Assembled structures of tetrakis(biimidazole)dirhodium complexes hydrogen-bonded with common inorganic anions

Eight new structures of dirhodium complexes, each with four biimidazole (H₂bim) ligands, were obtained: [Rh₂(H₂bim)₄(H₂O)₂](NO₃)₄·4H₂O (I), [Rh₂(H₂bim)₄(H₂O)₂](ClO₄)₄·5H₂O (II), [Rh₂(H₂bim)₄(MeOH)₂](ClO₄)₄ (III), [Rh₂(H₂bim)₄(DMF)₂](BF₄)₄ (IV), [Rh₂(H₂bim)₄(Mepy)₂](SiF₆)₂·8H₂O (V), [{Rh₂(H₂bim)₄(pz)}₂(μ-pz)](SiF₆)(ClO₄)₆·12.7H₂O (VI), [{Rh₂(H₂bim)₄(pz)}₂(μ-pz)](ClO₄)₈·11.4H₂O (VII) and [Rh₂(H₂bim)₄(μ-pz)](SiF₆)₂·6H₂O (VIII). The unbridged Rh—Rh bond distances range between 2.6313 (8) and 2.7052 (5) Å. The dirhodium units adopt a staggered conformation with torsion angles N—Rh—Rh—N of 37.6 (4)–48.98 (8)°. Various assembled structures were constructed by hydrogen bonding between the complexes and the anions: a discrete structure in (IV), one-dimensional structure in (II), two-dimensional structures in (I), (III), (VI), (VII) and (VIII) and a three-dimensional structure in (V).

S1. Experimental

S1.1. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1.

S2. Results and discussion

Computing details

For all compounds, data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).

(I)

Crystal data

C24H28N16O2Rh2·4(NO3)·4(H2O)	Dx = 1.891 Mg m^−3
Mr = 1098.55	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pbcn	Cell parameters from 9401 reflections
a = 18.843 (3) Å	θ = 3.0–27.5°
b = 16.642 (3) Å	µ = 0.96 mm^−1
c = 12.307 (2) Å	T = 123 K
V = 3859.2 (11) Å^3	Prismatic, green
Z = 4	0.66 × 0.12 × 0.10 mm
F(000) = 2216

Data collection

Rigaku/MSC Mercury CCD diffractometer	4413 independent reflections
Radiation source: rotating-anode X-ray tube	4134 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.2°
ω scans	h = −24→17
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −21→19
Tmin = 0.809, Tmax = 0.956	l = −15→11
29049 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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.080	H atoms treated by a mixture of independent and constrained refinement
S = 1.32	w = 1/[σ^2(Fo^2) + (0.0208P)^2 + 3.7755P] where P = (Fo^2 + 2Fc^2)/3
4416 reflections	(Δ/σ)max = 0.001
313 parameters	Δρmax = 0.79 e Å^−3
0 restraints	Δρmin = −0.57 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	0.496293 (11)	0.284327 (13)	0.641384 (16)	0.01116 (7)
N1	0.59822 (13)	0.32611 (15)	0.62505 (18)	0.0135 (5)
C1	0.64592 (15)	0.26794 (19)	0.6126 (2)	0.0150 (6)
N2	0.71109 (13)	0.29788 (15)	0.59918 (19)	0.0171 (5)
H2N	0.7504	0.2701	0.5908	0.021*
C2	0.70526 (16)	0.38076 (19)	0.6009 (2)	0.0195 (6)
H2	0.7426	0.4186	0.5927	0.023*
C3	0.63508 (16)	0.39728 (18)	0.6166 (2)	0.0161 (6)
H3	0.6149	0.4495	0.6211	0.019*
N3	0.55025 (13)	0.17784 (15)	0.63014 (18)	0.0140 (5)
C4	0.61985 (16)	0.18639 (19)	0.6143 (2)	0.0151 (6)
N4	0.65146 (14)	0.11611 (16)	0.59794 (19)	0.0189 (6)
H4N	0.6969	0.1083	0.5852	0.023*
C5	0.60030 (17)	0.0581 (2)	0.6046 (2)	0.0216 (7)
H5	0.6070	0.0018	0.5968	0.026*
C6	0.53747 (17)	0.09677 (19)	0.6246 (2)	0.0186 (6)
H6	0.4926	0.0717	0.6333	0.022*
N5	0.44123 (13)	0.39047 (15)	0.64183 (17)	0.0134 (5)
C7	0.37062 (15)	0.38177 (19)	0.6380 (2)	0.0151 (6)
N6	0.33816 (14)	0.45272 (16)	0.63229 (18)	0.0183 (5)
H6N	0.2921	0.4608	0.6291	0.022*
C8	0.38953 (17)	0.5106 (2)	0.6324 (2)	0.0197 (6)
H8	0.3823	0.5670	0.6294	0.024*
C9	0.45320 (17)	0.47192 (19)	0.6375 (2)	0.0176 (6)
H9	0.4984	0.4971	0.6380	0.021*
N7	0.39421 (13)	0.24234 (15)	0.64234 (18)	0.0138 (5)
C10	0.34518 (16)	0.30002 (19)	0.6403 (2)	0.0156 (6)
N8	0.27952 (13)	0.26823 (17)	0.63876 (19)	0.0194 (6)
H8N	0.2392	0.2950	0.6377	0.023*
C11	0.28727 (17)	0.1858 (2)	0.6392 (2)	0.0205 (7)
H11	0.2501	0.1471	0.6388	0.025*
C12	0.35840 (16)	0.17020 (19)	0.6402 (2)	0.0170 (6)
H12	0.3796	0.1184	0.6394	0.020*
O1	0.49336 (12)	0.28149 (15)	0.45463 (17)	0.0175 (4)
H1A	0.465 (2)	0.316 (3)	0.433 (3)	0.045 (13)*
H1B	0.4778 (19)	0.241 (2)	0.436 (3)	0.020 (10)*
N9	0.84385 (14)	0.12376 (17)	0.61933 (19)	0.0211 (6)
O2	0.83313 (13)	0.19829 (15)	0.61922 (19)	0.0303 (6)
O3	0.79334 (13)	0.07548 (17)	0.6175 (2)	0.0383 (6)
O4	0.90598 (11)	0.09783 (14)	0.62123 (17)	0.0235 (5)
N10	0.14816 (15)	0.44192 (18)	0.6615 (2)	0.0246 (6)
O5	0.19275 (12)	0.48324 (16)	0.61076 (19)	0.0310 (6)
O6	0.16805 (15)	0.38192 (16)	0.7156 (2)	0.0397 (7)
O7	0.08408 (13)	0.46105 (16)	0.65985 (19)	0.0312 (6)
O8	0.12766 (14)	0.21130 (17)	0.6437 (2)	0.0309 (6)
H8A	0.088 (3)	0.216 (3)	0.618 (4)	0.072 (18)*
H8B	0.117 (3)	0.227 (3)	0.709 (4)	0.070 (17)*
O9	0.45282 (18)	0.13651 (18)	0.3771 (2)	0.0390 (7)
H9A	0.495 (3)	0.116 (4)	0.358 (4)	0.10 (3)*
H9B	0.423 (3)	0.130 (3)	0.327 (4)	0.073 (18)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.00905 (12)	0.01098 (12)	0.01346 (11)	0.00023 (8)	−0.00001 (8)	−0.00033 (8)
N1	0.0118 (12)	0.0141 (13)	0.0145 (11)	0.0007 (10)	−0.0005 (9)	−0.0008 (9)
C1	0.0121 (14)	0.0179 (16)	0.0149 (13)	0.0021 (12)	0.0004 (10)	0.0017 (11)
N2	0.0122 (13)	0.0193 (15)	0.0197 (12)	−0.0003 (11)	0.0018 (9)	−0.0020 (10)
C2	0.0152 (15)	0.0201 (17)	0.0231 (15)	−0.0038 (13)	0.0015 (12)	0.0006 (12)
C3	0.0186 (15)	0.0128 (16)	0.0167 (14)	−0.0022 (12)	−0.0007 (11)	0.0016 (11)
N3	0.0129 (12)	0.0121 (13)	0.0171 (11)	0.0009 (10)	−0.0003 (9)	−0.0012 (9)
C4	0.0135 (15)	0.0170 (16)	0.0148 (13)	0.0028 (12)	0.0008 (11)	−0.0021 (11)
N4	0.0133 (13)	0.0190 (15)	0.0245 (13)	0.0042 (11)	0.0033 (10)	−0.0016 (10)
C5	0.0226 (17)	0.0136 (16)	0.0286 (16)	−0.0007 (13)	0.0040 (12)	−0.0003 (12)
C6	0.0179 (16)	0.0150 (16)	0.0229 (15)	−0.0003 (12)	0.0019 (12)	0.0014 (12)
N5	0.0128 (12)	0.0138 (13)	0.0136 (11)	0.0012 (10)	−0.0006 (9)	−0.0006 (9)
C7	0.0124 (14)	0.0219 (17)	0.0109 (12)	0.0012 (12)	−0.0014 (10)	−0.0001 (11)
N6	0.0164 (13)	0.0192 (14)	0.0191 (12)	0.0054 (11)	0.0005 (10)	0.0016 (10)
C8	0.0232 (17)	0.0161 (17)	0.0198 (14)	0.0023 (13)	−0.0004 (12)	0.0006 (12)
C9	0.0199 (16)	0.0154 (16)	0.0175 (13)	−0.0016 (12)	−0.0013 (11)	−0.0004 (12)
N7	0.0115 (12)	0.0147 (13)	0.0154 (11)	−0.0013 (10)	−0.0010 (9)	−0.0010 (9)
C10	0.0124 (14)	0.0219 (17)	0.0124 (13)	0.0015 (12)	−0.0010 (10)	−0.0004 (11)
N8	0.0106 (12)	0.0265 (16)	0.0211 (13)	0.0000 (11)	−0.0023 (10)	0.0012 (11)
C11	0.0177 (16)	0.0230 (18)	0.0209 (15)	−0.0061 (13)	−0.0037 (12)	0.0008 (12)
C12	0.0185 (16)	0.0135 (16)	0.0189 (14)	−0.0038 (12)	−0.0006 (11)	−0.0009 (12)
O1	0.0188 (12)	0.0146 (12)	0.0191 (10)	−0.0006 (11)	−0.0034 (8)	−0.0023 (9)
N9	0.0189 (14)	0.0251 (16)	0.0192 (13)	0.0056 (12)	0.0019 (10)	0.0018 (11)
O2	0.0278 (14)	0.0243 (14)	0.0387 (14)	0.0104 (11)	0.0004 (10)	0.0032 (10)
O3	0.0166 (13)	0.0301 (16)	0.0682 (18)	0.0006 (11)	0.0009 (12)	0.0007 (13)
O4	0.0130 (11)	0.0236 (13)	0.0339 (12)	0.0050 (9)	0.0020 (9)	0.0058 (10)
N10	0.0187 (15)	0.0254 (16)	0.0297 (14)	0.0028 (12)	−0.0048 (11)	−0.0067 (12)
O5	0.0195 (13)	0.0347 (16)	0.0390 (14)	0.0026 (11)	−0.0030 (10)	−0.0006 (11)
O6	0.0371 (16)	0.0309 (16)	0.0512 (15)	0.0140 (13)	−0.0038 (12)	0.0083 (12)
O7	0.0176 (12)	0.0341 (15)	0.0419 (14)	0.0075 (11)	−0.0006 (10)	−0.0036 (11)
O8	0.0206 (14)	0.0416 (17)	0.0306 (14)	0.0014 (12)	−0.0053 (11)	−0.0027 (12)
O9	0.0394 (18)	0.0331 (17)	0.0445 (16)	−0.0040 (14)	−0.0044 (14)	−0.0108 (13)

Geometric parameters (Å, º)

Rh1—N7	2.047 (2)	C7—C10	1.443 (4)
Rh1—N3	2.048 (2)	N6—C8	1.365 (4)
Rh1—N5	2.049 (2)	N6—H6N	0.8800
Rh1—N1	2.053 (2)	C8—C9	1.363 (4)
Rh1—O1	2.299 (2)	C8—H8	0.9500
Rh1—Rh1^i	2.6771 (6)	C9—H9	0.9500
N1—C1	1.330 (4)	N7—C10	1.333 (4)
N1—C3	1.377 (4)	N7—C12	1.377 (4)
C1—N2	1.336 (4)	C10—N8	1.346 (4)
C1—C4	1.443 (4)	N8—C11	1.380 (4)
N2—C2	1.384 (4)	N8—H8N	0.8800
N2—H2N	0.8800	C11—C12	1.365 (4)
C2—C3	1.365 (4)	C11—H11	0.9500
C2—H2	0.9500	C12—H12	0.9500
C3—H3	0.9500	O1—H1A	0.83 (5)
N3—C4	1.333 (4)	O1—H1B	0.78 (4)
N3—C6	1.372 (4)	N9—O3	1.246 (4)
C4—N4	1.328 (4)	N9—O4	1.248 (3)
N4—C5	1.367 (4)	N9—O2	1.257 (4)
N4—H4N	0.8800	N10—O7	1.249 (3)
C5—C6	1.370 (4)	N10—O5	1.253 (4)
C5—H5	0.9500	N10—O6	1.257 (4)
C6—H6	0.9500	O8—H8A	0.81 (6)
N5—C7	1.339 (4)	O8—H8B	0.87 (5)
N5—C9	1.375 (4)	O9—H9A	0.90 (6)
C7—N6	1.332 (4)	O9—H9B	0.83 (5)
N7—Rh1—N3	99.88 (10)	C5—C6—H6	125.7
N7—Rh1—N5	79.53 (10)	N3—C6—H6	125.7
N3—Rh1—N5	176.24 (9)	C7—N5—C9	105.6 (3)
N7—Rh1—N1	174.71 (9)	C7—N5—Rh1	114.2 (2)
N3—Rh1—N1	79.74 (10)	C9—N5—Rh1	140.1 (2)
N5—Rh1—N1	100.49 (10)	N6—C7—N5	111.2 (3)
N7—Rh1—O1	88.63 (8)	N6—C7—C10	133.2 (3)
N3—Rh1—O1	85.80 (9)	N5—C7—C10	115.6 (3)
N5—Rh1—O1	90.47 (9)	C7—N6—C8	107.4 (3)
N1—Rh1—O1	86.07 (8)	C7—N6—H6N	126.3
N7—Rh1—Rh1^i	92.48 (6)	C8—N6—H6N	126.3
N3—Rh1—Rh1^i	92.38 (6)	C9—C8—N6	107.0 (3)
N5—Rh1—Rh1^i	91.36 (6)	C9—C8—H8	126.5
N1—Rh1—Rh1^i	92.81 (6)	N6—C8—H8	126.5
O1—Rh1—Rh1^i	178.00 (6)	C8—C9—N5	108.8 (3)
C1—N1—C3	106.1 (2)	C8—C9—H9	125.6
C1—N1—Rh1	113.4 (2)	N5—C9—H9	125.6
C3—N1—Rh1	140.4 (2)	C10—N7—C12	106.7 (2)
N1—C1—N2	111.4 (3)	C10—N7—Rh1	113.9 (2)
N1—C1—C4	116.9 (3)	C12—N7—Rh1	139.3 (2)
N2—C1—C4	131.7 (3)	N7—C10—N8	110.8 (3)
C1—N2—C2	107.3 (3)	N7—C10—C7	116.7 (3)
C1—N2—H2N	126.4	N8—C10—C7	132.5 (3)
C2—N2—H2N	126.4	C10—N8—C11	107.1 (3)
C3—C2—N2	106.2 (3)	C10—N8—H8N	126.5
C3—C2—H2	126.9	C11—N8—H8N	126.5
N2—C2—H2	126.9	C12—C11—N8	107.0 (3)
C2—C3—N1	109.0 (3)	C12—C11—H11	126.5
C2—C3—H3	125.5	N8—C11—H11	126.5
N1—C3—H3	125.5	C11—C12—N7	108.4 (3)
C4—N3—C6	105.7 (3)	C11—C12—H12	125.8
C4—N3—Rh1	113.9 (2)	N7—C12—H12	125.8
C6—N3—Rh1	140.1 (2)	Rh1—O1—H1A	109 (3)
N4—C4—N3	111.7 (3)	Rh1—O1—H1B	109 (3)
N4—C4—C1	132.3 (3)	H1A—O1—H1B	105 (4)
N3—C4—C1	115.9 (3)	O3—N9—O4	119.6 (3)
C4—N4—C5	107.3 (3)	O3—N9—O2	120.9 (3)
C4—N4—H4N	126.4	O4—N9—O2	119.5 (3)
C5—N4—H4N	126.4	O7—N10—O5	120.0 (3)
N4—C5—C6	106.8 (3)	O7—N10—O6	120.0 (3)
N4—C5—H5	126.6	O5—N10—O6	120.0 (3)
C6—C5—H5	126.6	H8A—O8—H8B	97 (4)
C5—C6—N3	108.6 (3)	H9A—O9—H9B	110 (5)
N1—Rh1—Rh1^i—N5^i	39.77 (10)	Rh1—N3—C6—C5	172.7 (2)
N3—Rh1—Rh1^i—N7^i	40.03 (10)	N7—Rh1—N5—C7	−2.58 (18)
N7—Rh1—N1—C1	−84.5 (11)	N3—Rh1—N5—C7	78.8 (15)
N3—Rh1—N1—C1	1.87 (18)	N1—Rh1—N5—C7	172.04 (18)
N5—Rh1—N1—C1	−174.31 (18)	O1—Rh1—N5—C7	85.94 (19)
O1—Rh1—N1—C1	−84.56 (19)	Rh1^i—Rh1—N5—C7	−94.85 (18)
Rh1^i—Rh1—N1—C1	93.79 (18)	N7—Rh1—N5—C9	−176.7 (3)
N7—Rh1—N1—C3	90.7 (11)	N3—Rh1—N5—C9	−95.3 (15)
N3—Rh1—N1—C3	177.1 (3)	N1—Rh1—N5—C9	−2.0 (3)
N5—Rh1—N1—C3	0.9 (3)	O1—Rh1—N5—C9	−88.1 (3)
O1—Rh1—N1—C3	90.7 (3)	Rh1^i—Rh1—N5—C9	91.1 (3)
Rh1^i—Rh1—N1—C3	−91.0 (3)	C9—N5—C7—N6	−0.4 (3)
C3—N1—C1—N2	1.4 (3)	Rh1—N5—C7—N6	−176.45 (17)
Rh1—N1—C1—N2	178.23 (18)	C9—N5—C7—C10	179.3 (2)
C3—N1—C1—C4	−177.9 (2)	Rh1—N5—C7—C10	3.3 (3)
Rh1—N1—C1—C4	−1.1 (3)	N5—C7—N6—C8	0.0 (3)
N1—C1—N2—C2	−1.3 (3)	C10—C7—N6—C8	−179.7 (3)
C4—C1—N2—C2	177.9 (3)	C7—N6—C8—C9	0.4 (3)
C1—N2—C2—C3	0.6 (3)	N6—C8—C9—N5	−0.7 (3)
N2—C2—C3—N1	0.3 (3)	C7—N5—C9—C8	0.7 (3)
C1—N1—C3—C2	−1.0 (3)	Rh1—N5—C9—C8	175.0 (2)
Rh1—N1—C3—C2	−176.4 (2)	N3—Rh1—N7—C10	−174.82 (19)
N7—Rh1—N3—C4	172.17 (19)	N5—Rh1—N7—C10	1.40 (18)
N5—Rh1—N3—C4	91.4 (15)	N1—Rh1—N7—C10	−89.4 (11)
N1—Rh1—N3—C4	−2.47 (19)	O1—Rh1—N7—C10	−89.33 (19)
O1—Rh1—N3—C4	84.29 (19)	Rh1^i—Rh1—N7—C10	92.33 (18)
Rh1^i—Rh1—N3—C4	−94.90 (19)	N3—Rh1—N7—C12	1.8 (3)
N7—Rh1—N3—C6	−0.6 (3)	N5—Rh1—N7—C12	178.0 (3)
N5—Rh1—N3—C6	−81.3 (15)	N1—Rh1—N7—C12	87.2 (11)
N1—Rh1—N3—C6	−175.2 (3)	O1—Rh1—N7—C12	87.3 (3)
O1—Rh1—N3—C6	−88.4 (3)	Rh1^i—Rh1—N7—C12	−91.1 (3)
Rh1^i—Rh1—N3—C6	92.4 (3)	C12—N7—C10—N8	1.0 (3)
C6—N3—C4—N4	0.7 (3)	Rh1—N7—C10—N8	178.68 (17)
Rh1—N3—C4—N4	−174.43 (18)	C12—N7—C10—C7	−177.8 (2)
C6—N3—C4—C1	177.8 (2)	Rh1—N7—C10—C7	−0.1 (3)
Rh1—N3—C4—C1	2.7 (3)	N6—C7—C10—N7	177.5 (3)
N1—C1—C4—N4	175.3 (3)	N5—C7—C10—N7	−2.2 (4)
N2—C1—C4—N4	−3.8 (5)	N6—C7—C10—N8	−0.9 (5)
N1—C1—C4—N3	−1.1 (4)	N5—C7—C10—N8	179.4 (3)
N2—C1—C4—N3	179.8 (3)	N7—C10—N8—C11	−0.3 (3)
N3—C4—N4—C5	−0.7 (3)	C7—C10—N8—C11	178.2 (3)
C1—C4—N4—C5	−177.2 (3)	C10—N8—C11—C12	−0.5 (3)
C4—N4—C5—C6	0.4 (3)	N8—C11—C12—N7	1.1 (3)
N4—C5—C6—N3	0.0 (3)	C10—N7—C12—C11	−1.3 (3)
C4—N3—C6—C5	−0.5 (3)	Rh1—N7—C12—C11	−178.0 (2)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O2	0.88	1.99	2.845 (3)	162
N4—H4N···O3	0.88	1.94	2.768 (4)	157
N6—H6N···O5	0.88	1.92	2.799 (4)	175
N8—H8N···O6	0.88	2.19	2.981 (4)	149
N8—H8N···O8	0.88	2.52	3.015 (4)	116
O1—H1A···N9^ii	0.83 (5)	2.57 (5)	3.354 (4)	158 (4)
O1—H1A···O2^ii	0.83 (5)	2.57 (4)	3.171 (3)	130 (4)
O1—H1A···O4^ii	0.83 (5)	1.93 (5)	2.760 (3)	174 (4)
O1—H1B···O9	0.78 (4)	1.93 (4)	2.705 (4)	171 (4)
O8—H8A···O1^ii	0.81 (6)	2.00 (6)	2.808 (3)	174 (5)
O8—H8B···O2^i	0.87 (5)	2.36 (5)	3.017 (4)	133 (4)
O9—H9A···O7^iii	0.90 (6)	2.12 (7)	2.993 (4)	164 (6)
O9—H9B···O6^iv	0.83 (5)	2.21 (6)	3.038 (4)	170 (5)
O9—H9B···O7^iv	0.83 (5)	2.56 (5)	3.204 (4)	135 (5)

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

(II)

