A ferric-cyanide-bridged one-dimensional dirhodium complex with (18-­crown-6)­potassium cations

The crystal structure of the title compound, catena-poly[bis[aqua(18-crown-6)­potassium] di­aqua(18-crown-6)­potassium [[tetra-μ-benzoato-2:3κ⁸O:O′-μ-cyano-1:2κ²C:N-tetra­cyano-1κC-irondirhodium(Rh—Rh)]-μ-cyano-1κC:3′κN] octahydrate], [K(18-crown-6)(H₂O)]₂[K(18-crown-6)(H₂O)₂]­[FeRh₂(C₇H₅O₂)₄(CN)₆]·8H₂O, where (18-crown-6) is 1,4,7,10,13,16-hexaoxa­cyclo­octa­decane (C₁₂H₂₄O₆), has been determined. Ferric cyanides connect the dirhodium units to form a one-dimensional chain compound. [K(18-crown-6-ether)(H₂O)₂] cations (with inversion symmetry) and [K(18-crown-6-ether)(H₂O)] cations (in general positions) are located between the chains.

S1. Comment

Metal cyanide compounds have been used to synthesize coordination polymers (Ward, 1995; Vahrenkamp et al., 1997, and references therein). Hexacyanometallate ions [M(CN)]^n- can provide one- (Colacio et al., 2000), two- (Miyasaka et al., 1997) and three-dimensional polymers (Miyasaka et al., 1998a,b; Langenberg et al., 1997) since cyano groups are directed to all three axes. Dirhodium acetate units are connected by Co(CN)₆^3- to form a two-dimensional sheet (Lu et al., 1996). It was the first example for dimetal units to be connected by a metal cyanide. Diruthenium units are also bridged by Co(CN)₆^3- to form a pentanuclear complex (Kim et al., 1998).

Ferric cyanide can also be used as a metal cyanide to connect dimetal units to form one-, two-, or three-dimensional compounds. Only the potassium salt among the ferric cyanides is water-soluble. 18-Crown-6-ether can help increase the solubility of a ferric cyanide (Miyasaka et al., 1998a).

Only trans-cyano groups of the ferric cyanide connect dirhodium units to form an one-dimensional chain compound. The Rh—Rh distance is 2.4109 (4) Å which is a little longer than the typical Rh—Rh distance in tetracarboxylatodirhodium(II,II) complexes. Rh—N(bridging cyano group) distances are 2.208 (3) and 2.200 (3) Å. The chain is not linear with angles of 168.1 (3) and 170.7 (3)° for C5—N1—Rh1 and C10—N6—Rh2ⁱⁱ (ii = x, 3/2 - y, z - 1/2), repectively. The benzoate groups of a dirhodium unit are staggered with those of the next dirhodium unit, and also twisted to the four Fe—CN bonds. The Fe—CN bonds of a ferric cyanide are eclipsed with those bonds of the next ferric cyanide. Actually, the ferric cyanide has the possibility to make three-dimensional network structures since all six cyano groups can connect some complex units. However, a benzoate bridging ligand of a dirhodium complex is too bulky to make a two- or three-dimensional compound. Potassium cations encapsulated by crownether are located between anion chains. Two K atoms K1 and K2 are on general positions whereas K3 and K4 are on inversion centres. The asymmetric unit therefore contains 3 crownether molecules. Each K1 and K2 has a water molecule on the one axial site and the other axial site interact with the phenyl group of the benzoate bridging ligand. K3 and K4 have water molecules on both axial sites since it has an inversion centre on the K atom. There are hydrogen bondings between hydrogen atoms of water molecules bonded to the potassium, K3 and K4, and nitrogen atoms, N2, N3, N4 and N5 of free cyano groups.

Related literature

For related literature, see: Colacio et al. (2000); Kim et al. (1998); Langenberg et al. (1997); Lu et al. (1996); Miyasaka et al. (1997, 1998a, 1998b); Vahrenkamp et al. (1997); Ward (1995).

S2. Experimental

A methanol solution of Rh₂(O₂CC₆H₅)₄(CH₃OH)₂ was added to a methanol solution of [K(18-crown-6-ether)(H₂O)₂][Fe(CN)₆]3H₂O. The mixture solution was allowed to stand for several days in the dark room until almost all the solvent was evaporated. Small brown block crystals for X-ray data collection were obtained. IR(KBr): ν(C≡N) 2112.77 cm^-1

S3. Refinement

All H atoms except water molecule hydrogen atoms were inserted at calculated positions and treated as riding with isotropic displacement parameters.

Computing details

Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures

Fig. 1. ORTEP drawing of compound (I). All H atoms are omitted except the water hydrogen atoms.

[{K(18-crown-6-ether)(H₂O)}₂{K(18-crown-6-ether)(H₂O)₂}] [Rh₂(O₂CC₆H₅)₄Fe(CN)₆]8H₂O (18-crown-6-ether = 1,4,7,10,13,16-hexaoxacyclooctadecane)

Crystal data

[K(C12H24O6)(H2O)]2[K(C12H24O6)(H2O)2][FeRh2(C7H5O2)4 (CN)6]·8H2O	F(000) = 4220
Mr = 2028.66	Dx = 1.447 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.0884 (4) Å	Cell parameters from 75952 reflections
b = 23.1083 (5) Å	θ = 2.6–27.0°
c = 25.8233 (6) Å	µ = 0.72 mm^−1
β = 104.090 (1)°	T = 150 K
V = 9311.6 (4) Å^3	Block, brown
Z = 4	0.25 × 0.15 × 0.14 mm

Data collection

Nonius Kappa-CCD diffractometer	20305 independent reflections
Radiation source: fine-focus sealed tube	13576 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
φ scans and ω scans with κ offsets	θmax = 27.0°, θmin = 2.6°
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	h = −21→20
Tmin = 0.840, Tmax = 0.906	k = −30→29
75952 measured reflections	l = −32→31

