A zigzag chain structure in catena-poly[[[tetra-μ-acetamidato-κ⁴N:O;κ⁴O:N-dirhodium(II,III)]-μ-chloro] methanol solvate]

In {[Rh₂(C₂H₄NO)₄Cl]·CH₃OH}_n, the cationic dirhodium complex and bridging chloro ligands form a one-dimensional zigzag chain, [Rh₂(acam)₄(μ-Cl)] (Hacam is acetamide). There is a large difference between the two Rh—Cl distances [2.6076 (14) and 2.5027 (14) Å]. Neighboring chains are connected by two N—H...O hydrogen bonds per link between the amidate ligands.

S1. Comment

A halide-bridged one-dimensional chain is commonly observed in structures with metal–metal-bonded paddlewheel complexes such as K[Mo₂(O₂CH)₄Cl] (Robbins & Martin, 1984), [Pt₂(S₂CR)₄I] (Bellitto et al., 1983; Kitagawa et al., 2001; Mitsumi et al., 2002) and [Ru₂(O₂CR)₄X] (X = Cl and Br; Angaridis, 2005). The chain in K[Mo₂(O₂CH)₄Cl] is a zigzag one, that in [Pt₂(S₂CR)₄I] is linear and [Ru₂(O₂CR)₄X] contains both types. We have reported assemblies of acetamidate-bridged dirhodium paddlewheel complexes with halide linkers, viz. one-dimensional chain structures in [Rh₂(acam)₄(µ-X)].nH₂O (Hacam is acetamide; X = Cl, Br and I; n = 0, 2, 3 and 7; Yang et al., 2000, 2001), a two-dimensional honeycomb structure in [{Rh₂(acam)₄}₃(µ₃-Cl)₂]·4H₂O (Takazaki et al., 2003), and a three-dimensional diamondoid structure in [{Rh₂(acam)₄}₂(µ₄-I)]·6H₂O (Fuma et al., 2004). In the zigzag chain structure of [Rh₂(acam)₄(µ-X)].nH₂O, the Rh—Cl—Rh angle varies with the hydrogen bonding involving the water molecules. We have attempted to synthesize the chain structure with solvent molecules other than water. In this paper, we report the zigzag chain structure of [Rh₂(acam)₄(µ-Cl)]·CH₃OH, (I).

The structure of (I) is shown in Fig. 1. There are one independent [Rh₂(acam)₄Cl] unit and one methanol molecule in the asymmetric unit. The bond distances in the [Rh₂(acam)₄] skeleton are similar to those observed previously for the cationic [Rh₂(acam)₄] unit (Yang et al., 2000, 2001, 2006; Ebihara & Fuma, 2006; Baranovskii et al., 1986). The [Rh₂(acam)₄Cl] unit forms an infinite zigzag chain structure (Fig. 2) as in [Rh₂(acam)₄(µ-Cl)] and [Rh₂(acam)₄(µ-Cl)]·7H₂O (Yang et al., 2000, 2001).

In the reported zigzag chain structures of [M₂L₄X] (M = Ru and Rh, L = O₂CR, HN(O)CR, and X = Cl, Br and I; Bennett et al., 1969; Togano et al., 1980; Kimura et al., 1982; Chakravarty & Cotton, 1985; Chakravarty et al., 1985; Das & Chakravarty, 1991; Abe et al., 1992; Barral et al., 1998, 1999, 2000, 2004; Cukiernik et al., 1998; Yang et al., 2000, 2001), the dimetal unit usually lies on an inversion center or on a twofold axis. For example, in the chain structure of [Rh₂(acam)₄(µ-Cl)] (Yang et al., 2001), which crystallizes in C2/c, the dirhodium unit lies on an inversion center and the Cl atom lies on a twofold axis. In the structure of [Ru₂(O₂CC₆H₄OMe)₄Cl] (Das & Chakravarty, 1991), there are three independent diruthenium units of which two lie on inversion centers and one occupies a general position. In the structure of (I), the chain is propagated along the c axis with each unit of the complex connected to adjacent units generated by the c-glide plane at y = 1/4. Compound (I) is the first example of a zigzag chain constructed from one independent paddlewheel complex that does not have any symmetry.