Crystal data

C24H28N16O2Rh2·4(ClO4)·5(H2O)	F(000) = 2544
Mr = 1266.32	Dx = 1.884 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71069 Å
a = 13.453 (2) Å	Cell parameters from 11005 reflections
b = 13.334 (2) Å	θ = 3.0–27.5°
c = 24.906 (4) Å	µ = 1.08 mm^−1
β = 91.749 (2)°	T = 296 K
V = 4465.5 (13) Å^3	Prismatic, green
Z = 4	0.41 × 0.35 × 0.34 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer	10190 independent reflections
Radiation source: rotating-anode X-ray tube	8188 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 = −17→16
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −14→17
Tmin = 0.731, Tmax = 0.815	l = −32→31
34616 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)] = 0.058	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.163	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0753P)^2 + 6.5586P] where P = (Fo^2 + 2Fc^2)/3
10190 reflections	(Δ/σ)max = 0.001
641 parameters	Δρmax = 0.78 e Å^−3
0 restraints	Δρmin = −0.74 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	Occ. (<1)
Rh1	0.53955 (2)	0.26880 (3)	0.600046 (13)	0.03340 (11)
Rh2	0.69975 (2)	0.26866 (3)	0.664573 (14)	0.03684 (12)
N1	0.4434 (3)	0.2821 (3)	0.66190 (15)	0.0390 (8)
C1	0.4049 (3)	0.1948 (4)	0.6768 (2)	0.0447 (10)
N2	0.3366 (3)	0.2092 (4)	0.7139 (2)	0.0639 (13)
H2N	0.3023	0.1631	0.7287	0.077*
C2	0.3304 (4)	0.3090 (5)	0.7241 (3)	0.0698 (17)
H2	0.2892	0.3401	0.7484	0.084*
C3	0.3976 (4)	0.3550 (4)	0.6912 (2)	0.0536 (12)
H3	0.4097	0.4235	0.6893	0.064*
N3	0.5097 (3)	0.1203 (3)	0.61424 (15)	0.0396 (8)
C4	0.4409 (3)	0.1066 (4)	0.6505 (2)	0.0442 (10)
N4	0.4204 (3)	0.0088 (3)	0.65627 (19)	0.0543 (11)
H4N	0.3783	−0.0167	0.6777	0.065*
C5	0.4781 (4)	−0.0421 (4)	0.6223 (2)	0.0582 (13)
H5	0.4799	−0.1113	0.6178	0.070*
C6	0.5336 (4)	0.0268 (4)	0.5956 (2)	0.0506 (12)
H6	0.5794	0.0128	0.5695	0.061*
N5	0.5593 (2)	0.4171 (3)	0.58141 (14)	0.0364 (8)
C7	0.6056 (3)	0.4311 (3)	0.53579 (18)	0.0385 (9)
N6	0.6104 (3)	0.5293 (3)	0.52416 (16)	0.0436 (9)
H6N	0.6375	0.5556	0.4967	0.052*
C8	0.5643 (3)	0.5798 (4)	0.5641 (2)	0.0463 (11)
H8	0.5557	0.6488	0.5668	0.056*
C9	0.5337 (3)	0.5098 (4)	0.59883 (19)	0.0428 (10)
H9	0.5001	0.5230	0.6301	0.051*
N7	0.6206 (3)	0.2559 (3)	0.53224 (15)	0.0390 (8)
C10	0.6384 (3)	0.3432 (4)	0.50845 (17)	0.0396 (9)
N8	0.6826 (3)	0.3280 (3)	0.46160 (17)	0.0536 (10)
H8N	0.7016	0.3736	0.4398	0.064*
C11	0.6920 (4)	0.2273 (4)	0.4549 (2)	0.0585 (14)
H11	0.7195	0.1953	0.4257	0.070*
C12	0.6539 (4)	0.1817 (4)	0.4986 (2)	0.0504 (11)
H12	0.6509	0.1130	0.5047	0.061*
N9	0.6384 (3)	0.3734 (3)	0.71439 (15)	0.0423 (8)
C13	0.5952 (4)	0.3336 (4)	0.7567 (2)	0.0512 (12)
N10	0.5627 (4)	0.4057 (4)	0.78885 (18)	0.0664 (13)
H10N	0.5319	0.3970	0.8182	0.080*
C14	0.5871 (5)	0.4961 (5)	0.7667 (2)	0.0676 (16)
H14	0.5738	0.5595	0.7804	0.081*
C15	0.6344 (4)	0.4748 (4)	0.7210 (2)	0.0531 (12)
H15	0.6601	0.5220	0.6976	0.064*
N11	0.6335 (3)	0.1765 (3)	0.71885 (15)	0.0453 (9)
C16	0.5913 (4)	0.2257 (4)	0.7586 (2)	0.0502 (12)
N12	0.5527 (3)	0.1611 (4)	0.79328 (18)	0.0635 (12)
H12N	0.5212	0.1765	0.8217	0.076*
C17	0.5720 (4)	0.0677 (5)	0.7758 (2)	0.0627 (15)
H17	0.5539	0.0082	0.7924	0.075*
C18	0.6224 (4)	0.0763 (4)	0.7299 (2)	0.0520 (12)
H18	0.6456	0.0234	0.7093	0.062*
N13	0.7779 (3)	0.3618 (3)	0.61590 (15)	0.0396 (8)
C19	0.8386 (3)	0.3131 (4)	0.58366 (19)	0.0442 (10)
N14	0.8953 (3)	0.3771 (4)	0.55698 (18)	0.0559 (11)
H14N	0.9392	0.3618	0.5340	0.067*
C20	0.8703 (4)	0.4718 (4)	0.5732 (2)	0.0602 (14)
H20	0.8976	0.5317	0.5614	0.072*
C21	0.7992 (4)	0.4617 (4)	0.6093 (2)	0.0489 (11)
H21	0.7689	0.5143	0.6271	0.059*
N15	0.7704 (3)	0.1651 (3)	0.61760 (16)	0.0429 (8)
C22	0.8347 (3)	0.2059 (4)	0.5846 (2)	0.0448 (10)
N16	0.8832 (3)	0.1360 (4)	0.55801 (19)	0.0566 (11)
H16N	0.9273	0.1460	0.5343	0.068*
C23	0.8496 (4)	0.0443 (4)	0.5755 (2)	0.0610 (14)
H23	0.8704	−0.0185	0.5641	0.073*
C24	0.7804 (4)	0.0632 (4)	0.6123 (2)	0.0519 (12)
H24	0.7454	0.0151	0.6311	0.062*
O1	0.3963 (3)	0.2753 (3)	0.54537 (15)	0.0538 (9)
O2	0.8362 (3)	0.2659 (4)	0.72130 (19)	0.0794 (14)
Cl1	0.82216 (13)	0.56104 (17)	0.41178 (8)	0.0877 (6)
O3	0.7225 (3)	0.5342 (4)	0.4201 (2)	0.0953 (16)
O4	0.8275 (8)	0.6651 (8)	0.4169 (5)	0.251 (6)
O5	0.8534 (5)	0.5347 (7)	0.3606 (3)	0.147 (3)
O6	0.8836 (5)	0.5176 (10)	0.4482 (3)	0.226 (6)
Cl2	0.62259 (12)	0.29621 (12)	0.31100 (6)	0.0670 (4)
O7	0.6129 (5)	0.3492 (7)	0.2641 (3)	0.176 (4)
O8	0.7027 (8)	0.3402 (10)	0.3378 (3)	0.247 (7)
O9	0.5418 (6)	0.2932 (5)	0.3436 (4)	0.160 (3)
O10	0.6425 (7)	0.1999 (5)	0.3012 (5)	0.220 (5)
Cl3	0.37165 (15)	0.4949 (2)	0.89392 (11)	0.1040 (7)
O11	0.4298 (10)	0.4154 (12)	0.8840 (6)	0.288 (7)
O12	0.2801 (5)	0.4730 (9)	0.8978 (6)	0.280 (8)
O13	0.3977 (9)	0.5226 (14)	0.9437 (4)	0.312 (9)
O14	0.4004 (10)	0.5565 (10)	0.8582 (5)	0.260 (6)
Cl4A	0.7636 (3)	0.2821 (2)	0.87174 (16)	0.0626 (10)	0.649 (8)
O15A	0.7851 (6)	0.3493 (5)	0.8278 (3)	0.081 (2)	0.649 (8)
Cl4B	0.7282 (6)	0.2572 (5)	0.8980 (4)	0.081 (2)	0.351 (8)
O15B	0.7235 (13)	0.1923 (12)	0.9389 (8)	0.119 (7)	0.351 (8)
O16	0.6564 (5)	0.3039 (5)	0.8873 (3)	0.123 (2)
O17	0.7675 (5)	0.1868 (4)	0.8526 (3)	0.113 (2)
O18	0.8267 (5)	0.3083 (5)	0.9135 (2)	0.121 (2)
O19	0.2799 (5)	0.0158 (4)	0.7481 (2)	0.115 (2)
O20	0.4216 (6)	0.2069 (7)	0.8760 (3)	0.168 (3)
O21	1.0149 (5)	0.2533 (5)	0.4893 (3)	0.116 (2)
O22	0.3310 (4)	0.0906 (4)	0.5107 (2)	0.1086 (18)
O23	1.0140 (5)	0.2828 (8)	0.6767 (4)	0.215 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.03611 (18)	0.0295 (2)	0.03494 (19)	−0.00147 (12)	0.00621 (13)	0.00278 (12)
Rh2	0.03811 (19)	0.0351 (2)	0.0374 (2)	0.00114 (13)	0.00349 (14)	0.00125 (13)
N1	0.0418 (18)	0.035 (2)	0.041 (2)	0.0015 (15)	0.0098 (15)	0.0033 (15)
C1	0.042 (2)	0.042 (3)	0.051 (3)	0.000 (2)	0.0099 (19)	0.011 (2)
N2	0.062 (3)	0.054 (3)	0.078 (3)	0.001 (2)	0.038 (2)	0.014 (2)
C2	0.076 (4)	0.056 (4)	0.080 (4)	0.016 (3)	0.045 (3)	0.010 (3)
C3	0.057 (3)	0.046 (3)	0.059 (3)	0.005 (2)	0.018 (2)	0.001 (2)
N3	0.0424 (18)	0.033 (2)	0.043 (2)	−0.0018 (15)	0.0060 (15)	0.0052 (16)
C4	0.042 (2)	0.040 (3)	0.051 (3)	−0.0022 (19)	0.0051 (19)	0.009 (2)
N4	0.054 (2)	0.035 (2)	0.075 (3)	−0.0118 (18)	0.014 (2)	0.009 (2)
C5	0.066 (3)	0.032 (3)	0.077 (4)	−0.007 (2)	0.005 (3)	0.000 (2)
C6	0.058 (3)	0.032 (3)	0.062 (3)	−0.003 (2)	0.012 (2)	−0.003 (2)
N5	0.0369 (17)	0.0322 (19)	0.0400 (19)	−0.0020 (14)	0.0016 (14)	0.0025 (15)
C7	0.0349 (19)	0.040 (2)	0.041 (2)	−0.0049 (17)	−0.0032 (17)	0.0070 (19)
N6	0.0450 (19)	0.037 (2)	0.049 (2)	−0.0069 (16)	0.0016 (17)	0.0136 (17)
C8	0.047 (2)	0.034 (2)	0.058 (3)	0.0000 (19)	−0.005 (2)	0.001 (2)
C9	0.045 (2)	0.040 (3)	0.043 (2)	0.0000 (18)	0.0010 (19)	−0.0013 (19)
N7	0.0411 (18)	0.041 (2)	0.0354 (19)	−0.0001 (15)	0.0044 (15)	0.0010 (15)
C10	0.039 (2)	0.044 (3)	0.036 (2)	−0.0044 (18)	0.0012 (17)	0.0027 (19)
N8	0.061 (2)	0.055 (3)	0.046 (2)	−0.004 (2)	0.0139 (19)	0.009 (2)
C11	0.074 (3)	0.060 (4)	0.042 (3)	0.006 (3)	0.020 (2)	−0.002 (2)
C12	0.059 (3)	0.045 (3)	0.048 (3)	0.004 (2)	0.010 (2)	−0.005 (2)
N9	0.051 (2)	0.038 (2)	0.038 (2)	0.0023 (16)	0.0038 (16)	−0.0031 (16)
C13	0.057 (3)	0.056 (3)	0.041 (2)	0.007 (2)	0.006 (2)	−0.005 (2)
N10	0.082 (3)	0.074 (4)	0.044 (2)	0.013 (3)	0.013 (2)	−0.010 (2)
C14	0.087 (4)	0.059 (4)	0.056 (3)	0.018 (3)	−0.003 (3)	−0.018 (3)
C15	0.065 (3)	0.045 (3)	0.049 (3)	0.002 (2)	0.000 (2)	−0.008 (2)
N11	0.047 (2)	0.047 (2)	0.042 (2)	0.0007 (17)	0.0046 (16)	0.0056 (18)
C16	0.057 (3)	0.059 (3)	0.035 (2)	0.003 (2)	0.007 (2)	0.009 (2)
N12	0.069 (3)	0.080 (4)	0.043 (2)	0.002 (3)	0.013 (2)	0.015 (2)
C17	0.069 (3)	0.061 (4)	0.058 (3)	−0.005 (3)	0.001 (3)	0.017 (3)
C18	0.057 (3)	0.048 (3)	0.052 (3)	−0.002 (2)	−0.001 (2)	0.010 (2)
N13	0.0406 (18)	0.037 (2)	0.042 (2)	−0.0040 (15)	0.0016 (15)	−0.0011 (16)
C19	0.039 (2)	0.045 (3)	0.048 (3)	−0.0065 (19)	0.0028 (19)	0.003 (2)
N14	0.048 (2)	0.062 (3)	0.059 (3)	−0.010 (2)	0.0158 (19)	0.007 (2)
C20	0.060 (3)	0.051 (3)	0.069 (4)	−0.011 (3)	0.003 (3)	0.006 (3)
C21	0.051 (3)	0.039 (3)	0.056 (3)	−0.004 (2)	−0.002 (2)	0.001 (2)
N15	0.0411 (18)	0.041 (2)	0.047 (2)	0.0057 (16)	0.0054 (16)	0.0005 (17)
C22	0.039 (2)	0.049 (3)	0.046 (3)	0.002 (2)	0.0083 (19)	−0.002 (2)
N16	0.050 (2)	0.056 (3)	0.064 (3)	0.008 (2)	0.016 (2)	−0.008 (2)
C23	0.060 (3)	0.044 (3)	0.080 (4)	0.009 (2)	0.007 (3)	−0.012 (3)
C24	0.058 (3)	0.036 (3)	0.061 (3)	0.004 (2)	0.003 (2)	0.002 (2)
O1	0.0518 (19)	0.054 (2)	0.056 (2)	−0.0092 (15)	−0.0046 (16)	0.0093 (16)
O2	0.056 (2)	0.114 (4)	0.068 (3)	0.008 (2)	−0.013 (2)	0.010 (2)
Cl1	0.0715 (10)	0.1087 (15)	0.0835 (12)	−0.0251 (10)	0.0136 (9)	0.0190 (11)
O3	0.067 (3)	0.102 (4)	0.119 (4)	−0.012 (3)	0.028 (3)	0.024 (3)
O4	0.266 (11)	0.140 (8)	0.354 (15)	−0.120 (8)	0.114 (11)	−0.082 (9)
O5	0.116 (4)	0.223 (9)	0.107 (5)	−0.024 (5)	0.053 (4)	−0.035 (5)
O6	0.088 (4)	0.432 (17)	0.159 (7)	0.027 (7)	−0.001 (5)	0.138 (9)
Cl2	0.0787 (9)	0.0601 (9)	0.0635 (8)	0.0045 (7)	0.0220 (7)	0.0035 (7)
O7	0.161 (6)	0.205 (8)	0.158 (6)	−0.067 (6)	−0.058 (5)	0.124 (6)
O8	0.259 (10)	0.385 (16)	0.094 (5)	−0.225 (11)	−0.034 (6)	0.052 (7)
O9	0.171 (7)	0.096 (5)	0.223 (8)	0.008 (4)	0.143 (6)	−0.011 (5)
O10	0.278 (11)	0.071 (4)	0.324 (12)	0.035 (5)	0.228 (10)	0.013 (6)
Cl3	0.0766 (12)	0.1158 (18)	0.1208 (18)	−0.0125 (11)	0.0247 (11)	0.0101 (15)
O11	0.252 (12)	0.311 (18)	0.310 (16)	0.114 (12)	0.134 (11)	−0.009 (13)
O12	0.080 (5)	0.300 (14)	0.46 (2)	−0.050 (7)	−0.047 (8)	0.141 (13)
O13	0.249 (12)	0.60 (3)	0.095 (7)	−0.103 (14)	0.065 (7)	−0.027 (11)
O14	0.350 (16)	0.210 (12)	0.222 (11)	−0.090 (11)	0.054 (11)	0.091 (9)
Cl4A	0.0759 (18)	0.0410 (15)	0.0700 (18)	0.0079 (12)	−0.0118 (14)	−0.0033 (12)
O15A	0.123 (6)	0.049 (4)	0.070 (4)	0.000 (4)	−0.011 (4)	0.010 (3)
Cl4B	0.077 (4)	0.048 (3)	0.117 (6)	0.003 (2)	−0.014 (4)	0.008 (3)
O15B	0.126 (13)	0.058 (9)	0.172 (18)	0.012 (9)	0.000 (12)	0.032 (11)
O16	0.148 (5)	0.116 (5)	0.106 (5)	0.035 (4)	−0.003 (4)	0.003 (4)
O17	0.140 (5)	0.061 (3)	0.138 (5)	−0.001 (3)	−0.020 (4)	−0.024 (3)
O18	0.160 (5)	0.110 (5)	0.091 (4)	−0.040 (4)	−0.013 (4)	−0.015 (4)
O19	0.164 (5)	0.058 (3)	0.126 (5)	−0.018 (3)	0.081 (4)	−0.003 (3)
O20	0.138 (6)	0.241 (10)	0.130 (6)	−0.021 (6)	0.080 (5)	−0.040 (6)
O21	0.122 (5)	0.123 (5)	0.107 (5)	−0.020 (4)	0.059 (4)	−0.017 (4)
O22	0.128 (4)	0.093 (4)	0.103 (4)	−0.012 (3)	−0.008 (3)	−0.006 (3)
O23	0.064 (3)	0.369 (14)	0.211 (9)	0.002 (5)	0.003 (4)	0.175 (9)

Geometric parameters (Å, º)

Rh1—N7	2.045 (4)	N10—H10N	0.8600
Rh1—N1	2.049 (4)	C14—C15	1.352 (8)
Rh1—N5	2.050 (4)	C14—H14	0.9300
Rh1—N3	2.054 (4)	C15—H15	0.9300
Rh1—O1	2.328 (3)	N11—C16	1.329 (6)
Rh1—Rh2	2.6488 (6)	N11—C18	1.373 (6)
Rh2—N13	2.048 (4)	C16—N12	1.336 (7)
Rh2—N11	2.051 (4)	N12—C17	1.347 (8)
Rh2—N9	2.057 (4)	N12—H12N	0.8600
Rh2—N15	2.061 (4)	C17—C18	1.354 (8)
Rh2—O2	2.282 (4)	C17—H17	0.9300
N1—C1	1.331 (6)	C18—H18	0.9300
N1—C3	1.373 (6)	N13—C19	1.332 (6)
C1—N2	1.337 (6)	N13—C21	1.374 (6)
C1—C4	1.436 (7)	C19—N14	1.335 (6)
N2—C2	1.357 (8)	C19—C22	1.430 (7)
N2—H2N	0.8600	N14—C20	1.372 (7)
C2—C3	1.382 (7)	N14—H14N	0.8600
C2—H2	0.9300	C20—C21	1.339 (7)
C3—H3	0.9300	C20—H20	0.9300
N3—C4	1.325 (6)	C21—H21	0.9300
N3—C6	1.371 (6)	N15—C22	1.327 (6)
C4—N4	1.342 (6)	N15—C24	1.372 (6)
N4—C5	1.348 (7)	C22—N16	1.327 (6)
N4—H4N	0.8600	N16—C23	1.379 (7)
C5—C6	1.369 (7)	N16—H16N	0.8600
C5—H5	0.9300	C23—C24	1.350 (8)
C6—H6	0.9300	C23—H23	0.9300
N5—C7	1.325 (6)	C24—H24	0.9300
N5—C9	1.359 (6)	Cl1—O6	1.340 (7)
C7—N6	1.343 (6)	Cl1—O4	1.395 (9)
C7—C10	1.432 (7)	Cl1—O5	1.399 (6)
N6—C8	1.366 (6)	Cl1—O3	1.409 (4)
N6—H6N	0.8600	Cl2—O10	1.336 (7)
C8—C9	1.345 (7)	Cl2—O7	1.368 (6)
C8—H8	0.9300	Cl2—O9	1.376 (6)
C9—H9	0.9300	Cl2—O8	1.381 (7)
N7—C10	1.332 (6)	Cl3—O12	1.273 (7)
N7—C12	1.379 (6)	Cl3—O14	1.278 (9)
C10—N8	1.341 (6)	Cl3—O13	1.330 (11)
N8—C11	1.359 (7)	Cl3—O11	1.344 (12)
N8—H8N	0.8600	Cl4A—O17	1.360 (6)
C11—C12	1.360 (7)	Cl4A—O18	1.367 (6)
C11—H11	0.9300	Cl4A—O15A	1.449 (8)
C12—H12	0.9300	Cl4A—O16	1.532 (8)
N9—C13	1.330 (6)	Cl4B—O16	1.173 (8)
N9—C15	1.364 (6)	Cl4B—O15B	1.34 (2)
C13—N10	1.334 (7)	Cl4B—O18	1.529 (9)
C13—C16	1.440 (8)	Cl4B—O17	1.574 (11)
N10—C14	1.370 (8)
O20···O11	2.790 (18)	O18···O22^ii	2.770 (8)
O22···O1	2.744 (6)	O23···O7^ii	3.070 (12)
O23···O2	2.678 (8)	O21···O15B^iii	3.193 (18)
O19···O7^i	2.916 (9)	O22···O12^iv	3.177 (14)
O19···O8^i	3.146 (11)	O21···O4^v	3.291 (13)
O19···O5^i	3.018 (9)	O23···O5^v	3.173 (12)
O20···O21^i	3.100 (10)	O23···O4^v	3.281 (15)
O20···O8^i	3.131 (12)
N7—Rh1—N1	173.08 (14)	C15—N9—Rh2	139.8 (4)
N7—Rh1—N5	79.53 (15)	N9—C13—N10	110.3 (5)
N1—Rh1—N5	100.15 (15)	N9—C13—C16	116.2 (4)
N7—Rh1—N3	99.95 (15)	N10—C13—C16	133.5 (5)
N1—Rh1—N3	79.78 (15)	C13—N10—C14	107.8 (5)
N5—Rh1—N3	175.18 (13)	C13—N10—H10N	126.1
N7—Rh1—O1	88.46 (14)	C14—N10—H10N	126.1
N1—Rh1—O1	84.62 (14)	C15—C14—N10	106.2 (5)
N5—Rh1—O1	86.72 (12)	C15—C14—H14	126.9
N3—Rh1—O1	88.48 (13)	N10—C14—H14	126.9
N7—Rh1—Rh2	93.23 (10)	C14—C15—N9	109.3 (5)
N1—Rh1—Rh2	93.69 (10)	C14—C15—H15	125.3
N5—Rh1—Rh2	91.67 (9)	N9—C15—H15	125.3
N3—Rh1—Rh2	93.14 (10)	C16—N11—C18	106.3 (4)
O1—Rh1—Rh2	177.42 (10)	C16—N11—Rh2	113.5 (3)
N13—Rh2—N11	174.14 (14)	C18—N11—Rh2	140.1 (4)
N13—Rh2—N9	99.67 (16)	N11—C16—N12	110.3 (5)
N11—Rh2—N9	79.56 (17)	N11—C16—C13	116.9 (4)
N13—Rh2—N15	79.41 (16)	N12—C16—C13	132.8 (5)
N11—Rh2—N15	100.95 (17)	C16—N12—C17	107.7 (5)
N9—Rh2—N15	176.01 (14)	C16—N12—H12N	126.1
N13—Rh2—O2	87.62 (16)	C17—N12—H12N	126.1
N11—Rh2—O2	86.54 (16)	N12—C17—C18	107.6 (5)
N9—Rh2—O2	88.12 (16)	N12—C17—H17	126.2
N15—Rh2—O2	87.96 (16)	C18—C17—H17	126.2
N13—Rh2—Rh1	93.64 (9)	C17—C18—N11	108.1 (5)
N11—Rh2—Rh1	92.20 (10)	C17—C18—H18	126.0
N9—Rh2—Rh1	91.82 (10)	N11—C18—H18	126.0
N15—Rh2—Rh1	92.11 (10)	C19—N13—C21	105.5 (4)
O2—Rh2—Rh1	178.73 (13)	C19—N13—Rh2	113.3 (3)
C1—N1—C3	106.6 (4)	C21—N13—Rh2	140.5 (3)
C1—N1—Rh1	113.2 (3)	N13—C19—N14	111.0 (5)
C3—N1—Rh1	139.9 (3)	N13—C19—C22	117.0 (4)
N1—C1—N2	110.3 (5)	N14—C19—C22	132.0 (5)
N1—C1—C4	116.7 (4)	C19—N14—C20	107.1 (5)
N2—C1—C4	132.9 (5)	C19—N14—H14N	126.5
C1—N2—C2	108.6 (4)	C20—N14—H14N	126.5
C1—N2—H2N	125.7	C21—C20—N14	106.9 (5)
C2—N2—H2N	125.7	C21—C20—H20	126.5
N2—C2—C3	106.1 (5)	N14—C20—H20	126.5
N2—C2—H2	126.9	C20—C21—N13	109.5 (5)
C3—C2—H2	126.9	C20—C21—H21	125.3
N1—C3—C2	108.3 (5)	N13—C21—H21	125.3
N1—C3—H3	125.9	C22—N15—C24	106.2 (4)
C2—C3—H3	125.9	C22—N15—Rh2	113.4 (3)
C4—N3—C6	106.4 (4)	C24—N15—Rh2	140.0 (4)
C4—N3—Rh1	113.2 (3)	N16—C22—N15	111.2 (5)
C6—N3—Rh1	140.2 (3)	N16—C22—C19	132.4 (5)
N3—C4—N4	110.9 (4)	N15—C22—C19	116.4 (4)
N3—C4—C1	116.8 (4)	C22—N16—C23	107.1 (5)
N4—C4—C1	132.3 (5)	C22—N16—H16N	126.5
C4—N4—C5	107.3 (4)	C23—N16—H16N	126.5
C4—N4—H4N	126.3	C24—C23—N16	106.7 (5)
C5—N4—H4N	126.3	C24—C23—H23	126.6
N4—C5—C6	107.4 (5)	N16—C23—H23	126.6
N4—C5—H5	126.3	C23—C24—N15	108.8 (5)
C6—C5—H5	126.3	C23—C24—H24	125.6
C5—C6—N3	108.0 (5)	N15—C24—H24	125.6
C5—C6—H6	126.0	O6—Cl1—O4	109.8 (8)
N3—C6—H6	126.0	O6—Cl1—O5	108.1 (6)
C7—N5—C9	106.0 (4)	O4—Cl1—O5	108.5 (6)
C7—N5—Rh1	113.5 (3)	O6—Cl1—O3	111.1 (4)
C9—N5—Rh1	140.3 (3)	O4—Cl1—O3	106.6 (5)
N5—C7—N6	110.5 (4)	O5—Cl1—O3	112.6 (4)
N5—C7—C10	116.8 (4)	O10—Cl2—O7	110.8 (7)
N6—C7—C10	132.7 (4)	O10—Cl2—O9	104.2 (4)
C7—N6—C8	107.3 (4)	O7—Cl2—O9	117.5 (5)
C7—N6—H6N	126.3	O10—Cl2—O8	109.8 (8)
C8—N6—H6N	126.3	O7—Cl2—O8	104.3 (5)
C9—C8—N6	106.3 (4)	O9—Cl2—O8	110.2 (6)
C9—C8—H8	126.9	O12—Cl3—O14	120.9 (8)
N6—C8—H8	126.9	O12—Cl3—O13	102.8 (9)
C8—C9—N5	110.0 (4)	O14—Cl3—O13	113.1 (9)
C8—C9—H9	125.0	O12—Cl3—O11	113.8 (10)
N5—C9—H9	125.0	O14—Cl3—O11	100.8 (9)
C10—N7—C12	106.9 (4)	O13—Cl3—O11	104.6 (10)
C10—N7—Rh1	113.7 (3)	O17—Cl4A—O18	118.4 (4)
C12—N7—Rh1	138.9 (3)	O17—Cl4A—O15A	107.6 (5)
N7—C10—N8	110.2 (4)	O18—Cl4A—O15A	106.4 (5)
N7—C10—C7	116.2 (4)	O17—Cl4A—O16	108.2 (5)
N8—C10—C7	133.5 (4)	O18—Cl4A—O16	109.1 (4)
C10—N8—C11	107.5 (4)	O15A—Cl4A—O16	106.6 (4)
C10—N8—H8N	126.2	O16—Cl4B—O15B	117.3 (12)
C11—N8—H8N	126.2	O16—Cl4B—O18	121.4 (7)
N8—C11—C12	107.8 (5)	O15B—Cl4B—O18	99.1 (9)
N8—C11—H11	126.1	O16—Cl4B—O17	116.4 (7)
C12—C11—H11	126.1	O15B—Cl4B—O17	100.8 (9)
C11—C12—N7	107.6 (5)	O18—Cl4B—O17	98.0 (6)
C11—C12—H12	126.2	Cl4B—O16—Cl4A	35.2 (5)
N7—C12—H12	126.2	Cl4A—O17—Cl4B	34.2 (3)
C13—N9—C15	106.3 (4)	Cl4A—O18—Cl4B	35.1 (3)
C13—N9—Rh2	113.6 (3)
N7—Rh1—Rh2—N13	42.27 (15)	C12—N7—C10—C7	177.6 (4)
N1—Rh1—Rh2—N13	−137.62 (15)	Rh1—N7—C10—C7	4.7 (5)
N5—Rh1—Rh2—N13	−37.33 (15)	N5—C7—C10—N7	−1.2 (5)
N3—Rh1—Rh2—N13	142.43 (15)	N6—C7—C10—N7	−179.8 (4)
O1—Rh1—Rh2—N13	−89 (2)	N5—C7—C10—N8	176.7 (4)
N7—Rh1—Rh2—N11	−138.30 (16)	N6—C7—C10—N8	−2.0 (8)
N1—Rh1—Rh2—N11	41.81 (16)	N7—C10—N8—C11	0.9 (5)
N5—Rh1—Rh2—N11	142.10 (16)	C7—C10—N8—C11	−177.0 (5)
N3—Rh1—Rh2—N11	−38.13 (16)	C10—N8—C11—C12	−0.7 (6)
O1—Rh1—Rh2—N11	91 (2)	N8—C11—C12—N7	0.2 (6)
N7—Rh1—Rh2—N9	142.09 (16)	C10—N7—C12—C11	0.3 (6)
N1—Rh1—Rh2—N9	−37.81 (15)	Rh1—N7—C12—C11	170.3 (4)
N5—Rh1—Rh2—N9	62.48 (15)	N13—Rh2—N9—C13	−169.7 (3)
N3—Rh1—Rh2—N9	−117.75 (15)	N11—Rh2—N9—C13	4.4 (3)
O1—Rh1—Rh2—N9	11 (2)	N15—Rh2—N9—C13	−93 (2)
N7—Rh1—Rh2—N15	−37.25 (16)	O2—Rh2—N9—C13	−82.4 (3)
N1—Rh1—Rh2—N15	142.86 (15)	Rh1—Rh2—N9—C13	96.3 (3)
N5—Rh1—Rh2—N15	−116.85 (15)	N13—Rh2—N9—C15	2.8 (5)
N3—Rh1—Rh2—N15	62.91 (15)	N11—Rh2—N9—C15	176.9 (5)
O1—Rh1—Rh2—N15	−168 (2)	N15—Rh2—N9—C15	79 (2)
N7—Rh1—Rh2—O2	−131 (6)	O2—Rh2—N9—C15	90.1 (5)
N1—Rh1—Rh2—O2	49 (6)	Rh1—Rh2—N9—C15	−91.2 (5)
N5—Rh1—Rh2—O2	150 (6)	C15—N9—C13—N10	1.2 (6)
N3—Rh1—Rh2—O2	−31 (6)	Rh2—N9—C13—N10	176.1 (3)
O1—Rh1—Rh2—O2	98 (6)	C15—N9—C13—C16	−179.7 (4)
N7—Rh1—N1—C1	83.3 (13)	Rh2—N9—C13—C16	−4.7 (5)
N5—Rh1—N1—C1	170.0 (3)	N9—C13—N10—C14	−0.8 (6)
N3—Rh1—N1—C1	−5.1 (3)	C16—C13—N10—C14	−179.8 (5)
O1—Rh1—N1—C1	84.3 (3)	C13—N10—C14—C15	0.1 (6)
Rh2—Rh1—N1—C1	−97.6 (3)	N10—C14—C15—N9	0.6 (6)
N7—Rh1—N1—C3	−89.2 (13)	C13—N9—C15—C14	−1.1 (6)
N5—Rh1—N1—C3	−2.5 (5)	Rh2—N9—C15—C14	−174.0 (4)
N3—Rh1—N1—C3	−177.6 (5)	N13—Rh2—N11—C16	79.6 (16)
O1—Rh1—N1—C3	−88.2 (5)	N9—Rh2—N11—C16	−3.4 (3)
Rh2—Rh1—N1—C3	89.9 (5)	N15—Rh2—N11—C16	172.5 (3)
C3—N1—C1—N2	0.3 (6)	O2—Rh2—N11—C16	85.3 (3)
Rh1—N1—C1—N2	−174.6 (3)	Rh1—Rh2—N11—C16	−94.9 (3)
C3—N1—C1—C4	179.1 (4)	N13—Rh2—N11—C18	−95.4 (16)
Rh1—N1—C1—C4	4.1 (5)	N9—Rh2—N11—C18	−178.4 (5)
N1—C1—N2—C2	−0.5 (6)	N15—Rh2—N11—C18	−2.5 (5)
C4—C1—N2—C2	−179.0 (5)	O2—Rh2—N11—C18	−89.7 (5)
C1—N2—C2—C3	0.5 (7)	Rh1—Rh2—N11—C18	90.1 (5)
C1—N1—C3—C2	0.0 (6)	C18—N11—C16—N12	−1.2 (6)
Rh1—N1—C3—C2	172.8 (4)	Rh2—N11—C16—N12	−177.9 (3)
N2—C2—C3—N1	−0.3 (7)	C18—N11—C16—C13	178.7 (4)
N7—Rh1—N3—C4	−167.6 (3)	Rh2—N11—C16—C13	2.0 (5)
N1—Rh1—N3—C4	5.4 (3)	N9—C13—C16—N11	1.8 (7)
N5—Rh1—N3—C4	−84.2 (18)	N10—C13—C16—N11	−179.3 (5)
O1—Rh1—N3—C4	−79.4 (3)	N9—C13—C16—N12	−178.3 (5)
Rh2—Rh1—N3—C4	98.6 (3)	N10—C13—C16—N12	0.7 (10)
N7—Rh1—N3—C6	6.8 (5)	N11—C16—N12—C17	1.0 (6)
N1—Rh1—N3—C6	179.7 (5)	C13—C16—N12—C17	−178.9 (5)
N5—Rh1—N3—C6	90.1 (18)	C16—N12—C17—C18	−0.3 (6)
O1—Rh1—N3—C6	94.9 (5)	N12—C17—C18—N11	−0.4 (6)
Rh2—Rh1—N3—C6	−87.1 (5)	C16—N11—C18—C17	1.0 (5)
C6—N3—C4—N4	0.6 (5)	Rh2—N11—C18—C17	176.2 (4)
Rh1—N3—C4—N4	176.8 (3)	N11—Rh2—N13—C19	88.5 (16)
C6—N3—C4—C1	178.9 (4)	N9—Rh2—N13—C19	170.5 (3)
Rh1—N3—C4—C1	−4.9 (5)	N15—Rh2—N13—C19	−5.5 (3)
N1—C1—C4—N3	0.5 (6)	O2—Rh2—N13—C19	82.8 (3)
N2—C1—C4—N3	178.9 (5)	Rh1—Rh2—N13—C19	−97.0 (3)
N1—C1—C4—N4	178.4 (5)	N11—Rh2—N13—C21	−80.3 (17)
N2—C1—C4—N4	−3.2 (9)	N9—Rh2—N13—C21	1.7 (5)
N3—C4—N4—C5	−0.2 (6)	N15—Rh2—N13—C21	−174.4 (5)
C1—C4—N4—C5	−178.1 (5)	O2—Rh2—N13—C21	−86.0 (5)
C4—N4—C5—C6	−0.3 (6)	Rh1—Rh2—N13—C21	94.2 (5)
N4—C5—C6—N3	0.6 (6)	C21—N13—C19—N14	−0.8 (5)
C4—N3—C6—C5	−0.7 (5)	Rh2—N13—C19—N14	−173.4 (3)
Rh1—N3—C6—C5	−175.3 (4)	C21—N13—C19—C22	177.3 (4)
N7—Rh1—N5—C7	4.2 (3)	Rh2—N13—C19—C22	4.7 (5)
N1—Rh1—N5—C7	−168.8 (3)	N13—C19—N14—C20	0.5 (5)
N3—Rh1—N5—C7	−80.1 (18)	C22—C19—N14—C20	−177.2 (5)
O1—Rh1—N5—C7	−84.9 (3)	C19—N14—C20—C21	0.0 (6)
Rh2—Rh1—N5—C7	97.1 (3)	N14—C20—C21—N13	−0.5 (6)
N7—Rh1—N5—C9	177.6 (4)	C19—N13—C21—C20	0.8 (5)
N1—Rh1—N5—C9	4.6 (4)	Rh2—N13—C21—C20	170.2 (4)
N3—Rh1—N5—C9	93.3 (18)	N13—Rh2—N15—C22	5.7 (3)
O1—Rh1—N5—C9	88.5 (4)	N11—Rh2—N15—C22	−168.4 (3)
Rh2—Rh1—N5—C9	−89.5 (4)	N9—Rh2—N15—C22	−71 (2)
C9—N5—C7—N6	0.3 (4)	O2—Rh2—N15—C22	−82.3 (3)
Rh1—N5—C7—N6	176.0 (2)	Rh1—Rh2—N15—C22	99.0 (3)
C9—N5—C7—C10	−178.6 (3)	N13—Rh2—N15—C24	177.1 (5)
Rh1—N5—C7—C10	−3.0 (4)	N11—Rh2—N15—C24	3.1 (5)
N5—C7—N6—C8	−0.5 (5)	N9—Rh2—N15—C24	100 (2)
C10—C7—N6—C8	178.2 (4)	O2—Rh2—N15—C24	89.2 (5)
C7—N6—C8—C9	0.4 (5)	Rh1—Rh2—N15—C24	−89.6 (5)
N6—C8—C9—N5	−0.2 (5)	C24—N15—C22—N16	1.4 (5)
C7—N5—C9—C8	−0.1 (5)	Rh2—N15—C22—N16	175.7 (3)
Rh1—N5—C9—C8	−173.8 (3)	C24—N15—C22—C19	−179.3 (4)
N1—Rh1—N7—C10	83.2 (13)	Rh2—N15—C22—C19	−5.0 (5)
N5—Rh1—N7—C10	−4.8 (3)	N13—C19—C22—N16	179.4 (5)
N3—Rh1—N7—C10	170.3 (3)	N14—C19—C22—N16	−3.0 (9)
O1—Rh1—N7—C10	82.1 (3)	N13—C19—C22—N15	0.2 (6)
Rh2—Rh1—N7—C10	−95.9 (3)	N14—C19—C22—N15	177.8 (5)
N1—Rh1—N7—C12	−86.3 (13)	N15—C22—N16—C23	−1.1 (6)
N5—Rh1—N7—C12	−174.3 (5)	C19—C22—N16—C23	179.7 (5)
N3—Rh1—N7—C12	0.8 (5)	C22—N16—C23—C24	0.4 (6)
O1—Rh1—N7—C12	−87.4 (5)	N16—C23—C24—N15	0.4 (6)
Rh2—Rh1—N7—C12	94.6 (5)	C22—N15—C24—C23	−1.1 (6)
C12—N7—C10—N8	−0.8 (5)	Rh2—N15—C24—C23	−172.9 (4)
Rh1—N7—C10—N8	−173.6 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O19	0.86	2.05	2.829 (7)	151
N4—H4N···O19	0.86	2.27	3.013 (7)	145
N4—H4N···O10^vi	0.86	2.52	3.104 (8)	126
N6—H6N···O3	0.86	2.27	3.038 (7)	149
N6—H6N···O1^vii	0.86	2.52	3.128 (5)	128
N8—H8N···O3	0.86	2.22	2.991 (7)	150
N8—H8N···O8	0.86	2.58	3.107 (8)	121
N10—H10N···O11	0.86	2.18	3.014 (13)	163
N12—H12N···O20	0.86	1.97	2.819 (8)	167
N14—H14N···O21	0.86	2.11	2.884 (8)	150
N16—H16N···O21	0.86	2.18	2.949 (8)	148