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)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.116	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0364P)^2 + 9.4629P] where P = (Fo^2 + 2Fc^2)/3
20305 reflections	(Δ/σ)max = 0.003
1156 parameters	Δρmax = 1.33 e Å^−3
64 restraints	Δρmin = −0.69 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Rh1	0.236786 (18)	0.739165 (11)	0.705813 (10)	0.01490 (7)
Rh2	0.253935 (18)	0.752744 (11)	0.800397 (10)	0.01520 (7)
Fe1	0.24944 (3)	0.73350 (2)	0.503479 (18)	0.01547 (11)
O1	0.11733 (16)	0.77579 (10)	0.69407 (9)	0.0201 (6)
O2	0.13363 (16)	0.78642 (10)	0.78280 (9)	0.0216 (6)
O3	0.18367 (16)	0.66008 (10)	0.71555 (9)	0.0197 (6)
O4	0.19748 (16)	0.67472 (10)	0.80386 (9)	0.0212 (6)
O5	0.35729 (16)	0.70515 (10)	0.72340 (9)	0.0206 (6)
O6	0.37202 (16)	0.71459 (10)	0.81248 (9)	0.0188 (6)
O7	0.29242 (16)	0.81762 (10)	0.70228 (9)	0.0205 (6)
O8	0.31019 (16)	0.83076 (10)	0.79098 (9)	0.0190 (6)
N1	0.22889 (19)	0.72957 (12)	0.61971 (11)	0.0178 (7)
N2	0.0523 (2)	0.73853 (13)	0.45991 (12)	0.0281 (8)
N3	0.2475 (2)	0.59918 (14)	0.50097 (12)	0.0252 (7)
N4	0.4473 (2)	0.73304 (13)	0.54512 (12)	0.0260 (7)
N5	0.2524 (2)	0.86766 (14)	0.50746 (13)	0.0331 (8)
N6	0.2647 (2)	0.73666 (12)	0.38643 (11)	0.0192 (7)
C1	0.0902 (2)	0.78816 (15)	0.73472 (14)	0.0204 (8)
C2	0.1752 (2)	0.64517 (15)	0.76112 (14)	0.0193 (8)
C3	0.3993 (2)	0.70123 (14)	0.77173 (14)	0.0182 (8)
C4	0.3194 (2)	0.84587 (15)	0.74553 (13)	0.0184 (8)
C5	0.2366 (2)	0.73104 (14)	0.57660 (13)	0.0172 (8)
C6	0.1254 (3)	0.73576 (15)	0.47697 (13)	0.0199 (8)
C7	0.2483 (2)	0.64940 (16)	0.50164 (13)	0.0175 (7)
C8	0.3736 (3)	0.73266 (15)	0.52894 (13)	0.0201 (8)
C9	0.2512 (2)	0.81767 (16)	0.50631 (14)	0.0217 (8)
C10	0.2597 (2)	0.73493 (14)	0.43002 (14)	0.0188 (8)
C11	−0.0028 (3)	0.80440 (15)	0.72577 (14)	0.0228 (9)
C12	−0.0453 (3)	0.79096 (18)	0.76569 (16)	0.0340 (10)
H12A	−0.0146	0.7748	0.7986	0.041*
C13	−0.1328 (3)	0.8014 (2)	0.75665 (17)	0.0429 (12)
H13A	−0.1623	0.7916	0.7831	0.051*
C14	−0.1768 (3)	0.82610 (19)	0.70915 (17)	0.0404 (12)
H14A	−0.2365	0.8333	0.7030	0.049*
C15	−0.1338 (3)	0.84038 (17)	0.67046 (16)	0.0330 (10)
H15A	−0.1642	0.8581	0.6382	0.040*
C16	−0.0473 (3)	0.82901 (16)	0.67838 (15)	0.0258 (9)
H16A	−0.0185	0.8381	0.6513	0.031*
C21	0.1352 (2)	0.58737 (14)	0.76547 (14)	0.0181 (8)
C22	0.1354 (3)	0.56430 (16)	0.81529 (15)	0.0270 (9)
H22A	0.1593	0.5859	0.8467	0.032*
C23	0.1010 (3)	0.51023 (17)	0.81937 (17)	0.0369 (11)
H23A	0.1015	0.4948	0.8535	0.044*
C24	0.0659 (3)	0.47844 (17)	0.77387 (17)	0.0350 (11)
H24A	0.0426	0.4411	0.7767	0.042*
C25	0.0651 (3)	0.50150 (16)	0.72409 (16)	0.0323 (10)
H25	0.0407	0.4799	0.6927	0.039*
C26	0.0995 (2)	0.55584 (15)	0.71984 (15)	0.0234 (9)
H26	0.0986	0.5714	0.6857	0.028*
C31	0.4898 (3)	0.68055 (15)	0.78177 (14)	0.0221 (9)
C32	0.5308 (3)	0.65630 (16)	0.83040 (15)	0.0293 (10)
H32A	0.5002	0.6503	0.8571	0.035*
C33	0.6158 (3)	0.64095 (18)	0.83988 (17)	0.0378 (11)
H33A	0.6432	0.6237	0.8731	0.045*
C36	0.5361 (3)	0.68937 (17)	0.74319 (15)	0.0291 (9)
H36A	0.5086	0.7056	0.7096	0.035*
C34	0.6619 (3)	0.65004 (18)	0.80225 (18)	0.0406 (12)
H34A	0.7207	0.6396	0.8095	0.049*
C35	0.6217 (3)	0.67460 (19)	0.75374 (17)	0.0380 (11)
H35A	0.6532	0.6813	0.7276	0.046*
C41	0.3649 (2)	0.90148 (15)	0.74198 (14)	0.0192 (8)
C42	0.3929 (3)	0.93573 (15)	0.78731 (14)	0.0259 (9)
H42	0.3855	0.9229	0.8209	0.031*
C43	0.4314 (3)	0.98871 (16)	0.78325 (16)	0.0306 (10)
H43	0.4493	1.0123	0.8141	0.037*
C44	0.4442 (3)	1.00758 (17)	0.73499 (16)	0.0327 (10)
H44A	0.4709	1.0438	0.7326	0.039*
C45	0.4176 (3)	0.97282 (17)	0.68994 (16)	0.0327 (10)
H45A	0.4265	0.9854	0.6567	0.039*
C46	0.3785 (3)	0.92021 (16)	0.69323 (15)	0.0271 (9)
H46A	0.3607	0.8967	0.6623	0.032*
K1	0.58215 (6)	0.95905 (4)	0.88792 (3)	0.0299 (2)
O11	0.62998 (18)	0.86742 (12)	0.82540 (11)	0.0352 (7)
O12	0.53774 (18)	0.84207 (11)	0.90339 (10)	0.0303 (7)
O13	0.43597 (18)	0.93303 (11)	0.92327 (10)	0.0292 (7)
O14	0.47653 (18)	1.04801 (11)	0.91375 (10)	0.0282 (6)
O15	0.59106 (18)	1.07197 (11)	0.85216 (10)	0.0299 (7)
O16	0.69074 (19)	0.98241 (12)	0.82399 (11)	0.0358 (7)
O17	0.6850 (2)	0.89236 (13)	0.97107 (13)	0.0525 (9)
H1W	0.7282 (11)	0.8807 (12)	0.9604 (7)	0.063*
H2W	0.6553 (8)	0.8631 (8)	0.9758 (10)	0.063*
C101	0.7011 (3)	0.9395 (2)	0.78678 (18)	0.0490 (13)
H10A	0.7530	0.9477	0.7739	0.059*
H10B	0.6510	0.9397	0.7557	0.059*
C102	0.7091 (3)	0.8818 (2)	0.81317 (19)	0.0461 (13)
H10C	0.7237	0.8522	0.7891	0.055*
H10D	0.7555	0.8827	0.8463	0.055*
C103	0.6342 (3)	0.81239 (18)	0.85130 (19)	0.0417 (12)
H10E	0.6812	0.8124	0.8842	0.050*
H10F	0.6461	0.7817	0.8274	0.050*
C104	0.5506 (3)	0.80076 (18)	0.86494 (18)	0.0409 (12)
H10G	0.5033	0.8034	0.8323	0.049*
H10H	0.5508	0.7612	0.8796	0.049*
C105	0.4581 (3)	0.83225 (16)	0.91679 (16)	0.0316 (10)
H10I	0.4597	0.7946	0.9354	0.038*
H10J	0.4112	0.8309	0.8839	0.038*
C106	0.4421 (3)	0.87977 (17)	0.95208 (16)	0.0353 (11)
