Bis[(1,4,7,10,13,16-hexa­oxacyclo­octa­decane)­potassium] carbonyl­tricyano­rhodate(I) acetonitrile solvate

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.

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

---

S1. Comment

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 Rh^I 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—C2≡N2 bond angle of 174.2 (3)°. The other trans cyanide ligand is more linear, with an Rh1—C4≡N4 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.

S2. Experimental

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.

S3. Refinement

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 U_iso(H) values were assigned as 1.5 times U_eq of the adjacent atom; the remaining U_iso(H) values were assigned as 1.2 times the adjacent U_eq. A final analysis of variance between observed and calculated structure factors showed little dependence on amplitude or resolution.

Computing details

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

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

Crystal data

[K(C12H24)]2[Rh(CN)3(CO)]·C2H3N	F(000) = 1784
Mr = 856.86	Dx = 1.441 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 949 reflections
a = 22.439 (6) Å	θ = 2.2–26.1°
b = 8.553 (2) Å	µ = 0.71 mm^−1
c = 20.576 (5) Å	T = 193 K
β = 90.178 (4)°	Tabular, yellow
V = 3948.9 (17) Å^3	0.40 × 0.18 × 0.10 mm
Z = 4

Data collection

Siemens SMART CCD diffractometer	9709 independent reflections
Radiation source: normal-focus sealed tube	7084 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.039
ω scans	θmax = 28.3°, θmin = 1.8°
Absorption correction: integration [XPREP in SHELXTL (Bruker, 2001)]	h = −29→29
Tmin = 0.775, Tmax = 0.935	k = −11→11
39007 measured reflections	l = −27→27