Symmetry codes: (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+1.

(III)

Crystal data

C26H32N16O2Rh2·4(ClO4)	Dx = 1.890 Mg m^−3
Mr = 1204.30	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pbcn	Cell parameters from 9792 reflections
a = 20.119 (5) Å	θ = 3.0–27.5°
b = 16.115 (4) Å	µ = 1.13 mm^−1
c = 13.055 (3) Å	T = 296 K
V = 4232.9 (17) Å^3	Prismatic, green
Z = 4	0.42 × 0.35 × 0.32 mm
F(000) = 2408

Data collection

Rigaku/MSC Mercury CCD diffractometer	4835 independent reflections
Radiation source: rotating-anode X-ray tube	4243 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.1°
ω scans	h = −26→25
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −20→20
Tmin = 0.740, Tmax = 0.803	l = −14→16
30878 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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.126	H atoms treated by a mixture of independent and constrained refinement
S = 1.16	w = 1/[σ^2(Fo^2) + (0.0552P)^2 + 4.7874P] where P = (Fo^2 + 2Fc^2)/3
4838 reflections	(Δ/σ)max = 0.001
302 parameters	Δρmax = 1.04 e Å^−3
1 restraint	Δρmin = −0.61 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	0.497490 (11)	0.271040 (16)	0.64762 (2)	0.03020 (11)
N1	0.59303 (14)	0.31328 (19)	0.6312 (2)	0.0338 (6)
C1	0.63709 (18)	0.2521 (2)	0.6151 (3)	0.0380 (8)
N2	0.69761 (15)	0.2844 (2)	0.5973 (3)	0.0477 (9)
H2N	0.7335	0.2569	0.5862	0.057*
C2	0.6918 (2)	0.3688 (3)	0.6000 (4)	0.0503 (10)
H2	0.7256	0.4073	0.5898	0.060*
C3	0.62670 (19)	0.3860 (3)	0.6206 (3)	0.0417 (9)
H3	0.6084	0.4387	0.6263	0.050*
N3	0.54734 (14)	0.16006 (18)	0.6369 (2)	0.0357 (7)
C4	0.61244 (18)	0.1688 (2)	0.6198 (3)	0.0386 (8)
N4	0.64145 (16)	0.0952 (2)	0.6080 (3)	0.0475 (8)
H4N	0.6830	0.0865	0.5969	0.057*
C5	0.5934 (2)	0.0364 (3)	0.6169 (4)	0.0520 (10)
H5	0.5992	−0.0207	0.6116	0.062*
C6	0.5351 (2)	0.0768 (2)	0.6348 (3)	0.0432 (9)
H6	0.4938	0.0518	0.6440	0.052*
N5	0.44682 (15)	0.38132 (19)	0.6460 (2)	0.0353 (7)
C7	0.38098 (18)	0.3726 (2)	0.6400 (3)	0.0369 (8)
N6	0.35148 (16)	0.4461 (2)	0.6299 (3)	0.0471 (8)
H6N	0.3094	0.4548	0.6254	0.057*
C8	0.4001 (2)	0.5049 (3)	0.6282 (4)	0.0504 (10)
H8	0.3940	0.5619	0.6216	0.061*
C9	0.4589 (2)	0.4646 (2)	0.6377 (3)	0.0429 (9)
H9	0.5006	0.4894	0.6385	0.052*
N7	0.40188 (15)	0.22891 (19)	0.6486 (2)	0.0353 (7)
C10	0.35631 (18)	0.2885 (3)	0.6435 (3)	0.0388 (8)
N8	0.29523 (16)	0.2558 (2)	0.6397 (3)	0.0453 (8)
H8N	0.2584	0.2829	0.6377	0.054*
C11	0.30196 (19)	0.1716 (3)	0.6396 (3)	0.0483 (10)
H11	0.2678	0.1327	0.6365	0.058*
C12	0.36819 (19)	0.1555 (3)	0.6448 (3)	0.0432 (9)
H12	0.3874	0.1030	0.6457	0.052*
O1	0.49253 (15)	0.2775 (2)	0.4713 (3)	0.0576 (8)
H1	0.4653 (19)	0.313 (2)	0.461 (4)	0.069*
C13	0.4931 (5)	0.2148 (6)	0.4038 (6)	0.161 (5)
H13	0.5125	0.1666	0.4351	0.242*
H13A	0.5189	0.2304	0.3449	0.242*
H13B	0.4484	0.2024	0.3830	0.242*
Cl1	0.83630 (5)	0.13164 (7)	0.64406 (9)	0.0534 (3)
O2	0.8199 (3)	0.1982 (4)	0.5815 (4)	0.142 (3)
O3	0.7906 (2)	0.0702 (4)	0.6377 (7)	0.189 (4)
O4	0.89949 (15)	0.1003 (2)	0.6126 (3)	0.0670 (9)
O5	0.8381 (3)	0.1616 (4)	0.7444 (3)	0.128 (2)
Cl2	0.16651 (6)	0.41641 (8)	0.65875 (11)	0.0644 (4)
O6	0.2100 (2)	0.4742 (3)	0.6073 (5)	0.133 (2)
O7	0.17426 (18)	0.3388 (2)	0.6079 (3)	0.0777 (11)
O8	0.1864 (3)	0.4092 (5)	0.7603 (4)	0.161 (3)
O9	0.10097 (16)	0.4456 (2)	0.6486 (3)	0.0785 (12)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.02584 (16)	0.03121 (17)	0.03355 (18)	0.00317 (10)	−0.00061 (10)	−0.00026 (11)
N1	0.0301 (14)	0.0357 (15)	0.0355 (17)	−0.0002 (12)	0.0006 (12)	0.0013 (13)
C1	0.0297 (17)	0.044 (2)	0.040 (2)	0.0057 (15)	0.0032 (16)	0.0006 (17)
N2	0.0302 (16)	0.058 (2)	0.055 (2)	0.0031 (14)	0.0065 (15)	0.0012 (17)
C2	0.044 (2)	0.053 (2)	0.054 (3)	−0.0092 (19)	0.0025 (19)	0.003 (2)
C3	0.0382 (19)	0.042 (2)	0.045 (2)	0.0005 (16)	0.0004 (17)	0.0030 (17)
N3	0.0319 (15)	0.0367 (15)	0.0386 (18)	0.0044 (12)	−0.0018 (12)	−0.0008 (13)
C4	0.0352 (18)	0.042 (2)	0.039 (2)	0.0054 (16)	0.0045 (15)	−0.0017 (16)
N4	0.0411 (17)	0.0464 (19)	0.055 (2)	0.0148 (15)	0.0071 (16)	−0.0017 (16)
C5	0.056 (2)	0.040 (2)	0.060 (3)	0.0080 (19)	0.004 (2)	0.000 (2)
C6	0.045 (2)	0.0354 (19)	0.049 (2)	0.0029 (16)	0.0010 (17)	0.0003 (17)
N5	0.0334 (15)	0.0373 (16)	0.0352 (17)	0.0059 (13)	−0.0016 (12)	0.0008 (13)
C7	0.0355 (18)	0.0396 (19)	0.036 (2)	0.0081 (15)	0.0000 (15)	−0.0037 (16)
N6	0.0407 (17)	0.0470 (19)	0.054 (2)	0.0168 (15)	−0.0052 (15)	−0.0008 (16)
C8	0.057 (2)	0.035 (2)	0.060 (3)	0.0108 (18)	−0.007 (2)	0.0002 (19)
C9	0.046 (2)	0.0375 (19)	0.046 (2)	0.0004 (17)	−0.0039 (17)	−0.0014 (17)
N7	0.0295 (15)	0.0398 (17)	0.0368 (18)	0.0027 (12)	−0.0029 (12)	−0.0020 (13)
C10	0.0276 (17)	0.052 (2)	0.036 (2)	0.0052 (16)	−0.0011 (14)	−0.0002 (17)
N8	0.0265 (15)	0.0531 (19)	0.056 (2)	0.0049 (14)	−0.0023 (14)	−0.0023 (16)
C11	0.0346 (19)	0.052 (2)	0.059 (3)	−0.0052 (17)	−0.0038 (17)	−0.001 (2)
C12	0.0386 (19)	0.0384 (19)	0.053 (3)	−0.0019 (16)	−0.0006 (17)	−0.0070 (17)
O1	0.0607 (19)	0.069 (2)	0.0430 (19)	0.0178 (15)	−0.0112 (15)	0.0015 (16)
C13	0.244 (13)	0.168 (9)	0.071 (5)	0.132 (8)	−0.051 (6)	−0.050 (5)
Cl1	0.0412 (5)	0.0613 (6)	0.0577 (7)	0.0131 (5)	0.0093 (5)	0.0090 (5)
O2	0.142 (4)	0.179 (5)	0.105 (4)	0.120 (4)	0.052 (3)	0.074 (4)
O3	0.062 (3)	0.129 (5)	0.375 (12)	−0.032 (3)	0.062 (4)	−0.073 (5)
O4	0.0462 (17)	0.063 (2)	0.092 (3)	0.0149 (15)	0.0173 (17)	0.0094 (18)
O5	0.122 (4)	0.193 (6)	0.068 (3)	0.064 (4)	0.005 (3)	−0.019 (3)
Cl2	0.0445 (6)	0.0644 (7)	0.0841 (9)	0.0197 (5)	−0.0173 (5)	−0.0218 (6)
O6	0.059 (2)	0.074 (3)	0.265 (7)	−0.006 (2)	−0.011 (3)	0.000 (4)
O7	0.070 (2)	0.066 (2)	0.097 (3)	0.0290 (18)	−0.018 (2)	−0.018 (2)
O8	0.166 (5)	0.220 (7)	0.096 (4)	0.102 (5)	−0.070 (4)	−0.064 (4)
O9	0.0445 (17)	0.078 (2)	0.114 (3)	0.0212 (17)	−0.0125 (18)	−0.020 (2)

Geometric parameters (Å, º)

Rh1—N7	2.040 (3)	N6—C8	1.362 (6)
Rh1—N5	2.049 (3)	N6—H6N	0.8600
Rh1—N1	2.050 (3)	C8—C9	1.357 (6)
Rh1—N3	2.055 (3)	C8—H8	0.9300
Rh1—O1	2.307 (4)	C9—H9	0.9300
Rh1—Rh1^i	2.6752 (9)	N7—C10	1.330 (5)
N1—C1	1.343 (5)	N7—C12	1.365 (5)
N1—C3	1.360 (5)	C10—N8	1.339 (5)
C1—N2	1.345 (5)	N8—C11	1.363 (5)
C1—C4	1.432 (5)	N8—H8N	0.8600
N2—C2	1.366 (5)	C11—C12	1.359 (5)
N2—H2N	0.8600	C11—H11	0.9300
C2—C3	1.364 (5)	C12—H12	0.9300
C2—H2	0.9300	O1—C13	1.341 (8)
C3—H3	0.9300	O1—H1	0.805 (19)
N3—C4	1.336 (5)	C13—H13	0.9600
N3—C6	1.365 (5)	C13—H13A	0.9600
C4—N4	1.331 (5)	C13—H13B	0.9600
N4—C5	1.359 (5)	Cl1—O3	1.354 (5)
N4—H4N	0.8600	Cl1—O2	1.389 (4)
C5—C6	1.362 (6)	Cl1—O5	1.396 (5)
C5—H5	0.9300	Cl1—O4	1.428 (3)
C6—H6	0.9300	Cl2—O8	1.389 (5)
N5—C7	1.334 (5)	Cl2—O9	1.406 (3)
N5—C9	1.368 (5)	Cl2—O7	1.424 (4)
C7—N6	1.330 (5)	Cl2—O6	1.443 (5)
C7—C10	1.444 (6)
N7—Rh1—N5	79.61 (12)	N6—C7—N5	110.8 (3)
N7—Rh1—N1	174.38 (12)	N6—C7—C10	133.2 (3)
N5—Rh1—N1	100.22 (12)	N5—C7—C10	116.0 (3)
N7—Rh1—N3	99.84 (12)	C7—N6—C8	107.5 (3)
N5—Rh1—N3	175.47 (12)	C7—N6—H6N	126.2
N1—Rh1—N3	79.88 (12)	C8—N6—H6N	126.2
N7—Rh1—O1	88.90 (12)	C9—C8—N6	106.9 (4)
N5—Rh1—O1	85.94 (11)	C9—C8—H8	126.5
N1—Rh1—O1	85.49 (12)	N6—C8—H8	126.5
N3—Rh1—O1	89.56 (12)	C8—C9—N5	108.8 (4)
N7—Rh1—Rh1^i	91.67 (9)	C8—C9—H9	125.6
N5—Rh1—Rh1^i	91.66 (8)	N5—C9—H9	125.6
N1—Rh1—Rh1^i	93.95 (9)	C10—N7—C12	106.4 (3)
N3—Rh1—Rh1^i	92.85 (9)	C10—N7—Rh1	114.2 (3)
O1—Rh1—Rh1^i	177.39 (8)	C12—N7—Rh1	139.2 (3)
C1—N1—C3	106.7 (3)	N7—C10—N8	110.5 (4)
C1—N1—Rh1	113.0 (2)	N7—C10—C7	116.3 (3)
C3—N1—Rh1	139.8 (3)	N8—C10—C7	133.2 (4)
N1—C1—N2	109.9 (3)	C10—N8—C11	107.6 (3)
N1—C1—C4	116.9 (3)	C10—N8—H8N	126.2
N2—C1—C4	133.2 (3)	C11—N8—H8N	126.2
C1—N2—C2	107.7 (3)	C12—C11—N8	106.7 (4)
C1—N2—H2N	126.2	C12—C11—H11	126.6
C2—N2—H2N	126.2	N8—C11—H11	126.6
C3—C2—N2	106.8 (4)	C11—C12—N7	108.8 (4)
C3—C2—H2	126.6	C11—C12—H12	125.6
N2—C2—H2	126.6	N7—C12—H12	125.6
N1—C3—C2	108.9 (4)	C13—O1—Rh1	128.4 (5)
N1—C3—H3	125.6	C13—O1—H1	116 (4)
C2—C3—H3	125.6	Rh1—O1—H1	103 (4)
C4—N3—C6	106.1 (3)	O1—C13—H13	109.5
C4—N3—Rh1	113.4 (2)	O1—C13—H13A	109.5
C6—N3—Rh1	140.2 (3)	H13—C13—H13A	109.5
N4—C4—N3	110.8 (3)	O1—C13—H13B	109.5
N4—C4—C1	132.7 (3)	H13—C13—H13B	109.5
N3—C4—C1	116.5 (3)	H13A—C13—H13B	109.5
C4—N4—C5	107.4 (3)	O3—Cl1—O2	111.6 (5)
C4—N4—H4N	126.3	O3—Cl1—O5	109.1 (4)
C5—N4—H4N	126.3	O2—Cl1—O5	106.9 (4)
N4—C5—C6	107.1 (4)	O3—Cl1—O4	109.1 (3)
N4—C5—H5	126.4	O2—Cl1—O4	108.4 (2)
C6—C5—H5	126.4	O5—Cl1—O4	111.6 (3)
C5—C6—N3	108.5 (4)	O8—Cl2—O9	112.8 (3)
C5—C6—H6	125.7	O8—Cl2—O7	109.9 (3)
N3—C6—H6	125.7	O9—Cl2—O7	110.6 (2)
C7—N5—C9	105.9 (3)	O8—Cl2—O6	108.8 (4)
C7—N5—Rh1	113.8 (2)	O9—Cl2—O6	108.0 (3)
C9—N5—Rh1	139.7 (3)	O7—Cl2—O6	106.5 (3)
N1—Rh1—Rh1^i—N5^i	40.76 (12)	N3—Rh1—N5—C7
N3—Rh1—Rh1^i—N7^i	41.15 (12)	O1—Rh1—N5—C7
N7—Rh1—N1—C1		Rh1—Rh1^i—N5—C7
N5—Rh1—N1—C1		N7—Rh1—N5—C9
N3—Rh1—N1—C1		N1—Rh1—N5—C9
O1—Rh1—N1—C1		N3—Rh1—N5—C9
Rh1—Rh1^i—N1—C1		O1—Rh1—N5—C9
N7—Rh1—N1—C3		Rh1—Rh1^i—N5—C9
N5—Rh1—N1—C3		C9—N5—C7—N6
N3—Rh1—N1—C3		Rh1—N5—C7—N6
O1—Rh1—N1—C3		C9—N5—C7—C10
Rh1—Rh1^i—N1—C3		Rh1—N5—C7—C10
C3—N1—C1—N2		N5—C7—N6—C8
Rh1—N1—C1—N2		C10—C7—N6—C8
C3—N1—C1—C4		C7—N6—C8—C9
Rh1—N1—C1—C4		N6—C8—C9—N5
N1—C1—N2—C2		C7—N5—C9—C8
C4—C1—N2—C2		Rh1—N5—C9—C8
C1—N2—C2—C3		N5—Rh1—N7—C10
C1—N1—C3—C2		N1—Rh1—N7—C10
Rh1—N1—C3—C2		N3—Rh1—N7—C10
N2—C2—C3—N1		O1—Rh1—N7—C10
N7—Rh1—N3—C4		Rh1—Rh1^i—N7—C10
N5—Rh1—N3—C4		N5—Rh1—N7—C12
N1—Rh1—N3—C4		N1—Rh1—N7—C12
O1—Rh1—N3—C4		N3—Rh1—N7—C12
Rh1—Rh1^i—N3—C4		O1—Rh1—N7—C12
N7—Rh1—N3—C6		Rh1—Rh1^i—N7—C12
N5—Rh1—N3—C6		C12—N7—C10—N8
N1—Rh1—N3—C6		Rh1—N7—C10—N8
O1—Rh1—N3—C6		C12—N7—C10—C7
Rh1—Rh1^i—N3—C6		Rh1—N7—C10—C7
C6—N3—C4—N4		N6—C7—C10—N7
Rh1—N3—C4—N4		N5—C7—C10—N7
C6—N3—C4—C1		N6—C7—C10—N8
Rh1—N3—C4—C1		N5—C7—C10—N8
N1—C1—C4—N4		N7—C10—N8—C11
N2—C1—C4—N4		C7—C10—N8—C11
N1—C1—C4—N3		C10—N8—C11—C12
N2—C1—C4—N3		N8—C11—C12—N7
N3—C4—N4—C5		C10—N7—C12—C11
C1—C4—N4—C5		Rh1—N7—C12—C11
C4—N4—C5—C6		N7—Rh1—O1—C13
N4—C5—C6—N3		N5—Rh1—O1—C13
C4—N3—C6—C5		N1—Rh1—O1—C13
Rh1—N3—C6—C5		N3—Rh1—O1—C13
N7—Rh1—N5—C7		Rh1—Rh1^i—O1—C13
N1—Rh1—N5—C7

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O2	0.86	1.98	2.833 (5)	172
N4—H4N···O3	0.86	2.25	3.053 (6)	156
N6—H6N···O6	0.86	2.04	2.897 (5)	177
N8—H8N···O7	0.86	1.96	2.808 (5)	170
O1—H1···O4^ii	0.81 (2)	2.15 (2)	2.929 (4)	163 (5)

Symmetry code: (ii) x−1/2, −y+1/2, −z+1.