H10K	0.3882	0.8724	0.9630	0.042*
H10L	0.4897	0.8818	0.9846	0.042*
C107	0.3965 (3)	0.97713 (17)	0.94772 (16)	0.0345 (10)
H10M	0.4304	0.9840	0.9847	0.041*
H10N	0.3381	0.9650	0.9491	0.041*
C108	0.3922 (3)	1.03115 (17)	0.91548 (17)	0.0350 (11)
H10O	0.3572	1.0243	0.8788	0.042*
H10P	0.3649	1.0624	0.9317	0.042*
C109	0.4792 (3)	1.10354 (16)	0.88979 (16)	0.0326 (10)
H10Q	0.4605	1.1338	0.9117	0.039*
H10R	0.4400	1.1042	0.8537	0.039*
C110	0.5679 (3)	1.11517 (16)	0.88608 (16)	0.0336 (11)
H11A	0.5717	1.1542	0.8710	0.040*
H11B	0.6075	1.1136	0.9220	0.040*
C111	0.6745 (3)	1.08168 (18)	0.84384 (17)	0.0374 (11)
H11C	0.7186	1.0758	0.8776	0.045*
H11D	0.6792	1.1218	0.8315	0.045*
C112	0.6868 (3)	1.0398 (2)	0.80284 (18)	0.0436 (12)
H11D'	0.6387	1.0428	0.7707	0.052*
H11E	0.7406	1.0488	0.7923	0.052*
K2	−0.08470 (6)	0.53804 (3)	0.61407 (3)	0.0281 (2)
O21	−0.05323 (19)	0.65457 (11)	0.59088 (11)	0.0328 (7)
O22	0.06294 (18)	0.56599 (11)	0.58148 (10)	0.0294 (7)
O23	0.01956 (18)	0.44957 (11)	0.58681 (10)	0.0303 (7)
O24	−0.08988 (19)	0.42395 (11)	0.65138 (11)	0.0354 (7)
O25	−0.1796 (2)	0.51358 (13)	0.68865 (12)	0.0457 (8)
O26	−0.1323 (2)	0.62670 (12)	0.67511 (12)	0.0427 (8)
O27	−0.2086 (2)	0.51995 (12)	0.52878 (12)	0.0396 (8)
H3W	−0.2270 (15)	0.4866 (3)	0.5169 (10)	0.047*
H4W	−0.2442 (15)	0.5455 (4)	0.5131 (10)	0.047*
C201	−0.1507 (4)	0.6779 (2)	0.6442 (2)	0.0630 (17)
H20A	−0.1676	0.7090	0.6660	0.076*
H20B	−0.1992	0.6708	0.6130	0.076*
C202	−0.0762 (4)	0.69632 (19)	0.6260 (2)	0.0531 (14)
H20C	−0.0887	0.7338	0.6071	0.064*
H20D	−0.0273	0.7021	0.6572	0.064*
C203	0.0312 (3)	0.66586 (17)	0.58450 (17)	0.0333 (10)
H20E	0.0721	0.6679	0.6199	0.040*
H20F	0.0321	0.7035	0.5663	0.040*
C204	0.0568 (3)	0.61907 (17)	0.55250 (17)	0.0360 (11)
H20G	0.0138	0.6153	0.5180	0.043*
H20H	0.1128	0.6284	0.5450	0.043*
C205	0.1015 (3)	0.52209 (17)	0.55647 (15)	0.0314 (10)
H20I	0.1603	0.5339	0.5557	0.038*
H20J	0.0679	0.5166	0.5192	0.038*
C206	0.1045 (3)	0.46691 (17)	0.58654 (16)	0.0344 (10)
H20K	0.1322	0.4365	0.5696	0.041*
H20L	0.1387	0.4723	0.6237	0.041*
C207	0.0166 (3)	0.39343 (16)	0.60943 (16)	0.0341 (11)
H20M	0.0573	0.3914	0.6449	0.041*
H20N	0.0332	0.3637	0.5862	0.041*
C208	−0.0722 (3)	0.38219 (17)	0.61470 (16)	0.0382 (12)
H20O	−0.1137	0.3861	0.5796	0.046*
H20P	−0.0767	0.3425	0.6283	0.046*
C209	−0.1716 (3)	0.41590 (19)	0.6623 (2)	0.0468 (13)
H20Q	−0.1787	0.3752	0.6724	0.056*
H20R	−0.2177	0.4254	0.6305	0.056*
C210	−0.1752 (3)	0.4552 (2)	0.7072 (2)	0.0501 (14)
H21A	−0.2263	0.4462	0.7207	0.060*
H21B	−0.1236	0.4499	0.7368	0.060*
C211	−0.1765 (4)	0.5557 (2)	0.7291 (2)	0.0560 (14)
H21C	−0.1191	0.5556	0.7542	0.067*
H21D	−0.2196	0.5465	0.7495	0.067*
C212	−0.1945 (4)	0.6135 (2)	0.7037 (2)	0.0632 (16)
H21E	−0.2522	0.6135	0.6790	0.076*
H21F	−0.1934	0.6432	0.7314	0.076*
K3	0.0000	1.0000	0.5000	0.0314 (3)
O31	−0.1395 (2)	1.04363 (13)	0.42965 (12)	0.0462 (8)
O32	−0.1418 (2)	0.92572 (14)	0.46211 (14)	0.0533 (9)
O33	−0.0085 (2)	0.88973 (13)	0.55412 (12)	0.0439 (8)
O34	−0.0924 (2)	1.07034 (13)	0.55466 (12)	0.0489 (9)
H5W	−0.0609 (7)	1.0978 (8)	0.5697 (11)	0.059*
H6W	−0.1366 (11)	1.0832 (11)	0.5328 (5)	0.059*
C301	−0.2047 (4)	1.0041 (2)	0.4061 (2)	0.0729 (19)
H30A	−0.1883	0.9831	0.3766	0.087*
H30B	−0.2587	1.0253	0.3910	0.087*
C302	−0.2177 (3)	0.9614 (2)	0.4482 (2)	0.0668 (17)
H30C	−0.2260	0.9823	0.4800	0.080*
H30D	−0.2690	0.9373	0.4338	0.080*
C303	−0.1519 (4)	0.8831 (2)	0.5007 (2)	0.0649 (16)
H30E	−0.1977	0.8554	0.4843	0.078*
H30F	−0.1679	0.9021	0.5312	0.078*
C304	−0.0678 (3)	0.8519 (2)	0.5193 (2)	0.0539 (14)
H30G	−0.0760	0.8162	0.5386	0.065*
H30H	−0.0452	0.8410	0.4883	0.065*
C305	0.0734 (3)	0.86427 (19)	0.56982 (18)	0.0446 (13)
H30I	0.0941	0.8538	0.5379	0.054*
H30J	0.0708	0.8286	0.5907	0.054*
C306	0.1329 (3)	0.9070 (2)	0.60315 (18)	0.0495 (13)
H30K	0.1106	0.9191	0.6340	0.059*
H30L	0.1901	0.8893	0.6169	0.059*
K4	0.5000	1.0000	0.5000	0.0354 (3)
O41	0.6303 (2)	0.98949 (12)	0.59337 (11)	0.0397 (8)
O42	0.54822 (19)	1.09840 (11)	0.56555 (11)	0.0344 (7)
O43	0.44526 (19)	1.11088 (12)	0.45939 (11)	0.0382 (7)
O44	0.3935 (2)	0.94414 (13)	0.55597 (12)	0.0489 (9)
H7W	0.3471 (9)	0.9345 (13)	0.5339 (5)	0.059*
H8W	0.4189 (9)	0.9137 (9)	0.5706 (12)	0.059*
C401	0.6344 (3)	1.03636 (18)	0.63010 (16)	0.0406 (11)
H40A	0.6877	1.0338	0.6588	0.049*
H40B	0.5849	1.0346	0.6466	0.049*
C402	0.6326 (3)	1.09211 (18)	0.59992 (17)	0.0398 (11)
H40C	0.6457	1.1251	0.6251	0.048*
H40D	0.6760	1.0912	0.5785	0.048*
C403	0.5393 (3)	1.15149 (17)	0.53662 (17)	0.0380 (11)
H40E	0.5829	1.1538	0.5155	0.046*
H40F	0.5479	1.1846	0.5617	0.046*
C404	0.4517 (3)	1.15404 (18)	0.50043 (17)	0.0393 (11)
H40G	0.4082	1.1467	0.5210	0.047*
H40H	0.4412	1.1929	0.4841	0.047*
C405	0.3643 (3)	1.1117 (2)	0.42157 (19)	0.0495 (13)
H40I	0.3545	1.1500	0.4040	0.059*
H40J	0.3178	1.1044	0.4398	0.059*
C406	0.3640 (3)	1.06560 (19)	0.38076 (18)	0.0459 (12)
H40K	0.3107	1.0679	0.3520	0.055*
H40L	0.4133	1.0710	0.3646	0.055*