The Rh—Cl—Rh angles in [Rh₂(acam)₄(µ-Cl)] and [Rh₂(acam)₄(µ-Cl)]·7H₂O are 115.48 (10) and 153.50 (6)°, respectively. Since the corresponding angle in (I) is 114.59 (5)°, the chain structure in (I) more closely resembles that in [Rh₂(acam)₄(µ-Cl)]. The hydrogen bonds from NH of the acam ligands to O atoms of the next complexes along the chain [N1···O4ⁱ and N3···O2ⁱⁱ; symmetry codes: (i) x, −y + 1/2, z − 1/2; (ii) x, −y + 1/2, z + 1/2; Table 2] also support the chain structure, as was observed in [Rh₂(acam)₄(µ-Cl)] (Yang et al., 2001). The CH₃OH molecule lies beside the chain, accepting a hydrogen bond from an N atom of an acam ligand (N2) and donating a hydrogen bond to an O atom of a neighboring complex (O2ⁱⁱ).

The Rh—Rh—Cl angles in (I) (Table 1) are slightly more bent than that in [Rh₂(acam)₄(µ-Cl)] [174.52 (4)°]. Rh1—Cl1 and Rh2—Cl1ⁱ (Table 1) are both different from the corresponding value in [Rh₂(acam)₄(µ-Cl)] [2.581 (1) Å]. The difference between these Rh—Cl distances is very large (ca 0.1 Å). In the previously reported chain structures, the largest differences (ca 0.04 Å) between M—Cl bonds were observed in [Ru₂{HN(O)CC₆H₄R}₄(µ-Cl)] [R = H (Chakravarty & Cotton, 1985) and R = Cl (Chakravarty et al., 1985). The long–short pattern of the M—Cl bonds in the Cl—MM—Cl—MM—Cl unit is long–long–short–short for [Ru₂(HN(O)CC₆H₄R)₄(µ-Cl)] since two independent diruthenium units lie on inversion centers, but long–short–long–short for (I).

The chains are mutually parallel and are connected to each other by a pair of hydrogen bonds [N4···O3ⁱⁱⁱ and N4ⁱⁱⁱ···O3; symmetry code: (iii) −x + 1, −y + 1, −z + 1]. These interchain hydrogen bonds were not observed in other chain structures with amidate-bridged paddlewheel complexes (Chakravarty & Cotton, 1985; Chakravarty et al., 1985; Yang et al., 2000, 2001).

S2. Experimental

[Rh₂(acam)₄(H₂O)₂]ClO₄ was prepared by the method described by Baranovskii et al. (1986). Into a methanol solution of [Rh₂(acam)₄(H₂O)₂]ClO₄ (3.1 mmol l⁻¹), a methanol solution of CoCl₂·6H₂O (0.21 mol l⁻¹) was diffused slowly. After several days, brown crystals of (I) were obtained.

S3. Refinement

The positional parameters of the H atom attached to O were refined with U_iso(H) values of 1.5U_eq(O). All other H atoms were placed in idealized positions and treated as riding atoms, with C—H distances of 0.98 Å and U_iso(H) values of 1.5U_eq(C), and with N—H distances of 0.88 Å and U_iso(H) of 1.2U_eq(N).

Computing details

Data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 and TEXSAN.

Figures

	Fig. 1. The molecular structure of (I), showing the atom-labeling scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. [Symmetry code: (i) x, −y + 1/2, −1/2 + z.]
	Fig. 2. Crystal structure of (I). Hydrogen bonds were drawn as thin lines. [symmetry codes: (i) x, −y + 1/2, z − 1/2; (ii) x, −y + 1/2, z + 1/2; (iii) −x + 1, −y + 1, −z + 1.]

poly[µ-chloro-tetra-µ-acetamidato-κ4 N:O;κ4O:N-dirhodium(II,III) methanol solvate]

Crystal data

[Rh2Cl(C2H4NO)4]·CH4O	F(000) = 996
Mr = 505.56	Dx = 2.189 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 4776 reflections
a = 8.601 (4) Å	θ = 3.0–27.5°
b = 14.254 (7) Å	µ = 2.35 mm^−1
c = 12.664 (7) Å	T = 173 K
β = 98.854 (5)°	Prism, brown
V = 1534.1 (13) Å^3	0.30 × 0.10 × 0.10 mm
Z = 4