(IV)

Crystal data

C30H38N18O2Rh2·4(BF4)	F(000) = 2456
Mr = 1235.84	Dx = 1.754 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
a = 16.073 (10) Å	Cell parameters from 4208 reflections
b = 19.104 (11) Å	θ = 3.0–27.5°
c = 16.399 (10) Å	µ = 0.82 mm^−1
β = 111.673 (6)°	T = 296 K
V = 4679 (5) Å^3	Prismatic, green
Z = 4	0.47 × 0.38 × 0.23 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer	5356 independent reflections
Radiation source: rotating-anode X-ray tube	3475 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.056
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.0°
ω scans	h = −20→20
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −22→24
Tmin = 0.765, Tmax = 0.891	l = −20→21
17721 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)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.213	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.1143P)^2 + 8.0854P] where P = (Fo^2 + 2Fc^2)/3
5356 reflections	(Δ/σ)max < 0.001
392 parameters	Δρmax = 2.60 e Å^−3
474 restraints	Δρmin = −0.94 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	Occ. (<1)
Rh1	0.41335 (3)	0.249529 (18)	0.23305 (3)	0.03572 (19)
N1	0.4147 (3)	0.1473 (2)	0.2727 (3)	0.0445 (10)
C1	0.3907 (4)	0.1019 (3)	0.2065 (4)	0.0484 (13)
N2	0.3880 (4)	0.0366 (3)	0.2348 (4)	0.0600 (14)
H2N	0.3739	−0.0006	0.2031	0.072*
C2	0.4115 (5)	0.0404 (3)	0.3226 (4)	0.0667 (18)
H2	0.4163	0.0031	0.3605	0.080*
C3	0.4269 (4)	0.1089 (3)	0.3455 (4)	0.0547 (15)
H3	0.4432	0.1265	0.4022	0.066*
N3	0.3833 (3)	0.1988 (2)	0.1155 (3)	0.0461 (10)
C4	0.3711 (4)	0.1304 (3)	0.1198 (4)	0.0491 (13)
N4	0.3405 (3)	0.1017 (3)	0.0403 (3)	0.0596 (13)
H4N	0.3281	0.0582	0.0281	0.071*
C5	0.3327 (4)	0.1545 (4)	−0.0182 (4)	0.0645 (17)
H5	0.3131	0.1502	−0.0789	0.077*
C6	0.3589 (4)	0.2139 (3)	0.0285 (4)	0.0576 (15)
H6	0.3601	0.2581	0.0052	0.069*
N5	0.4278 (3)	0.2999 (2)	0.3473 (3)	0.0448 (10)
C7	0.4072 (4)	0.3678 (3)	0.3355 (4)	0.0482 (13)
N6	0.4012 (4)	0.3952 (3)	0.4078 (3)	0.0696 (16)
H6N	0.3886	0.4380	0.4148	0.084*
C8	0.4183 (5)	0.3433 (4)	0.4682 (4)	0.075 (2)
H8	0.4197	0.3476	0.5252	0.090*
C9	0.4330 (4)	0.2843 (3)	0.4305 (4)	0.0551 (14)
H9	0.4447	0.2404	0.4566	0.066*
N7	0.4008 (3)	0.3510 (2)	0.1913 (3)	0.0442 (10)
C10	0.3940 (4)	0.3959 (3)	0.2500 (4)	0.0494 (13)
N8	0.3768 (5)	0.4606 (3)	0.2165 (4)	0.0656 (15)
H8N	0.3695	0.4976	0.2431	0.079*
C11	0.3732 (5)	0.4568 (3)	0.1329 (4)	0.0699 (19)
H11	0.3625	0.4938	0.0935	0.084*
C12	0.3880 (4)	0.3886 (3)	0.1169 (4)	0.0517 (14)
H12	0.3892	0.3710	0.0645	0.062*
O1	0.2648 (3)	0.2572 (2)	0.2061 (3)	0.0508 (11)
C13	0.2404 (4)	0.2318 (4)	0.2615 (5)	0.0620 (17)
H13	0.2794	0.2013	0.3020	0.074*
N9	0.1626 (4)	0.2445 (3)	0.2685 (5)	0.0694 (18)
C14	0.1026 (7)	0.2945 (7)	0.2105 (7)	0.133 (5)
H14	0.1353	0.3358	0.2074	0.200*
H14A	0.0567	0.3066	0.2324	0.200*
H14B	0.0756	0.2745	0.1530	0.200*
C15	0.1370 (6)	0.2101 (6)	0.3350 (6)	0.102 (3)
H15	0.1793	0.1738	0.3628	0.154*
H15A	0.0784	0.1900	0.3079	0.154*
H15B	0.1363	0.2438	0.3782	0.154*
B1	0.3728 (6)	0.5813 (4)	0.3763 (5)	0.084 (2)
F1	0.3661 (4)	0.6447 (2)	0.4079 (3)	0.119 (2)
F2A	0.3234 (11)	0.5794 (7)	0.2867 (6)	0.097 (5)	0.54 (3)
F3A	0.4522 (8)	0.5549 (8)	0.3920 (12)	0.135 (6)	0.54 (3)
F4A	0.3269 (15)	0.5346 (6)	0.4113 (12)	0.135 (6)	0.54 (3)
F2B	0.3065 (11)	0.5591 (12)	0.3080 (13)	0.138 (8)	0.46 (3)
F3B	0.4468 (12)	0.5868 (13)	0.3499 (17)	0.162 (8)	0.46 (3)
F4B	0.399 (3)	0.5367 (7)	0.4449 (9)	0.159 (10)	0.46 (3)
B2A	0.3488 (12)	−0.0920 (9)	0.0443 (9)	0.116 (6)	0.421 (17)
B2B	0.3638 (10)	−0.0916 (7)	0.0493 (8)	0.118 (5)	0.579 (17)
F5	0.3608 (7)	−0.0812 (4)	0.1280 (4)	0.204 (4)
F6A	0.2633 (11)	−0.1049 (16)	−0.0042 (11)	0.216 (11)	0.421 (17)
F7A	0.3754 (16)	−0.0348 (8)	0.0129 (11)	0.149 (8)	0.421 (17)
F8A	0.3993 (17)	−0.1463 (9)	0.0386 (12)	0.149 (9)	0.421 (17)
F6B	0.4504 (8)	−0.0890 (11)	0.0576 (10)	0.202 (8)	0.579 (17)
F7B	0.3295 (13)	−0.1534 (6)	0.0162 (9)	0.167 (8)	0.579 (17)
F8B	0.3172 (11)	−0.0413 (7)	−0.0046 (9)	0.176 (7)	0.579 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0436 (3)	0.0330 (3)	0.0329 (3)	−0.00020 (14)	0.0169 (2)	0.00079 (13)
N1	0.059 (3)	0.031 (2)	0.045 (2)	−0.0035 (19)	0.021 (2)	0.0014 (18)
C1	0.058 (3)	0.035 (3)	0.057 (3)	−0.005 (2)	0.027 (3)	0.003 (2)
N2	0.087 (4)	0.031 (3)	0.067 (3)	−0.008 (2)	0.034 (3)	−0.002 (2)
C2	0.094 (5)	0.041 (3)	0.070 (4)	−0.001 (3)	0.036 (4)	0.013 (3)
C3	0.064 (3)	0.059 (4)	0.045 (3)	−0.005 (3)	0.025 (3)	0.006 (3)
N3	0.053 (2)	0.043 (3)	0.042 (2)	0.0028 (19)	0.018 (2)	−0.0011 (19)
C4	0.062 (3)	0.039 (3)	0.046 (3)	−0.003 (2)	0.020 (3)	−0.005 (2)
N4	0.077 (3)	0.046 (3)	0.049 (3)	−0.007 (2)	0.016 (2)	−0.010 (2)
C5	0.084 (4)	0.068 (4)	0.045 (3)	−0.008 (3)	0.026 (3)	−0.009 (3)
C6	0.080 (4)	0.050 (4)	0.049 (3)	−0.001 (3)	0.030 (3)	0.006 (3)
N5	0.055 (2)	0.041 (2)	0.041 (2)	0.0014 (19)	0.022 (2)	0.0005 (18)
C7	0.064 (3)	0.043 (3)	0.042 (3)	0.005 (3)	0.025 (3)	0.001 (2)
N6	0.115 (5)	0.052 (3)	0.057 (3)	0.008 (3)	0.049 (3)	−0.006 (2)
C8	0.116 (6)	0.067 (5)	0.053 (4)	0.006 (4)	0.044 (4)	0.000 (3)
C9	0.073 (4)	0.054 (4)	0.048 (3)	−0.003 (3)	0.034 (3)	0.001 (3)
N7	0.055 (2)	0.039 (2)	0.038 (2)	−0.0002 (19)	0.0163 (19)	0.0001 (18)
C10	0.067 (3)	0.034 (3)	0.050 (3)	0.004 (2)	0.025 (3)	−0.003 (2)
N8	0.115 (5)	0.028 (3)	0.056 (3)	0.012 (3)	0.034 (3)	0.006 (2)
C11	0.112 (6)	0.043 (4)	0.057 (4)	0.010 (3)	0.032 (4)	0.010 (3)
C12	0.069 (4)	0.046 (3)	0.039 (3)	0.004 (3)	0.018 (3)	0.007 (2)
O1	0.052 (2)	0.057 (3)	0.052 (3)	−0.0021 (16)	0.030 (2)	0.0060 (17)
C13	0.051 (3)	0.070 (4)	0.064 (4)	0.003 (3)	0.020 (3)	0.000 (3)
N9	0.066 (4)	0.093 (5)	0.070 (4)	0.006 (3)	0.049 (3)	0.015 (3)
C14	0.096 (6)	0.196 (13)	0.131 (9)	0.061 (8)	0.069 (7)	0.075 (9)
C15	0.106 (6)	0.124 (8)	0.104 (6)	0.009 (6)	0.070 (6)	0.026 (6)
B1	0.125 (6)	0.065 (5)	0.059 (4)	0.031 (5)	0.029 (4)	−0.009 (3)
F1	0.190 (5)	0.070 (3)	0.084 (3)	0.045 (3)	0.033 (3)	−0.010 (2)
F2A	0.144 (11)	0.071 (6)	0.065 (5)	0.021 (6)	0.026 (5)	−0.003 (4)
F3A	0.124 (7)	0.107 (11)	0.141 (13)	0.045 (7)	0.012 (7)	−0.043 (10)
F4A	0.207 (15)	0.101 (7)	0.114 (11)	0.026 (8)	0.077 (11)	0.021 (7)
F2B	0.096 (8)	0.176 (18)	0.130 (11)	0.011 (10)	0.027 (9)	−0.077 (12)
F3B	0.126 (10)	0.23 (2)	0.143 (16)	0.007 (11)	0.067 (11)	−0.048 (13)
F4B	0.31 (3)	0.066 (7)	0.087 (8)	0.068 (12)	0.062 (12)	0.000 (6)
B2A	0.173 (14)	0.068 (12)	0.114 (11)	−0.016 (11)	0.060 (13)	−0.041 (13)
B2B	0.193 (12)	0.062 (10)	0.097 (10)	−0.016 (10)	0.051 (12)	−0.014 (9)
F5	0.363 (11)	0.135 (6)	0.136 (5)	−0.021 (6)	0.118 (6)	−0.060 (4)
F6A	0.185 (14)	0.16 (2)	0.252 (19)	−0.056 (12)	0.026 (15)	−0.046 (16)
F7A	0.23 (2)	0.056 (8)	0.185 (16)	−0.011 (10)	0.106 (17)	−0.026 (9)
F8A	0.27 (2)	0.073 (10)	0.141 (15)	0.035 (14)	0.119 (16)	0.009 (10)
F6B	0.162 (9)	0.212 (19)	0.198 (14)	0.002 (10)	0.025 (9)	−0.054 (13)
F7B	0.261 (19)	0.065 (6)	0.140 (10)	−0.024 (9)	0.035 (13)	−0.046 (6)
F8B	0.218 (15)	0.074 (8)	0.171 (9)	0.021 (9)	−0.002 (11)	−0.013 (7)

Geometric parameters (Å, º)

Rh1—N7	2.041 (5)	N7—C12	1.364 (7)
Rh1—N5	2.042 (4)	C10—N8	1.339 (7)
Rh1—N3	2.049 (4)	N8—C11	1.353 (9)
Rh1—N1	2.057 (4)	N8—H8N	0.8600
Rh1—O1	2.266 (5)	C11—C12	1.366 (9)
Rh1—Rh1^i	2.6313 (18)	C11—H11	0.9300
N1—C1	1.331 (7)	C12—H12	0.9300
N1—C3	1.352 (7)	O1—C13	1.216 (9)
C1—N2	1.337 (7)	C13—N9	1.319 (9)
C1—C4	1.444 (8)	C13—H13	0.9300
N2—C2	1.350 (8)	N9—C14	1.439 (11)
N2—H2N	0.8600	N9—C15	1.458 (10)
C2—C3	1.358 (9)	C14—H14	0.9600
C2—H2	0.9300	C14—H14A	0.9600
C3—H3	0.9300	C14—H14B	0.9600
N3—C4	1.328 (7)	C15—H15	0.9600
N3—C6	1.363 (7)	C15—H15A	0.9600
C4—N4	1.331 (7)	C15—H15B	0.9600
N4—C5	1.365 (8)	B1—F2B	1.300 (11)
N4—H4N	0.8600	B1—F3A	1.306 (10)
C5—C6	1.348 (9)	B1—F1	1.338 (8)
C5—H5	0.9300	B1—F4B	1.349 (10)
C6—H6	0.9300	B1—F2A	1.389 (10)
N5—C7	1.336 (7)	B1—F4A	1.408 (11)
N5—C9	1.368 (7)	B1—F3B	1.412 (12)
C7—N6	1.332 (7)	B2A—F5	1.330 (13)
C7—C10	1.442 (8)	B2A—F6A	1.333 (14)
N6—C8	1.357 (8)	B2A—F8A	1.341 (14)
N6—H6N	0.8600	B2A—F7A	1.344 (14)
C8—C9	1.348 (9)	B2B—F5	1.324 (13)
C8—H8	0.9300	B2B—F7B	1.331 (13)
C9—H9	0.9300	B2B—F8B	1.333 (13)
N7—C10	1.324 (7)	B2B—F6B	1.350 (13)
N7—Rh1—N5	79.88 (18)	N5—C9—H9	125.7
N7—Rh1—N3	99.97 (18)	C10—N7—C12	106.4 (5)
N5—Rh1—N3	173.40 (17)	C10—N7—Rh1	113.3 (4)
N7—Rh1—N1	175.25 (17)	C12—N7—Rh1	139.9 (4)
N5—Rh1—N1	99.96 (18)	N7—C10—N8	111.1 (5)
N3—Rh1—N1	79.63 (18)	N7—C10—C7	116.3 (5)
N7—Rh1—O1	84.66 (16)	N8—C10—C7	132.5 (6)
N5—Rh1—O1	84.44 (17)	C10—N8—C11	106.9 (5)
N3—Rh1—O1	88.97 (17)	C10—N8—H8N	126.6
N1—Rh1—O1	90.60 (16)	C11—N8—H8N	126.6
N7—Rh1—Rh1^i	92.08 (13)	N8—C11—C12	107.5 (5)
N5—Rh1—Rh1^i	93.04 (13)	N8—C11—H11	126.3
N3—Rh1—Rh1^i	93.55 (13)	C12—C11—H11	126.3
N1—Rh1—Rh1^i	92.67 (13)	N7—C12—C11	108.1 (5)
O1—Rh1—Rh1^i	176.18 (10)	N7—C12—H12	125.9
C1—N1—C3	105.8 (5)	C11—C12—H12	125.9
C1—N1—Rh1	113.2 (4)	C13—O1—Rh1	115.8 (4)
C3—N1—Rh1	140.8 (4)	O1—C13—N9	124.7 (7)
N1—C1—N2	111.1 (5)	O1—C13—H13	117.7
N1—C1—C4	116.7 (5)	N9—C13—H13	117.7
N2—C1—C4	132.1 (6)	C13—N9—C14	119.4 (7)
C1—N2—C2	106.7 (5)	C13—N9—C15	121.4 (7)
C1—N2—H2N	126.6	C14—N9—C15	119.2 (7)
C2—N2—H2N	126.6	N9—C14—H14	109.5
N2—C2—C3	107.3 (5)	N9—C14—H14A	109.5
N2—C2—H2	126.3	H14—C14—H14A	109.5
C3—C2—H2	126.3	N9—C14—H14B	109.5
N1—C3—C2	109.0 (5)	H14—C14—H14B	109.5
N1—C3—H3	125.5	H14A—C14—H14B	109.5
C2—C3—H3	125.5	N9—C15—H15	109.5
C4—N3—C6	105.8 (5)	N9—C15—H15A	109.5
C4—N3—Rh1	113.7 (4)	H15—C15—H15A	109.5
C6—N3—Rh1	139.6 (4)	N9—C15—H15B	109.5
N3—C4—N4	111.2 (5)	H15—C15—H15B	109.5
N3—C4—C1	116.2 (5)	H15A—C15—H15B	109.5
N4—C4—C1	132.6 (6)	F2B—B1—F1	118.2 (10)
C4—N4—C5	106.8 (5)	F3A—B1—F1	119.1 (9)
C4—N4—H4N	126.6	F2B—B1—F4B	114.8 (11)
C5—N4—H4N	126.6	F1—B1—F4B	107.1 (7)
C6—C5—N4	107.1 (5)	F3A—B1—F2A	109.5 (9)
C6—C5—H5	126.5	F1—B1—F2A	109.7 (7)
N4—C5—H5	126.5	F3A—B1—F4A	107.2 (8)
C5—C6—N3	109.0 (6)	F1—B1—F4A	106.6 (8)
C5—C6—H6	125.5	F2A—B1—F4A	103.5 (9)
N3—C6—H6	125.5	F2B—B1—F3B	106.0 (10)
C7—N5—C9	106.1 (5)	F1—B1—F3B	104.4 (9)
C7—N5—Rh1	112.7 (3)	F4B—B1—F3B	105.0 (9)
C9—N5—Rh1	139.2 (4)	F5—B2A—F6A	111.6 (13)
N6—C7—N5	110.4 (5)	F5—B2A—F8A	109.3 (12)
N6—C7—C10	133.3 (6)	F6A—B2A—F8A	109.5 (13)
N5—C7—C10	116.3 (5)	F5—B2A—F7A	108.9 (12)
C7—N6—C8	107.5 (5)	F6A—B2A—F7A	109.0 (13)
C7—N6—H6N	126.2	F8A—B2A—F7A	108.4 (12)
C8—N6—H6N	126.2	F5—B2B—F7B	111.9 (12)
C9—C8—N6	107.4 (6)	F5—B2B—F8B	108.9 (12)
C9—C8—H8	126.3	F7B—B2B—F8B	108.8 (12)
N6—C8—H8	126.3	F5—B2B—F6B	107.7 (11)
C8—C9—N5	108.6 (6)	F7B—B2B—F6B	109.3 (12)
C8—C9—H9	125.7	F8B—B2B—F6B	110.2 (12)
N1—Rh1—Rh1^i—N3^i	−43.72 (18)	O1—Rh1—N5—C7	−74.8 (4)
N5—Rh1—Rh1^i—N7^i	−43.72 (17)	Rh1^i—Rh1—N5—C7	102.3 (4)
N7—Rh1—N1—C1	81 (2)	N7—Rh1—N5—C9	171.5 (6)
N5—Rh1—N1—C1	169.0 (4)	N3—Rh1—N5—C9	82.2 (16)
N3—Rh1—N1—C1	−4.3 (4)	N1—Rh1—N5—C9	−3.7 (6)
O1—Rh1—N1—C1	84.5 (4)	O1—Rh1—N5—C9	85.9 (6)
Rh1^i—Rh1—N1—C1	−97.4 (4)	Rh1^i—Rh1—N5—C9	−97.0 (6)
N7—Rh1—N1—C3	−93 (2)	C9—N5—C7—N6	1.2 (7)
N5—Rh1—N1—C3	−5.4 (7)	Rh1—N5—C7—N6	168.2 (4)
N3—Rh1—N1—C3	−178.7 (7)	C9—N5—C7—C10	−177.3 (5)
O1—Rh1—N1—C3	−89.8 (6)	Rh1—N5—C7—C10	−10.3 (7)
Rh1^i—Rh1—N1—C3	88.2 (6)	N5—C7—N6—C8	0.0 (8)
C3—N1—C1—N2	−0.4 (7)	C10—C7—N6—C8	178.1 (7)
Rh1—N1—C1—N2	−176.7 (4)	C7—N6—C8—C9	−1.2 (9)
C3—N1—C1—C4	178.4 (5)	N6—C8—C9—N5	1.9 (8)
Rh1—N1—C1—C4	2.1 (7)	C7—N5—C9—C8	−1.9 (7)
N1—C1—N2—C2	−0.3 (8)	Rh1—N5—C9—C8	−163.4 (5)
C4—C1—N2—C2	−178.8 (7)	N5—Rh1—N7—C10	−9.7 (4)
C1—N2—C2—C3	0.9 (8)	N3—Rh1—N7—C10	163.6 (4)
C1—N1—C3—C2	1.0 (7)	N1—Rh1—N7—C10	79 (2)
Rh1—N1—C3—C2	175.6 (5)	O1—Rh1—N7—C10	75.6 (4)
N2—C2—C3—N1	−1.2 (8)	Rh1^i—Rh1—N7—C10	−102.4 (4)
N7—Rh1—N3—C4	−169.1 (4)	N5—Rh1—N7—C12	179.1 (6)
N5—Rh1—N3—C4	−81.0 (15)	N3—Rh1—N7—C12	−7.5 (6)
N1—Rh1—N3—C4	6.1 (4)	N1—Rh1—N7—C12	−92 (2)
O1—Rh1—N3—C4	−84.7 (4)	O1—Rh1—N7—C12	−95.6 (6)
Rh1^i—Rh1—N3—C4	98.2 (4)	Rh1^i—Rh1—N7—C12	86.4 (6)
N7—Rh1—N3—C6	−1.4 (7)	C12—N7—C10—N8	0.4 (7)
N5—Rh1—N3—C6	86.7 (16)	Rh1—N7—C10—N8	−173.7 (4)
N1—Rh1—N3—C6	173.8 (7)	C12—N7—C10—C7	−178.7 (5)
O1—Rh1—N3—C6	83.0 (6)	Rh1—N7—C10—C7	7.2 (7)
Rh1^i—Rh1—N3—C6	−94.2 (6)	N6—C7—C10—N7	−175.9 (7)
C6—N3—C4—N4	0.2 (7)	N5—C7—C10—N7	2.1 (8)
Rh1—N3—C4—N4	171.9 (4)	N6—C7—C10—N8	5.1 (13)
C6—N3—C4—C1	−178.6 (5)	N5—C7—C10—N8	−176.8 (7)
Rh1—N3—C4—C1	−6.9 (7)	N7—C10—N8—C11	−0.5 (8)
N1—C1—C4—N3	3.2 (8)	C7—C10—N8—C11	178.5 (7)
N2—C1—C4—N3	−178.3 (6)	C10—N8—C11—C12	0.3 (9)
N1—C1—C4—N4	−175.2 (6)	C10—N7—C12—C11	−0.2 (7)
N2—C1—C4—N4	3.3 (12)	Rh1—N7—C12—C11	171.3 (5)
N3—C4—N4—C5	0.0 (7)	N8—C11—C12—N7	−0.1 (8)
C1—C4—N4—C5	178.5 (7)	N7—Rh1—O1—C13	−136.6 (5)
C4—N4—C5—C6	−0.2 (7)	N5—Rh1—O1—C13	−56.3 (5)
N4—C5—C6—N3	0.3 (8)	N3—Rh1—O1—C13	123.3 (5)
C4—N3—C6—C5	−0.3 (7)	N1—Rh1—O1—C13	43.7 (5)
Rh1—N3—C6—C5	−168.5 (5)	Rh1^i—Rh1—O1—C13	−105.3 (17)
N7—Rh1—N5—C7	10.7 (4)	Rh1—O1—C13—N9	163.8 (6)
N3—Rh1—N5—C7	−78.6 (15)	O1—C13—N9—C14	−3.6 (13)
N1—Rh1—N5—C7	−164.4 (4)	O1—C13—N9—C15	177.8 (8)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···F5	0.86	1.93	2.786 (8)	170
N4—H4N···F8B	0.86	1.97	2.818 (15)	171
N4—H4N···F7A	0.86	1.98	2.738 (17)	146
N6—H6N···F4B	0.86	1.94	2.773 (13)	163
N6—H6N···F4A	0.86	2.09	2.927 (16)	166
N6—H6N···F3A	0.86	2.54	3.19 (2)	134
N8—H8N···F2A	0.86	1.97	2.817 (15)	167
N8—H8N···F2B	0.86	2.08	2.884 (19)	155
N8—H8N···F3B	0.86	2.43	3.169 (19)	144
N8—H8N···F3A	0.86	2.56	3.227 (15)	136

(V)

Crystal data

C36H38N18Rh2·2(SiF6)·8(H2O)	Dx = 1.726 Mg m^−3
Mr = 1356.97	Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I4122	Cell parameters from 14243 reflections
a = 17.6300 (5) Å	θ = 3.0–27.5°
c = 16.8037 (6) Å	µ = 0.79 mm^−1
V = 5222.9 (3) Å^3	T = 296 K
Z = 4	Prismatic, red
F(000) = 2744	0.41 × 0.40 × 0.40 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer	3004 independent reflections
Radiation source: rotating-anode X-ray tube	2952 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
ω scans	h = −22→21
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −22→22
Tmin = 0.727, Tmax = 0.814	l = −14→21
20508 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.027	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.073	w = 1/[σ^2(Fo^2) + (0.0493P)^2 + 1.975P] where P = (Fo^2 + 2Fc^2)/3
S = 1.12	(Δ/σ)max = 0.001
3004 reflections	Δρmax = 0.80 e Å^−3
220 parameters	Δρmin = −0.36 e Å^−3
15 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.02 (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	Occ. (<1)
Rh1	0.445750 (10)	0.445750 (10)	0.0000	0.02735 (9)
N1	0.36851 (12)	0.51661 (12)	0.05284 (12)	0.0312 (4)
C1	0.36143 (16)	0.50496 (15)	0.13091 (16)	0.0367 (5)
N2	0.30158 (14)	0.54327 (15)	0.15982 (15)	0.0441 (5)
H2N	0.2866	0.5440	0.2085	0.053*
C2	0.26894 (16)	0.58083 (16)	0.09758 (19)	0.0423 (6)
H2	0.2263	0.6118	0.0999	0.051*
C3	0.31059 (14)	0.56455 (15)	0.03147 (18)	0.0365 (5)
H3	0.3014	0.5828	−0.0195	0.044*
N3	0.46441 (13)	0.42079 (13)	0.11796 (13)	0.0353 (4)
C4	0.41519 (17)	0.45467 (15)	0.16714 (15)	0.0387 (5)
N4	0.42891 (19)	0.43573 (15)	0.24257 (14)	0.0550 (6)
H4N	0.4047	0.4516	0.2838	0.066*
C5	0.4885 (2)	0.3865 (2)	0.2420 (2)	0.0606 (9)
H5	0.5104	0.3636	0.2863	0.073*
C6	0.5098 (2)	0.37689 (17)	0.16603 (18)	0.0465 (6)
H6	0.5490	0.3456	0.1487	0.056*
N5	0.35452 (13)	0.35452 (13)	0.0000	0.0423 (6)
C7	0.3687 (2)	0.2847 (3)	0.0156 (5)	0.124 (3)
H7	0.4187	0.2714	0.0266	0.148*
C8	0.3152 (3)	0.2287 (3)	0.0172 (6)	0.157 (4)
H8	0.3298	0.1796	0.0307	0.189*
C9	0.2425 (2)	0.2425 (2)	0.0000	0.0865 (19)
C10	0.1817 (3)	0.1817 (3)	0.0000	0.163 (6)
H10A	0.1340	0.2038	−0.0150	0.245*	0.50
H10B	0.1776	0.1602	0.0523	0.245*	0.50
H10C	0.1951	0.1427	−0.0373	0.245*	0.50
Si1	0.22790 (15)	0.54844 (14)	0.3697 (2)	0.0739 (10)	0.50
F1	0.1635 (7)	0.4809 (4)	0.3825 (6)	0.146 (4)	0.50
F2	0.2708 (7)	0.5186 (7)	0.4520 (4)	0.128 (4)	0.50
F3	0.2914 (7)	0.6168 (6)	0.3578 (7)	0.149 (4)	0.50
F4	0.2837 (6)	0.4894 (4)	0.3167 (4)	0.096 (2)	0.50
F5	0.1905 (6)	0.5772 (7)	0.2878 (4)	0.131 (3)	0.50
F6	0.1762 (6)	0.6065 (5)	0.4258 (5)	0.114 (3)	0.50
O1	0.34398 (18)	0.7500	0.1250	0.0542 (7)
O2	0.23366 (16)	0.73366 (16)	0.2500	0.0739 (10)
O4	0.4094 (13)	0.4941 (15)	0.5655 (11)	0.270 (11)	0.50
O3	0.4212 (10)	0.4807 (14)	0.3987 (10)	0.242 (10)	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.03114 (10)	0.03114 (10)	0.01978 (12)	0.00846 (8)	0.00059 (6)	−0.00059 (6)
N1	0.0344 (10)	0.0350 (10)	0.0241 (9)	0.0057 (8)	0.0019 (8)	−0.0024 (7)
C1	0.0447 (13)	0.0372 (12)	0.0282 (12)	0.0073 (11)	0.0093 (10)	−0.0024 (10)
N2	0.0462 (12)	0.0473 (13)	0.0388 (13)	0.0053 (10)	0.0173 (10)	−0.0091 (10)
C2	0.0355 (12)	0.0398 (13)	0.0517 (17)	0.0075 (10)	0.0066 (12)	−0.0097 (12)
C3	0.0339 (11)	0.0322 (12)	0.0434 (13)	0.0047 (9)	−0.0044 (10)	−0.0007 (10)
N3	0.0436 (11)	0.0369 (10)	0.0255 (10)	0.0085 (9)	0.0007 (8)	0.0007 (8)
C4	0.0529 (14)	0.0397 (13)	0.0234 (11)	0.0061 (11)	0.0068 (10)	0.0002 (10)
N4	0.0895 (19)	0.0537 (14)	0.0219 (10)	0.0183 (11)	0.0079 (12)	0.0059 (10)
C5	0.091 (2)	0.0585 (17)	0.0322 (16)	0.0159 (17)	−0.0100 (17)	0.0105 (15)
C6	0.0608 (18)	0.0420 (15)	0.0368 (14)	0.0142 (12)	−0.0055 (13)	0.0068 (12)
N5	0.0424 (9)	0.0424 (9)	0.0421 (16)	0.0122 (12)	0.0013 (11)	−0.0013 (11)
C7	0.0434 (18)	0.068 (3)	0.260 (9)	0.0111 (17)	0.022 (3)	0.080 (4)
C8	0.063 (2)	0.063 (2)	0.347 (13)	0.0024 (19)	0.011 (5)	0.086 (5)
C9	0.0553 (16)	0.0553 (16)	0.149 (6)	−0.006 (2)	0.008 (3)	−0.008 (3)
C10	0.087 (4)	0.087 (4)	0.316 (17)	−0.044 (4)	0.042 (8)	−0.042 (8)
Si1	0.115 (3)	0.0649 (11)	0.0414 (12)	−0.0008 (13)	0.028 (2)	0.0082 (11)
F1	0.207 (11)	0.115 (6)	0.116 (6)	−0.060 (7)	0.097 (8)	−0.005 (5)
F2	0.167 (10)	0.170 (10)	0.047 (4)	0.078 (8)	0.031 (5)	−0.001 (5)
F3	0.178 (10)	0.093 (5)	0.175 (12)	−0.025 (6)	0.051 (8)	0.005 (7)
F4	0.146 (7)	0.088 (4)	0.053 (4)	0.004 (5)	0.043 (4)	−0.001 (3)
F5	0.158 (8)	0.171 (8)	0.064 (4)	0.007 (6)	0.019 (4)	0.034 (5)
F6	0.158 (9)	0.103 (5)	0.079 (5)	0.051 (6)	0.021 (5)	−0.008 (4)
O1	0.0447 (16)	0.0604 (18)	0.0574 (18)	0.000	0.000	−0.0204 (14)
O2	0.0829 (16)	0.0829 (16)	0.0561 (19)	−0.0102 (19)	0.0072 (16)	−0.0072 (16)
O4	0.28 (2)	0.39 (3)	0.144 (14)	0.09 (2)	−0.007 (15)	−0.026 (18)
O3	0.173 (13)	0.39 (3)	0.158 (13)	0.105 (17)	0.023 (10)	−0.118 (15)