O1W	0.0634 (2)	0.82464 (13)	0.37229 (12)	0.0445 (8)
H9W	0.069 (3)	0.7999 (13)	0.3973 (11)	0.053*
H10W	0.098 (2)	0.8163 (16)	0.3532 (14)	0.053*
O2W	−0.1266 (2)	0.74026 (15)	0.41203 (16)	0.0589 (10)
H11W	−0.0722 (4)	0.7388 (19)	0.4218 (19)	0.071*
H12W	−0.142 (2)	0.7702 (13)	0.3929 (17)	0.071*
O3W	0.4301 (2)	0.79917 (19)	0.64301 (15)	0.0707 (12)
H13W	0.3824 (16)	0.795 (2)	0.6510 (18)	0.085*
H14W	0.429 (3)	0.782 (2)	0.6137 (11)	0.085*
O4W	−0.1165 (2)	0.85601 (17)	0.36766 (17)	0.0683 (11)
H15W	−0.0687 (16)	0.850 (2)	0.360 (2)	0.082*
H16W	−0.113 (3)	0.8860 (14)	0.3874 (18)	0.082*
O5W	0.5858 (3)	0.83273 (17)	0.70291 (17)	0.0731 (12)
H17W	0.5334 (8)	0.825 (2)	0.689 (2)	0.088*
H18W	0.617 (2)	0.8062 (17)	0.695 (2)	0.088*
O6W	−0.1807 (2)	0.68322 (19)	0.49241 (18)	0.0776 (12)
H19W	−0.1326 (15)	0.674 (2)	0.5127 (18)	0.093*
H20W	−0.174 (3)	0.7097 (19)	0.4709 (17)	0.093*
O7W	0.6227 (3)	0.7408 (2)	0.6205 (3)	0.1100 (17)
H21W	0.621 (4)	0.770 (2)	0.641 (2)	0.132*
H22W	0.5727 (19)	0.736 (3)	0.600 (2)	0.132*
O8W	0.2612 (8)	1.2259 (3)	0.4509 (4)	0.223 (4)
H23W	0.249 (9)	1.225 (5)	0.481 (3)	0.267*
H24W	0.270 (9)	1.2609 (18)	0.443 (5)	0.267*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.01781 (17)	0.01860 (14)	0.00902 (13)	−0.00044 (12)	0.00465 (11)	−0.00224 (11)
Rh2	0.01895 (16)	0.01851 (14)	0.00912 (13)	−0.00088 (12)	0.00529 (11)	−0.00235 (11)
Fe1	0.0201 (3)	0.0181 (3)	0.0094 (2)	0.0004 (2)	0.0060 (2)	0.0003 (2)
O1	0.0194 (15)	0.0273 (14)	0.0144 (12)	0.0049 (11)	0.0054 (11)	−0.0013 (11)
O2	0.0173 (15)	0.0313 (15)	0.0164 (13)	0.0039 (11)	0.0047 (11)	−0.0056 (11)
O3	0.0283 (16)	0.0193 (13)	0.0125 (12)	−0.0019 (11)	0.0067 (11)	−0.0021 (10)
O4	0.0277 (17)	0.0243 (14)	0.0127 (12)	−0.0049 (11)	0.0073 (11)	−0.0023 (10)
O5	0.0208 (15)	0.0274 (14)	0.0139 (13)	0.0030 (11)	0.0049 (11)	−0.0040 (11)
O6	0.0208 (15)	0.0237 (13)	0.0123 (12)	0.0016 (11)	0.0046 (11)	−0.0018 (10)
O7	0.0260 (16)	0.0215 (13)	0.0148 (13)	−0.0054 (11)	0.0065 (11)	−0.0027 (10)
O8	0.0261 (16)	0.0194 (13)	0.0125 (12)	−0.0029 (11)	0.0065 (11)	−0.0029 (10)
N1	0.0231 (18)	0.0208 (16)	0.0107 (14)	−0.0032 (13)	0.0062 (13)	−0.0027 (12)
N2	0.024 (2)	0.0308 (19)	0.0285 (18)	0.0009 (16)	0.0049 (16)	−0.0025 (15)
N3	0.027 (2)	0.0256 (18)	0.0247 (17)	−0.0026 (15)	0.0101 (14)	−0.0012 (15)
N4	0.027 (2)	0.0258 (18)	0.0251 (17)	0.0013 (15)	0.0068 (16)	0.0013 (14)
N5	0.029 (2)	0.026 (2)	0.046 (2)	−0.0003 (16)	0.0126 (18)	−0.0008 (16)
N6	0.0242 (19)	0.0227 (16)	0.0119 (14)	0.0048 (13)	0.0068 (13)	0.0049 (13)
C1	0.025 (2)	0.0164 (18)	0.0193 (19)	−0.0005 (16)	0.0048 (17)	−0.0029 (15)
C2	0.019 (2)	0.0223 (19)	0.0169 (18)	0.0033 (16)	0.0054 (16)	−0.0009 (15)
C3	0.023 (2)	0.0142 (18)	0.0186 (19)	−0.0023 (15)	0.0067 (17)	−0.0025 (15)
C4	0.017 (2)	0.0202 (19)	0.0175 (19)	0.0031 (15)	0.0041 (16)	−0.0020 (15)
C5	0.020 (2)	0.0154 (18)	0.0167 (18)	−0.0015 (15)	0.0056 (16)	0.0005 (14)
C6	0.025 (2)	0.0217 (19)	0.0140 (17)	−0.0002 (17)	0.0072 (17)	0.0016 (15)
C7	0.016 (2)	0.026 (2)	0.0118 (16)	−0.0008 (16)	0.0063 (14)	0.0010 (16)
C8	0.030 (2)	0.0188 (19)	0.0154 (17)	0.0020 (17)	0.0124 (17)	0.0022 (15)
C9	0.017 (2)	0.027 (2)	0.023 (2)	0.0008 (17)	0.0082 (17)	0.0027 (17)
C10	0.019 (2)	0.0172 (18)	0.0203 (19)	0.0044 (15)	0.0052 (16)	0.0035 (15)
C11	0.024 (2)	0.024 (2)	0.0203 (19)	0.0038 (17)	0.0043 (17)	−0.0050 (16)
C12	0.025 (3)	0.052 (3)	0.025 (2)	0.010 (2)	0.0080 (19)	−0.0004 (19)
C13	0.036 (3)	0.061 (3)	0.034 (3)	0.010 (2)	0.014 (2)	−0.002 (2)
C14	0.027 (3)	0.053 (3)	0.040 (3)	0.012 (2)	0.006 (2)	−0.015 (2)
C15	0.034 (3)	0.030 (2)	0.033 (2)	0.0106 (19)	0.003 (2)	−0.0004 (18)
C16	0.026 (2)	0.026 (2)	0.025 (2)	0.0045 (17)	0.0071 (18)	−0.0051 (17)
C21	0.017 (2)	0.0171 (18)	0.0216 (19)	0.0012 (15)	0.0064 (16)	−0.0009 (15)
C22	0.032 (3)	0.026 (2)	0.024 (2)	−0.0007 (18)	0.0108 (19)	−0.0002 (17)
C23	0.050 (3)	0.028 (2)	0.035 (2)	−0.001 (2)	0.016 (2)	0.0100 (19)
C24	0.037 (3)	0.020 (2)	0.047 (3)	−0.0034 (19)	0.009 (2)	0.005 (2)
C25	0.038 (3)	0.022 (2)	0.033 (2)	−0.0014 (19)	0.001 (2)	−0.0055 (18)
C26	0.025 (2)	0.021 (2)	0.023 (2)	−0.0004 (17)	0.0050 (17)	−0.0005 (16)
C31	0.026 (2)	0.0209 (19)	0.0186 (19)	0.0018 (16)	0.0045 (17)	−0.0077 (15)
C32	0.037 (3)	0.026 (2)	0.025 (2)	0.0080 (19)	0.007 (2)	−0.0036 (17)
C33	0.038 (3)	0.040 (3)	0.029 (2)	0.015 (2)	−0.004 (2)	−0.003 (2)
C36	0.026 (3)	0.039 (2)	0.023 (2)	0.0019 (19)	0.0069 (19)	−0.0045 (18)
C34	0.025 (3)	0.045 (3)	0.048 (3)	0.016 (2)	0.000 (2)	−0.012 (2)
C35	0.030 (3)	0.049 (3)	0.038 (3)	0.006 (2)	0.014 (2)	−0.008 (2)
C41	0.018 (2)	0.0209 (19)	0.0186 (18)	0.0027 (15)	0.0034 (16)	0.0025 (15)
C42	0.034 (3)	0.025 (2)	0.0185 (19)	−0.0037 (18)	0.0060 (18)	−0.0001 (16)
C43	0.034 (3)	0.027 (2)	0.028 (2)	−0.0066 (19)	0.002 (2)	−0.0017 (18)
C44	0.035 (3)	0.026 (2)	0.034 (2)	−0.0082 (19)	0.004 (2)	0.0047 (19)
C45	0.037 (3)	0.036 (2)	0.025 (2)	−0.005 (2)	0.008 (2)	0.0103 (19)
C46	0.031 (3)	0.030 (2)	0.020 (2)	−0.0035 (18)	0.0061 (18)	0.0016 (17)