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.081	H-atom parameters not refined
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0376P)^2 + 0.650P] where P = (Fo^2 + 2Fc^2)/3
9709 reflections	(Δ/σ)max = 0.001
452 parameters	Δρmax = 0.65 e Å^−3
0 restraints	Δρmin = −0.27 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	0.31857 (11)	0.4631 (3)	0.45378 (11)	0.0374 (5)
C2	0.29937 (11)	0.2486 (3)	0.54646 (12)	0.0436 (6)
C3	0.17146 (12)	0.2831 (3)	0.51821 (10)	0.0372 (5)
C4	0.20208 (10)	0.5043 (3)	0.42098 (11)	0.0332 (5)
C5	0.54676 (11)	0.2815 (3)	0.67632 (13)	0.0467 (6)
H5A	0.5663	0.2258	0.7128	0.056*
H5B	0.5611	0.3910	0.6762	0.056*
C6	0.56204 (11)	0.2047 (3)	0.61387 (13)	0.0475 (6)
H6A	0.5413	0.2579	0.5775	0.057*
H6B	0.6055	0.2115	0.6063	0.057*
C7	0.56500 (12)	−0.0415 (3)	0.56224 (13)	0.0517 (7)
H7A	0.6089	−0.0335	0.5594	0.062*
H7B	0.5476	0.0017	0.5218	0.062*
C8	0.54711 (13)	−0.2083 (3)	0.56989 (13)	0.0562 (8)
H8A	0.5612	−0.2697	0.5322	0.067*
H8B	0.5655	−0.2522	0.6097	0.067*
C9	0.46425 (17)	−0.3753 (3)	0.58089 (15)	0.0693 (10)
H9A	0.4826	−0.4230	0.6200	0.083*
H9B	0.4767	−0.4368	0.5425	0.083*
C10	0.39816 (18)	−0.3782 (4)	0.58675 (15)	0.0727 (10)
H10A	0.3798	−0.3199	0.5503	0.087*
H10B	0.3836	−0.4874	0.5853	0.087*
C11	0.31963 (13)	−0.3122 (4)	0.65649 (16)	0.0648 (9)
H11A	0.3054	−0.4217	0.6553	0.078*
H11B	0.2992	−0.2534	0.6215	0.078*
C12	0.30564 (12)	−0.2413 (3)	0.72043 (14)	0.0554 (7)
H12A	0.2625	−0.2512	0.7295	0.067*
H12B	0.3280	−0.2958	0.7553	0.067*
C13	0.30712 (12)	−0.0012 (4)	0.77658 (14)	0.0551 (7)
H13A	0.3299	−0.0448	0.8137	0.066*
H13B	0.2641	−0.0132	0.7858	0.066*
C14	0.32187 (12)	0.1655 (3)	0.76785 (15)	0.0563 (8)
H14A	0.3012	0.2066	0.7289	0.068*
H14B	0.3082	0.2259	0.8061	0.068*
C15	0.40007 (12)	0.3432 (3)	0.74927 (13)	0.0492 (7)
H15A	0.3863	0.4085	0.7860	0.059*
H15B	0.3805	0.3810	0.7091	0.059*
C16	0.46622 (12)	0.3553 (3)	0.74277 (13)	0.0473 (6)
H16A	0.4783	0.4666	0.7413	0.057*
H16B	0.4859	0.3058	0.7806	0.057*
C17	−0.00508 (10)	0.4871 (3)	0.33507 (11)	0.0360 (5)
H17A	−0.0176	0.3771	0.3411	0.043*
H17B	−0.0393	0.5467	0.3174	0.043*
C18	0.01399 (11)	0.5552 (3)	0.39893 (11)	0.0364 (5)
H18A	−0.0182	0.5428	0.4314	0.044*
H18B	0.0499	0.5003	0.4152	0.044*
C19	0.04607 (11)	0.7895 (3)	0.44790 (11)	0.0393 (6)
H19A	0.0854	0.7474	0.4611	0.047*
H19B	0.0173	0.7686	0.4832	0.047*
C20	0.05061 (11)	0.9617 (3)	0.43606 (11)	0.0410 (6)
H20A	0.0117	1.0027	0.4210	0.049*
H20B	0.0614	1.0159	0.4770	0.049*
C21	0.09742 (11)	1.1525 (2)	0.37091 (12)	0.0399 (6)
H21A	0.1019	1.2173	0.4105	0.048*
H21B	0.0601	1.1837	0.3486	0.048*
C22	0.14905 (11)	1.1774 (3)	0.32720 (12)	0.0414 (6)
H22A	0.1532	1.2901	0.3173	0.050*
H22B	0.1861	1.1416	0.3488	0.050*
C23	0.18951 (10)	1.1018 (3)	0.22593 (12)	0.0387 (6)
H23A	0.2244	1.0494	0.2459	0.046*
H23B	0.1998	1.2130	0.2187	0.046*