Geometric parameters (Å, º)

Rh1—N1^i	2.0502 (19)	C5—C6	1.342 (5)
Rh1—N1	2.0502 (18)	C5—H5	0.9300
Rh1—N3^i	2.057 (2)	C6—H6	0.9300
Rh1—N3	2.057 (2)	N5—C7^i	1.283 (4)
Rh1—N5	2.275 (3)	N5—C7	1.283 (4)
Rh1—Rh1^ii	2.7052 (5)	C7—C8	1.367 (7)
N1—C1	1.334 (3)	C7—H7	0.9300
N1—C3	1.373 (3)	C8—C9	1.337 (6)
C1—N2	1.344 (3)	C8—H8	0.9300
C1—C4	1.434 (4)	C9—C8^i	1.337 (6)
N2—C2	1.365 (4)	C9—C10	1.514 (8)
N2—H2N	0.8600	C10—H10A	0.9600
C2—C3	1.362 (4)	C10—H10B	0.9600
C2—H2	0.9300	C10—H10C	0.9600
C3—H3	0.9300	Si1—F5	1.607 (8)
N3—C4	1.339 (3)	Si1—F3	1.658 (10)
N3—C6	1.376 (3)	Si1—F1	1.659 (8)
C4—N4	1.333 (3)	Si1—F2	1.662 (8)
N4—C5	1.363 (5)	Si1—F6	1.664 (7)
N4—H4N	0.8600	Si1—F4	1.687 (7)
N1^i—Rh1—N1	175.55 (12)	C6—C5—N4	107.6 (3)
N1^i—Rh1—N3^i	79.59 (8)	C6—C5—H5	126.2
N1—Rh1—N3^i	100.24 (8)	N4—C5—H5	126.2
N1^i—Rh1—N3	100.24 (8)	C5—C6—N3	108.9 (3)
N1—Rh1—N3	79.59 (8)	C5—C6—H6	125.5
N3^i—Rh1—N3	175.62 (13)	N3—C6—H6	125.5
N1^i—Rh1—N5	87.78 (6)	C7^i—N5—C7	114.6 (5)
N1—Rh1—N5	87.78 (6)	C7^i—N5—Rh1	122.7 (2)
N3^i—Rh1—N5	87.81 (7)	C7—N5—Rh1	122.7 (2)
N3—Rh1—N5	87.81 (7)	N5—C7—C8	124.2 (4)
N1^i—Rh1—Rh1^ii	92.22 (6)	N5—C7—H7	117.9
N1—Rh1—Rh1^ii	92.23 (6)	C8—C7—H7	117.9
N3^i—Rh1—Rh1^ii	92.19 (7)	C9—C8—C7	121.8 (4)
N3—Rh1—Rh1^ii	92.19 (7)	C9—C8—H8	119.1
N5—Rh1—Rh1^ii	180.0	C7—C8—H8	119.1
C1—N1—C3	106.4 (2)	C8—C9—C8^i	113.3 (5)
C1—N1—Rh1	113.22 (16)	C8—C9—C10	123.3 (3)
C3—N1—Rh1	139.08 (18)	C8^i—C9—C10	123.3 (3)
N1—C1—N2	110.6 (3)	C9—C10—H10A	109.5
N1—C1—C4	116.8 (2)	C9—C10—H10B	109.5
N2—C1—C4	132.6 (3)	H10A—C10—H10B	109.5
C1—N2—C2	107.3 (2)	C9—C10—H10C	109.5
C1—N2—H2N	126.3	H10A—C10—H10C	109.5
C2—N2—H2N	126.3	H10B—C10—H10C	109.5
C3—C2—N2	107.2 (2)	F5—Si1—F3	86.8 (6)
C3—C2—H2	126.4	F5—Si1—F1	93.3 (6)
N2—C2—H2	126.4	F3—Si1—F1	179.1 (6)
C2—C3—N1	108.5 (2)	F5—Si1—F2	177.1 (5)
C2—C3—H3	125.8	F3—Si1—F2	91.3 (8)
N1—C3—H3	125.8	F1—Si1—F2	88.6 (7)
C4—N3—C6	105.4 (2)	F5—Si1—F6	93.8 (5)
C4—N3—Rh1	113.30 (17)	F3—Si1—F6	89.5 (6)
C6—N3—Rh1	141.2 (2)	F1—Si1—F6	89.6 (5)
N4—C4—N3	111.0 (3)	F2—Si1—F6	88.4 (4)
N4—C4—C1	132.7 (3)	F5—Si1—F4	89.0 (5)
N3—C4—C1	116.3 (2)	F3—Si1—F4	89.5 (5)
C4—N4—C5	107.0 (3)	F1—Si1—F4	91.4 (4)
C4—N4—H4N	126.5	F2—Si1—F4	88.8 (4)
C5—N4—H4N	126.5	F6—Si1—F4	177.0 (6)
N1—Rh1^ii—Rh1^ii—N3		Rh1^ii—Rh1—N3—C6	−86.0 (3)
N1^i—Rh1—N1—C1	79.98 (19)	C6—N3—C4—N4	1.6 (3)
N3^i—Rh1—N1—C1	167.35 (19)	Rh1—N3—C4—N4	179.0 (2)
N3—Rh1—N1—C1	−8.20 (19)	C6—N3—C4—C1	179.3 (3)
N5—Rh1—N1—C1	79.98 (19)	Rh1—N3—C4—C1	−3.3 (3)
Rh1^ii—Rh1—N1—C1	−100.02 (19)	N1—C1—C4—N4	173.2 (3)
N1^i—Rh1—N1—C3	−84.6 (3)	N2—C1—C4—N4	−8.7 (6)
N3^i—Rh1—N1—C3	2.7 (3)	N1—C1—C4—N3	−3.9 (4)
N3—Rh1—N1—C3	−172.8 (3)	N2—C1—C4—N3	174.2 (3)
N5—Rh1—N1—C3	−84.6 (3)	N3—C4—N4—C5	−1.2 (4)
Rh1^ii—Rh1—N1—C3	95.4 (3)	C1—C4—N4—C5	−178.4 (3)
C3—N1—C1—N2	0.1 (3)	C4—N4—C5—C6	0.3 (4)
Rh1—N1—C1—N2	−169.46 (19)	N4—C5—C6—N3	0.7 (4)
C3—N1—C1—C4	178.6 (2)	C4—N3—C6—C5	−1.4 (4)
Rh1—N1—C1—C4	9.0 (3)	Rh1—N3—C6—C5	−177.6 (3)
N1—C1—N2—C2	0.1 (3)	N1^i—Rh1—N5—C7^i	−140.2 (5)
C4—C1—N2—C2	−178.0 (3)	N1—Rh1—N5—C7^i	39.8 (5)
C1—N2—C2—C3	−0.3 (3)	N3^i—Rh1—N5—C7^i	−60.6 (5)
N2—C2—C3—N1	0.4 (3)	N3—Rh1—N5—C7^i	119.4 (5)
C1—N1—C3—C2	−0.3 (3)	Rh1^ii—Rh1—N5—C7^i	−165.9 (5)
Rh1—N1—C3—C2	165.0 (2)	N1^i—Rh1—N5—C7	39.8 (5)
N1^i—Rh1—N3—C4	−169.34 (19)	N1—Rh1—N5—C7	−140.2 (5)
N1—Rh1—N3—C4	6.14 (19)	N3^i—Rh1—N5—C7	119.4 (5)
N3^i—Rh1—N3—C4	−82.00 (19)	N3—Rh1—N5—C7	−60.6 (5)
N5—Rh1—N3—C4	−82.00 (19)	Rh1^ii—Rh1—N5—C7	14.1 (5)
Rh1^ii—Rh1—N3—C4	98.00 (19)	C7^i—N5—C7—C8	−0.9 (7)
N1^i—Rh1—N3—C6	6.6 (4)	Rh1—N5—C7—C8	179.1 (7)
N1—Rh1—N3—C6	−177.9 (4)	N5—C7—C8—C9	2.0 (14)
N3^i—Rh1—N3—C6	94.0 (3)	C7—C8—C9—C8^i	−0.9 (6)
N5—Rh1—N3—C6	94.0 (3)	C7—C8—C9—C10	179.1 (6)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···F2^iii	0.86	1.87	2.684 (7)	158
N2—H2N···F4	0.86	2.06	2.819 (8)	147
N2—H2N···F5	0.86	2.23	2.970 (10)	144
N2—H2N···F6^iii	0.86	2.33	3.004 (9)	136
N4—H4N···F1^iii	0.86	1.92	2.774 (7)	171
N4—H4N···F4	0.86	2.30	2.999 (9)	138
N4—H4N···O3	0.86	2.02	2.744 (14)	141

Symmetry code: (iii) −x+1/2, y, −z+3/4.

(VI)

Crystal data

C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O)	Dx = 1.777 Mg m^−3
Mr = 2692.69	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pbca	Cell parameters from 25234 reflections
a = 20.170 (2) Å	θ = 3.3–27.5°
b = 21.875 (3) Å	µ = 0.94 mm^−1
c = 22.541 (3) Å	T = 296 K
V = 9946 (2) Å^3	Prismatic, red
Z = 4	0.50 × 0.42 × 0.31 mm
F(000) = 5420

Data collection

Rigaku/MSC Mercury CCD diffractometer	11352 independent reflections
Radiation source: rotating-anode X-ray tube	10339 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
ω scans	h = −26→24
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −28→27
Tmin = 0.832, Tmax = 0.894	l = −22→29
71587 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)] = 0.059	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.180	H atoms treated by a mixture of independent and constrained refinement
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0782P)^2 + 29.1806P] where P = (Fo^2 + 2Fc^2)/3
11379 reflections	(Δ/σ)max = 0.002
712 parameters	Δρmax = 1.65 e Å^−3
12 restraints	Δρmin = −1.44 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	Occ. (<1)
Rh1	0.285008 (17)	0.702100 (16)	0.559554 (17)	0.03460 (12)
Rh2	0.376560 (16)	0.616341 (15)	0.534188 (16)	0.03148 (11)
N1	0.3360 (2)	0.76822 (18)	0.5135 (2)	0.0413 (9)
C1	0.3731 (3)	0.8043 (2)	0.5486 (3)	0.0506 (14)
N2	0.3990 (3)	0.8501 (2)	0.5177 (3)	0.0626 (14)
H2N	0.4239	0.8787	0.5315	0.075*
C2	0.3789 (3)	0.8436 (3)	0.4604 (4)	0.0656 (18)
H2	0.3902	0.8688	0.4287	0.079*
C3	0.3394 (3)	0.7937 (3)	0.4580 (3)	0.0545 (14)
H3	0.3180	0.7790	0.4243	0.065*
N3	0.3427 (2)	0.7378 (2)	0.6263 (2)	0.0458 (10)
C4	0.3773 (3)	0.7869 (3)	0.6097 (3)	0.0501 (13)
N4	0.4128 (3)	0.8083 (3)	0.6558 (3)	0.0730 (17)
H4N	0.4392	0.8392	0.6555	0.088*
C5	0.3990 (4)	0.7722 (4)	0.7025 (4)	0.079 (2)
H5	0.4164	0.7765	0.7405	0.095*
C6	0.3562 (4)	0.7291 (3)	0.6854 (3)	0.0631 (17)
H6	0.3387	0.6985	0.7093	0.076*
N5	0.2228 (2)	0.66996 (19)	0.4944 (2)	0.0429 (9)
C7	0.1756 (3)	0.6327 (2)	0.5148 (3)	0.0510 (14)
N6	0.1355 (3)	0.6166 (2)	0.4703 (3)	0.0705 (18)
H6N	0.1017	0.5927	0.4729	0.085*
C8	0.1569 (4)	0.6441 (3)	0.4209 (4)	0.0706 (19)
H8	0.1377	0.6409	0.3835	0.085*
C9	0.2110 (3)	0.6775 (3)	0.4346 (3)	0.0528 (14)
H9	0.2358	0.7012	0.4086	0.063*
N7	0.2288 (2)	0.6413 (2)	0.6074 (2)	0.0501 (11)
C10	0.1784 (3)	0.6188 (3)	0.5767 (4)	0.0589 (16)
N8	0.1395 (3)	0.5844 (3)	0.6119 (4)	0.080 (2)
H8N	0.1047	0.5645	0.6013	0.095*
C11	0.1657 (4)	0.5870 (4)	0.6673 (4)	0.085 (3)
H11	0.1486	0.5681	0.7009	0.102*
C12	0.2208 (4)	0.6218 (3)	0.6650 (3)	0.0684 (19)
H12	0.2485	0.6310	0.6967	0.082*
N9	0.4529 (2)	0.67712 (17)	0.5442 (2)	0.0386 (9)
C13	0.4819 (3)	0.6748 (2)	0.5972 (3)	0.0441 (11)
N10	0.5328 (2)	0.7140 (2)	0.5997 (3)	0.0558 (12)
H10N	0.5582	0.7205	0.6297	0.067*
C14	0.5368 (3)	0.7418 (3)	0.5457 (3)	0.0593 (15)
H14	0.5677	0.7712	0.5346	0.071*
C15	0.4883 (3)	0.7190 (2)	0.5112 (3)	0.0483 (12)
H15	0.4800	0.7296	0.4720	0.058*
N11	0.3992 (2)	0.60354 (19)	0.6218 (2)	0.0406 (9)
C16	0.4538 (3)	0.6336 (2)	0.6395 (2)	0.0442 (11)
N12	0.4687 (3)	0.6182 (2)	0.6952 (2)	0.0594 (13)
H12N	0.5012	0.6325	0.7156	0.071*
C17	0.4242 (4)	0.5764 (3)	0.7142 (3)	0.0635 (16)
H17	0.4233	0.5576	0.7512	0.076*
C18	0.3805 (3)	0.5670 (3)	0.6687 (3)	0.0530 (13)
H18	0.3445	0.5405	0.6693	0.064*
N13	0.3605 (2)	0.62420 (18)	0.44503 (19)	0.0384 (9)
C19	0.3217 (3)	0.5808 (2)	0.4229 (2)	0.0438 (11)
N14	0.3198 (3)	0.5833 (3)	0.3638 (2)	0.0680 (15)
H14N	0.2975	0.5598	0.3406	0.082*
C20	0.3604 (4)	0.6306 (3)	0.3470 (3)	0.0718 (19)
H20	0.3694	0.6429	0.3083	0.086*
C21	0.3847 (3)	0.6560 (3)	0.3971 (3)	0.0540 (13)
H21	0.4131	0.6894	0.3989	0.065*
N15	0.30583 (19)	0.54976 (18)	0.52193 (19)	0.0380 (8)
C22	0.2900 (3)	0.5411 (2)	0.4654 (2)	0.0432 (11)
N16	0.2459 (3)	0.4958 (2)	0.4603 (3)	0.0556 (12)
H16N	0.2284	0.4827	0.4280	0.067*
C23	0.2340 (3)	0.4744 (3)	0.5157 (3)	0.0571 (15)
H23	0.2058	0.4423	0.5255	0.069*
C24	0.2701 (3)	0.5075 (2)	0.5537 (3)	0.0481 (12)
H24	0.2709	0.5027	0.5947	0.058*
N17	0.2080 (2)	0.77348 (19)	0.5770 (2)	0.0437 (10)
C25	0.1788 (4)	0.7800 (3)	0.6296 (3)	0.0644 (17)
H25	0.1909	0.7545	0.6608	0.077*
C26	0.1309 (4)	0.8240 (4)	0.6385 (4)	0.085 (3)
H26	0.1119	0.8275	0.6759	0.102*
N18	0.1107 (3)	0.8616 (3)	0.5956 (3)	0.0786 (18)
C27	0.1400 (4)	0.8545 (3)	0.5440 (3)	0.0680 (18)
H27	0.1277	0.8799	0.5129	0.082*
C28	0.1882 (3)	0.8112 (3)	0.5342 (3)	0.0530 (13)
H28	0.2074	0.8082	0.4968	0.064*
N19	0.45273 (18)	0.54441 (17)	0.51296 (19)	0.0361 (8)
C29	0.4560 (3)	0.4916 (2)	0.5429 (2)	0.0421 (11)
H29	0.4258	0.4842	0.5732	0.051*
C30	0.4973 (2)	0.5519 (2)	0.4700 (2)	0.0406 (11)
H30	0.4968	0.5879	0.4480	0.049*
Cl1	0.2778 (2)	0.58238 (11)	0.19874 (16)	0.1522 (17)
O1	0.2233 (6)	0.5459 (5)	0.1986 (7)	0.218 (6)
O2	0.3269 (9)	0.5550 (5)	0.2311 (6)	0.286 (10)
O3	0.2965 (8)	0.5927 (6)	0.1370 (5)	0.235 (7)
O4	0.2651 (5)	0.6388 (4)	0.2261 (5)	0.164 (4)
Cl2	0.50273 (10)	0.69105 (11)	0.83968 (9)	0.0785 (5)
O5	0.4665 (8)	0.6378 (7)	0.8369 (5)	0.256 (9)
O6	0.5326 (4)	0.6946 (4)	0.8946 (3)	0.122 (3)
O7	0.4637 (8)	0.7368 (7)	0.8328 (5)	0.267 (9)
O8	0.5462 (3)	0.6853 (4)	0.7924 (3)	0.113 (2)
Cl3	0.64557 (13)	0.59097 (13)	0.63762 (11)	0.0989 (8)
O9	0.6837 (6)	0.6371 (5)	0.6036 (5)	0.188 (5)
O10	0.6148 (3)	0.6242 (4)	0.6822 (3)	0.117 (3)
O11	0.6952 (4)	0.5514 (3)	0.6597 (4)	0.124 (3)
O12	0.6029 (4)	0.5617 (5)	0.6002 (5)	0.161 (4)
Si1	0.0000	0.5000	0.5000	0.0809 (10)
F1	0.0061 (3)	0.5712 (3)	0.4753 (6)	0.196 (5)
F2	0.0731 (3)	0.4893 (3)	0.4715 (5)	0.172 (4)
F3	0.0333 (6)	0.5196 (6)	0.5631 (5)	0.243 (6)
O1W	0.3069 (5)	0.8489 (5)	0.3071 (4)	0.149 (3)
O2W	0.2339 (5)	0.7416 (4)	0.3008 (4)	0.145 (3)
O3W	0.5974 (4)	0.7635 (3)	0.7008 (3)	0.103 (2)
O4W	0.1611 (6)	0.4761 (5)	0.3607 (5)	0.191 (5)
O5W	0.5199 (19)	0.8690 (15)	0.701 (2)	0.15 (2)	0.26 (3)
O6W	0.6244 (17)	0.9272 (13)	0.7204 (11)	0.233 (12)	0.50
O7W	0.4936 (11)	0.9107 (10)	0.6510 (13)	0.303 (17)	0.74 (3)
O8W	0.4435 (18)	0.5109 (17)	0.2650 (18)	0.29 (3)	0.50 (4)
O9W	0.5150 (19)	0.5739 (16)	0.2977 (16)	0.20 (2)	0.35 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0332 (2)	0.03079 (19)	0.0399 (2)	0.00056 (13)	0.00202 (14)	−0.00012 (13)
Rh2	0.03014 (19)	0.02803 (18)	0.0363 (2)	−0.00111 (12)	0.00235 (13)	−0.00109 (13)
N1	0.038 (2)	0.034 (2)	0.052 (3)	−0.0003 (16)	0.0027 (18)	0.0032 (17)
C1	0.038 (3)	0.036 (3)	0.078 (4)	0.001 (2)	0.001 (3)	−0.007 (3)
N2	0.050 (3)	0.039 (2)	0.099 (5)	−0.008 (2)	0.010 (3)	−0.004 (3)
C2	0.069 (4)	0.045 (3)	0.083 (5)	0.002 (3)	0.018 (4)	0.015 (3)
C3	0.062 (4)	0.045 (3)	0.056 (3)	0.003 (3)	0.012 (3)	0.005 (2)
N3	0.047 (2)	0.042 (2)	0.049 (3)	0.0094 (18)	−0.0012 (19)	−0.0065 (19)
C4	0.045 (3)	0.042 (3)	0.063 (4)	0.003 (2)	−0.010 (2)	−0.013 (2)
N4	0.067 (4)	0.060 (3)	0.092 (5)	0.004 (3)	−0.023 (3)	−0.030 (3)
C5	0.092 (5)	0.084 (5)	0.061 (4)	0.023 (4)	−0.024 (4)	−0.024 (4)
C6	0.081 (4)	0.065 (4)	0.043 (3)	0.026 (3)	−0.004 (3)	−0.011 (3)
N5	0.036 (2)	0.038 (2)	0.055 (3)	0.0017 (16)	−0.0005 (18)	−0.0040 (18)
C7	0.032 (2)	0.040 (3)	0.081 (4)	−0.006 (2)	0.004 (3)	−0.009 (3)
N6	0.041 (3)	0.054 (3)	0.116 (6)	−0.010 (2)	−0.019 (3)	−0.010 (3)
C8	0.063 (4)	0.071 (4)	0.078 (5)	0.006 (3)	−0.025 (4)	−0.020 (4)
C9	0.050 (3)	0.054 (3)	0.054 (3)	0.004 (2)	−0.011 (2)	−0.007 (3)
N7	0.048 (2)	0.039 (2)	0.063 (3)	0.0046 (19)	0.019 (2)	0.007 (2)
C10	0.040 (3)	0.042 (3)	0.094 (5)	0.003 (2)	0.021 (3)	0.006 (3)
N8	0.061 (3)	0.056 (3)	0.122 (6)	−0.010 (3)	0.038 (4)	0.015 (4)
C11	0.086 (5)	0.067 (4)	0.104 (7)	0.008 (4)	0.049 (5)	0.031 (4)
C12	0.079 (5)	0.057 (4)	0.069 (4)	0.015 (3)	0.030 (4)	0.017 (3)
N9	0.037 (2)	0.0292 (18)	0.050 (2)	−0.0010 (15)	0.0033 (17)	−0.0020 (16)
C13	0.039 (2)	0.041 (3)	0.052 (3)	−0.001 (2)	−0.003 (2)	−0.005 (2)
N10	0.039 (2)	0.060 (3)	0.069 (3)	−0.012 (2)	−0.005 (2)	−0.013 (2)
C14	0.048 (3)	0.049 (3)	0.082 (4)	−0.013 (3)	0.007 (3)	−0.003 (3)
C15	0.039 (3)	0.042 (3)	0.063 (4)	−0.006 (2)	0.008 (2)	0.001 (2)
N11	0.040 (2)	0.037 (2)	0.045 (2)	0.0022 (16)	0.0006 (18)	−0.0015 (17)
C16	0.047 (3)	0.043 (3)	0.043 (3)	0.004 (2)	−0.004 (2)	−0.003 (2)
N12	0.063 (3)	0.066 (3)	0.049 (3)	0.002 (2)	−0.015 (2)	−0.002 (2)
C17	0.075 (4)	0.067 (4)	0.048 (3)	0.003 (3)	0.003 (3)	0.009 (3)
C18	0.063 (4)	0.053 (3)	0.044 (3)	0.004 (3)	0.002 (2)	0.003 (2)
N13	0.040 (2)	0.036 (2)	0.039 (2)	0.0014 (16)	0.0022 (17)	−0.0014 (16)
C19	0.049 (3)	0.041 (3)	0.042 (3)	0.002 (2)	0.000 (2)	−0.004 (2)
N14	0.090 (4)	0.069 (3)	0.044 (3)	−0.016 (3)	−0.004 (3)	−0.005 (2)
C20	0.101 (6)	0.073 (4)	0.042 (3)	−0.016 (4)	0.003 (3)	0.008 (3)
C21	0.060 (3)	0.053 (3)	0.049 (3)	−0.005 (3)	0.003 (3)	0.008 (3)
N15	0.0339 (19)	0.0321 (19)	0.048 (2)	−0.0005 (15)	0.0031 (17)	−0.0007 (16)
C22	0.042 (3)	0.039 (3)	0.049 (3)	−0.001 (2)	0.000 (2)	−0.009 (2)
N16	0.051 (3)	0.047 (3)	0.069 (3)	−0.014 (2)	−0.006 (2)	−0.011 (2)
C23	0.045 (3)	0.048 (3)	0.078 (4)	−0.012 (2)	0.006 (3)	−0.005 (3)
C24	0.046 (3)	0.038 (3)	0.060 (3)	−0.008 (2)	0.008 (2)	0.001 (2)
N17	0.042 (2)	0.037 (2)	0.052 (3)	0.0079 (17)	−0.0004 (19)	−0.0009 (19)
C25	0.075 (4)	0.058 (3)	0.060 (4)	0.026 (3)	0.009 (3)	0.005 (3)
C26	0.094 (6)	0.078 (5)	0.083 (6)	0.035 (4)	0.032 (4)	0.001 (4)
N18	0.080 (4)	0.069 (4)	0.087 (5)	0.032 (3)	0.010 (4)	0.001 (3)
C27	0.072 (4)	0.060 (4)	0.072 (5)	0.031 (3)	−0.007 (3)	0.007 (3)
C28	0.052 (3)	0.051 (3)	0.056 (3)	0.010 (3)	0.003 (3)	0.004 (3)
N19	0.0327 (19)	0.0295 (18)	0.046 (2)	0.0030 (14)	0.0027 (16)	−0.0020 (16)
C29	0.040 (2)	0.035 (2)	0.051 (3)	0.0040 (19)	0.013 (2)	0.006 (2)
C30	0.039 (2)	0.034 (2)	0.048 (3)	0.0020 (19)	0.011 (2)	0.005 (2)
Cl1	0.255 (4)	0.0656 (13)	0.136 (3)	−0.0206 (19)	−0.112 (3)	−0.0087 (14)
O1	0.217 (11)	0.174 (10)	0.265 (15)	−0.123 (9)	0.011 (10)	−0.057 (10)
O2	0.51 (3)	0.163 (10)	0.187 (12)	0.131 (13)	−0.222 (15)	−0.074 (8)
O3	0.354 (19)	0.247 (14)	0.103 (7)	−0.143 (14)	−0.059 (9)	−0.002 (8)
O4	0.209 (10)	0.094 (5)	0.189 (10)	0.003 (6)	−0.085 (8)	−0.050 (6)
Cl2	0.0714 (11)	0.1059 (15)	0.0583 (10)	0.0127 (10)	0.0067 (8)	−0.0187 (10)
O5	0.318 (16)	0.307 (16)	0.142 (9)	−0.220 (15)	0.070 (10)	−0.096 (10)
O6	0.122 (6)	0.182 (8)	0.063 (4)	0.004 (5)	−0.009 (4)	−0.032 (4)
O7	0.333 (17)	0.351 (18)	0.116 (8)	0.277 (16)	−0.003 (9)	−0.013 (9)
O8	0.102 (5)	0.170 (7)	0.066 (4)	0.001 (5)	0.024 (3)	−0.022 (4)
Cl3	0.0959 (15)	0.1162 (18)	0.0847 (15)	0.0401 (14)	−0.0151 (12)	−0.0281 (13)
O9	0.217 (11)	0.194 (10)	0.153 (9)	−0.046 (9)	0.044 (8)	0.065 (8)
O10	0.094 (5)	0.153 (7)	0.102 (5)	0.034 (4)	0.004 (4)	−0.049 (5)
O11	0.127 (6)	0.112 (5)	0.133 (6)	0.050 (5)	−0.030 (5)	−0.015 (5)
O12	0.122 (6)	0.186 (9)	0.175 (9)	0.015 (6)	−0.052 (6)	−0.092 (7)
Si1	0.0410 (12)	0.0498 (14)	0.152 (3)	−0.0023 (10)	0.0031 (16)	−0.0129 (17)
F1	0.077 (4)	0.065 (3)	0.447 (16)	0.011 (3)	0.063 (6)	0.026 (6)
F2	0.076 (4)	0.098 (4)	0.340 (12)	0.009 (3)	0.064 (5)	−0.018 (6)
F3	0.224 (11)	0.302 (15)	0.203 (10)	−0.066 (10)	−0.083 (9)	−0.075 (10)
O1W	0.178 (8)	0.165 (8)	0.104 (6)	−0.023 (7)	0.020 (6)	−0.039 (6)
O2W	0.134 (7)	0.139 (7)	0.163 (8)	0.026 (5)	0.050 (6)	0.014 (6)
O3W	0.120 (5)	0.104 (5)	0.086 (4)	−0.020 (4)	−0.016 (4)	−0.010 (4)
O4W	0.243 (12)	0.155 (8)	0.174 (9)	0.030 (8)	−0.116 (9)	−0.062 (7)
O5W	0.16 (3)	0.09 (2)	0.20 (4)	−0.02 (2)	−0.06 (3)	0.02 (2)
O6W	0.35 (3)	0.23 (2)	0.125 (15)	0.082 (19)	−0.004 (16)	−0.036 (15)
O7W	0.27 (2)	0.22 (2)	0.42 (4)	−0.156 (19)	−0.13 (2)	0.08 (2)
O8W	0.27 (3)	0.28 (3)	0.33 (4)	0.08 (2)	0.01 (2)	−0.01 (2)
O9W	0.22 (4)	0.18 (3)	0.19 (4)	−0.01 (3)	0.05 (3)	−0.03 (2)