K1	0.0332 (6)	0.0269 (5)	0.0341 (5)	−0.0003 (4)	0.0169 (4)	0.0039 (4)
O11	0.0283 (18)	0.0378 (17)	0.0431 (18)	−0.0030 (13)	0.0157 (15)	−0.0086 (14)
O12	0.0320 (18)	0.0297 (15)	0.0318 (15)	−0.0061 (13)	0.0125 (13)	−0.0034 (12)
O13	0.0325 (18)	0.0319 (15)	0.0274 (15)	0.0016 (13)	0.0154 (13)	0.0042 (12)
O14	0.0325 (18)	0.0247 (14)	0.0274 (15)	0.0005 (12)	0.0077 (13)	0.0018 (12)
O15	0.0314 (18)	0.0273 (15)	0.0304 (15)	−0.0092 (13)	0.0062 (13)	−0.0004 (12)
O16	0.0368 (19)	0.0408 (17)	0.0342 (16)	−0.0065 (14)	0.0175 (14)	0.0000 (14)
O17	0.044 (2)	0.0415 (19)	0.067 (2)	−0.0037 (16)	0.0028 (18)	−0.0074 (17)
C101	0.049 (3)	0.064 (3)	0.044 (3)	−0.010 (3)	0.030 (3)	−0.010 (2)
C102	0.034 (3)	0.054 (3)	0.057 (3)	−0.008 (2)	0.024 (3)	−0.024 (2)
C103	0.039 (3)	0.032 (2)	0.054 (3)	0.006 (2)	0.012 (2)	−0.016 (2)
C104	0.049 (3)	0.031 (2)	0.047 (3)	−0.009 (2)	0.017 (2)	−0.011 (2)
C105	0.033 (3)	0.028 (2)	0.034 (2)	−0.0071 (19)	0.008 (2)	0.0075 (18)
C106	0.033 (3)	0.040 (3)	0.038 (3)	0.000 (2)	0.017 (2)	0.012 (2)
C107	0.033 (3)	0.043 (3)	0.032 (2)	0.002 (2)	0.018 (2)	0.000 (2)
C108	0.034 (3)	0.034 (2)	0.040 (3)	0.005 (2)	0.015 (2)	−0.004 (2)
C109	0.045 (3)	0.020 (2)	0.030 (2)	0.0049 (19)	0.004 (2)	−0.0004 (17)
C110	0.048 (3)	0.020 (2)	0.028 (2)	−0.0033 (19)	0.000 (2)	−0.0028 (17)
C111	0.031 (3)	0.034 (2)	0.045 (3)	−0.010 (2)	0.004 (2)	0.016 (2)
C112	0.028 (3)	0.063 (3)	0.045 (3)	−0.003 (2)	0.019 (2)	0.021 (2)
K2	0.0305 (6)	0.0244 (5)	0.0319 (5)	−0.0027 (4)	0.0123 (4)	0.0009 (4)
O21	0.0381 (19)	0.0235 (15)	0.0412 (17)	−0.0034 (13)	0.0180 (15)	−0.0055 (12)
O22	0.0330 (18)	0.0296 (15)	0.0282 (15)	−0.0021 (13)	0.0127 (13)	0.0010 (12)
O23	0.0326 (18)	0.0290 (15)	0.0280 (15)	−0.0012 (13)	0.0049 (13)	0.0006 (12)
O24	0.0313 (19)	0.0290 (16)	0.0450 (18)	−0.0098 (13)	0.0077 (15)	−0.0006 (13)
O25	0.053 (2)	0.0419 (19)	0.050 (2)	−0.0049 (16)	0.0288 (17)	0.0077 (16)
O26	0.048 (2)	0.0375 (18)	0.052 (2)	0.0026 (15)	0.0305 (17)	−0.0051 (15)
O27	0.041 (2)	0.0293 (16)	0.0479 (19)	−0.0010 (14)	0.0102 (16)	−0.0048 (14)
C201	0.084 (5)	0.035 (3)	0.090 (4)	0.009 (3)	0.058 (4)	−0.005 (3)
C202	0.083 (4)	0.029 (2)	0.061 (3)	−0.003 (3)	0.043 (3)	−0.012 (2)
C203	0.035 (3)	0.028 (2)	0.037 (2)	−0.0095 (19)	0.009 (2)	0.0060 (19)
C204	0.035 (3)	0.037 (2)	0.040 (3)	0.000 (2)	0.018 (2)	0.011 (2)
C205	0.030 (3)	0.040 (2)	0.027 (2)	−0.003 (2)	0.011 (2)	−0.0056 (19)
C206	0.036 (3)	0.036 (2)	0.030 (2)	0.005 (2)	0.007 (2)	−0.0080 (19)
C207	0.047 (3)	0.021 (2)	0.030 (2)	0.003 (2)	0.002 (2)	−0.0026 (18)
C208	0.050 (3)	0.022 (2)	0.033 (2)	−0.008 (2)	−0.008 (2)	0.0037 (18)
C209	0.032 (3)	0.036 (3)	0.071 (4)	−0.007 (2)	0.009 (3)	0.018 (2)
C210	0.033 (3)	0.056 (3)	0.066 (3)	−0.002 (2)	0.022 (3)	0.033 (3)
C211	0.061 (4)	0.067 (4)	0.054 (3)	0.001 (3)	0.040 (3)	−0.001 (3)
C212	0.075 (4)	0.062 (4)	0.070 (4)	−0.005 (3)	0.051 (3)	−0.010 (3)
K3	0.0287 (8)	0.0310 (7)	0.0322 (7)	0.0012 (6)	0.0028 (6)	−0.0017 (5)
O31	0.041 (2)	0.0426 (19)	0.0468 (19)	0.0065 (16)	−0.0051 (16)	0.0020 (15)
O32	0.042 (2)	0.044 (2)	0.070 (2)	−0.0007 (16)	0.0058 (19)	−0.0012 (17)
O33	0.047 (2)	0.0389 (18)	0.050 (2)	0.0076 (16)	0.0196 (17)	0.0035 (15)
O34	0.051 (2)	0.057 (2)	0.0350 (18)	0.0165 (17)	0.0047 (16)	0.0000 (15)
C301	0.064 (4)	0.061 (4)	0.069 (4)	0.002 (3)	−0.031 (3)	0.001 (3)
C302	0.033 (3)	0.056 (3)	0.100 (5)	−0.003 (3)	−0.008 (3)	0.003 (3)
C303	0.054 (4)	0.051 (3)	0.087 (4)	−0.019 (3)	0.012 (3)	0.008 (3)
C304	0.058 (4)	0.036 (3)	0.064 (3)	−0.008 (3)	0.009 (3)	0.003 (2)
C305	0.054 (3)	0.041 (3)	0.048 (3)	0.018 (2)	0.028 (3)	0.018 (2)
C306	0.049 (4)	0.059 (3)	0.038 (3)	0.014 (3)	0.004 (3)	0.013 (2)
K4	0.0361 (9)	0.0343 (7)	0.0330 (7)	−0.0018 (6)	0.0027 (6)	−0.0062 (6)
O41	0.047 (2)	0.0379 (17)	0.0318 (16)	−0.0065 (15)	0.0050 (15)	−0.0020 (14)
O42	0.038 (2)	0.0343 (16)	0.0313 (16)	−0.0111 (14)	0.0093 (14)	−0.0026 (13)
O43	0.037 (2)	0.0360 (17)	0.0396 (17)	−0.0002 (14)	0.0055 (15)	−0.0016 (14)
O44	0.048 (2)	0.055 (2)	0.044 (2)	−0.0078 (17)	0.0098 (17)	−0.0093 (16)
C401	0.040 (3)	0.050 (3)	0.031 (2)	−0.007 (2)	0.006 (2)	−0.008 (2)
C402	0.040 (3)	0.043 (3)	0.038 (3)	−0.011 (2)	0.013 (2)	−0.010 (2)
C403	0.054 (3)	0.029 (2)	0.038 (2)	−0.008 (2)	0.024 (2)	−0.007 (2)
C404	0.046 (3)	0.029 (2)	0.046 (3)	0.001 (2)	0.017 (2)	0.003 (2)
C405	0.042 (3)	0.047 (3)	0.055 (3)	0.005 (2)	0.001 (3)	0.007 (2)
C406	0.046 (3)	0.046 (3)	0.039 (3)	−0.004 (2)	−0.003 (2)	0.005 (2)
O1W	0.053 (2)	0.046 (2)	0.0377 (19)	0.0091 (16)	0.0172 (17)	0.0127 (15)
O2W	0.032 (2)	0.052 (2)	0.086 (3)	0.0006 (17)	0.001 (2)	0.0068 (19)
O3W	0.051 (3)	0.111 (3)	0.056 (2)	−0.027 (2)	0.025 (2)	−0.051 (2)
O4W	0.056 (3)	0.062 (3)	0.076 (3)	0.004 (2)	−0.005 (2)	−0.006 (2)
O5W	0.055 (3)	0.081 (3)	0.079 (3)	−0.015 (2)	0.008 (3)	0.013 (2)
O6W	0.042 (3)	0.084 (3)	0.096 (3)	−0.013 (2)	−0.005 (2)	0.030 (2)
O7W	0.084 (4)	0.084 (4)	0.146 (5)	−0.004 (3)	−0.003 (3)	0.009 (3)
O8W	0.240 (10)	0.154 (7)	0.295 (12)	0.019 (7)	0.104 (10)	0.040 (7)

