)
H20A0.01171.00270.42100.049*
H20B0.06141.01590.47700.049*
C210.09742 (11)1.1525 (2)0.37091 (12)0.0399 (6)
H21A0.10191.21730.41050.048*
H21B0.06011.18370.34860.048*
C220.14905 (11)1.1774 (3)0.32720 (12)0.0414 (6)
H22A0.15321.29010.31730.050*
H22B0.18611.14160.34880.050*
C230.18951 (10)1.1018 (3)0.22593 (12)0.0387 (6)
H23A0.22441.04940.24590.046*
H23B0.19981.21300.21870.046*
C240.17487 (10)1.0262 (3)0.16292 (12)0.0379 (5)
H24A0.13881.07500.14380.045*
H24B0.20831.03990.13210.045*
C250.15042 (11)0.7832 (3)0.11550 (11)0.0444 (6)
H25A0.18270.79850.08340.053*
H25B0.11300.82520.09680.053*
C260.14332 (11)0.6129 (3)0.13001 (12)0.0453 (6)
H26A0.13620.55410.08930.054*
H26B0.18000.57190.15070.054*
C270.08351 (11)0.4340 (3)0.18739 (11)0.0368 (5)
H27A0.11880.38910.20950.044*
H27B0.07650.37480.14670.044*
C280.03024 (11)0.4220 (3)0.23047 (11)0.0360 (5)
H28A0.00430.47440.20980.043*
H28B0.01990.31070.23740.043*
K20.41763 (2)0.01588 (6)0.64526 (2)0.03286 (12)
K40.11693 (2)0.76142 (5)0.29493 (2)0.03016 (11)
N20.33164 (11)0.1784 (3)0.57816 (12)0.0668 (7)
N30.12678 (11)0.2346 (3)0.53609 (10)0.0532 (6)
N40.17687 (9)0.5791 (2)0.38304 (10)0.0446 (5)
O10.36257 (9)0.5153 (2)0.43544 (9)0.0590 (5)
O20.48381 (7)0.27863 (18)0.68453 (7)0.0384 (4)
O30.54409 (7)0.04487 (19)0.61690 (8)0.0429 (4)
O40.48392 (8)0.21791 (19)0.57430 (8)0.0475 (4)
O50.38257 (8)0.3080 (2)0.64668 (8)0.0499 (5)
O60.32203 (8)0.0821 (2)0.71854 (8)0.0476 (4)
O70.38472 (7)0.18370 (19)0.76048 (8)0.0411 (4)
O80.04352 (6)0.49446 (17)0.29121 (7)0.0321 (3)
O90.02666 (7)0.71612 (17)0.38950 (7)0.0330 (3)
O100.09486 (7)0.99053 (17)0.38818 (7)0.0351 (4)
O110.13994 (7)1.09131 (17)0.26813 (7)0.0348 (4)
O120.16451 (7)0.86317 (17)0.17404 (7)0.0345 (4)
O130.09383 (7)0.59454 (17)0.17282 (7)0.0361 (4)
Rh10.249547 (8)0.37748 (2)0.484600 (8)0.03074 (6)
C290.26588 (12)0.9266 (3)0.41004 (14)0.0495 (7)
C300.23603 (13)0.8992 (3)0.47084 (13)0.0566 (7)
H30A0.25790.95160.50590.085*
H30B0.23450.78660.47950.085*
H30C0.19540.94080.46850.085*
N10.28940 (13)0.9483 (3)0.36234 (14)0.0753 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0391 (14)0.0380 (13)0.0350 (13)0.0012 (11)0.0073 (11)0.0040 (10)
C20.0478 (15)0.0405 (14)0.0424 (14)0.0046 (12)0.0098 (12)0.0063 (11)
C30.0491 (16)0.0387 (13)0.0239 (11)0.0052 (12)0.0033 (11)0.0010 (10)
C40.0315 (12)0.0296 (11)0.0383 (13)0.0027 (10)0.0015 (10)0.0007 (10)
C50.0332 (14)0.0402 (14)0.0665 (18)0.0083 (11)0.0074 (12)0.0085 (13)
C60.0320 (14)0.0491 (16)0.0615 (17)0.0029 (12)0.0076 (12)0.0156 (13)