Geometric parameters (Å, º)

Rh1—N7	2.053 (4)	N12—C17	1.354 (9)
Rh1—N1	2.056 (4)	N12—H12N	0.8600
Rh1—N3	2.056 (5)	C17—C18	1.367 (9)
Rh1—N5	2.056 (4)	C17—H17	0.9300
Rh1—N17	2.238 (4)	C18—H18	0.9300
Rh1—Rh2	2.6943 (5)	N13—C19	1.327 (7)
Rh2—N13	2.044 (4)	N13—C21	1.375 (7)
Rh2—N11	2.047 (4)	C19—N14	1.335 (7)
Rh2—N9	2.048 (4)	C19—C22	1.442 (8)
Rh2—N15	2.058 (4)	N14—C20	1.373 (9)
Rh2—N19	2.251 (4)	N14—H14N	0.8600
N1—C1	1.345 (7)	C20—C21	1.352 (9)
N1—C3	1.372 (7)	C20—H20	0.9300
C1—N2	1.327 (8)	C21—H21	0.9300
C1—C4	1.433 (9)	N15—C22	1.329 (7)
N2—C2	1.363 (10)	N15—C24	1.375 (7)
N2—H2N	0.8600	C22—N16	1.336 (7)
C2—C3	1.354 (9)	N16—C23	1.356 (9)
C2—H2	0.9300	N16—H16N	0.8600
C3—H3	0.9300	C23—C24	1.338 (8)
N3—C4	1.334 (7)	C23—H23	0.9300
N3—C6	1.375 (8)	C24—H24	0.9300
C4—N4	1.347 (8)	N17—C25	1.331 (8)
N4—C5	1.346 (11)	N17—C28	1.332 (7)
N4—H4N	0.8600	C25—C26	1.379 (9)
C5—C6	1.336 (11)	C25—H25	0.9300
C5—H5	0.9300	C26—N18	1.334 (10)
C6—H6	0.9300	C26—H26	0.9300
N5—C7	1.335 (7)	N18—C27	1.314 (10)
N5—C9	1.378 (8)	C27—C28	1.376 (8)
C7—N6	1.338 (8)	C27—H27	0.9300
C7—C10	1.429 (10)	C28—H28	0.9300
N6—C8	1.337 (10)	N19—C30	1.332 (6)
N6—H6N	0.8600	N19—C29	1.340 (6)
C8—C9	1.349 (9)	C29—C30^i	1.370 (7)
C8—H8	0.9300	C29—H29	0.9300
C9—H9	0.9300	C30—C29^i	1.370 (7)
N7—C10	1.325 (9)	C30—H30	0.9300
N7—C12	1.376 (8)	Cl1—O1	1.358 (9)
C10—N8	1.347 (8)	Cl1—O2	1.369 (11)
N8—C11	1.356 (12)	Cl1—O4	1.403 (8)
N8—H8N	0.8600	Cl1—O3	1.460 (12)
C11—C12	1.350 (11)	Cl2—O7	1.284 (9)
C11—H11	0.9300	Cl2—O5	1.376 (11)
C12—H12	0.9300	Cl2—O6	1.379 (7)
N9—C13	1.330 (7)	Cl2—O8	1.386 (6)
N9—C15	1.379 (7)	Cl3—O12	1.365 (8)
C13—N10	1.340 (7)	Cl3—O10	1.388 (6)
C13—C16	1.430 (8)	Cl3—O11	1.413 (7)
N10—C14	1.362 (9)	Cl3—O9	1.483 (9)
N10—H10N	0.8600	Si1—F2^ii	1.625 (6)
C14—C15	1.346 (9)	Si1—F2	1.625 (6)
C14—H14	0.9300	Si1—F3	1.631 (9)
C15—H15	0.9300	Si1—F3^ii	1.631 (9)
N11—C16	1.344 (7)	Si1—F1	1.660 (6)
N11—C18	1.379 (7)	Si1—F1^ii	1.660 (6)
C16—N12	1.334 (7)
N7—Rh1—N1	175.44 (17)	N9—C15—H15	125.9
N7—Rh1—N3	100.0 (2)	C16—N11—C18	106.2 (5)
N1—Rh1—N3	79.56 (18)	C16—N11—Rh2	113.8 (4)
N7—Rh1—N5	79.5 (2)	C18—N11—Rh2	139.4 (4)
N1—Rh1—N5	100.68 (18)	N12—C16—N11	110.0 (5)
N3—Rh1—N5	176.52 (16)	N12—C16—C13	134.3 (5)
N7—Rh1—N17	88.62 (17)	N11—C16—C13	115.7 (5)
N1—Rh1—N17	86.84 (16)	C16—N12—C17	108.6 (5)
N3—Rh1—N17	89.94 (17)	C16—N12—H12N	125.7
N5—Rh1—N17	86.61 (17)	C17—N12—H12N	125.7
N7—Rh1—Rh2	92.24 (12)	N12—C17—C18	106.9 (6)
N1—Rh1—Rh2	92.31 (11)	N12—C17—H17	126.5
N3—Rh1—Rh2	91.83 (12)	C18—C17—H17	126.5
N5—Rh1—Rh2	91.63 (12)	C17—C18—N11	108.2 (6)
N17—Rh1—Rh2	177.87 (13)	C17—C18—H18	125.9
N13—Rh2—N11	175.11 (16)	N11—C18—H18	125.9
N13—Rh2—N9	99.99 (17)	C19—N13—C21	106.0 (5)
N11—Rh2—N9	79.30 (17)	C19—N13—Rh2	113.8 (3)
N13—Rh2—N15	79.47 (17)	C21—N13—Rh2	139.4 (4)
N11—Rh2—N15	100.81 (17)	N13—C19—N14	111.3 (5)
N9—Rh2—N15	175.04 (16)	N13—C19—C22	116.3 (5)
N13—Rh2—N19	87.60 (16)	N14—C19—C22	132.4 (5)
N11—Rh2—N19	87.54 (16)	C19—N14—C20	106.8 (5)
N9—Rh2—N19	87.93 (15)	C19—N14—H14N	126.6
N15—Rh2—N19	87.12 (15)	C20—N14—H14N	126.6
N13—Rh2—Rh1	92.36 (11)	C21—C20—N14	107.2 (6)
N11—Rh2—Rh1	92.50 (12)	C21—C20—H20	126.4
N9—Rh2—Rh1	92.30 (11)	N14—C20—H20	126.4
N15—Rh2—Rh1	92.65 (11)	C20—C21—N13	108.7 (5)
N19—Rh2—Rh1	179.77 (10)	C20—C21—H21	125.7
C1—N1—C3	105.6 (5)	N13—C21—H21	125.7
C1—N1—Rh1	113.3 (4)	C22—N15—C24	106.2 (4)
C3—N1—Rh1	140.5 (4)	C22—N15—Rh2	113.4 (3)
N2—C1—N1	110.8 (6)	C24—N15—Rh2	140.4 (4)
N2—C1—C4	133.0 (6)	N15—C22—N16	110.3 (5)
N1—C1—C4	116.2 (5)	N15—C22—C19	116.4 (4)
C1—N2—C2	107.5 (5)	N16—C22—C19	133.3 (5)
C1—N2—H2N	126.2	C22—N16—C23	107.2 (5)
C2—N2—H2N	126.2	C22—N16—H16N	126.4
C3—C2—N2	107.2 (6)	C23—N16—H16N	126.4
C3—C2—H2	126.4	C24—C23—N16	107.9 (5)
N2—C2—H2	126.4	C24—C23—H23	126.1
C2—C3—N1	108.8 (6)	N16—C23—H23	126.1
C2—C3—H3	125.6	C23—C24—N15	108.4 (6)
N1—C3—H3	125.6	C23—C24—H24	125.8
C4—N3—C6	106.2 (5)	N15—C24—H24	125.8
C4—N3—Rh1	113.4 (4)	C25—N17—C28	116.6 (5)
C6—N3—Rh1	140.3 (5)	C25—N17—Rh1	122.6 (4)
N3—C4—N4	110.1 (6)	C28—N17—Rh1	120.8 (4)
N3—C4—C1	116.9 (5)	N17—C25—C26	120.9 (6)
N4—C4—C1	132.9 (6)	N17—C25—H25	119.5
C5—N4—C4	106.8 (6)	C26—C25—H25	119.5
C5—N4—H4N	126.6	N18—C26—C25	122.7 (7)
C4—N4—H4N	126.6	N18—C26—H26	118.7
C6—C5—N4	108.8 (6)	C25—C26—H26	118.7
C6—C5—H5	125.6	C27—N18—C26	115.5 (6)
N4—C5—H5	125.6	N18—C27—C28	122.9 (6)
C5—C6—N3	108.1 (7)	N18—C27—H27	118.6
C5—C6—H6	126.0	C28—C27—H27	118.6
N3—C6—H6	126.0	N17—C28—C27	121.4 (6)
C7—N5—C9	106.7 (5)	N17—C28—H28	119.3
C7—N5—Rh1	113.4 (4)	C27—C28—H28	119.3
C9—N5—Rh1	139.8 (4)	C30—N19—C29	116.0 (4)
N5—C7—N6	109.5 (6)	C30—N19—Rh2	122.0 (3)
N5—C7—C10	116.0 (5)	C29—N19—Rh2	122.0 (3)
N6—C7—C10	134.5 (6)	N19—C29—C30^i	121.8 (5)
C8—N6—C7	108.1 (5)	N19—C29—H29	119.1
C8—N6—H6N	126.0	C30^i—C29—H29	119.1
C7—N6—H6N	126.0	N19—C30—C29^i	122.2 (5)
N6—C8—C9	108.3 (6)	N19—C30—H30	118.9
N6—C8—H8	125.9	C29^i—C30—H30	118.9
C9—C8—H8	125.9	O1—Cl1—O2	109.3 (10)
C8—C9—N5	107.5 (6)	O1—Cl1—O4	111.7 (8)
C8—C9—H9	126.3	O2—Cl1—O4	106.4 (6)
N5—C9—H9	126.3	O1—Cl1—O3	107.3 (8)
C10—N7—C12	106.7 (6)	O2—Cl1—O3	112.9 (11)
C10—N7—Rh1	113.0 (4)	O4—Cl1—O3	109.3 (8)
C12—N7—Rh1	139.6 (5)	O7—Cl2—O5	109.2 (12)
N7—C10—N8	110.4 (7)	O7—Cl2—O6	109.5 (7)
N7—C10—C7	117.4 (5)	O5—Cl2—O6	108.6 (8)
N8—C10—C7	132.2 (7)	O7—Cl2—O8	111.5 (7)
C10—N8—C11	107.0 (7)	O5—Cl2—O8	103.0 (6)
C10—N8—H8N	126.5	O6—Cl2—O8	114.7 (5)
C11—N8—H8N	126.5	O12—Cl3—O10	114.3 (5)
C12—C11—N8	108.0 (7)	O12—Cl3—O11	112.2 (6)
C12—C11—H11	126.0	O10—Cl3—O11	112.4 (5)
N8—C11—H11	126.0	O12—Cl3—O9	109.0 (8)
C11—C12—N7	107.9 (8)	O10—Cl3—O9	104.5 (7)
C11—C12—H12	126.0	O11—Cl3—O9	103.4 (7)
N7—C12—H12	126.0	F2^ii—Si1—F2	179.998 (2)
C13—N9—C15	106.4 (4)	F2^ii—Si1—F3	89.5 (6)
C13—N9—Rh2	113.9 (3)	F2—Si1—F3	90.5 (6)
C15—N9—Rh2	139.6 (4)	F2^ii—Si1—F3^ii	90.5 (6)
N9—C13—N10	110.5 (5)	F2—Si1—F3^ii	89.5 (6)
N9—C13—C16	116.7 (5)	F3—Si1—F3^ii	180.0 (7)
N10—C13—C16	132.8 (5)	F2^ii—Si1—F1	93.7 (3)
C13—N10—C14	107.1 (5)	F2—Si1—F1	86.3 (3)
C13—N10—H10N	126.5	F3—Si1—F1	90.9 (6)
C14—N10—H10N	126.5	F3^ii—Si1—F1	89.1 (6)
C15—C14—N10	107.9 (5)	F2^ii—Si1—F1^ii	86.3 (3)
C15—C14—H14	126.1	F2—Si1—F1^ii	93.7 (3)
N10—C14—H14	126.1	F3—Si1—F1^ii	89.1 (6)
C14—C15—N9	108.1 (6)	F3^ii—Si1—F1^ii	90.9 (6)
C14—C15—H15	125.9	F1—Si1—F1^ii	179.998 (1)
N7—Rh1—Rh2—N13	118.86 (19)	Rh1—Rh2—N9—C13	97.6 (3)
N1—Rh1—Rh2—N13	−61.41 (17)	N13—Rh2—N9—C15	4.9 (5)
N3—Rh1—Rh2—N13	−141.03 (18)	N11—Rh2—N9—C15	180.0 (6)
N5—Rh1—Rh2—N13	39.35 (17)	N15—Rh2—N9—C15	88 (2)
N17—Rh1—Rh2—N13	5 (3)	N19—Rh2—N9—C15	92.1 (5)
N7—Rh1—Rh2—N11	−61.7 (2)	Rh1—Rh2—N9—C15	−87.9 (5)
N1—Rh1—Rh2—N11	118.08 (17)	C15—N9—C13—N10	1.3 (6)
N3—Rh1—Rh2—N11	38.46 (18)	Rh2—N9—C13—N10	177.6 (3)
N5—Rh1—Rh2—N11	−141.16 (17)	C15—N9—C13—C16	−179.5 (5)
N17—Rh1—Rh2—N11	−175 (23)	Rh2—N9—C13—C16	−3.2 (6)
N7—Rh1—Rh2—N9	−141.0 (2)	N9—C13—N10—C14	−0.8 (6)
N1—Rh1—Rh2—N9	38.70 (18)	C16—C13—N10—C14	−179.8 (6)
N3—Rh1—Rh2—N9	−40.92 (18)	C13—N10—C14—C15	0.0 (7)
N5—Rh1—Rh2—N9	139.46 (18)	N10—C14—C15—N9	0.8 (7)
N17—Rh1—Rh2—N9	105 (3)	C13—N9—C15—C14	−1.3 (6)
N7—Rh1—Rh2—N15	39.3 (2)	Rh2—N9—C15—C14	−176.1 (4)
N1—Rh1—Rh2—N15	−140.97 (18)	N13—Rh2—N11—C16	75 (2)
N3—Rh1—Rh2—N15	139.41 (18)	N9—Rh2—N11—C16	−7.0 (3)
N5—Rh1—Rh2—N15	−40.21 (18)	N15—Rh2—N11—C16	168.0 (3)
N17—Rh1—Rh2—N15	−74 (3)	N19—Rh2—N11—C16	81.4 (4)
N7—Rh1—Rh2—N19	37 (27)	Rh1—Rh2—N11—C16	−98.9 (3)
N1—Rh1—Rh2—N19	−144 (34)	N13—Rh2—N11—C18	−94 (2)
N3—Rh1—Rh2—N19	137 (34)	N9—Rh2—N11—C18	−176.3 (6)
N5—Rh1—Rh2—N19	−43 (27)	N15—Rh2—N11—C18	−1.3 (6)
N17—Rh1—Rh2—N19	−77 (27)	N19—Rh2—N11—C18	−87.9 (6)
N7—Rh1—N1—C1	78 (3)	Rh1—Rh2—N11—C18	91.8 (5)
N3—Rh1—N1—C1	−7.0 (3)	C18—N11—C16—N12	−1.2 (6)
N5—Rh1—N1—C1	169.4 (3)	Rh2—N11—C16—N12	−174.0 (4)
N17—Rh1—N1—C1	83.5 (4)	C18—N11—C16—C13	−179.8 (5)
Rh2—Rh1—N1—C1	−98.5 (3)	Rh2—N11—C16—C13	7.4 (6)
N7—Rh1—N1—C3	−91 (3)	N9—C13—C16—N12	179.1 (6)
N3—Rh1—N1—C3	−176.4 (6)	N10—C13—C16—N12	−2.0 (11)
N5—Rh1—N1—C3	0.0 (6)	N9—C13—C16—N11	−2.8 (7)
N17—Rh1—N1—C3	−85.9 (6)	N10—C13—C16—N11	176.1 (5)
Rh2—Rh1—N1—C3	92.1 (6)	N11—C16—N12—C17	1.3 (7)
C3—N1—C1—N2	−0.1 (6)	C13—C16—N12—C17	179.5 (6)
Rh1—N1—C1—N2	−173.1 (4)	C16—N12—C17—C18	−0.9 (7)
C3—N1—C1—C4	179.9 (5)	N12—C17—C18—N11	0.1 (7)
Rh1—N1—C1—C4	6.9 (6)	C16—N11—C18—C17	0.7 (6)
N1—C1—N2—C2	−0.8 (7)	Rh2—N11—C18—C17	170.5 (5)
C4—C1—N2—C2	179.2 (6)	N11—Rh2—N13—C19	86 (2)
C1—N2—C2—C3	1.3 (7)	N9—Rh2—N13—C19	167.3 (4)
N2—C2—C3—N1	−1.3 (7)	N15—Rh2—N13—C19	−7.7 (4)
C1—N1—C3—C2	0.9 (6)	N19—Rh2—N13—C19	79.9 (4)
Rh1—N1—C3—C2	170.7 (5)	Rh1—Rh2—N13—C19	−99.9 (3)
N7—Rh1—N3—C4	−169.3 (4)	N11—Rh2—N13—C21	−82 (2)
N1—Rh1—N3—C4	6.1 (4)	N9—Rh2—N13—C21	−0.4 (6)
N5—Rh1—N3—C4	−88 (3)	N15—Rh2—N13—C21	−175.4 (6)
N17—Rh1—N3—C4	−80.7 (4)	N19—Rh2—N13—C21	−87.8 (6)
Rh2—Rh1—N3—C4	98.1 (4)	Rh1—Rh2—N13—C21	92.4 (6)
N7—Rh1—N3—C6	7.3 (6)	C21—N13—C19—N14	−0.2 (6)
N1—Rh1—N3—C6	−177.3 (6)	Rh2—N13—C19—N14	−171.9 (4)
N5—Rh1—N3—C6	88 (3)	C21—N13—C19—C22	−179.8 (5)
N17—Rh1—N3—C6	95.9 (6)	Rh2—N13—C19—C22	8.5 (6)
Rh2—Rh1—N3—C6	−85.3 (6)	N13—C19—N14—C20	0.8 (8)
C6—N3—C4—N4	1.2 (6)	C22—C19—N14—C20	−179.7 (6)
Rh1—N3—C4—N4	178.9 (4)	C19—N14—C20—C21	−1.1 (9)
C6—N3—C4—C1	177.9 (5)	N14—C20—C21—N13	1.0 (9)
Rh1—N3—C4—C1	−4.4 (6)	C19—N13—C21—C20	−0.5 (7)
N2—C1—C4—N3	178.2 (6)	Rh2—N13—C21—C20	167.8 (5)
N1—C1—C4—N3	−1.8 (7)	N13—Rh2—N15—C22	5.6 (3)
N2—C1—C4—N4	−5.9 (11)	N11—Rh2—N15—C22	−169.5 (3)
N1—C1—C4—N4	174.1 (6)	N9—Rh2—N15—C22	−79 (2)
N3—C4—N4—C5	−1.0 (7)	N19—Rh2—N15—C22	−82.5 (4)
C1—C4—N4—C5	−177.1 (6)	Rh1—Rh2—N15—C22	97.5 (3)
C4—N4—C5—C6	0.4 (8)	N13—Rh2—N15—C24	−178.6 (6)
N4—C5—C6—N3	0.3 (8)	N11—Rh2—N15—C24	6.4 (6)
C4—N3—C6—C5	−0.9 (7)	N9—Rh2—N15—C24	97 (2)
Rh1—N3—C6—C5	−177.6 (5)	N19—Rh2—N15—C24	93.3 (5)
N7—Rh1—N5—C7	5.9 (4)	Rh1—Rh2—N15—C24	−86.7 (5)
N1—Rh1—N5—C7	−169.5 (4)	C24—N15—C22—N16	0.4 (6)
N3—Rh1—N5—C7	−76 (3)	Rh2—N15—C22—N16	177.6 (4)
N17—Rh1—N5—C7	−83.3 (4)	C24—N15—C22—C19	179.9 (5)
Rh2—Rh1—N5—C7	97.9 (4)	Rh2—N15—C22—C19	−2.8 (6)
N7—Rh1—N5—C9	−179.5 (6)	N13—C19—C22—N15	−3.8 (7)
N1—Rh1—N5—C9	5.1 (6)	N14—C19—C22—N15	176.7 (6)
N3—Rh1—N5—C9	99 (3)	N13—C19—C22—N16	175.6 (6)
N17—Rh1—N5—C9	91.2 (6)	N14—C19—C22—N16	−3.9 (11)
Rh2—Rh1—N5—C9	−87.6 (6)	N15—C22—N16—C23	−0.9 (7)
C9—N5—C7—N6	0.4 (6)	C19—C22—N16—C23	179.7 (6)
Rh1—N5—C7—N6	176.7 (4)	C22—N16—C23—C24	1.0 (7)
C9—N5—C7—C10	−179.8 (5)	N16—C23—C24—N15	−0.8 (7)
Rh1—N5—C7—C10	−3.4 (6)	C22—N15—C24—C23	0.3 (6)
N5—C7—N6—C8	−0.4 (7)	Rh2—N15—C24—C23	−175.7 (4)
C10—C7—N6—C8	179.7 (6)	N7—Rh1—N17—C25	41.6 (5)
C7—N6—C8—C9	0.3 (8)	N1—Rh1—N17—C25	−138.0 (5)
N6—C8—C9—N5	−0.1 (7)	N3—Rh1—N17—C25	−58.4 (5)
C7—N5—C9—C8	−0.2 (6)	N5—Rh1—N17—C25	121.1 (5)
Rh1—N5—C9—C8	−175.0 (5)	Rh2—Rh1—N17—C25	155 (3)
N1—Rh1—N7—C10	85 (3)	N7—Rh1—N17—C28	−137.2 (5)
N3—Rh1—N7—C10	168.9 (4)	N1—Rh1—N17—C28	43.3 (5)
N5—Rh1—N7—C10	−7.6 (4)	N3—Rh1—N17—C28	122.8 (5)
N17—Rh1—N7—C10	79.2 (4)	N5—Rh1—N17—C28	−57.6 (5)
Rh2—Rh1—N7—C10	−98.8 (4)	Rh2—Rh1—N17—C28	−23 (3)
N1—Rh1—N7—C12	−84 (3)	C28—N17—C25—C26	−0.3 (11)
N3—Rh1—N7—C12	0.8 (6)	Rh1—N17—C25—C26	−179.1 (6)
N5—Rh1—N7—C12	−175.7 (6)	N17—C25—C26—N18	0.7 (14)
N17—Rh1—N7—C12	−88.9 (6)	C25—C26—N18—C27	−0.7 (14)
Rh2—Rh1—N7—C12	93.1 (6)	C26—N18—C27—C28	0.3 (13)
C12—N7—C10—N8	−1.6 (7)	C25—N17—C28—C27	0.0 (10)
Rh1—N7—C10—N8	−173.6 (4)	Rh1—N17—C28—C27	178.8 (5)
C12—N7—C10—C7	−179.8 (5)	N18—C27—C28—N17	0.0 (12)
Rh1—N7—C10—C7	8.2 (6)	N13—Rh2—N19—C30	45.3 (4)
N5—C7—C10—N7	−3.3 (8)	N11—Rh2—N19—C30	−134.2 (4)
N6—C7—C10—N7	176.6 (6)	N9—Rh2—N19—C30	−54.8 (4)
N5—C7—C10—N8	179.1 (6)	N15—Rh2—N19—C30	124.9 (4)
N6—C7—C10—N8	−1.1 (12)	Rh1—Rh2—N19—C30	128 (26)
N7—C10—N8—C11	1.8 (7)	N13—Rh2—N19—C29	−134.8 (4)
C7—C10—N8—C11	179.6 (6)	N11—Rh2—N19—C29	45.7 (4)
C10—N8—C11—C12	−1.2 (8)	N9—Rh2—N19—C29	125.1 (4)
N8—C11—C12—N7	0.3 (8)	N15—Rh2—N19—C29	−55.3 (4)
C10—N7—C12—C11	0.8 (7)	Rh1—Rh2—N19—C29	−53 (27)
Rh1—N7—C12—C11	169.4 (5)	C30—N19—C29—C30^i	0.2 (9)
N13—Rh2—N9—C13	−169.6 (3)	Rh2—N19—C29—C30^i	−179.6 (4)
N11—Rh2—N9—C13	5.5 (3)	C29—N19—C30—C29^i	−0.2 (9)
N15—Rh2—N9—C13	−86 (2)	Rh2—N19—C30—C29^i	179.6 (4)
N19—Rh2—N9—C13	−82.4 (4)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···F1^iii	0.86	1.99	2.767 (7)	149
N4—H4N···O7W	0.86	1.91	2.773 (17)	176
N4—H4N···O5W	0.86	2.03	2.73 (3)	138
N6—H6N···F1	0.86	1.99	2.794 (8)	156
N6—H6N···F2	0.86	2.34	3.056 (9)	142
N8—H8N···F3	0.86	1.94	2.794 (11)	170
N10—H10N···O3W	0.86	2.02	2.841 (8)	159
N12—H12N···O8	0.86	2.27	3.067 (9)	154
N12—H12N···O10	0.86	2.42	2.965 (9)	122
N14—H14N···O11^i	0.86	2.44	3.011 (10)	125
N14—H14N···O2	0.86	2.54	3.058 (13)	119
N16—H16N···O4W	0.86	2.04	2.856 (10)	158
N16—H16N···O11^i	0.86	2.62	3.131 (10)	120

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

(VII)

Crystal data

C60H60N38Rh4·8(ClO4)·11.41(H2O)	Dx = 1.847 Mg m^−3
Mr = 2726.26	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pbca	Cell parameters from 19919 reflections
a = 20.289 (4) Å	θ = 3.1–27.5°
b = 21.524 (5) Å	µ = 0.99 mm^−1
c = 22.450 (5) Å	T = 296 K
V = 9804 (4) Å^3	Prismatic, red
Z = 4	0.42 × 0.35 × 0.25 mm
F(000) = 5488

Data collection

Rigaku/MSC Mercury CCD diffractometer	11220 independent reflections
Radiation source: rotating-anode X-ray tube	8509 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.104
Detector resolution: 14.6306 pixels mm^-1	θmax = 27.5°, θmin = 3.1°
ω scans	h = −25→26
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −17→27
Tmin = 0.807, Tmax = 0.884	l = −29→29
72426 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)] = 0.092	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.231	H atoms treated by a mixture of independent and constrained refinement
S = 1.15	w = 1/[σ^2(Fo^2) + (0.0905P)^2 + 33.6829P] where P = (Fo^2 + 2Fc^2)/3
11220 reflections	(Δ/σ)max = 0.001
706 parameters	Δρmax = 1.49 e Å^−3
19 restraints	Δρmin = −1.06 e Å^−3

Special details

Experimental. ????