C24	0.17487 (10)	1.0262 (3)	0.16292 (12)	0.0379 (5)
H24A	0.1388	1.0750	0.1438	0.045*
H24B	0.2083	1.0399	0.1321	0.045*
C25	0.15042 (11)	0.7832 (3)	0.11550 (11)	0.0444 (6)
H25A	0.1827	0.7985	0.0834	0.053*
H25B	0.1130	0.8252	0.0968	0.053*
C26	0.14332 (11)	0.6129 (3)	0.13001 (12)	0.0453 (6)
H26A	0.1362	0.5541	0.0893	0.054*
H26B	0.1800	0.5719	0.1507	0.054*
C27	0.08351 (11)	0.4340 (3)	0.18739 (11)	0.0368 (5)
H27A	0.1188	0.3891	0.2095	0.044*
H27B	0.0765	0.3748	0.1467	0.044*
C28	0.03024 (11)	0.4220 (3)	0.23047 (11)	0.0360 (5)
H28A	−0.0043	0.4744	0.2098	0.043*
H28B	0.0199	0.3107	0.2374	0.043*
K2	0.41763 (2)	0.01588 (6)	0.64526 (2)	0.03286 (12)
K4	0.11693 (2)	0.76142 (5)	0.29493 (2)	0.03016 (11)
N2	0.33164 (11)	0.1784 (3)	0.57816 (12)	0.0668 (7)
N3	0.12678 (11)	0.2346 (3)	0.53609 (10)	0.0532 (6)
N4	0.17687 (9)	0.5791 (2)	0.38304 (10)	0.0446 (5)
O1	0.36257 (9)	0.5153 (2)	0.43544 (9)	0.0590 (5)
O2	0.48381 (7)	0.27863 (18)	0.68453 (7)	0.0384 (4)
O3	0.54409 (7)	0.04487 (19)	0.61690 (8)	0.0429 (4)
O4	0.48392 (8)	−0.21791 (19)	0.57430 (8)	0.0475 (4)
O5	0.38257 (8)	−0.3080 (2)	0.64668 (8)	0.0499 (5)
O6	0.32203 (8)	−0.0821 (2)	0.71854 (8)	0.0476 (4)
O7	0.38472 (7)	0.18370 (19)	0.76048 (8)	0.0411 (4)
O8	0.04352 (6)	0.49446 (17)	0.29121 (7)	0.0321 (3)
O9	0.02666 (7)	0.71612 (17)	0.38950 (7)	0.0330 (3)
O10	0.09486 (7)	0.99053 (17)	0.38818 (7)	0.0351 (4)
O11	0.13994 (7)	1.09131 (17)	0.26813 (7)	0.0348 (4)
O12	0.16451 (7)	0.86317 (17)	0.17404 (7)	0.0345 (4)
O13	0.09383 (7)	0.59454 (17)	0.17282 (7)	0.0361 (4)
Rh1	0.249547 (8)	0.37748 (2)	0.484600 (8)	0.03074 (6)
C29	0.26588 (12)	0.9266 (3)	0.41004 (14)	0.0495 (7)
C30	0.23603 (13)	0.8992 (3)	0.47084 (13)	0.0566 (7)
H30A	0.2579	0.9516	0.5059	0.085*
H30B	0.2345	0.7866	0.4795	0.085*
H30C	0.1954	0.9408	0.4685	0.085*
N1	0.28940 (13)	0.9483 (3)	0.36234 (14)	0.0753 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0391 (14)	0.0380 (13)	0.0350 (13)	0.0012 (11)	−0.0073 (11)	0.0040 (10)
C2	0.0478 (15)	0.0405 (14)	0.0424 (14)	−0.0046 (12)	−0.0098 (12)	0.0063 (11)
C3	0.0491 (16)	0.0387 (13)	0.0239 (11)	−0.0052 (12)	−0.0033 (11)	−0.0010 (10)
C4	0.0315 (12)	0.0296 (11)	0.0383 (13)	−0.0027 (10)	−0.0015 (10)	−0.0007 (10)
C5	0.0332 (14)	0.0402 (14)	0.0665 (18)	−0.0083 (11)	−0.0074 (12)	0.0085 (13)
C6	0.0320 (14)	0.0491 (16)	0.0615 (17)	−0.0029 (12)	0.0076 (12)	0.0156 (13)
C7	0.0359 (14)	0.077 (2)	0.0426 (15)	0.0085 (14)	0.0101 (12)	0.0018 (14)
C8	0.066 (2)	0.0594 (18)	0.0435 (15)	0.0249 (15)	0.0055 (14)	−0.0075 (14)
C9	0.125 (3)	0.0349 (15)	0.0483 (17)	0.0040 (17)	0.0225 (19)	−0.0113 (13)
C10	0.117 (3)	0.0513 (18)	0.0500 (18)	−0.0338 (19)	0.0037 (19)	−0.0105 (15)
C11	0.0538 (19)	0.0578 (18)	0.083 (2)	−0.0260 (15)	−0.0260 (16)	0.0124 (17)
C12	0.0362 (15)	0.0635 (18)	0.0666 (19)	−0.0179 (13)	−0.0049 (13)	0.0220 (16)
C13	0.0336 (14)	0.082 (2)	0.0498 (17)	−0.0006 (14)	0.0116 (12)	0.0077 (16)