Data collection

Rigaku/MSC Mercury CCD diffractometer	3496 independent reflections
Radiation source: rotating-anode X-ray tube	3246 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.0°
ω scans	h = −10→11
Absorption correction: integration (NUMABS; Higashi, 1999)	k = −13→18
Tmin = 0.624, Tmax = 0.755	l = −14→16
12335 measured reflections

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.071	H atoms treated by a mixture of independent and constrained refinement
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0256P)^2 + 3.6476P] where P = (Fo^2 + 2Fc^2)/3
3496 reflections	(Δ/σ)max = 0.001
198 parameters	Δρmax = 0.95 e Å^−3
0 restraints	Δρmin = −0.80 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	0.55116 (3)	0.223511 (18)	0.65224 (2)	0.01191 (8)
Rh2	0.56671 (3)	0.312306 (18)	0.49089 (2)	0.01183 (8)
Cl1	0.56444 (11)	0.10902 (6)	0.81398 (7)	0.01671 (18)
N1	0.4437 (4)	0.2088 (2)	0.4147 (3)	0.0163 (6)
H1	0.4170	0.2134	0.3450	0.020*
O1	0.4298 (3)	0.12200 (17)	0.5627 (2)	0.0167 (5)
N2	0.7552 (4)	0.1693 (2)	0.6306 (3)	0.0153 (6)
H2	0.7994	0.1290	0.6788	0.018*
O2	0.7716 (3)	0.24327 (18)	0.4741 (2)	0.0179 (5)
N3	0.6648 (4)	0.3294 (2)	0.7305 (3)	0.0164 (6)
H3	0.6817	0.3272	0.8007	0.020*
O3	0.6972 (3)	0.41216 (18)	0.5816 (2)	0.0180 (5)
N4	0.3756 (4)	0.3777 (2)	0.5188 (2)	0.0155 (6)
H4	0.3407	0.4247	0.4768	0.019*
O4	0.3415 (3)	0.28888 (18)	0.6625 (2)	0.0168 (5)
C1	0.3999 (4)	0.1342 (3)	0.4617 (3)	0.0154 (7)
C2	0.3105 (5)	0.0573 (3)	0.3979 (3)	0.0243 (9)
H5	0.3835	0.0189	0.3642	0.036*
H6	0.2315	0.0849	0.3427	0.036*
H7	0.2581	0.0180	0.4453	0.036*
C3	0.8296 (4)	0.1878 (2)	0.5514 (3)	0.0160 (7)
C4	0.9870 (5)	0.1445 (3)	0.5449 (4)	0.0253 (9)
H8	0.9855	0.1163	0.4741	0.038*
H9	1.0096	0.0959	0.5999	0.038*
H10	1.0687	0.1930	0.5564	0.038*
C5	0.7162 (4)	0.4023 (2)	0.6840 (3)	0.0156 (7)
C6	0.8015 (5)	0.4796 (3)	0.7496 (3)	0.0222 (8)
H11	0.8884	0.5022	0.7147	0.033*
H12	0.8433	0.4556	0.8209	0.033*
H13	0.7285	0.5313	0.7561	0.033*
C7	0.2973 (4)	0.3556 (3)	0.5961 (3)	0.0163 (7)