Geometric parameters (Å, º)

Rh1—O7	2.034 (2)	O14—C108	1.422 (5)
Rh1—O5	2.038 (2)	O14—C109	1.430 (4)
Rh1—O1	2.054 (2)	O15—C111	1.427 (5)
Rh1—O3	2.059 (2)	O15—C110	1.435 (4)
Rh1—N1	2.207 (3)	O16—C101	1.419 (5)
Rh1—Rh2	2.4109 (4)	O16—C112	1.430 (5)
Rh2—O4	2.031 (2)	C101—C102	1.489 (6)
Rh2—O2	2.032 (2)	C103—C104	1.495 (6)
Rh2—O6	2.048 (2)	C105—C106	1.489 (5)
Rh2—O8	2.058 (2)	C107—C108	1.493 (5)
Rh2—N6^i	2.200 (3)	C109—C110	1.479 (6)
Fe1—C7	1.944 (4)	C111—C112	1.483 (6)
Fe1—C10	1.944 (3)	K2—O27	2.620 (3)
Fe1—C8	1.944 (4)	K2—O22	2.782 (3)
Fe1—C9	1.946 (4)	K2—O25	2.791 (3)
Fe1—C6	1.947 (4)	K2—O26	2.803 (3)
Fe1—C5	1.950 (3)	K2—O24	2.815 (3)
O1—C1	1.264 (4)	K2—O21	2.831 (3)
O2—C1	1.268 (4)	K2—O23	2.840 (3)
O3—C2	1.265 (4)	O21—C203	1.431 (5)
O4—C2	1.273 (4)	O21—C202	1.432 (5)
O5—C3	1.270 (4)	O22—C205	1.424 (4)
O6—C3	1.273 (4)	O22—C204	1.428 (4)
O7—C4	1.275 (4)	O23—C206	1.425 (5)
O8—C4	1.267 (4)	O23—C207	1.428 (4)
N1—C5	1.150 (4)	O24—C209	1.423 (5)
N2—C6	1.152 (5)	O24—C208	1.428 (5)
N3—C7	1.161 (4)	O25—C211	1.420 (5)
N4—C8	1.158 (5)	O25—C210	1.427 (5)
N5—C9	1.156 (5)	O26—C212	1.413 (5)
N6—C10	1.148 (4)	O26—C201	1.417 (5)
N6—Rh2^ii	2.200 (3)	C201—C202	1.454 (6)
C1—C11	1.504 (5)	C203—C204	1.479 (5)
C2—C21	1.499 (5)	C205—C206	1.488 (5)
C3—C31	1.494 (5)	C207—C208	1.490 (6)
C4—C41	1.493 (5)	C209—C210	1.485 (6)
C11—C16	1.381 (5)	C211—C212	1.486 (7)
C11—C12	1.404 (5)	K3—O31	2.715 (3)
C12—C13	1.390 (6)	K3—O31^iii	2.715 (3)
C13—C14	1.382 (6)	K3—O34^iii	2.804 (3)
C14—C15	1.385 (6)	K3—O34	2.804 (3)
C15—C16	1.383 (5)	K3—O32	2.832 (3)
C21—C26	1.385 (5)	K3—O32^iii	2.832 (3)
C21—C22	1.392 (5)	K3—O33	2.925 (3)
C22—C23	1.381 (5)	K3—O33^iii	2.925 (3)
C23—C24	1.384 (6)	O31—C301	1.412 (6)
C24—C25	1.388 (5)	O31—C306^iii	1.440 (5)
C25—C26	1.388 (5)	O32—C303	1.437 (6)
C31—C32	1.386 (5)	O32—C302	1.445 (6)
C31—C36	1.396 (5)	O33—C305	1.410 (5)
C32—C33	1.377 (6)	O33—C304	1.436 (5)
C33—C34	1.374 (6)	C301—C302	1.520 (7)
C36—C35	1.380 (6)	C303—C304	1.505 (7)
C34—C35	1.384 (6)	C305—C306	1.494 (6)
C41—C42	1.394 (5)	C306—O31^iii	1.440 (5)
C41—C46	1.397 (5)	K4—O41^iv	2.794 (3)
C42—C43	1.388 (5)	K4—O41	2.794 (3)
C43—C44	1.382 (5)	K4—O44^iv	2.810 (3)
C44—C45	1.393 (5)	K4—O44	2.810 (3)
C45—C46	1.381 (5)	K4—O43	2.827 (3)
K1—O16	2.734 (3)	K4—O43^iv	2.827 (3)
K1—O15	2.783 (3)	K4—O42^iv	2.828 (3)
K1—O13	2.788 (3)	K4—O42	2.828 (3)
K1—O17	2.827 (3)	O41—C406^iv	1.430 (5)
K1—O14	2.848 (3)	O41—C401	1.431 (5)
K1—O12	2.849 (3)	O42—C403	1.425 (5)
K1—O11	2.879 (3)	O42—C402	1.438 (5)
O11—C102	1.424 (5)	O43—C405	1.425 (5)
O11—C103	1.431 (5)	O43—C404	1.441 (5)
O12—C105	1.424 (5)	C401—C402	1.502 (6)
O12—C104	1.428 (5)	C403—C404	1.490 (6)
O13—C107	1.426 (4)	C405—C406	1.497 (6)
O13—C106	1.429 (4)	C406—O41^iv	1.430 (5)
O7—Rh1—O5	87.05 (10)	O12—C104—C103	109.5 (3)
O7—Rh1—O1	91.85 (10)	O12—C105—C106	109.3 (3)
O5—Rh1—O1	175.56 (9)	O13—C106—C105	108.5 (3)
O7—Rh1—O3	175.69 (9)	O13—C107—C108	108.4 (3)
O5—Rh1—O3	91.78 (10)	O14—C108—C107	109.4 (3)
O1—Rh1—O3	89.00 (10)	O14—C109—C110	108.8 (3)
O7—Rh1—N1	87.84 (10)	O15—C110—C109	108.1 (3)
O5—Rh1—N1	90.23 (10)	O15—C111—C112	107.4 (3)
O1—Rh1—N1	94.03 (10)	O16—C112—C111	109.5 (3)
O3—Rh1—N1	96.32 (9)	O27—K2—O22	108.29 (9)
O7—Rh1—Rh2	89.22 (6)	O27—K2—O25	96.65 (10)
O5—Rh1—Rh2	87.50 (6)	O22—K2—O25	155.00 (9)
O1—Rh1—Rh2	88.18 (6)	O27—K2—O26	109.46 (10)
O3—Rh1—Rh2	86.58 (6)	O22—K2—O26	111.75 (9)
N1—Rh1—Rh2	176.38 (8)	O25—K2—O26	59.32 (9)
O4—Rh2—O2	86.45 (10)	O27—K2—O24	93.35 (9)
O4—Rh2—O6	91.10 (10)	O22—K2—O24	114.80 (9)
O2—Rh2—O6	175.17 (9)	O25—K2—O24	60.50 (9)
O4—Rh2—O8	175.77 (9)	O26—K2—O24	117.21 (9)
O2—Rh2—O8	93.46 (10)	O27—K2—O21	96.47 (9)
O6—Rh2—O8	88.67 (10)	O22—K2—O21	60.35 (8)