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	Occ. (<1)
Rh1	0.28661 (3)	0.70345 (3)	0.56605 (2)	0.03821 (17)
Rh2	0.37753 (3)	0.61688 (2)	0.53858 (2)	0.03527 (16)
N1	0.3341 (3)	0.7707 (3)	0.5160 (3)	0.0470 (15)
C1	0.3720 (4)	0.8078 (4)	0.5485 (4)	0.056 (2)
N2	0.3962 (4)	0.8542 (3)	0.5151 (4)	0.069 (2)
H2N	0.4211	0.8839	0.5272	0.083*
C2	0.3738 (5)	0.8453 (4)	0.4581 (5)	0.070 (3)
H2	0.3832	0.8698	0.4250	0.085*
C3	0.3359 (4)	0.7950 (4)	0.4595 (4)	0.056 (2)
H3	0.3137	0.7786	0.4269	0.067*
N3	0.3474 (3)	0.7431 (3)	0.6295 (3)	0.0490 (15)
C4	0.3805 (4)	0.7923 (4)	0.6101 (4)	0.058 (2)
N4	0.4179 (4)	0.8155 (4)	0.6541 (4)	0.075 (2)
H4N	0.4441	0.8469	0.6518	0.090*
C5	0.4067 (6)	0.7801 (6)	0.7024 (5)	0.084 (3)
H5	0.4259	0.7856	0.7397	0.101*
C6	0.3633 (5)	0.7357 (5)	0.6880 (4)	0.067 (3)
H6	0.3469	0.7052	0.7134	0.081*
N5	0.2218 (3)	0.6667 (3)	0.5047 (3)	0.0408 (13)
C7	0.1783 (4)	0.6287 (4)	0.5302 (4)	0.0507 (19)
N6	0.1350 (4)	0.6086 (4)	0.4889 (4)	0.063 (2)
H6N	0.1020	0.5843	0.4950	0.076*
C8	0.1532 (5)	0.6340 (5)	0.4357 (5)	0.066 (3)
H8	0.1327	0.6271	0.3993	0.080*
C9	0.2064 (4)	0.6710 (4)	0.4450 (4)	0.055 (2)
H9	0.2282	0.6947	0.4166	0.065*
N7	0.2356 (3)	0.6428 (3)	0.6188 (3)	0.0467 (15)
C10	0.1848 (4)	0.6171 (3)	0.5927 (4)	0.0485 (18)
N8	0.1505 (4)	0.5832 (4)	0.6319 (4)	0.065 (2)
H8N	0.1164	0.5609	0.6240	0.078*
C11	0.1791 (5)	0.5902 (5)	0.6865 (4)	0.068 (3)
H11	0.1648	0.5736	0.7224	0.082*
C12	0.2316 (5)	0.6258 (4)	0.6776 (4)	0.063 (2)
H12	0.2615	0.6375	0.7069	0.075*
N9	0.4530 (3)	0.6796 (3)	0.5470 (3)	0.0398 (13)
C13	0.4828 (4)	0.6769 (4)	0.5995 (4)	0.0489 (18)
N10	0.5329 (3)	0.7177 (3)	0.6013 (3)	0.0581 (18)
H10N	0.5583	0.7251	0.6311	0.070*
C14	0.5356 (4)	0.7451 (4)	0.5460 (4)	0.063 (2)
H14	0.5656	0.7752	0.5340	0.076*
C15	0.4881 (4)	0.7213 (3)	0.5132 (4)	0.0519 (19)
H15	0.4797	0.7312	0.4736	0.062*
N11	0.4022 (3)	0.6039 (3)	0.6265 (3)	0.0423 (14)
C16	0.4560 (4)	0.6349 (3)	0.6425 (3)	0.0439 (17)
N12	0.4732 (4)	0.6189 (4)	0.6979 (3)	0.064 (2)
H12N	0.5058	0.6336	0.7179	0.077*
C17	0.4302 (5)	0.5754 (4)	0.7169 (4)	0.064 (2)
H17	0.4309	0.5554	0.7536	0.076*
C18	0.3861 (4)	0.5661 (4)	0.6727 (3)	0.0526 (19)
H18	0.3508	0.5385	0.6737	0.063*
N13	0.3591 (3)	0.6256 (3)	0.4492 (3)	0.0412 (13)
C19	0.3220 (4)	0.5800 (4)	0.4277 (3)	0.0471 (17)
N14	0.3204 (4)	0.5829 (4)	0.3681 (3)	0.065 (2)
H14N	0.2993	0.5582	0.3448	0.078*
C20	0.3580 (6)	0.6318 (5)	0.3510 (4)	0.073 (3)
H20	0.3657	0.6451	0.3122	0.088*
C21	0.3821 (4)	0.6571 (4)	0.4014 (4)	0.055 (2)
H21	0.4104	0.6911	0.4031	0.066*
N15	0.3074 (3)	0.5487 (3)	0.5275 (3)	0.0393 (13)
C22	0.2913 (4)	0.5394 (3)	0.4711 (4)	0.0447 (17)
N16	0.2485 (4)	0.4928 (3)	0.4661 (3)	0.0596 (18)
H16N	0.2311	0.4796	0.4335	0.072*
C23	0.2372 (5)	0.4700 (4)	0.5209 (4)	0.062 (2)
H23	0.2102	0.4366	0.5306	0.074*
C24	0.2732 (4)	0.5052 (4)	0.5594 (4)	0.0519 (19)
H24	0.2744	0.5005	0.6006	0.062*
N17	0.2086 (3)	0.7745 (3)	0.5835 (3)	0.0459 (14)
C25	0.1804 (5)	0.7835 (4)	0.6359 (4)	0.060 (2)
H25	0.1938	0.7600	0.6684	0.072*
C26	0.1315 (6)	0.8271 (5)	0.6430 (5)	0.081 (3)
H26	0.1135	0.8323	0.6807	0.097*
N18	0.1088 (4)	0.8620 (4)	0.5992 (4)	0.075 (2)
C27	0.1375 (5)	0.8526 (4)	0.5473 (4)	0.063 (2)
H27	0.1239	0.8759	0.5147	0.076*
C28	0.1870 (4)	0.8094 (4)	0.5397 (4)	0.057 (2)
H28	0.2057	0.8049	0.5021	0.068*
N19	0.4529 (3)	0.5445 (3)	0.5144 (3)	0.0393 (13)
C29	0.4577 (4)	0.4910 (3)	0.5438 (3)	0.0413 (16)
H29	0.4287	0.4832	0.5750	0.050*
C30	0.4959 (4)	0.5532 (3)	0.4705 (3)	0.0445 (17)
H30	0.4946	0.5901	0.4489	0.053*
Cl1	0.2784 (2)	0.58212 (17)	0.20406 (19)	0.1286 (15)
O1	0.2231 (7)	0.5460 (6)	0.2042 (7)	0.187 (6)
O2	0.3295 (8)	0.5535 (5)	0.2354 (6)	0.193 (7)
O3	0.2972 (8)	0.5916 (7)	0.1422 (5)	0.198 (7)
O4	0.2645 (7)	0.6403 (4)	0.2322 (5)	0.165 (5)
Cl2	0.50756 (14)	0.69240 (14)	0.84318 (12)	0.0789 (7)
O5	0.4635 (8)	0.6450 (8)	0.8381 (6)	0.220 (8)
O6	0.5378 (5)	0.6906 (6)	0.8985 (4)	0.137 (4)
O7	0.4742 (8)	0.7450 (7)	0.8379 (5)	0.217 (8)
O8	0.5518 (4)	0.6851 (5)	0.7955 (4)	0.111 (3)
Cl3	0.64676 (16)	0.59659 (16)	0.63272 (13)	0.0886 (9)
O9	0.6855 (6)	0.6403 (6)	0.5983 (5)	0.158 (5)
O10	0.6163 (4)	0.6302 (4)	0.6793 (4)	0.104 (3)
O11	0.6923 (5)	0.5536 (4)	0.6566 (4)	0.125 (3)
O12	0.6007 (5)	0.5672 (5)	0.5943 (5)	0.140 (4)
Cl4	0.00139 (18)	0.48605 (18)	0.59243 (19)	0.1097 (11)
O13	−0.0592 (5)	0.5080 (6)	0.5705 (7)	0.178 (6)
O14	0.0024 (5)	0.4208 (4)	0.5774 (6)	0.152 (5)
O15	0.0519 (6)	0.5168 (7)	0.5621 (6)	0.191 (6)
O16	0.0074 (9)	0.4967 (7)	0.6545 (6)	0.214 (7)
O1W	0.3173 (6)	0.8456 (6)	0.3115 (4)	0.142 (4)
O2W	0.2372 (6)	0.7423 (6)	0.3120 (5)	0.156 (4)
O3W	0.5991 (5)	0.7671 (4)	0.7013 (4)	0.119 (3)
O4W	0.1792 (6)	0.4799 (7)	0.3533 (6)	0.190 (6)
O5W	0.523 (2)	0.8785 (19)	0.702 (3)	0.18 (2)	0.30 (3)
O6W	0.6142 (17)	0.9137 (13)	0.7117 (11)	0.277 (18)	0.70 (3)
O7W	0.4892 (16)	0.9167 (16)	0.770 (2)	0.34 (2)	0.70 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0368 (3)	0.0390 (3)	0.0388 (3)	0.0020 (2)	−0.0010 (2)	−0.0019 (2)
Rh2	0.0337 (3)	0.0343 (3)	0.0378 (3)	−0.0003 (2)	0.0013 (2)	−0.0016 (2)
N1	0.045 (4)	0.041 (3)	0.055 (4)	0.000 (3)	0.005 (3)	−0.002 (3)
C1	0.045 (4)	0.046 (4)	0.076 (6)	0.010 (4)	0.005 (4)	−0.003 (4)
N2	0.061 (5)	0.041 (4)	0.105 (7)	−0.007 (3)	0.017 (5)	−0.005 (4)
C2	0.067 (6)	0.053 (5)	0.091 (8)	0.006 (4)	0.022 (6)	0.002 (5)
C3	0.057 (5)	0.052 (5)	0.060 (5)	−0.001 (4)	0.008 (4)	0.005 (4)
N3	0.044 (3)	0.053 (4)	0.050 (4)	0.004 (3)	−0.005 (3)	−0.015 (3)
C4	0.047 (5)	0.051 (5)	0.076 (6)	0.006 (4)	−0.011 (4)	−0.020 (4)
N4	0.069 (5)	0.071 (5)	0.084 (6)	−0.001 (4)	−0.018 (5)	−0.030 (5)
C5	0.079 (7)	0.101 (8)	0.072 (7)	0.016 (6)	−0.019 (6)	−0.042 (7)
C6	0.063 (6)	0.085 (7)	0.053 (5)	0.019 (5)	−0.007 (4)	−0.018 (5)
N5	0.042 (3)	0.039 (3)	0.042 (3)	0.002 (3)	0.001 (3)	−0.002 (3)
C7	0.037 (4)	0.047 (4)	0.068 (5)	−0.003 (3)	−0.002 (4)	−0.018 (4)
N6	0.051 (4)	0.063 (5)	0.076 (5)	−0.007 (3)	−0.009 (4)	−0.012 (4)
C8	0.053 (5)	0.075 (6)	0.072 (6)	0.018 (5)	−0.023 (5)	−0.024 (5)
C9	0.058 (5)	0.051 (5)	0.054 (5)	0.015 (4)	−0.009 (4)	−0.003 (4)
N7	0.052 (4)	0.047 (4)	0.041 (3)	0.010 (3)	0.008 (3)	0.002 (3)
C10	0.045 (4)	0.040 (4)	0.061 (5)	0.008 (3)	0.009 (4)	−0.004 (4)
N8	0.049 (4)	0.063 (5)	0.082 (6)	−0.003 (3)	0.023 (4)	0.006 (4)
C11	0.078 (7)	0.081 (7)	0.046 (5)	0.016 (5)	0.021 (5)	0.016 (5)
C12	0.078 (6)	0.058 (5)	0.052 (5)	0.013 (5)	0.013 (5)	0.009 (4)
N9	0.039 (3)	0.031 (3)	0.049 (3)	0.005 (2)	0.000 (3)	−0.002 (2)
C13	0.047 (4)	0.049 (4)	0.050 (4)	−0.003 (3)	−0.005 (4)	−0.009 (4)
N10	0.046 (4)	0.064 (4)	0.064 (5)	−0.002 (3)	−0.012 (3)	−0.016 (4)
C14	0.051 (5)	0.052 (5)	0.086 (7)	−0.010 (4)	0.010 (5)	−0.005 (5)
C15	0.046 (4)	0.039 (4)	0.070 (5)	−0.004 (3)	0.009 (4)	0.000 (4)
N11	0.046 (3)	0.041 (3)	0.040 (3)	0.000 (3)	0.002 (3)	−0.005 (3)
C16	0.035 (4)	0.048 (4)	0.048 (4)	0.009 (3)	−0.004 (3)	−0.011 (3)
N12	0.056 (4)	0.077 (5)	0.060 (4)	0.005 (4)	−0.018 (4)	−0.008 (4)
C17	0.080 (6)	0.062 (5)	0.049 (5)	−0.002 (5)	−0.004 (5)	0.001 (4)
C18	0.055 (5)	0.058 (5)	0.045 (4)	0.001 (4)	0.004 (4)	0.001 (4)
N13	0.039 (3)	0.043 (3)	0.041 (3)	0.002 (3)	0.004 (3)	−0.003 (3)
C19	0.047 (4)	0.052 (4)	0.043 (4)	−0.008 (3)	−0.003 (3)	−0.004 (3)
N14	0.079 (5)	0.071 (5)	0.045 (4)	−0.018 (4)	−0.005 (4)	−0.007 (4)
C20	0.096 (8)	0.072 (6)	0.052 (5)	−0.020 (6)	−0.001 (5)	0.014 (5)
C21	0.058 (5)	0.060 (5)	0.048 (4)	−0.003 (4)	0.002 (4)	0.009 (4)
N15	0.035 (3)	0.041 (3)	0.041 (3)	−0.002 (2)	0.005 (2)	0.001 (3)
C22	0.041 (4)	0.035 (4)	0.058 (5)	−0.001 (3)	−0.004 (3)	−0.012 (3)
N16	0.055 (4)	0.056 (4)	0.068 (5)	−0.017 (3)	−0.007 (4)	−0.018 (4)
C23	0.060 (5)	0.053 (5)	0.072 (6)	−0.021 (4)	0.012 (5)	−0.005 (4)
C24	0.042 (4)	0.053 (5)	0.060 (5)	0.004 (3)	0.013 (4)	0.004 (4)
N17	0.039 (3)	0.042 (3)	0.056 (4)	0.007 (3)	−0.004 (3)	0.000 (3)
C25	0.063 (5)	0.058 (5)	0.060 (5)	0.024 (4)	0.005 (4)	0.003 (4)
C26	0.097 (8)	0.083 (7)	0.064 (6)	0.024 (6)	0.027 (6)	−0.003 (5)
N18	0.083 (6)	0.071 (5)	0.071 (5)	0.035 (4)	0.010 (4)	0.006 (4)
C27	0.073 (6)	0.058 (5)	0.059 (5)	0.026 (5)	0.008 (5)	0.011 (4)
C28	0.052 (5)	0.065 (5)	0.053 (5)	0.014 (4)	0.002 (4)	0.003 (4)
N19	0.040 (3)	0.033 (3)	0.044 (3)	−0.001 (2)	0.005 (3)	−0.001 (2)
C29	0.043 (4)	0.041 (4)	0.040 (4)	0.007 (3)	0.008 (3)	0.006 (3)
C30	0.042 (4)	0.036 (4)	0.055 (4)	0.007 (3)	0.003 (3)	0.008 (3)
Cl1	0.189 (4)	0.079 (2)	0.118 (3)	−0.028 (2)	−0.069 (3)	−0.004 (2)
O1	0.190 (12)	0.153 (11)	0.219 (14)	−0.105 (10)	0.013 (10)	−0.046 (10)
O2	0.303 (18)	0.129 (9)	0.147 (10)	0.042 (11)	−0.126 (12)	−0.020 (8)
O3	0.308 (18)	0.201 (13)	0.085 (7)	−0.123 (13)	−0.023 (9)	−0.010 (8)
O4	0.251 (13)	0.068 (5)	0.177 (11)	−0.004 (7)	−0.120 (10)	−0.037 (6)
Cl2	0.0708 (16)	0.099 (2)	0.0673 (15)	0.0153 (14)	0.0043 (12)	−0.0202 (14)
O5	0.260 (17)	0.245 (16)	0.154 (11)	−0.161 (15)	0.061 (11)	−0.075 (11)
O6	0.131 (8)	0.215 (12)	0.065 (5)	0.030 (8)	−0.015 (5)	−0.040 (6)
O7	0.299 (18)	0.232 (15)	0.120 (9)	0.196 (15)	0.014 (10)	0.000 (9)
O8	0.091 (6)	0.167 (9)	0.075 (5)	0.020 (6)	0.024 (5)	−0.016 (5)
Cl3	0.090 (2)	0.103 (2)	0.0733 (17)	0.0298 (17)	−0.0069 (15)	−0.0128 (16)
O9	0.157 (10)	0.180 (11)	0.136 (9)	−0.052 (9)	0.016 (8)	0.050 (9)
O10	0.084 (5)	0.152 (8)	0.076 (5)	0.048 (5)	0.000 (4)	−0.032 (5)
O11	0.155 (9)	0.103 (7)	0.117 (7)	0.061 (6)	−0.032 (6)	−0.019 (6)
O12	0.122 (8)	0.179 (11)	0.119 (8)	−0.001 (7)	−0.045 (6)	−0.061 (8)
Cl4	0.093 (2)	0.109 (3)	0.128 (3)	−0.013 (2)	0.006 (2)	−0.034 (2)
O13	0.091 (8)	0.150 (10)	0.293 (17)	0.043 (7)	−0.045 (9)	−0.057 (11)
O14	0.101 (7)	0.078 (6)	0.277 (15)	−0.003 (5)	0.031 (8)	−0.048 (8)
O15	0.149 (11)	0.220 (14)	0.202 (13)	−0.125 (10)	0.049 (9)	−0.019 (10)
O16	0.32 (2)	0.222 (15)	0.097 (8)	0.027 (15)	−0.015 (11)	−0.050 (9)
O1W	0.162 (10)	0.171 (10)	0.094 (7)	0.000 (8)	−0.006 (7)	−0.023 (7)
O2W	0.133 (10)	0.170 (11)	0.165 (11)	0.029 (8)	0.026 (8)	0.018 (9)
O3W	0.135 (8)	0.115 (7)	0.108 (7)	−0.020 (6)	−0.019 (6)	−0.038 (6)
O4W	0.152 (11)	0.260 (15)	0.159 (11)	0.061 (11)	−0.066 (9)	−0.104 (11)
O5W	0.18 (4)	0.14 (3)	0.23 (4)	−0.11 (3)	−0.06 (3)	0.02 (3)
O6W	0.42 (4)	0.26 (3)	0.150 (19)	0.14 (3)	−0.02 (2)	−0.012 (18)
O7W	0.29 (3)	0.28 (3)	0.44 (4)	−0.10 (2)	0.08 (3)	0.13 (3)

Geometric parameters (Å, º)