C70.0359 (14)0.077 (2)0.0426 (15)0.0085 (14)0.0101 (12)0.0018 (14)
C80.066 (2)0.0594 (18)0.0435 (15)0.0249 (15)0.0055 (14)0.0075 (14)
C90.125 (3)0.0349 (15)0.0483 (17)0.0040 (17)0.0225 (19)0.0113 (13)
C100.117 (3)0.0513 (18)0.0500 (18)0.0338 (19)0.0037 (19)0.0105 (15)
C110.0538 (19)0.0578 (18)0.083 (2)0.0260 (15)0.0260 (16)0.0124 (17)
C120.0362 (15)0.0635 (18)0.0666 (19)0.0179 (13)0.0049 (13)0.0220 (16)
C130.0336 (14)0.082 (2)0.0498 (17)0.0006 (14)0.0116 (12)0.0077 (16)
C140.0338 (15)0.072 (2)0.0637 (19)0.0129 (14)0.0098 (13)0.0069 (15)
C150.0589 (18)0.0406 (15)0.0480 (16)0.0121 (12)0.0017 (13)0.0098 (12)
C160.0576 (17)0.0372 (14)0.0472 (15)0.0045 (12)0.0037 (13)0.0074 (11)
C170.0308 (12)0.0295 (12)0.0477 (14)0.0034 (10)0.0024 (10)0.0026 (10)
C180.0392 (14)0.0347 (12)0.0353 (13)0.0007 (10)0.0068 (10)0.0073 (10)
C190.0470 (15)0.0451 (14)0.0257 (12)0.0047 (12)0.0026 (10)0.0037 (10)
C200.0464 (15)0.0439 (14)0.0326 (13)0.0052 (12)0.0013 (11)0.0112 (11)
C210.0536 (16)0.0278 (12)0.0383 (13)0.0065 (11)0.0108 (12)0.0072 (10)
C220.0469 (15)0.0280 (11)0.0491 (15)0.0039 (11)0.0163 (12)0.0017 (11)
C230.0261 (12)0.0295 (12)0.0604 (16)0.0025 (10)0.0002 (11)0.0057 (11)
C240.0286 (12)0.0376 (13)0.0475 (14)0.0044 (10)0.0070 (10)0.0132 (11)
C250.0418 (15)0.0618 (17)0.0297 (13)0.0025 (13)0.0095 (11)0.0047 (12)
C260.0395 (14)0.0551 (16)0.0413 (14)0.0000 (12)0.0120 (11)0.0191 (12)
C270.0423 (14)0.0325 (12)0.0355 (13)0.0059 (10)0.0035 (11)0.0081 (10)
C280.0408 (14)0.0294 (11)0.0379 (13)0.0025 (10)0.0103 (11)0.0037 (10)
K20.0317 (3)0.0329 (3)0.0341 (3)0.0010 (2)0.0015 (2)0.0024 (2)
K40.0348 (3)0.0277 (2)0.0280 (2)0.0028 (2)0.00089 (19)0.00160 (19)
N20.0628 (17)0.0679 (16)0.0694 (17)0.0018 (13)0.0242 (13)0.0271 (14)
N30.0596 (15)0.0655 (15)0.0344 (12)0.0211 (13)0.0032 (11)0.0011 (11)
N40.0420 (12)0.0403 (12)0.0514 (13)0.0028 (10)0.0106 (10)0.0088 (10)
O10.0464 (12)0.0709 (14)0.0597 (12)0.0106 (10)0.0009 (10)0.0125 (10)
O20.0347 (9)0.0372 (9)0.0434 (9)0.0034 (7)0.0035 (7)0.0042 (7)
O30.0390 (10)0.0450 (10)0.0447 (10)0.0025 (8)0.0101 (8)0.0066 (8)
O40.0602 (12)0.0377 (10)0.0444 (10)0.0056 (9)0.0075 (9)0.0001 (8)
O50.0613 (12)0.0448 (10)0.0436 (10)0.0164 (9)0.0052 (9)0.0012 (8)
O60.0410 (10)0.0549 (11)0.0470 (11)0.0118 (8)0.0031 (8)0.0115 (9)
O70.0327 (9)0.0441 (9)0.0465 (10)0.0067 (7)0.0019 (7)0.0020 (8)
O80.0285 (8)0.0349 (8)0.0330 (8)0.0044 (7)0.0009 (6)0.0049 (7)
O90.0400 (9)0.0310 (8)0.0280 (8)0.0030 (7)0.0014 (7)0.0013 (6)
O100.0424 (9)0.0286 (8)0.0344 (9)0.0043 (7)0.0010 (7)0.0047 (7)