C14	0.0338 (15)	0.072 (2)	0.0637 (19)	0.0129 (14)	0.0098 (13)	−0.0069 (15)
C15	0.0589 (18)	0.0406 (15)	0.0480 (16)	0.0121 (12)	0.0017 (13)	−0.0098 (12)
C16	0.0576 (17)	0.0372 (14)	0.0472 (15)	−0.0045 (12)	−0.0037 (13)	−0.0074 (11)
C17	0.0308 (12)	0.0295 (12)	0.0477 (14)	−0.0034 (10)	0.0024 (10)	0.0026 (10)
C18	0.0392 (14)	0.0347 (12)	0.0353 (13)	0.0007 (10)	0.0068 (10)	0.0073 (10)
C19	0.0470 (15)	0.0451 (14)	0.0257 (12)	0.0047 (12)	0.0026 (10)	−0.0037 (10)
C20	0.0464 (15)	0.0439 (14)	0.0326 (13)	0.0052 (12)	0.0013 (11)	−0.0112 (11)
C21	0.0536 (16)	0.0278 (12)	0.0383 (13)	0.0065 (11)	−0.0108 (12)	−0.0072 (10)
C22	0.0469 (15)	0.0280 (11)	0.0491 (15)	−0.0039 (11)	−0.0163 (12)	−0.0017 (11)
C23	0.0261 (12)	0.0295 (12)	0.0604 (16)	−0.0025 (10)	0.0002 (11)	0.0057 (11)
C24	0.0286 (12)	0.0376 (13)	0.0475 (14)	0.0044 (10)	0.0070 (10)	0.0132 (11)
C25	0.0418 (15)	0.0618 (17)	0.0297 (13)	−0.0025 (13)	0.0095 (11)	−0.0047 (12)
C26	0.0395 (14)	0.0551 (16)	0.0413 (14)	0.0000 (12)	0.0120 (11)	−0.0191 (12)
C27	0.0423 (14)	0.0325 (12)	0.0355 (13)	0.0059 (10)	−0.0035 (11)	−0.0081 (10)
C28	0.0408 (14)	0.0294 (11)	0.0379 (13)	−0.0025 (10)	−0.0103 (11)	−0.0037 (10)
K2	0.0317 (3)	0.0329 (3)	0.0341 (3)	−0.0010 (2)	−0.0015 (2)	0.0024 (2)
K4	0.0348 (3)	0.0277 (2)	0.0280 (2)	0.0028 (2)	0.00089 (19)	0.00160 (19)
N2	0.0628 (17)	0.0679 (16)	0.0694 (17)	0.0018 (13)	−0.0242 (13)	0.0271 (14)
N3	0.0596 (15)	0.0655 (15)	0.0344 (12)	−0.0211 (13)	0.0032 (11)	0.0011 (11)
N4	0.0420 (12)	0.0403 (12)	0.0514 (13)	0.0028 (10)	−0.0106 (10)	0.0088 (10)
O1	0.0464 (12)	0.0709 (14)	0.0597 (12)	−0.0106 (10)	0.0009 (10)	0.0125 (10)
O2	0.0347 (9)	0.0372 (9)	0.0434 (9)	−0.0034 (7)	−0.0035 (7)	−0.0042 (7)
O3	0.0390 (10)	0.0450 (10)	0.0447 (10)	0.0025 (8)	0.0101 (8)	0.0066 (8)
O4	0.0602 (12)	0.0377 (10)	0.0444 (10)	0.0056 (9)	0.0075 (9)	0.0001 (8)
O5	0.0613 (12)	0.0448 (10)	0.0436 (10)	−0.0164 (9)	−0.0052 (9)	−0.0012 (8)
O6	0.0410 (10)	0.0549 (11)	0.0470 (11)	−0.0118 (8)	0.0031 (8)	0.0115 (9)
O7	0.0327 (9)	0.0441 (9)	0.0465 (10)	0.0067 (7)	0.0019 (7)	−0.0020 (8)
O8	0.0285 (8)	0.0349 (8)	0.0330 (8)	−0.0044 (7)	0.0009 (6)	−0.0049 (7)
O9	0.0400 (9)	0.0310 (8)	0.0280 (8)	0.0030 (7)	0.0014 (7)	−0.0013 (6)
O10	0.0424 (9)	0.0286 (8)	0.0344 (9)	0.0043 (7)	0.0010 (7)	−0.0047 (7)
O11	0.0317 (9)	0.0325 (8)	0.0402 (9)	−0.0052 (7)	−0.0014 (7)	−0.0025 (7)
O12	0.0377 (9)	0.0357 (8)	0.0301 (8)	0.0002 (7)	0.0026 (7)	0.0026 (7)
O13	0.0366 (9)	0.0348 (9)	0.0370 (9)	0.0029 (7)	0.0051 (7)	−0.0046 (7)
Rh1	0.03406 (10)	0.02909 (9)	0.02903 (10)	0.00036 (8)	−0.00592 (7)	0.00219 (8)
C29	0.0452 (16)	0.0535 (16)	0.0498 (17)	0.0084 (13)	−0.0031 (13)	−0.0002 (13)
C30	0.067 (2)	0.0557 (18)	0.0468 (16)	−0.0127 (15)	0.0086 (14)	−0.0091 (13)
N1	0.079 (2)	0.087 (2)	0.0608 (17)	0.0155 (16)	0.0169 (15)	0.0062 (16)