O4—Rh2—N6^i	88.88 (10)	O25—K2—O21	119.64 (9)
O2—Rh2—N6^i	91.12 (10)	O26—K2—O21	60.73 (8)
O6—Rh2—N6^i	92.99 (10)	O24—K2—O21	170.05 (9)
O8—Rh2—N6^i	95.35 (10)	O27—K2—O23	92.95 (9)
O4—Rh2—Rh1	89.25 (6)	O22—K2—O23	59.52 (8)
O2—Rh2—Rh1	87.44 (6)	O25—K2—O23	118.73 (9)
O6—Rh2—Rh1	88.37 (6)	O26—K2—O23	157.58 (9)
O8—Rh2—Rh1	86.53 (6)	O24—K2—O23	58.61 (8)
N6^i—Rh2—Rh1	177.71 (8)	O21—K2—O23	119.04 (8)
C7—Fe1—C10	89.76 (14)	C203—O21—C202	110.4 (3)
C7—Fe1—C8	90.06 (15)	C203—O21—K2	114.9 (2)
C10—Fe1—C8	90.34 (14)	C202—O21—K2	114.8 (2)
C7—Fe1—C9	179.26 (15)	C205—O22—C204	110.9 (3)
C10—Fe1—C9	90.90 (14)	C205—O22—K2	118.0 (2)
C8—Fe1—C9	89.61 (15)	C204—O22—K2	113.7 (2)
C7—Fe1—C6	90.89 (15)	C206—O23—C207	112.6 (3)
C10—Fe1—C6	88.85 (14)	C206—O23—K2	115.1 (2)
C8—Fe1—C6	178.74 (15)	C207—O23—K2	118.2 (2)
C9—Fe1—C6	89.44 (15)	C209—O24—C208	112.7 (3)
C7—Fe1—C5	89.54 (13)	C209—O24—K2	107.2 (2)
C10—Fe1—C5	178.66 (15)	C208—O24—K2	112.2 (2)
C8—Fe1—C5	90.81 (14)	C211—O25—C210	114.2 (4)
C9—Fe1—C5	89.81 (14)	C211—O25—K2	116.3 (3)
C6—Fe1—C5	90.02 (14)	C210—O25—K2	115.6 (3)
C1—O1—Rh1	118.1 (2)	C212—O26—C201	113.4 (4)
C1—O2—Rh2	119.9 (2)	C212—O26—K2	117.4 (3)
C2—O3—Rh1	119.8 (2)	C201—O26—K2	110.0 (2)
C2—O4—Rh2	118.2 (2)	O26—C201—C202	110.6 (4)
C3—O5—Rh1	119.8 (2)	O21—C202—C201	111.6 (4)
C3—O6—Rh2	118.2 (2)	O21—C203—C204	109.4 (3)
C4—O7—Rh1	118.5 (2)	O22—C204—C203	109.2 (3)
C4—O8—Rh2	120.3 (2)	O22—C205—C206	109.7 (3)
C5—N1—Rh1	168.1 (3)	O23—C206—C205	109.5 (3)
C10—N6—Rh2^ii	170.7 (3)	O23—C207—C208	108.9 (3)
O1—C1—O2	125.9 (3)	O24—C208—C207	107.0 (3)
O1—C1—C11	117.4 (3)	O24—C209—C210	106.8 (4)
O2—C1—C11	116.7 (3)	O25—C210—C209	109.0 (4)
O3—C2—O4	126.1 (3)	O25—C211—C212	108.7 (4)
O3—C2—C21	117.3 (3)	O26—C212—C211	109.8 (4)
O4—C2—C21	116.6 (3)	O31—K3—O31^iii	180.000 (1)
O5—C3—O6	125.9 (3)	O31—K3—O34^iii	109.37 (9)
O5—C3—C31	117.2 (3)	O31^iii—K3—O34^iii	70.63 (9)
O6—C3—C31	116.9 (3)	O31—K3—O34	70.63 (9)
O8—C4—O7	125.4 (3)	O31^iii—K3—O34	109.37 (9)
O8—C4—C41	117.6 (3)	O34^iii—K3—O34	180.000 (1)
O7—C4—C41	117.0 (3)	O31—K3—O32	61.88 (9)
N1—C5—Fe1	179.8 (4)	O31^iii—K3—O32	118.12 (9)
N2—C6—Fe1	177.5 (3)	O34^iii—K3—O32	87.48 (10)
N3—C7—Fe1	179.4 (3)	O34—K3—O32	92.52 (10)
N4—C8—Fe1	178.3 (3)	O31—K3—O32^iii	118.12 (9)
N5—C9—Fe1	179.3 (3)	O31^iii—K3—O32^iii	61.88 (9)
N6—C10—Fe1	178.7 (3)	O34^iii—K3—O32^iii	92.52 (10)
C16—C11—C12	120.1 (4)	O34—K3—O32^iii	87.48 (10)
C16—C11—C1	121.4 (3)	O32—K3—O32^iii	180.00 (10)
C12—C11—C1	118.4 (3)	O31—K3—O33	121.07 (10)
C13—C12—C11	119.5 (4)	O31^iii—K3—O33	58.93 (10)
C14—C13—C12	120.0 (4)	O34^iii—K3—O33	80.08 (9)
C13—C14—C15	120.1 (4)	O34—K3—O33	99.92 (9)
C16—C15—C14	120.6 (4)	O32—K3—O33	60.64 (9)
C11—C16—C15	119.7 (4)	O32^iii—K3—O33	119.36 (9)
C26—C21—C22	119.5 (3)	O31—K3—O33^iii	58.93 (10)
C26—C21—C2	120.1 (3)	O31^iii—K3—O33^iii	121.07 (10)
C22—C21—C2	120.4 (3)	O34^iii—K3—O33^iii	99.92 (9)
C23—C22—C21	120.4 (4)	O34—K3—O33^iii	80.08 (9)
C22—C23—C24	120.2 (4)	O32—K3—O33^iii	119.36 (9)
C23—C24—C25	119.5 (4)	O32^iii—K3—O33^iii	60.64 (9)
C26—C25—C24	120.4 (4)	O33—K3—O33^iii	180.000 (1)
C21—C26—C25	120.0 (3)	C301—O31—C306^iii	114.3 (4)
C32—C31—C36	119.2 (4)	C301—O31—K3	117.1 (3)
C32—C31—C3	120.9 (3)	C306^iii—O31—K3	121.4 (3)
C36—C31—C3	119.7 (3)	C303—O32—C302	109.4 (4)
C33—C32—C31	119.8 (4)	C303—O32—K3	113.1 (3)
C34—C33—C32	121.2 (4)	C302—O32—K3	107.5 (3)
C35—C36—C31	120.2 (4)	C305—O33—C304	111.0 (4)
C33—C34—C35	119.3 (4)	C305—O33—K3	110.6 (2)
C36—C35—C34	120.3 (4)	C304—O33—K3	109.4 (3)
C42—C41—C46	119.5 (3)	O31—C301—C302	109.2 (4)
C42—C41—C4	120.0 (3)	O32—C302—C301	107.1 (5)
C46—C41—C4	120.6 (3)	O32—C303—C304	107.8 (4)
C43—C42—C41	119.7 (3)	O33—C304—C303	108.5 (4)