C8	0.1492 (5)	0.4072 (3)	0.6069 (3)	0.0232 (9)
H14	0.0858	0.3694	0.6490	0.035*
H15	0.0894	0.4187	0.5358	0.035*
H16	0.1756	0.4672	0.6430	0.035*
O5	0.9595 (4)	0.1373 (2)	0.8394 (3)	0.0309 (7)
H17	0.885 (7)	0.157 (4)	0.871 (5)	0.046*
C9	1.0613 (5)	0.2118 (3)	0.8249 (4)	0.0316 (10)
H18	0.9994	0.2662	0.7959	0.047*
H19	1.1319	0.1926	0.7751	0.047*
H20	1.1236	0.2284	0.8938	0.047*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.01449 (14)	0.01280 (14)	0.00845 (14)	−0.00139 (10)	0.00178 (10)	0.00018 (10)
Rh2	0.01393 (15)	0.01311 (14)	0.00857 (14)	0.00078 (10)	0.00210 (10)	0.00066 (10)
Cl1	0.0248 (5)	0.0152 (4)	0.0106 (4)	−0.0016 (3)	0.0041 (3)	−0.0010 (3)
N1	0.0201 (17)	0.0180 (15)	0.0107 (15)	0.0003 (12)	0.0014 (13)	−0.0028 (12)
O1	0.0199 (13)	0.0169 (12)	0.0128 (13)	−0.0010 (10)	0.0008 (11)	0.0004 (10)
N2	0.0184 (16)	0.0155 (14)	0.0113 (15)	0.0023 (12)	0.0004 (12)	0.0018 (11)
O2	0.0177 (13)	0.0215 (13)	0.0151 (14)	0.0037 (10)	0.0045 (11)	0.0030 (10)
N3	0.0215 (17)	0.0171 (15)	0.0102 (15)	−0.0040 (12)	0.0009 (13)	−0.0019 (11)
O3	0.0219 (14)	0.0173 (13)	0.0149 (14)	−0.0039 (10)	0.0032 (11)	−0.0007 (10)
N4	0.0193 (16)	0.0167 (15)	0.0101 (15)	0.0043 (12)	0.0008 (12)	0.0021 (11)
O4	0.0196 (14)	0.0198 (13)	0.0117 (13)	0.0007 (10)	0.0050 (11)	0.0005 (10)
C1	0.0150 (17)	0.0167 (17)	0.0144 (18)	0.0020 (13)	0.0018 (14)	−0.0037 (14)
C2	0.032 (2)	0.0196 (19)	0.019 (2)	−0.0041 (16)	−0.0030 (18)	−0.0034 (15)
C3	0.0171 (18)	0.0149 (17)	0.0153 (19)	−0.0007 (14)	0.0006 (15)	−0.0023 (14)
C4	0.023 (2)	0.029 (2)	0.025 (2)	0.0076 (17)	0.0060 (17)	0.0017 (17)
C5	0.0158 (18)	0.0158 (17)	0.0145 (19)	0.0027 (14)	0.0002 (15)	−0.0029 (13)
C6	0.026 (2)	0.0175 (18)	0.022 (2)	−0.0049 (15)	−0.0004 (17)	−0.0009 (15)
C7	0.0175 (18)	0.0181 (17)	0.0130 (18)	0.0011 (14)	0.0012 (14)	−0.0034 (14)
C8	0.022 (2)	0.030 (2)	0.019 (2)	0.0072 (16)	0.0051 (17)	−0.0011 (16)
O5	0.0249 (16)	0.0379 (18)	0.0305 (18)	0.0038 (14)	0.0060 (14)	0.0041 (14)
C9	0.028 (2)	0.033 (2)	0.032 (3)	−0.0028 (18)	0.001 (2)	−0.0047 (19)