Geometric parameters (Å, º)

C1—O1	1.149 (3)	C18—H18B	0.9900
C1—Rh1	1.828 (3)	C19—O9	1.423 (3)
C2—N2	1.144 (3)	C19—C20	1.497 (3)
C2—Rh1	2.019 (2)	C19—H19A	0.9900
C3—N3	1.147 (3)	C19—H19B	0.9900
C3—Rh1	2.051 (3)	C20—O10	1.422 (3)
C4—N4	1.155 (3)	C20—H20A	0.9900
C4—Rh1	2.004 (2)	C20—H20B	0.9900
C5—O2	1.423 (3)	C21—O10	1.432 (3)
C5—C6	1.484 (4)	C21—C22	1.484 (3)
C5—H5A	0.9900	C21—H21A	0.9900
C5—H5B	0.9900	C21—H21B	0.9900
C6—O3	1.427 (3)	C22—O11	1.435 (3)
C6—H6A	0.9900	C22—H22A	0.9900
C6—H6B	0.9900	C22—H22B	0.9900
C7—O3	1.426 (3)	C23—O11	1.416 (3)
C7—C8	1.490 (4)	C23—C24	1.485 (3)
C7—H7A	0.9900	C23—H23A	0.9900
C7—H7B	0.9900	C23—H23B	0.9900
C8—O4	1.423 (3)	C24—O12	1.432 (3)
C8—H8A	0.9900	C24—H24A	0.9900
C8—H8B	0.9900	C24—H24B	0.9900
C9—O4	1.424 (3)	C25—O12	1.420 (3)
C9—C10	1.488 (5)	C25—C26	1.495 (3)
C9—H9A	0.9900	C25—H25A	0.9900
C9—H9B	0.9900	C25—H25B	0.9900
C10—O5	1.416 (3)	C26—O13	1.428 (3)
C10—H10A	0.9900	C26—H26A	0.9900
C10—H10B	0.9900	C26—H26B	0.9900
C11—O5	1.428 (3)	C27—O13	1.424 (3)
C11—C12	1.483 (4)	C27—C28	1.494 (3)
C11—H11A	0.9900	C27—H27A	0.9900
C11—H11B	0.9900	C27—H27B	0.9900
C12—O6	1.412 (3)	C28—O8	1.426 (3)
C12—H12A	0.9900	C28—H28A	0.9900
C12—H12B	0.9900	C28—H28B	0.9900
C13—O6	1.421 (3)	K2—N2	2.747 (2)
C13—C14	1.476 (4)	K2—O6	2.7563 (18)
C13—H13A	0.9900	K2—O2	2.8110 (17)
C13—H13B	0.9900	K2—O7	2.8699 (18)
C14—O7	1.427 (3)	K2—O5	2.8801 (19)
C14—H14A	0.9900	K2—O4	2.8908 (18)
C14—H14B	0.9900	K2—O3	2.9094 (18)
C15—O7	1.426 (3)	K4—N4	2.741 (2)
C15—C16	1.494 (4)	K4—O10	2.7880 (16)
C15—H15A	0.9900	K4—O8	2.8163 (16)
C15—H15B	0.9900	K4—O9	2.8398 (16)
C16—O2	1.423 (3)	K4—O12	2.8462 (16)
C16—H16A	0.9900	K4—O11	2.9212 (17)
C16—H16B	0.9900	K4—O13	2.9343 (17)
C17—O8	1.419 (3)	C29—N1	1.131 (3)
C17—C18	1.498 (3)	C29—C30	1.440 (4)
C17—H17A	0.9900	C30—H30A	0.9800
C17—H17B	0.9900	C30—H30B	0.9800
C18—O9	1.419 (3)	C30—H30C	0.9800
C18—H18A	0.9900
O1—C1—Rh1	178.6 (2)	O12—C24—H24B	110.0
N2—C2—Rh1	174.2 (3)	C23—C24—H24B	110.0
N3—C3—Rh1	177.7 (2)	H24A—C24—H24B	108.3
N4—C4—Rh1	177.2 (2)	O12—C25—C26	108.88 (19)
O2—C5—C6	109.1 (2)	O12—C25—H25A	109.9
O2—C5—H5A	109.9	C26—C25—H25A	109.9
C6—C5—H5A	109.9	O12—C25—H25B	109.9
O2—C5—H5B	109.9	C26—C25—H25B	109.9
C6—C5—H5B	109.9	H25A—C25—H25B	108.3