O110.0317 (9)0.0325 (8)0.0402 (9)0.0052 (7)0.0014 (7)0.0025 (7)
O120.0377 (9)0.0357 (8)0.0301 (8)0.0002 (7)0.0026 (7)0.0026 (7)
O130.0366 (9)0.0348 (9)0.0370 (9)0.0029 (7)0.0051 (7)0.0046 (7)
Rh10.03406 (10)0.02909 (9)0.02903 (10)0.00036 (8)0.00592 (7)0.00219 (8)
C290.0452 (16)0.0535 (16)0.0498 (17)0.0084 (13)0.0031 (13)0.0002 (13)
C300.067 (2)0.0557 (18)0.0468 (16)0.0127 (15)0.0086 (14)0.0091 (13)
N10.079 (2)0.087 (2)0.0608 (17)0.0155 (16)0.0169 (15)0.0062 (16)
Geometric parameters (Å, º) top
C1—O11.149 (3)C18—H18B0.9900
C1—Rh11.828 (3)C19—O91.423 (3)
C2—N21.144 (3)C19—C201.497 (3)
C2—Rh12.019 (2)C19—H19A0.9900
C3—N31.147 (3)C19—H19B0.9900
C3—Rh12.051 (3)C20—O101.422 (3)
C4—N41.155 (3)C20—H20A0.9900
C4—Rh12.004 (2)C20—H20B0.9900
C5—O21.423 (3)C21—O101.432 (3)
C5—C61.484 (4)C21—C221.484 (3)
C5—H5A0.9900C21—H21A0.9900
C5—H5B0.9900C21—H21B0.9900
C6—O31.427 (3)C22—O111.435 (3)
C6—H6A0.9900C22—H22A0.9900
C6—H6B0.9900C22—H22B0.9900
C7—O31.426 (3)C23—O111.416 (3)
C7—C81.490 (4)C23—C241.485 (3)
C7—H7A0.9900C23—H23A0.9900
C7—H7B0.9900C23—H23B0.9900
C8—O41.423 (3)C24—O121.432 (3)
C8—H8A0.9900C24—H24A0.9900
C8—H8B0.9900C24—H24B0.9900
C9—O41.424 (3)C25—O121.420 (3)
C9—C101.488 (5)C25—C261.495 (3)
C9—H9A0.9900C25—H25A0.9900
C9—H9B0.9900C25—H25B0.9900
C10—O51.416 (3)C26—O131.428 (3)
C10—H10A0.9900C26—H26A0.9900
C10—H10B0.9900C26—H26B0.9900
C11—O51.428 (3)C27—O131.424 (3)
C11—C121.483 (4)C27—C281.494 (3)
C11—H11A0.9900C27—H27A0.9900
C11—H11B0.9900C27—H27B0.9900
C12—O61.412 (3)C28—O81.426 (3)
C12—H12A0.9900C28—H28A0.9900
C12—H12B0.9900C28—H28B0.9900
C13—O61.421 (3)K2—N22.747 (2)
C13—C141.476 (4)K2—O62.7563 (18)
C13—H13A0.9900K2—O22.8110 (17)
C13—H13B0.9900K2—O72.8699 (18)
C14—O71.427 (3)K2—O52.8801 (19)
C14—H14A0.9900K2—O42.8908 (18)
C14—H14B0.9900K2—O32.9094 (18)
C15—O71.426 (3)K4—N42.741 (2)
C15—C161.494 (4)K4—O102.7880 (16)
C15—H15A0.9900K4—O82.8163 (16)
C15—H15B0.9900K4—O92.8398 (16)
C16—O21.423 (3)K4—O122.8462 (16)
C16—H16A0.9900K4—O112.9212 (17)
C16—H16B0.9900K4—O132.9343 (17)
C17—O81.419 (3)C29—N11.131 (3)
C17—C181.498 (3)C29—C301.440 (4)
C17—H17A0.9900C30—H30A0.9800
C17—H17B0.9900C30—H30B0.9800
C18—O91.419 (3)C30—H30C0.9800
C18—H18A0.9900
O1—C1—Rh1178.6 (2)O12—C24—H24B110.0
N2—C2—Rh1174.2 (3)C23—C24—H24B110.0
N3—C3—Rh1177.7 (2)H24A—C24—H24B108.3
N4—C4—Rh1177.2 (2)O12—C25—C26108.88 (19)
O2—C5—C6109.1 (2)O12—C25—H25A109.9
O2—C5—H5A109.9C26—C25—H25A109.9
C6—C5—H5A109.9O12—C25—H25B109.9
O2—C5—H5B109.9C26—C25—H25B109.9