C44—C43—C42	120.9 (4)	O33—C305—C306	108.2 (4)
C43—C44—C45	119.2 (4)	O31^iii—C306—C305	108.3 (4)
C46—C45—C44	120.6 (4)	O41^iv—K4—O41	180.000 (1)
C45—C46—C41	120.1 (4)	O41^iv—K4—O44^iv	86.54 (9)
O16—K1—O15	61.47 (8)	O41—K4—O44^iv	93.46 (9)
O16—K1—O13	162.65 (9)	O41^iv—K4—O44	93.46 (9)
O15—K1—O13	115.25 (8)	O41—K4—O44	86.54 (9)
O16—K1—O17	102.96 (10)	O44^iv—K4—O44	180.00 (11)
O15—K1—O17	134.03 (9)	O41^iv—K4—O43	60.04 (8)
O13—K1—O17	91.05 (9)	O41—K4—O43	119.96 (8)
O16—K1—O14	120.28 (8)	O44^iv—K4—O43	64.32 (9)
O15—K1—O14	58.85 (8)	O44—K4—O43	115.68 (9)
O13—K1—O14	58.66 (8)	O41^iv—K4—O43^iv	119.96 (8)
O17—K1—O14	119.21 (9)	O41—K4—O43^iv	60.04 (8)
O16—K1—O12	119.41 (8)	O44^iv—K4—O43^iv	115.68 (9)
O15—K1—O12	166.18 (9)	O44—K4—O43^iv	64.32 (9)
O13—K1—O12	59.27 (8)	O43—K4—O43^iv	180.00 (11)
O17—K1—O12	59.79 (9)	O41^iv—K4—O42^iv	60.95 (8)
O14—K1—O12	117.89 (8)	O41—K4—O42^iv	119.05 (8)
O16—K1—O11	60.61 (8)	O44^iv—K4—O42^iv	100.04 (8)
O15—K1—O11	117.46 (8)	O44—K4—O42^iv	79.96 (8)
O13—K1—O11	112.77 (8)	O43—K4—O42^iv	119.43 (8)
O17—K1—O11	80.68 (9)	O43^iv—K4—O42^iv	60.57 (8)
O14—K1—O11	156.71 (9)	O41^iv—K4—O42	119.05 (8)
O12—K1—O11	59.41 (8)	O41—K4—O42	60.95 (8)
C102—O11—C103	111.5 (3)	O44^iv—K4—O42	79.96 (8)
C102—O11—K1	109.2 (2)	O44—K4—O42	100.04 (8)
C103—O11—K1	112.4 (2)	O43—K4—O42	60.57 (8)
C105—O12—C104	110.7 (3)	O43^iv—K4—O42	119.43 (8)
C105—O12—K1	117.2 (2)	O42^iv—K4—O42	180.00 (6)
C104—O12—K1	116.9 (2)	C406^iv—O41—C401	112.1 (3)
C107—O13—C106	111.5 (3)	C406^iv—O41—K4	115.4 (2)
C107—O13—K1	119.5 (2)	C401—O41—K4	114.2 (2)
C106—O13—K1	113.5 (2)	C403—O42—C402	111.7 (3)
C108—O14—C109	112.9 (3)	C403—O42—K4	113.6 (2)
C108—O14—K1	115.9 (2)	C402—O42—K4	111.6 (2)
C109—O14—K1	117.6 (2)	C405—O43—C404	112.7 (3)
C111—O15—C110	112.0 (3)	C405—O43—K4	114.6 (2)
C111—O15—K1	108.9 (2)	C404—O43—K4	113.2 (2)
C110—O15—K1	114.1 (2)	O41—C401—C402	108.2 (3)
C101—O16—C112	113.1 (3)	O42—C402—C401	107.6 (4)
C101—O16—K1	117.9 (2)	O42—C403—C404	108.8 (3)
C112—O16—K1	116.0 (2)	O43—C404—C403	108.8 (4)
O16—C101—C102	109.2 (4)	O43—C405—C406	108.6 (4)
O11—C102—C101	109.1 (4)	O41^iv—C406—C405	108.4 (4)
O11—C103—C104	109.1 (4)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2; (iii) −x, −y+2, −z+1; (iv) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O17—H1W···O6W^v	0.85 (1)	2.10 (1)	2.728 (5)	130 (1)
O17—H2W···O12	0.86 (1)	2.36 (2)	2.829 (4)	115 (1)
O27—H3W···N3^vi	0.86 (1)	2.04 (1)	2.885 (4)	168 (1)
O27—H4W···O17^vii	0.85 (1)	1.98 (1)	2.831 (4)	172 (4)
O34—H5W···O1W^iii	0.84 (1)	2.34 (1)	3.039 (4)	140 (1)
O34—H6W···N5^iii	0.85 (1)	2.21 (1)	3.040 (5)	166 (1)
O44—H7W···N5	0.85 (1)	2.16 (2)	2.909 (5)	147 (2)
O44—H8W···O43^iv	0.85 (1)	2.55 (1)	3.000 (5)	114 (1)
O1W—H9W···N2	0.85 (1)	2.21 (1)	3.051 (4)	167 (4)
O1W—H10W···O4^ii	0.85 (1)	2.28 (1)	3.104 (4)	162 (4)
O2W—H11W···N2	0.85 (1)	2.01 (1)	2.842 (5)	168 (5)
O2W—H12W···O4W	0.85 (1)	2.16 (2)	2.930 (5)	151 (4)
O3W—H13W···O7	0.85 (1)	2.25 (2)	3.014 (4)	150 (4)
O3W—H14W···N4	0.85 (1)	2.18 (1)	3.023 (4)	171 (5)
O4W—H15W···O1W	0.85 (1)	2.15 (2)	2.957 (5)	158 (6)
O4W—H16W···O32	0.85 (1)	2.29 (3)	3.032 (5)	146 (5)
O5W—H17W···O3W	0.85 (1)	1.89 (2)	2.717 (5)	164 (5)
O5W—H18W···O7W	0.85 (1)	2.46 (3)	3.164 (7)	140 (4)
O6W—H19W···O21	0.85 (1)	2.16 (3)	2.928 (5)	151 (5)
O6W—H20W···O2W	0.85 (1)	1.99 (3)	2.772 (5)	153 (6)
O7W—H21W···O5W	0.85 (1)	2.34 (2)	3.164 (7)	163 (7)
O7W—H22W···N4	0.86 (1)	2.17 (1)	3.019 (6)	173 (7)
O8W—H23W···O6W^iii	0.85 (1)	2.55 (12)	3.025 (10)	116 (10)

Symmetry codes: (ii) x, −y+3/2, z−1/2; (iii) −x, −y+2, −z+1; (iv) −x+1, −y+2, −z+1; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1; (vii) x−1, −y+3/2, z−1/2.