H5A—C5—H5B	108.3	O13—C26—C25	108.31 (19)
O3—C6—C5	108.7 (2)	O13—C26—H26A	110.0
O3—C6—H6A	110.0	C25—C26—H26A	110.0
C5—C6—H6A	110.0	O13—C26—H26B	110.0
O3—C6—H6B	110.0	C25—C26—H26B	110.0
C5—C6—H6B	110.0	H26A—C26—H26B	108.4
H6A—C6—H6B	108.3	O13—C27—C28	108.80 (18)
O3—C7—C8	108.8 (2)	O13—C27—H27A	109.9
O3—C7—H7A	109.9	C28—C27—H27A	109.9
C8—C7—H7A	109.9	O13—C27—H27B	109.9
O3—C7—H7B	109.9	C28—C27—H27B	109.9
C8—C7—H7B	109.9	H27A—C27—H27B	108.3
H7A—C7—H7B	108.3	O8—C28—C27	108.94 (18)
O4—C8—C7	109.3 (2)	O8—C28—H28A	109.9
O4—C8—H8A	109.8	C27—C28—H28A	109.9
C7—C8—H8A	109.8	O8—C28—H28B	109.9
O4—C8—H8B	109.8	C27—C28—H28B	109.9
C7—C8—H8B	109.8	H28A—C28—H28B	108.3
H8A—C8—H8B	108.3	N2—K2—O6	83.23 (7)
O4—C9—C10	109.4 (3)	N2—K2—O2	96.29 (7)
O4—C9—H9A	109.8	O6—K2—O2	119.81 (5)
C10—C9—H9A	109.8	N2—K2—O7	88.85 (7)
O4—C9—H9B	109.8	O6—K2—O7	59.83 (5)
C10—C9—H9B	109.8	O2—K2—O7	59.98 (5)
H9A—C9—H9B	108.2	N2—K2—O5	107.48 (7)
O5—C10—C9	108.2 (2)	O6—K2—O5	59.27 (6)
O5—C10—H10A	110.1	O2—K2—O5	155.53 (5)
C9—C10—H10A	110.1	O7—K2—O5	113.69 (5)
O5—C10—H10B	110.1	N2—K2—O4	117.26 (7)
C9—C10—H10B	110.1	O6—K2—O4	117.95 (6)
H10A—C10—H10B	108.4	O2—K2—O4	115.21 (5)
O5—C11—C12	109.1 (2)	O7—K2—O4	153.80 (5)
O5—C11—H11A	109.9	O5—K2—O4	58.72 (5)
C12—C11—H11A	109.9	N2—K2—O3	122.69 (7)
O5—C11—H11B	109.9	O6—K2—O3	153.74 (5)
C12—C11—H11B	109.9	O2—K2—O3	58.31 (5)
H11A—C11—H11B	108.3	O7—K2—O3	112.13 (5)
O6—C12—C11	108.3 (2)	O5—K2—O3	110.52 (5)
O6—C12—H12A	110.0	O4—K2—O3	56.90 (5)
C11—C12—H12A	110.0	N4—K4—O10	91.86 (6)
O6—C12—H12B	110.0	N4—K4—O8	80.94 (6)
C11—C12—H12B	110.0	O10—K4—O8	118.90 (5)
H12A—C12—H12B	108.4	N4—K4—O9	79.55 (6)
O6—C13—C14	108.3 (2)	O10—K4—O9	59.71 (5)
O6—C13—H13A	110.0	O8—K4—O9	59.31 (4)
C14—C13—H13A	110.0	N4—K4—O12	124.57 (6)
O6—C13—H13B	110.0	O10—K4—O12	117.03 (5)
C14—C13—H13B	110.0	O8—K4—O12	116.43 (5)
H13A—C13—H13B	108.4	O9—K4—O12	155.63 (5)
O7—C14—C13	109.9 (2)	N4—K4—O11	125.99 (6)
O7—C14—H14A	109.7	O10—K4—O11	58.86 (5)
C13—C14—H14A	109.7	O8—K4—O11	151.84 (5)
O7—C14—H14B	109.7	O9—K4—O11	112.83 (4)
C13—C14—H14B	109.7	O12—K4—O11	58.18 (4)
H14A—C14—H14B	108.2	N4—K4—O13	112.00 (6)
O7—C15—C16	108.8 (2)	O10—K4—O13	154.14 (5)
O7—C15—H15A	109.9	O8—K4—O13	58.71 (4)
C16—C15—H15A	109.9	O9—K4—O13	113.32 (5)