Geometric parameters (Å, º)

Rh1—Rh2	2.4247 (11)	O4—C7	1.287 (5)
Rh1—Cl1	2.6076 (14)	C1—C2	1.500 (5)
Rh1—O1	2.026 (3)	C2—H5	0.9800
Rh1—O4	2.052 (3)	C2—H6	0.9800
Rh1—N2	1.975 (3)	C2—H7	0.9800
Rh1—N3	1.979 (3)	C3—C4	1.501 (5)
Rh2—Cl1^i	2.5027 (14)	C4—H8	0.9800
Rh2—O2	2.057 (3)	C4—H9	0.9800
Rh2—O3	2.051 (3)	C4—H10	0.9800
Rh2—N1	1.978 (3)	C5—C6	1.501 (5)
Rh2—N4	1.968 (3)	C6—H11	0.9800
N1—C1	1.302 (5)	C6—H12	0.9800
N1—H1	0.8800	C6—H13	0.9800
O1—C1	1.277 (5)	C7—C8	1.495 (5)
N2—C3	1.297 (5)	C8—H14	0.9800
N2—H2	0.8800	C8—H15	0.9800
O2—C3	1.297 (5)	C8—H16	0.9800
N3—C5	1.304 (5)	O5—C9	1.406 (5)
N3—H3	0.8800	O5—H17	0.86 (6)
O3—C5	1.289 (5)	C9—H18	0.9800
N4—C7	1.310 (5)	C9—H19	0.9800
N4—H4	0.8800	C9—H20	0.9800
N2—Rh1—N3	89.26 (13)	Rh2—N4—H4	118.0
N2—Rh1—O1	92.00 (12)	C7—O4—Rh1	117.9 (2)
N3—Rh1—O1	175.59 (12)	O1—C1—N1	122.7 (3)
N2—Rh1—O4	174.29 (12)	O1—C1—C2	116.6 (3)
N3—Rh1—O4	89.61 (12)	N1—C1—C2	120.7 (3)
O1—Rh1—O4	88.72 (11)	C1—C2—H5	109.5
N2—Rh1—Rh2	85.51 (9)	C1—C2—H6	109.5
N3—Rh1—Rh2	86.36 (10)	H5—C2—H6	109.5
O1—Rh1—Rh2	89.52 (8)	C1—C2—H7	109.5
O4—Rh1—Rh2	88.83 (8)	H5—C2—H7	109.5
N2—Rh1—Cl1	86.09 (9)	H6—C2—H7	109.5
N3—Rh1—Cl1	97.21 (10)	O2—C3—N2	121.9 (3)
O1—Rh1—Cl1	87.09 (8)	O2—C3—C4	117.1 (3)
O4—Rh1—Cl1	99.61 (8)	N2—C3—C4	121.0 (3)
Rh2—Rh1—Cl1	170.82 (2)	C3—C4—H8	109.5
N4—Rh2—N1	92.43 (13)	C3—C4—H9	109.5
N4—Rh2—O3	88.32 (12)	H8—C4—H9	109.5
N1—Rh2—O3	174.91 (12)	C3—C4—H10	109.5
N4—Rh2—O2	175.61 (12)	H8—C4—H10	109.5
N1—Rh2—O2	89.72 (12)	H9—C4—H10	109.5
O3—Rh2—O2	89.21 (11)	O3—C5—N3	122.8 (3)
N4—Rh2—Rh1	86.54 (9)	O3—C5—C6	116.9 (3)
N1—Rh2—Rh1	85.79 (10)	N3—C5—C6	120.3 (3)
O3—Rh2—Rh1	89.23 (8)	C5—C6—H11	109.5
O2—Rh2—Rh1	89.80 (8)	C5—C6—H12	109.5
N4—Rh2—Cl1^i	93.28 (9)	H11—C6—H12	109.5
N1—Rh2—Cl1^i	88.16 (10)	C5—C6—H13	109.5
O3—Rh2—Cl1^i	96.82 (8)	H11—C6—H13	109.5
O2—Rh2—Cl1^i	90.62 (8)	H12—C6—H13	109.5
Rh1—Rh2—Cl1^i	173.94 (2)	O4—C7—N4	122.1 (3)
Rh2^ii—Cl1—Rh1	114.59 (5)	O4—C7—C8	118.3 (3)
C1—N1—Rh2	123.8 (3)	N4—C7—C8	119.6 (3)
C1—N1—H1	118.1	C7—C8—H14	109.5
Rh2—N1—H1	118.1	C7—C8—H15	109.5
C1—O1—Rh1	118.1 (2)	H14—C8—H15	109.5
C3—N2—Rh1	125.6 (3)	C7—C8—H16	109.5
C3—N2—H2	117.2	H14—C8—H16	109.5
Rh1—N2—H2	117.2	H15—C8—H16	109.5