C6—C5—H5B109.9H25A—C25—H25B108.3
H5A—C5—H5B108.3O13—C26—C25108.31 (19)
O3—C6—C5108.7 (2)O13—C26—H26A110.0
O3—C6—H6A110.0C25—C26—H26A110.0
C5—C6—H6A110.0O13—C26—H26B110.0
O3—C6—H6B110.0C25—C26—H26B110.0
C5—C6—H6B110.0H26A—C26—H26B108.4
H6A—C6—H6B108.3O13—C27—C28108.80 (18)
O3—C7—C8108.8 (2)O13—C27—H27A109.9
O3—C7—H7A109.9C28—C27—H27A109.9
C8—C7—H7A109.9O13—C27—H27B109.9
O3—C7—H7B109.9C28—C27—H27B109.9
C8—C7—H7B109.9H27A—C27—H27B108.3
H7A—C7—H7B108.3O8—C28—C27108.94 (18)
O4—C8—C7109.3 (2)O8—C28—H28A109.9
O4—C8—H8A109.8C27—C28—H28A109.9
C7—C8—H8A109.8O8—C28—H28B109.9
O4—C8—H8B109.8C27—C28—H28B109.9
C7—C8—H8B109.8H28A—C28—H28B108.3
H8A—C8—H8B108.3N2—K2—O683.23 (7)
O4—C9—C10109.4 (3)N2—K2—O296.29 (7)
O4—C9—H9A109.8O6—K2—O2119.81 (5)
C10—C9—H9A109.8N2—K2—O788.85 (7)
O4—C9—H9B109.8O6—K2—O759.83 (5)
C10—C9—H9B109.8O2—K2—O759.98 (5)
H9A—C9—H9B108.2N2—K2—O5107.48 (7)
O5—C10—C9108.2 (2)O6—K2—O559.27 (6)
O5—C10—H10A110.1O2—K2—O5155.53 (5)
C9—C10—H10A110.1O7—K2—O5113.69 (5)
O5—C10—H10B110.1N2—K2—O4117.26 (7)
C9—C10—H10B110.1O6—K2—O4117.95 (6)
H10A—C10—H10B108.4O2—K2—O4115.21 (5)
O5—C11—C12109.1 (2)O7—K2—O4153.80 (5)
O5—C11—H11A109.9O5—K2—O458.72 (5)
C12—C11—H11A109.9N2—K2—O3122.69 (7)
O5—C11—H11B109.9O6—K2—O3153.74 (5)
C12—C11—H11B109.9O2—K2—O358.31 (5)
H11A—C11—H11B108.3O7—K2—O3112.13 (5)
O6—C12—C11108.3 (2)O5—K2—O3110.52 (5)
O6—C12—H12A110.0O4—K2—O356.90 (5)
C11—C12—H12A110.0N4—K4—O1091.86 (6)
O6—C12—H12B110.0N4—K4—O880.94 (6)
C11—C12—H12B110.0O10—K4—O8118.90 (5)
H12A—C12—H12B108.4N4—K4—O979.55 (6)
O6—C13—C14108.3 (2)O10—K4—O959.71 (5)
O6—C13—H13A110.0O8—K4—O959.31 (4)
C14—C13—H13A110.0N4—K4—O12124.57 (6)
O6—C13—H13B110.0O10—K4—O12117.03 (5)
C14—C13—H13B110.0O8—K4—O12116.43 (5)
H13A—C13—H13B108.4O9—K4—O12155.63 (5)
O7—C14—C13109.9 (2)N4—K4—O11125.99 (6)
O7—C14—H14A109.7O10—K4—O1158.86 (5)
C13—C14—H14A109.7O8—K4—O11151.84 (5)
O7—C14—H14B109.7O9—K4—O11112.83 (4)
C13—C14—H14B109.7O12—K4—O1158.18 (4)
H14A—C14—H14B108.2N4—K4—O13112.00 (6)
O7—C15—C16108.8 (2)O10—K4—O13154.14 (5)
O7—C15—H15A109.9O8—K4—O1358.71 (4)
C16—C15—H15A109.9O9—K4—O13113.32 (5)
O7—C15—H15B109.9O12—K4—O1357.74 (5)
C16—C15—H15B109.9O11—K4—O13109.82 (5)
H15A—C15—H15B108.3C2—N2—K2174.3 (2)
O2—C16—C15108.8 (2)C4—N4—K4178.79 (19)
O2—C16—H16A109.9C16—O2—C5111.72 (19)
C15—C16—H16A109.9C16—O2—K2117.57 (14)
O2—C16—H16B109.9C5—O2—K2120.22 (13)
C15—C16—H16B109.9C7—O3—C6111.60 (19)
H16A—C16—H16B108.3C7—O3—K2115.95 (14)
O8—C17—C18108.82 (18)C6—O3—K2111.48 (13)
O8—C17—H17A109.9C8—O4—C9111.7 (2)
C18—C17—H17A109.9C8—O4—K2120.42 (15)