O7—C15—H15B	109.9	O12—K4—O13	57.74 (5)
C16—C15—H15B	109.9	O11—K4—O13	109.82 (5)
H15A—C15—H15B	108.3	C2—N2—K2	174.3 (2)
O2—C16—C15	108.8 (2)	C4—N4—K4	178.79 (19)
O2—C16—H16A	109.9	C16—O2—C5	111.72 (19)
C15—C16—H16A	109.9	C16—O2—K2	117.57 (14)
O2—C16—H16B	109.9	C5—O2—K2	120.22 (13)
C15—C16—H16B	109.9	C7—O3—C6	111.60 (19)
H16A—C16—H16B	108.3	C7—O3—K2	115.95 (14)
O8—C17—C18	108.82 (18)	C6—O3—K2	111.48 (13)
O8—C17—H17A	109.9	C8—O4—C9	111.7 (2)
C18—C17—H17A	109.9	C8—O4—K2	120.42 (15)
O8—C17—H17B	109.9	C9—O4—K2	116.48 (16)
C18—C17—H17B	109.9	C10—O5—C11	111.1 (2)
H17A—C17—H17B	108.3	C10—O5—K2	109.30 (15)
O9—C18—C17	108.29 (18)	C11—O5—K2	107.20 (16)
O9—C18—H18A	110.0	C12—O6—C13	112.6 (2)
C17—C18—H18A	110.0	C12—O6—K2	120.78 (16)
O9—C18—H18B	110.0	C13—O6—K2	119.85 (15)
C17—C18—H18B	110.0	C15—O7—C14	111.13 (19)
H18A—C18—H18B	108.4	C15—O7—K2	106.38 (14)
O9—C19—C20	108.52 (18)	C14—O7—K2	106.87 (15)
O9—C19—H19A	110.0	C17—O8—C28	112.28 (17)
C20—C19—H19A	110.0	C17—O8—K4	117.99 (12)
O9—C19—H19B	110.0	C28—O8—K4	119.80 (12)
C20—C19—H19B	110.0	C18—O9—C19	111.93 (16)
H19A—C19—H19B	108.4	C18—O9—K4	111.70 (12)
O10—C20—C19	109.34 (18)	C19—O9—K4	107.54 (13)
O10—C20—H20A	109.8	C20—O10—C21	111.60 (17)
C19—C20—H20A	109.8	C20—O10—K4	118.74 (12)
O10—C20—H20B	109.8	C21—O10—K4	120.14 (13)
C19—C20—H20B	109.8	C23—O11—C22	112.13 (17)
H20A—C20—H20B	108.3	C23—O11—K4	108.46 (12)
O10—C21—C22	108.73 (19)	C22—O11—K4	111.13 (12)
O10—C21—H21A	109.9	C25—O12—C24	111.69 (17)
C22—C21—H21A	109.9	C25—O12—K4	120.72 (13)
O10—C21—H21B	109.9	C24—O12—K4	119.92 (13)
C22—C21—H21B	109.9	C27—O13—C26	111.30 (17)
H21A—C21—H21B	108.3	C27—O13—K4	108.48 (12)
O11—C22—C21	109.29 (18)	C26—O13—K4	109.80 (13)
O11—C22—H22A	109.8	C1—Rh1—C4	90.33 (9)
C21—C22—H22A	109.8	C1—Rh1—C2	88.24 (10)
O11—C22—H22B	109.8	C4—Rh1—C2	178.16 (10)
C21—C22—H22B	109.8	C1—Rh1—C3	179.20 (10)
H22A—C22—H22B	108.3	C4—Rh1—C3	88.87 (9)
O11—C23—C24	109.61 (18)	C2—Rh1—C3	92.56 (10)
O11—C23—H23A	109.7	N1—C29—C30	179.9 (4)
C24—C23—H23A	109.7	C29—C30—H30A	109.5
O11—C23—H23B	109.7	C29—C30—H30B	109.5
C24—C23—H23B	109.7	H30A—C30—H30B	109.5
H23A—C23—H23B	108.2	C29—C30—H30C	109.5
O12—C24—C23	108.67 (18)	H30A—C30—H30C	109.5
O12—C24—H24A	110.0	H30B—C30—H30C	109.5
C23—C24—H24A	110.0