C3—O2—Rh2	116.8 (2)	C9—O5—H17	110 (4)
C5—N3—Rh1	123.9 (3)	O5—C9—H18	109.5
C5—N3—H3	118.1	O5—C9—H19	109.5
Rh1—N3—H3	118.1	H18—C9—H19	109.5
C5—O3—Rh2	117.5 (2)	O5—C9—H20	109.5
C7—N4—Rh2	124.1 (3)	H18—C9—H20	109.5
C7—N4—H4	118.0	H19—C9—H20	109.5
O1—Rh1—Rh2—N1	1.08 (12)	Rh1—Rh2—O2—C3	−6.1 (3)
N2—Rh1—Rh2—O2	3.40 (12)	Cl1^i—Rh2—O2—C3	179.9 (3)
N3—Rh1—Rh2—O3	3.73 (12)	N2—Rh1—N3—C5	82.1 (3)
O4—Rh1—Rh2—N4	5.04 (12)	O4—Rh1—N3—C5	−92.3 (3)
N2—Rh1—Rh2—N4	−174.18 (13)	Rh2—Rh1—N3—C5	−3.4 (3)
N3—Rh1—Rh2—N4	−84.64 (13)	Cl1—Rh1—N3—C5	168.1 (3)
O1—Rh1—Rh2—N4	93.78 (12)	N4—Rh2—O3—C5	81.2 (3)
N2—Rh1—Rh2—N1	93.13 (13)	O2—Rh2—O3—C5	−95.2 (3)
N3—Rh1—Rh2—N1	−177.33 (13)	Rh1—Rh2—O3—C5	−5.3 (3)
O4—Rh1—Rh2—N1	−87.65 (12)	Cl1^i—Rh2—O3—C5	174.3 (2)
N2—Rh1—Rh2—O3	−85.82 (12)	N1—Rh2—N4—C7	80.5 (3)
O1—Rh1—Rh2—O3	−177.86 (11)	O3—Rh2—N4—C7	−94.5 (3)
O4—Rh1—Rh2—O3	93.41 (11)	Rh1—Rh2—N4—C7	−5.2 (3)
N3—Rh1—Rh2—O2	92.94 (12)	Cl1^i—Rh2—N4—C7	168.8 (3)
O1—Rh1—Rh2—O2	−88.65 (11)	N3—Rh1—O4—C7	79.6 (3)
O4—Rh1—Rh2—O2	−177.38 (11)	O1—Rh1—O4—C7	−96.3 (3)
N2—Rh1—Cl1—Rh2^ii	119.27 (10)	Rh2—Rh1—O4—C7	−6.8 (3)
N3—Rh1—Cl1—Rh2^ii	30.51 (10)	Cl1—Rh1—O4—C7	176.9 (2)
O1—Rh1—Cl1—Rh2^ii	−148.52 (8)	Rh1—O1—C1—N1	−0.2 (5)
O4—Rh1—Cl1—Rh2^ii	−60.31 (8)	Rh1—O1—C1—C2	179.7 (3)
N4—Rh2—N1—C1	−88.1 (3)	Rh2—N1—C1—O1	1.6 (5)
O2—Rh2—N1—C1	88.1 (3)	Rh2—N1—C1—C2	−178.3 (3)
Rh1—Rh2—N1—C1	−1.8 (3)	Rh2—O2—C3—N2	6.6 (5)
Cl1^i—Rh2—N1—C1	178.7 (3)	Rh2—O2—C3—C4	−174.2 (3)
N2—Rh1—O1—C1	−86.3 (3)	Rh1—N2—C3—O2	−2.7 (5)
O4—Rh1—O1—C1	88.0 (3)	Rh1—N2—C3—C4	178.1 (3)
Rh2—Rh1—O1—C1	−0.8 (3)	Rh2—O3—C5—N3	4.4 (5)
Cl1—Rh1—O1—C1	−172.3 (3)	Rh2—O3—C5—C6	−175.5 (3)
N3—Rh1—N2—C3	−88.2 (3)	Rh1—N3—C5—O3	0.1 (5)
O1—Rh1—N2—C3	87.6 (3)	Rh1—N3—C5—C6	−180.0 (3)
Rh2—Rh1—N2—C3	−1.8 (3)	Rh1—O4—C7—N4	4.9 (5)
Cl1—Rh1—N2—C3	174.5 (3)	Rh1—O4—C7—C8	−176.6 (3)
N1—Rh2—O2—C3	−91.9 (3)	Rh2—N4—C7—O4	1.2 (5)
O3—Rh2—O2—C3	83.1 (3)	Rh2—N4—C7—C8	−177.2 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O4^i	0.88	2.30	3.180 (4)	175
N2—H2···O5	0.88	2.28	2.976 (5)	136
N3—H3···O2^ii	0.88	2.43	3.251 (5)	155
N4—H4···O3^iii	0.88	2.45	3.277 (4)	158
O5—H17···O2^ii	0.86 (6)	2.25 (6)	3.045 (4)	155 (5)

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