O8—C17—H17B109.9C9—O4—K2116.48 (16)
C18—C17—H17B109.9C10—O5—C11111.1 (2)
H17A—C17—H17B108.3C10—O5—K2109.30 (15)
O9—C18—C17108.29 (18)C11—O5—K2107.20 (16)
O9—C18—H18A110.0C12—O6—C13112.6 (2)
C17—C18—H18A110.0C12—O6—K2120.78 (16)
O9—C18—H18B110.0C13—O6—K2119.85 (15)
C17—C18—H18B110.0C15—O7—C14111.13 (19)
H18A—C18—H18B108.4C15—O7—K2106.38 (14)
O9—C19—C20108.52 (18)C14—O7—K2106.87 (15)
O9—C19—H19A110.0C17—O8—C28112.28 (17)
C20—C19—H19A110.0C17—O8—K4117.99 (12)
O9—C19—H19B110.0C28—O8—K4119.80 (12)
C20—C19—H19B110.0C18—O9—C19111.93 (16)
H19A—C19—H19B108.4C18—O9—K4111.70 (12)
O10—C20—C19109.34 (18)C19—O9—K4107.54 (13)
O10—C20—H20A109.8C20—O10—C21111.60 (17)
C19—C20—H20A109.8C20—O10—K4118.74 (12)
O10—C20—H20B109.8C21—O10—K4120.14 (13)
C19—C20—H20B109.8C23—O11—C22112.13 (17)
H20A—C20—H20B108.3C23—O11—K4108.46 (12)
O10—C21—C22108.73 (19)C22—O11—K4111.13 (12)
O10—C21—H21A109.9C25—O12—C24111.69 (17)
C22—C21—H21A109.9C25—O12—K4120.72 (13)
O10—C21—H21B109.9C24—O12—K4119.92 (13)
C22—C21—H21B109.9C27—O13—C26111.30 (17)
H21A—C21—H21B108.3C27—O13—K4108.48 (12)
O11—C22—C21109.29 (18)C26—O13—K4109.80 (13)
O11—C22—H22A109.8C1—Rh1—C490.33 (9)
C21—C22—H22A109.8C1—Rh1—C288.24 (10)
O11—C22—H22B109.8C4—Rh1—C2178.16 (10)
C21—C22—H22B109.8C1—Rh1—C3179.20 (10)
H22A—C22—H22B108.3C4—Rh1—C388.87 (9)
O11—C23—C24109.61 (18)C2—Rh1—C392.56 (10)
O11—C23—H23A109.7N1—C29—C30179.9 (4)
C24—C23—H23A109.7C29—C30—H30A109.5
O11—C23—H23B109.7C29—C30—H30B109.5
C24—C23—H23B109.7H30A—C30—H30B109.5
H23A—C23—H23B108.2C29—C30—H30C109.5
O12—C24—C23108.67 (18)H30A—C30—H30C109.5
O12—C24—H24A110.0H30B—C30—H30C109.5
C23—C24—H24A110.0

Experimental details

Crystal data
Chemical formula[K(C12H24)]2[Rh(CN)3(CO)]·C2H3N
Mr856.86
Crystal system, space groupMonoclinic, P21/c
Temperature (K)193
a, b, c (Å)22.439 (6), 8.553 (2), 20.576 (5)
β (°) 90.178 (4)
V3)3948.9 (17)
Z4
Radiation typeMo Kα
µ (mm1)0.71
Crystal size (mm)0.40 × 0.18 × 0.10
Data collection
DiffractometerSiemens SMART CCD
Absorption correctionIntegration
[XPREP in SHELXTL (Bruker, 2001)]
Tmin, Tmax0.775, 0.935
No. of measured, independent and
observed [I > 2σ(I)] reflections
39007, 9709, 7084
Rint0.039
(sin θ/λ)max1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.081, 1.02
No. of reflections9709
No. of parameters452
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.65, 0.27

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXTL (Bruker, 2001), CIFTAB in SHELXTL.

 

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