Rh1—N7	2.043 (6)	C16—N12	1.337 (10)
Rh1—N5	2.062 (6)	N12—C17	1.348 (11)
Rh1—N3	2.069 (6)	N12—H12N	0.8600
Rh1—N1	2.071 (6)	C17—C18	1.352 (12)
Rh1—N17	2.235 (6)	C17—H17	0.9300
Rh1—Rh2	2.6935 (8)	C18—H18	0.9300
Rh2—N13	2.049 (6)	N13—C19	1.327 (9)
Rh2—N9	2.050 (6)	N13—C21	1.354 (10)
Rh2—N11	2.056 (6)	C19—N14	1.341 (10)
Rh2—N15	2.059 (6)	C19—C22	1.449 (11)
Rh2—N19	2.248 (6)	N14—C20	1.354 (12)
N1—C1	1.327 (11)	N14—H14N	0.8600
N1—C3	1.372 (10)	C20—C21	1.348 (13)
C1—N2	1.341 (11)	C20—H20	0.9300
C1—C4	1.434 (13)	C21—H21	0.9300
N2—C2	1.371 (13)	N15—C22	1.323 (9)
N2—H2N	0.8600	N15—C24	1.367 (10)
C2—C3	1.329 (13)	C22—N16	1.332 (9)
C2—H2	0.9300	N16—C23	1.343 (11)
C3—H3	0.9300	N16—H16N	0.8600
N3—C4	1.328 (11)	C23—C24	1.364 (12)
N3—C6	1.361 (11)	C23—H23	0.9300
C4—N4	1.341 (11)	C24—H24	0.9300
N4—C5	1.345 (14)	N17—C28	1.314 (10)
N4—H4N	0.8600	N17—C25	1.323 (10)
C5—C6	1.341 (15)	C25—C26	1.374 (13)
C5—H5	0.9300	C25—H25	0.9300
C6—H6	0.9300	C26—N18	1.320 (13)
N5—C7	1.334 (10)	C26—H26	0.9300
N5—C9	1.379 (10)	N18—C27	1.319 (11)
C7—N6	1.347 (10)	C27—C28	1.379 (12)
C7—C10	1.432 (12)	C27—H27	0.9300
N6—C8	1.364 (13)	C28—H28	0.9300
N6—H6N	0.8600	N19—C30	1.331 (9)
C8—C9	1.356 (13)	N19—C29	1.331 (9)
C8—H8	0.9300	C29—C30^i	1.378 (10)
C9—H9	0.9300	C29—H29	0.9300
N7—C10	1.308 (10)	C30—C29^i	1.378 (10)
N7—C12	1.372 (10)	C30—H30	0.9300
C10—N8	1.339 (10)	Cl1—O1	1.365 (11)
N8—C11	1.365 (12)	Cl1—O2	1.396 (12)
N8—H8N	0.8600	Cl1—O4	1.431 (10)
C11—C12	1.327 (13)	Cl1—O3	1.454 (12)
C11—H11	0.9300	Cl2—O7	1.324 (11)
C12—H12	0.9300	Cl2—O5	1.361 (12)
N9—C13	1.325 (10)	Cl2—O6	1.385 (9)
N9—C15	1.375 (10)	Cl2—O8	1.406 (8)
C13—N10	1.344 (10)	Cl3—O10	1.413 (8)
C13—C16	1.430 (11)	Cl3—O11	1.413 (9)
N10—C14	1.374 (12)	Cl3—O12	1.421 (9)
N10—H10N	0.8600	Cl3—O9	1.449 (10)
C14—C15	1.316 (12)	Cl4—O15	1.396 (10)
C14—H14	0.9300	Cl4—O13	1.406 (11)
C15—H15	0.9300	Cl4—O16	1.418 (12)
N11—C16	1.329 (9)	Cl4—O14	1.444 (9)
N11—C18	1.357 (10)
N7—Rh1—N5	79.6 (3)	C15—C14—H14	126.0
N7—Rh1—N3	99.6 (3)	N10—C14—H14	126.0
N5—Rh1—N3	176.9 (2)	C14—C15—N9	108.9 (8)
N7—Rh1—N1	175.3 (2)	C14—C15—H15	125.5
N5—Rh1—N1	101.7 (3)	N9—C15—H15	125.5
N3—Rh1—N1	78.9 (3)	C16—N11—C18	107.0 (7)
N7—Rh1—N17	88.7 (2)	C16—N11—Rh2	113.0 (5)
N5—Rh1—N17	85.9 (2)	C18—N11—Rh2	139.1 (5)
N3—Rh1—N17	91.1 (2)	N11—C16—N12	109.6 (7)
N1—Rh1—N17	86.9 (2)	N11—C16—C13	116.6 (7)
N7—Rh1—Rh2	92.15 (17)	N12—C16—C13	133.8 (7)
N5—Rh1—Rh2	91.04 (16)	C16—N12—C17	107.8 (7)
N3—Rh1—Rh2	91.96 (18)	C16—N12—H12N	126.1
N1—Rh1—Rh2	92.34 (17)	C17—N12—H12N	126.1
N17—Rh1—Rh2	176.61 (17)	N12—C17—C18	107.4 (8)
N13—Rh2—N9	99.6 (2)	N12—C17—H17	126.3
N13—Rh2—N11	175.6 (2)	C18—C17—H17	126.3
N9—Rh2—N11	79.6 (2)	C17—C18—N11	108.2 (8)
N13—Rh2—N15	79.7 (2)	C17—C18—H18	125.9
N9—Rh2—N15	175.2 (2)	N11—C18—H18	125.9
N11—Rh2—N15	100.8 (2)	C19—N13—C21	106.2 (7)
N13—Rh2—N19	87.2 (2)	C19—N13—Rh2	113.1 (5)
N9—Rh2—N19	88.3 (2)	C21—N13—Rh2	139.3 (6)
N11—Rh2—N19	88.4 (2)	N13—C19—N14	110.0 (7)
N15—Rh2—N19	87.0 (2)	N13—C19—C22	116.3 (6)
N13—Rh2—Rh1	92.05 (17)	N14—C19—C22	133.7 (7)
N9—Rh2—Rh1	92.01 (16)	C19—N14—C20	107.8 (7)
N11—Rh2—Rh1	92.33 (17)	C19—N14—H14N	126.1
N15—Rh2—Rh1	92.72 (16)	C20—N14—H14N	126.1
N19—Rh2—Rh1	179.23 (16)	C21—C20—N14	106.3 (8)
C1—N1—C3	105.3 (7)	C21—C20—H20	126.9
C1—N1—Rh1	113.1 (6)	N14—C20—H20	126.9
C3—N1—Rh1	141.2 (6)	C20—C21—N13	109.7 (8)
N1—C1—N2	110.6 (9)	C20—C21—H21	125.1
N1—C1—C4	117.4 (8)	N13—C21—H21	125.1
N2—C1—C4	132.0 (9)	C22—N15—C24	105.9 (6)
C1—N2—C2	107.3 (8)	C22—N15—Rh2	113.1 (5)
C1—N2—H2N	126.3	C24—N15—Rh2	140.8 (6)
C2—N2—H2N	126.3	N15—C22—N16	110.8 (7)
C3—C2—N2	106.4 (9)	N15—C22—C19	116.6 (6)
C3—C2—H2	126.8	N16—C22—C19	132.6 (7)
N2—C2—H2	126.8	C22—N16—C23	108.0 (7)
C2—C3—N1	110.3 (9)	C22—N16—H16N	126.0
C2—C3—H3	124.8	C23—N16—H16N	126.0
N1—C3—H3	124.8	N16—C23—C24	106.6 (7)
C4—N3—C6	106.9 (8)	N16—C23—H23	126.7
C4—N3—Rh1	113.9 (6)	C24—C23—H23	126.7
C6—N3—Rh1	139.2 (7)	C23—C24—N15	108.7 (8)
N3—C4—N4	110.0 (9)	C23—C24—H24	125.7
N3—C4—C1	116.2 (7)	N15—C24—H24	125.7
N4—C4—C1	133.7 (10)	C28—N17—C25	115.9 (7)
C4—N4—C5	106.7 (9)	C28—N17—Rh1	119.8 (6)
C4—N4—H4N	126.6	C25—N17—Rh1	124.3 (5)
C5—N4—H4N	126.6	N17—C25—C26	121.1 (8)
C6—C5—N4	108.7 (9)	N17—C25—H25	119.5
C6—C5—H5	125.7	C26—C25—H25	119.5
N4—C5—H5	125.7	N18—C26—C25	123.7 (9)
C5—C6—N3	107.8 (10)	N18—C26—H26	118.2
C5—C6—H6	126.1	C25—C26—H26	118.2
N3—C6—H6	126.1	C27—N18—C26	114.6 (8)
C7—N5—C9	107.9 (7)	N18—C27—C28	122.4 (9)
C7—N5—Rh1	111.8 (5)	N18—C27—H27	118.8
C9—N5—Rh1	140.3 (6)	C28—C27—H27	118.8
N5—C7—N6	109.5 (8)	N17—C28—C27	122.4 (8)
N5—C7—C10	117.8 (7)	N17—C28—H28	118.8
N6—C7—C10	132.8 (8)	C27—C28—H28	118.8
C7—N6—C8	107.3 (8)	C30—N19—C29	116.2 (6)
C7—N6—H6N	126.3	C30—N19—Rh2	121.8 (5)
C8—N6—H6N	126.3	C29—N19—Rh2	122.0 (5)
C9—C8—N6	108.4 (8)	N19—C29—C30^i	122.2 (7)
C9—C8—H8	125.8	N19—C29—H29	118.9
N6—C8—H8	125.8	C30^i—C29—H29	118.9
C8—C9—N5	107.0 (8)	N19—C30—C29^i	121.6 (7)
C8—C9—H9	126.5	N19—C30—H30	119.2
N5—C9—H9	126.5	C29^i—C30—H30	119.2
C10—N7—C12	105.7 (7)	O1—Cl1—O2	111.0 (10)
C10—N7—Rh1	114.2 (5)	O1—Cl1—O4	109.6 (9)
C12—N7—Rh1	139.3 (6)	O2—Cl1—O4	108.0 (7)
N7—C10—N8	110.3 (8)	O1—Cl1—O3	107.3 (8)
N7—C10—C7	116.0 (7)	O2—Cl1—O3	110.4 (10)
N8—C10—C7	133.7 (8)	O4—Cl1—O3	110.5 (8)
C10—N8—C11	107.9 (8)	O7—Cl2—O5	107.2 (12)
C10—N8—H8N	126.1	O7—Cl2—O6	109.3 (8)
C11—N8—H8N	126.1	O5—Cl2—O6	110.2 (9)
C12—C11—N8	105.7 (8)	O7—Cl2—O8	110.8 (8)
C12—C11—H11	127.1	O5—Cl2—O8	105.7 (7)
N8—C11—H11	127.1	O6—Cl2—O8	113.4 (6)
C11—C12—N7	110.3 (9)	O10—Cl3—O11	109.9 (6)
C11—C12—H12	124.9	O10—Cl3—O12	113.0 (6)
N7—C12—H12	124.9	O11—Cl3—O12	111.6 (7)
C13—N9—C15	106.4 (7)	O10—Cl3—O9	107.3 (7)
C13—N9—Rh2	113.2 (5)	O11—Cl3—O9	105.9 (8)
C15—N9—Rh2	140.0 (6)	O12—Cl3—O9	108.8 (7)
N9—C13—N10	110.1 (7)	O15—Cl4—O13	108.2 (10)
N9—C13—C16	117.0 (7)	O15—Cl4—O16	109.8 (10)
N10—C13—C16	132.9 (8)	O13—Cl4—O16	111.4 (10)
C13—N10—C14	106.5 (7)	O15—Cl4—O14	109.6 (8)
C13—N10—H10N	126.8	O13—Cl4—O14	105.0 (7)
C14—N10—H10N	126.8	O16—Cl4—O14	112.6 (10)
C15—C14—N10	108.0 (8)
N7—Rh1—Rh2—N13	122.2 (3)	Rh1—Rh2—N9—C13	97.9 (5)
N5—Rh1—Rh2—N13	42.5 (2)	N13—Rh2—N9—C15	2.3 (8)
N3—Rh1—Rh2—N13	−138.2 (3)	N11—Rh2—N9—C15	177.8 (8)
N1—Rh1—Rh2—N13	−59.2 (3)	N15—Rh2—N9—C15	83 (3)
N17—Rh1—Rh2—N13	18 (3)	N19—Rh2—N9—C15	89.1 (8)
N7—Rh1—Rh2—N9	−138.1 (3)	Rh1—Rh2—N9—C15	−90.2 (8)
N5—Rh1—Rh2—N9	142.2 (2)	C15—N9—C13—N10	3.4 (9)
N3—Rh1—Rh2—N9	−38.5 (3)	Rh2—N9—C13—N10	178.0 (5)
N1—Rh1—Rh2—N9	40.5 (2)	C15—N9—C13—C16	−178.6 (7)
N17—Rh1—Rh2—N9	118 (3)	Rh2—N9—C13—C16	−4.0 (9)
N7—Rh1—Rh2—N11	−58.5 (3)	N9—C13—N10—C14	−2.4 (9)
N5—Rh1—Rh2—N11	−138.1 (2)	C16—C13—N10—C14	−180.0 (9)
N3—Rh1—Rh2—N11	41.2 (3)	C13—N10—C14—C15	0.4 (10)
N1—Rh1—Rh2—N11	120.1 (3)	N10—C14—C15—N9	1.6 (10)
N17—Rh1—Rh2—N11	−163 (3)	C13—N9—C15—C14	−3.1 (9)
N7—Rh1—Rh2—N15	42.4 (2)	Rh2—N9—C15—C14	−175.4 (6)
N5—Rh1—Rh2—N15	−37.2 (2)	N13—Rh2—N11—C16	73 (3)
N3—Rh1—Rh2—N15	142.1 (3)	N9—Rh2—N11—C16	−6.9 (5)
N1—Rh1—Rh2—N15	−139.0 (2)	N15—Rh2—N11—C16	168.2 (5)
N17—Rh1—Rh2—N15	−62 (3)	N19—Rh2—N11—C16	81.6 (5)
N7—Rh1—Rh2—N19	107 (11)	Rh1—Rh2—N11—C16	−98.6 (5)
N5—Rh1—Rh2—N19	27 (11)	N13—Rh2—N11—C18	−94 (3)
N3—Rh1—Rh2—N19	−153 (11)	N9—Rh2—N11—C18	−174.5 (8)
N1—Rh1—Rh2—N19	−74 (11)	N15—Rh2—N11—C18	0.7 (8)
N17—Rh1—Rh2—N19	3 (12)	N19—Rh2—N11—C18	−85.9 (8)
N7—Rh1—N1—C1	65 (3)	Rh1—Rh2—N11—C18	93.9 (8)
N5—Rh1—N1—C1	170.4 (5)	C18—N11—C16—N12	−1.5 (8)
N3—Rh1—N1—C1	−6.5 (5)	Rh2—N11—C16—N12	−173.0 (5)
N17—Rh1—N1—C1	85.3 (6)	C18—N11—C16—C13	178.5 (7)
Rh2—Rh1—N1—C1	−98.0 (5)	Rh2—N11—C16—C13	7.0 (8)
N7—Rh1—N1—C3	−107 (3)	N9—C13—C16—N11	−2.1 (10)
N5—Rh1—N1—C3	−1.3 (9)	N10—C13—C16—N11	175.3 (8)
N3—Rh1—N1—C3	−178.2 (9)	N9—C13—C16—N12	178.0 (8)
N17—Rh1—N1—C3	−86.5 (9)	N10—C13—C16—N12	−4.6 (16)
Rh2—Rh1—N1—C3	90.2 (9)	N11—C16—N12—C17	1.6 (9)
C3—N1—C1—N2	1.0 (9)	C13—C16—N12—C17	−178.4 (8)
Rh1—N1—C1—N2	−173.7 (5)	C16—N12—C17—C18	−1.1 (10)
C3—N1—C1—C4	−178.6 (7)	N12—C17—C18—N11	0.1 (10)
Rh1—N1—C1—C4	6.8 (9)	C16—N11—C18—C17	0.9 (9)
N1—C1—N2—C2	−1.5 (10)	Rh2—N11—C18—C17	168.8 (6)
C4—C1—N2—C2	177.9 (9)	N9—Rh2—N13—C19	165.5 (5)
C1—N2—C2—C3	1.4 (10)	N11—Rh2—N13—C19	86 (3)
N2—C2—C3—N1	−0.9 (10)	N15—Rh2—N13—C19	−9.7 (5)
C1—N1—C3—C2	0.0 (10)	N19—Rh2—N13—C19	77.7 (5)
Rh1—N1—C3—C2	172.1 (7)	Rh1—Rh2—N13—C19	−102.1 (5)
N7—Rh1—N3—C4	−170.1 (6)	N9—Rh2—N13—C21	1.5 (9)
N5—Rh1—N3—C4	−96 (5)	N11—Rh2—N13—C21	−78 (3)
N1—Rh1—N3—C4	5.4 (6)	N15—Rh2—N13—C21	−173.7 (9)
N17—Rh1—N3—C4	−81.3 (6)	N19—Rh2—N13—C21	−86.3 (8)
Rh2—Rh1—N3—C4	97.4 (5)	Rh1—Rh2—N13—C21	93.9 (8)
N7—Rh1—N3—C6	6.7 (9)	C21—N13—C19—N14	−1.1 (9)
N5—Rh1—N3—C6	81 (5)	Rh2—N13—C19—N14	−170.3 (6)
N1—Rh1—N3—C6	−177.8 (9)	C21—N13—C19—C22	−179.8 (7)
N17—Rh1—N3—C6	95.6 (9)	Rh2—N13—C19—C22	11.0 (9)
Rh2—Rh1—N3—C6	−85.8 (8)	N13—C19—N14—C20	0.4 (11)
C6—N3—C4—N4	1.4 (10)	C22—C19—N14—C20	178.7 (9)
Rh1—N3—C4—N4	179.2 (5)	C19—N14—C20—C21	0.5 (12)
C6—N3—C4—C1	178.7 (7)	N14—C20—C21—N13	−1.2 (12)
Rh1—N3—C4—C1	−3.5 (9)	C19—N13—C21—C20	1.4 (10)
N1—C1—C4—N3	−2.3 (11)	Rh2—N13—C21—C20	166.1 (7)
N2—C1—C4—N3	178.3 (8)	N13—Rh2—N15—C22	6.9 (5)
N1—C1—C4—N4	174.2 (9)	N9—Rh2—N15—C22	−75 (3)
N2—C1—C4—N4	−5.3 (17)	N11—Rh2—N15—C22	−168.6 (5)
N3—C4—N4—C5	−1.1 (11)	N19—Rh2—N15—C22	−80.8 (5)
C1—C4—N4—C5	−177.7 (9)	Rh1—Rh2—N15—C22	98.5 (5)
C4—N4—C5—C6	0.4 (12)	N13—Rh2—N15—C24	−178.8 (8)
N4—C5—C6—N3	0.4 (11)	N9—Rh2—N15—C24	99 (3)
C4—N3—C6—C5	−1.1 (10)	N11—Rh2—N15—C24	5.7 (8)
Rh1—N3—C6—C5	−178.1 (7)	N19—Rh2—N15—C24	93.5 (8)
N7—Rh1—N5—C7	5.5 (5)	Rh1—Rh2—N15—C24	−87.2 (8)
N3—Rh1—N5—C7	−69 (5)	C24—N15—C22—N16	0.5 (9)
N1—Rh1—N5—C7	−169.9 (5)	Rh2—N15—C22—N16	176.7 (5)
N17—Rh1—N5—C7	−83.9 (5)	C24—N15—C22—C19	−179.5 (7)
Rh2—Rh1—N5—C7	97.5 (5)	Rh2—N15—C22—C19	−3.2 (8)
N7—Rh1—N5—C9	−178.9 (8)	N13—C19—C22—N15	−5.3 (11)
N3—Rh1—N5—C9	106 (5)	N14—C19—C22—N15	176.5 (9)
N1—Rh1—N5—C9	5.7 (8)	N13—C19—C22—N16	174.8 (8)
N17—Rh1—N5—C9	91.7 (8)	N14—C19—C22—N16	−3.5 (16)
Rh2—Rh1—N5—C9	−86.9 (8)	N15—C22—N16—C23	−1.3 (10)
C9—N5—C7—N6	−0.4 (9)	C19—C22—N16—C23	178.7 (9)
Rh1—N5—C7—N6	176.7 (5)	C22—N16—C23—C24	1.5 (10)
C9—N5—C7—C10	179.9 (7)	N16—C23—C24—N15	−1.3 (10)
Rh1—N5—C7—C10	−3.1 (8)	C22—N15—C24—C23	0.5 (9)
N5—C7—N6—C8	1.4 (9)	Rh2—N15—C24—C23	−174.1 (6)
C10—C7—N6—C8	−179.0 (8)	N7—Rh1—N17—C28	−137.8 (7)
C7—N6—C8—C9	−1.8 (10)	N5—Rh1—N17—C28	−58.1 (7)
N6—C8—C9—N5	1.6 (10)	N3—Rh1—N17—C28	122.7 (7)
C7—N5—C9—C8	−0.8 (9)	N1—Rh1—N17—C28	43.9 (7)
Rh1—N5—C9—C8	−176.5 (6)	Rh2—Rh1—N17—C28	−34 (3)
N5—Rh1—N7—C10	−7.5 (5)	N7—Rh1—N17—C25	40.6 (7)
N3—Rh1—N7—C10	169.5 (5)	N5—Rh1—N17—C25	120.3 (7)
N1—Rh1—N7—C10	99 (3)	N3—Rh1—N17—C25	−58.9 (7)
N17—Rh1—N7—C10	78.6 (5)	N1—Rh1—N17—C25	−137.8 (7)
Rh2—Rh1—N7—C10	−98.1 (5)	Rh2—Rh1—N17—C25	145 (3)
N5—Rh1—N7—C12	−175.2 (9)	C28—N17—C25—C26	0.0 (14)
N3—Rh1—N7—C12	1.8 (9)	Rh1—N17—C25—C26	−178.4 (8)
N1—Rh1—N7—C12	−69 (4)	N17—C25—C26—N18	0.8 (18)
N17—Rh1—N7—C12	−89.1 (8)	C25—C26—N18—C27	−1.0 (18)
Rh2—Rh1—N7—C12	94.2 (8)	C26—N18—C27—C28	0.4 (16)
C12—N7—C10—N8	−2.0 (9)	C25—N17—C28—C27	−0.6 (14)
Rh1—N7—C10—N8	−173.7 (5)	Rh1—N17—C28—C27	177.9 (7)
C12—N7—C10—C7	179.8 (7)	N18—C27—C28—N17	0.4 (16)
Rh1—N7—C10—C7	8.1 (8)	N13—Rh2—N19—C30	45.7 (6)
N5—C7—C10—N7	−3.3 (10)	N9—Rh2—N19—C30	−54.0 (6)
N6—C7—C10—N7	177.0 (8)	N11—Rh2—N19—C30	−133.6 (6)
N5—C7—C10—N8	178.9 (8)	N15—Rh2—N19—C30	125.5 (6)
N6—C7—C10—N8	−0.7 (16)	Rh1—Rh2—N19—C30	61 (11)
N7—C10—N8—C11	3.1 (10)	N13—Rh2—N19—C29	−135.4 (6)
C7—C10—N8—C11	−179.1 (8)	N9—Rh2—N19—C29	124.9 (6)
C10—N8—C11—C12	−2.9 (10)	N11—Rh2—N19—C29	45.3 (6)
N8—C11—C12—N7	1.7 (10)	N15—Rh2—N19—C29	−55.6 (6)
C10—N7—C12—C11	0.1 (10)	Rh1—Rh2—N19—C29	−120 (11)
Rh1—N7—C12—C11	168.4 (7)	C30—N19—C29—C30^i	−0.4 (12)
N13—Rh2—N9—C13	−169.7 (5)	Rh2—N19—C29—C30^i	−179.4 (6)
N11—Rh2—N9—C13	5.9 (5)	C29—N19—C30—C29^i	0.4 (12)
N15—Rh2—N9—C13	−89 (3)	Rh2—N19—C30—C29^i	179.4 (6)
N19—Rh2—N9—C13	−82.8 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O14^ii	0.86	2.08	2.872 (13)	154
N4—H4N···O5W	0.86	2.08	2.75 (4)	135
N4—H4N···O14^ii	0.86	2.55	3.273 (16)	142
N6—H6N···O15	0.86	2.33	3.075 (14)	145
N6—H6N···O13^iii	0.86	2.62	3.233 (14)	129
N8—H8N···O15	0.86	2.13	2.915 (15)	151
N8—H8N···Cl4	0.86	2.92	3.782 (9)	178
N10—H10N···O3W	0.86	2.00	2.824 (11)	161
N10—H10N···O10	0.86	2.59	3.077 (11)	117
N12—H12N···O8	0.86	2.27	3.062 (12)	154
N12—H12N···O10	0.86	2.41	2.945 (11)	121
N14—H14N···O11^i	0.86	2.41	3.001 (12)	126
N14—H14N···O2	0.86	2.53	3.049 (14)	120
N16—H16N···O4W	0.86	2.09	2.910 (13)	160
N16—H16N···O11^i	0.86	2.65	3.167 (12)	120

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

(VIII)

Crystal data

C28H28F12N18Rh2·2(SiF6)·6(H2O)	F(000) = 2432
Mr = 1214.78	Dx = 1.887 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
a = 27.057 (5) Å	Cell parameters from 6156 reflections
b = 9.9832 (15) Å	θ = 3.0–27.5°
c = 18.718 (3) Å	µ = 0.95 mm^−1
β = 122.2560 (19)°	T = 296 K
V = 4275.6 (13) Å^3	Prismatic, red
Z = 4	0.59 × 0.39 × 0.21 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer	4873 independent reflections
Radiation source: rotating-anode X-ray tube	4409 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
Detector resolution: 14.62 pixels mm^-1	θmax = 27.5°, θmin = 3.8°
ω scans	h = −34→21
Absorption correction: numerical NUMABS (Higashi, 1999)	k = −12→10
Tmin = 0.747, Tmax = 0.867	l = −20→24
16660 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)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.136	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0767P)^2 + 22.3201P] where P = (Fo^2 + 2Fc^2)/3
4873 reflections	(Δ/σ)max < 0.001
309 parameters	Δρmax = 1.37 e Å^−3
0 restraints	Δρmin = −1.21 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	0.5000	0.48681 (4)	0.2500	0.02135 (13)
Rh2	0.5000	0.21732 (4)	0.2500	0.02278 (13)
N1	0.55449 (15)	0.4974 (3)	0.2053 (2)	0.0289 (7)
C1	0.61052 (18)	0.5151 (4)	0.2656 (3)	0.0316 (8)
N2	0.64316 (19)	0.5329 (5)	0.2329 (3)	0.0517 (11)
H2N	0.6803	0.5453	0.2606	0.062*
C2	0.6067 (3)	0.5277 (8)	0.1471 (4)	0.0673 (18)
H2	0.6173	0.5369	0.1076	0.081*
C3	0.5518 (2)	0.5066 (5)	0.1305 (3)	0.0464 (12)
H3	0.5181	0.4995	0.0770	0.056*
N3	0.58000 (14)	0.4915 (3)	0.3611 (2)	0.0264 (6)
C4	0.62451 (18)	0.5126 (4)	0.3513 (3)	0.0299 (8)
N4	0.67424 (16)	0.5295 (4)	0.4261 (2)	0.0421 (9)
H4N	0.7081	0.5452	0.4342	0.051*
C5	0.6616 (2)	0.5175 (5)	0.4866 (3)	0.0484 (12)
H5	0.6879	0.5234	0.5447	0.058*
C6	0.6035 (2)	0.4951 (4)	0.4465 (3)	0.0365 (9)
H6	0.5827	0.4839	0.4727	0.044*
N5	0.49934 (15)	0.2108 (3)	0.1393 (2)	0.0292 (7)
C7	0.55188 (19)	0.1931 (4)	0.1512 (3)	0.0344 (9)
N6	0.54808 (19)	0.1764 (5)	0.0777 (3)	0.0460 (9)
H6N	0.5769	0.1639	0.0712	0.055*
C8	0.4904 (2)	0.1825 (6)	0.0147 (3)	0.0472 (11)
H8	0.4747	0.1743	−0.0430	0.057*
C9	0.4605 (2)	0.2030 (4)	0.0536 (3)	0.0369 (9)
H9	0.4201	0.2106	0.0263	0.044*
N7	0.58799 (14)	0.2093 (3)	0.2966 (2)	0.0289 (7)
C10	0.60043 (18)	0.1946 (4)	0.2374 (3)	0.0345 (9)
N8	0.65797 (17)	0.1829 (5)	0.2720 (3)	0.0481 (10)
H8N	0.6756	0.1733	0.2453	0.058*
C11	0.6838 (2)	0.1889 (6)	0.3576 (4)	0.0525 (13)
H11	0.7236	0.1836	0.3980	0.063*
C12	0.64002 (19)	0.2042 (4)	0.3727 (3)	0.0383 (9)
H12	0.6447	0.2102	0.4256	0.046*
N9	0.5000	0.7202 (4)	0.2500	0.0237 (9)
C13	0.53399 (19)	0.7867 (4)	0.3200 (3)	0.0326 (9)
H13	0.5580	0.7402	0.3700	0.039*
C14	0.53457 (19)	0.9261 (4)	0.3204 (3)	0.0349 (9)
H14	0.5594	0.9718	0.3704	0.042*
N10	0.5000	0.9941 (4)	0.2500	0.0277 (9)
Si1	0.81273 (6)	0.5852 (2)	0.41399 (10)	0.0581 (4)
F1	0.8146 (7)	0.7193 (11)	0.3712 (7)	0.279 (7)
F2	0.8735 (4)	0.6493 (11)	0.4859 (6)	0.210 (5)
F3	0.8438 (4)	0.5230 (10)	0.3688 (7)	0.214 (5)
F4	0.7547 (3)	0.5092 (10)	0.3475 (7)	0.226 (6)
F5	0.7766 (5)	0.6599 (9)	0.4453 (10)	0.253 (7)
F6	0.8270 (8)	0.4585 (14)	0.4673 (8)	0.313 (8)
O1	0.5947 (3)	0.8697 (6)	0.1915 (4)	0.0985 (18)
O2	0.6770 (4)	0.8445 (8)	0.3646 (5)	0.138 (3)
O3	0.7085 (5)	0.7199 (9)	0.1683 (10)	0.198 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0230 (2)	0.01753 (19)	0.0232 (2)	0.000	0.01210 (17)	0.000
Rh2	0.0231 (2)	0.0165 (2)	0.0283 (2)	0.000	0.01339 (17)	0.000
N1	0.0305 (17)	0.0294 (16)	0.0290 (17)	−0.0016 (12)	0.0174 (15)	−0.0001 (12)
C1	0.0285 (19)	0.032 (2)	0.038 (2)	−0.0027 (15)	0.0203 (18)	0.0011 (16)
N2	0.038 (2)	0.081 (3)	0.046 (2)	−0.013 (2)	0.029 (2)	−0.006 (2)
C2	0.059 (3)	0.114 (5)	0.045 (3)	−0.023 (3)	0.039 (3)	−0.008 (3)
C3	0.047 (3)	0.066 (3)	0.031 (2)	−0.011 (2)	0.024 (2)	−0.005 (2)
N3	0.0275 (16)	0.0229 (15)	0.0263 (16)	−0.0010 (11)	0.0127 (13)	0.0002 (11)
C4	0.0264 (18)	0.0290 (19)	0.031 (2)	−0.0034 (14)	0.0132 (16)	−0.0007 (14)
N4	0.0259 (17)	0.055 (2)	0.036 (2)	−0.0086 (16)	0.0103 (16)	−0.0017 (17)
C5	0.042 (3)	0.058 (3)	0.031 (2)	−0.009 (2)	0.010 (2)	−0.001 (2)
C6	0.038 (2)	0.042 (2)	0.028 (2)	−0.0036 (17)	0.0166 (18)	0.0011 (16)
N5	0.0313 (17)	0.0236 (15)	0.0330 (17)	0.0009 (12)	0.0174 (15)	−0.0016 (12)
C7	0.036 (2)	0.032 (2)	0.040 (2)	0.0041 (17)	0.0234 (19)	−0.0026 (17)
N6	0.046 (2)	0.058 (2)	0.044 (2)	0.0068 (19)	0.031 (2)	−0.0056 (19)
C8	0.051 (3)	0.057 (3)	0.035 (2)	0.005 (2)	0.024 (2)	−0.004 (2)
C9	0.038 (2)	0.036 (2)	0.034 (2)	0.0031 (17)	0.0169 (19)	−0.0016 (16)
N7	0.0267 (16)	0.0215 (15)	0.0377 (18)	0.0013 (11)	0.0166 (15)	−0.0002 (12)
C10	0.0277 (19)	0.032 (2)	0.045 (2)	0.0039 (16)	0.0201 (18)	−0.0016 (17)
N8	0.0290 (19)	0.060 (2)	0.057 (3)	0.0052 (18)	0.0243 (19)	−0.006 (2)
C11	0.027 (2)	0.060 (3)	0.056 (3)	0.009 (2)	0.013 (2)	−0.002 (3)
C12	0.030 (2)	0.037 (2)	0.039 (2)	0.0032 (16)	0.0119 (18)	0.0007 (17)
N9	0.026 (2)	0.022 (2)	0.023 (2)	0.000	0.0129 (18)	0.000
C13	0.040 (2)	0.0222 (19)	0.0237 (19)	0.0040 (15)	0.0086 (17)	0.0028 (13)
C14	0.038 (2)	0.0219 (19)	0.031 (2)	0.0025 (15)	0.0092 (17)	−0.0006 (15)
N10	0.025 (2)	0.027 (2)	0.028 (2)	0.000	0.0115 (19)	0.000
Si1	0.0305 (7)	0.0998 (14)	0.0438 (8)	−0.0039 (7)	0.0197 (6)	0.0054 (8)
F1	0.49 (2)	0.151 (9)	0.217 (12)	−0.006 (11)	0.207 (14)	0.057 (8)
F2	0.115 (6)	0.308 (14)	0.129 (6)	−0.012 (6)	0.012 (5)	−0.095 (7)
F3	0.197 (8)	0.295 (11)	0.265 (10)	−0.140 (8)	0.201 (8)	−0.178 (9)
F4	0.063 (4)	0.219 (9)	0.288 (12)	−0.032 (4)	0.021 (5)	−0.121 (8)
F5	0.226 (10)	0.194 (9)	0.50 (2)	−0.052 (7)	0.306 (13)	−0.127 (10)
F6	0.46 (2)	0.270 (14)	0.240 (13)	0.083 (14)	0.208 (15)	0.175 (11)
O1	0.092 (4)	0.099 (4)	0.100 (5)	−0.008 (3)	0.048 (4)	−0.008 (3)
O2	0.170 (8)	0.126 (7)	0.115 (6)	0.047 (5)	0.075 (6)	0.036 (4)
O3	0.203 (10)	0.126 (7)	0.370 (17)	−0.035 (7)	0.222 (12)	−0.012 (9)

Geometric parameters (Å, º)

Rh1—N1	2.049 (3)	C7—N6	1.334 (6)
Rh1—N1^i	2.049 (3)	C7—C10	1.437 (6)
Rh1—N3	2.051 (3)	N6—C8	1.366 (7)
Rh1—N3^i	2.051 (3)	N6—H6N	0.8600
Rh1—N9	2.330 (4)	C8—C9	1.362 (7)
Rh1—Rh2	2.6904 (7)	C8—H8	0.9300
Rh2—N7^i	2.054 (3)	C9—H9	0.9300
Rh2—N7	2.054 (3)	N7—C10	1.328 (6)
Rh2—N5^i	2.063 (3)	N7—C12	1.368 (6)
Rh2—N5	2.063 (3)	C10—N8	1.334 (6)
Rh2—N10^ii	2.228 (5)	N8—C11	1.365 (7)
N1—C1	1.333 (6)	N8—H8N	0.8600
N1—C3	1.367 (6)	C11—C12	1.364 (7)
C1—N2	1.329 (6)	C11—H11	0.9300
C1—C4	1.438 (6)	C12—H12	0.9300
N2—C2	1.365 (7)	N9—C13^i	1.310 (4)
N2—H2N	0.8600	N9—C13	1.310 (4)
C2—C3	1.361 (8)	C13—C14	1.391 (6)
C2—H2	0.9300	C13—H13	0.9300
C3—H3	0.9300	C14—N10	1.325 (5)
N3—C4	1.328 (5)	C14—H14	0.9300
N3—C6	1.369 (5)	N10—C14^i	1.325 (5)
C4—N4	1.337 (6)	N10—Rh2^iii	2.228 (4)
N4—C5	1.352 (7)	Si1—F6	1.528 (9)
N4—H4N	0.8600	Si1—F5	1.570 (6)
C5—C6	1.352 (7)	Si1—F1	1.575 (9)
C5—H5	0.9300	Si1—F4	1.582 (6)
C6—H6	0.9300	Si1—F2	1.601 (8)
N5—C7	1.328 (5)	Si1—F3	1.602 (6)
N5—C9	1.374 (6)
O1···O2	2.797 (10)	O3···F4^iv	3.120 (14)
O1···F3^iv	2.895 (15)	O3···F6^iv	3.23 (1)
O2···F5	2.931 (13)	O3···F3^iv	3.254 (14)
O2···F5^v	3.08 (1)
N1—Rh1—N1^i	174.10 (18)	N3—C6—H6	125.3
N1—Rh1—N3	79.22 (14)	C7—N5—C9	105.8 (4)
N1^i—Rh1—N3	100.64 (14)	C7—N5—Rh2	113.7 (3)
N1—Rh1—N3^i	100.64 (14)	C9—N5—Rh2	140.0 (3)
N1^i—Rh1—N3^i	79.22 (14)	N5—C7—N6	111.0 (4)
N3—Rh1—N3^i	177.39 (17)	N5—C7—C10	116.2 (4)
N1—Rh1—N9	87.05 (9)	N6—C7—C10	132.8 (4)
N1^i—Rh1—N9	87.05 (9)	C7—N6—C8	108.0 (4)
N3—Rh1—N9	88.70 (8)	C7—N6—H6N	126.0
N3^i—Rh1—N9	88.70 (8)	C8—N6—H6N	126.0
N1—Rh1—Rh2	92.95 (9)	C9—C8—N6	106.1 (4)
N1^i—Rh1—Rh2	92.95 (9)	C9—C8—H8	127.0
N3—Rh1—Rh2	91.30 (8)	N6—C8—H8	127.0
N3^i—Rh1—Rh2	91.30 (8)	C8—C9—N5	109.3 (4)
N9—Rh1—Rh2	180.000 (1)	C8—C9—H9	125.4
N7^i—Rh2—N7	175.53 (17)	N5—C9—H9	125.4
N7^i—Rh2—N5^i	79.18 (14)	C10—N7—C12	106.6 (4)
N7—Rh2—N5^i	100.67 (14)	C10—N7—Rh2	113.7 (3)
N7^i—Rh2—N5	100.67 (14)	C12—N7—Rh2	139.4 (3)
N7—Rh2—N5	79.18 (14)	N7—C10—N8	110.7 (4)
N5^i—Rh2—N5	176.37 (17)	N7—C10—C7	116.8 (4)
N7^i—Rh2—N10^ii	87.77 (8)	N8—C10—C7	132.5 (4)
N7—Rh2—N10^ii	87.77 (8)	C10—N8—C11	107.5 (4)
N5^i—Rh2—N10^ii	88.18 (9)	C10—N8—H8N	126.3
N5—Rh2—N10^ii	88.19 (9)	C11—N8—H8N	126.3
N7^i—Rh2—Rh1	92.23 (8)	C12—C11—N8	106.9 (4)
N7—Rh2—Rh1	92.23 (8)	C12—C11—H11	126.6
N5^i—Rh2—Rh1	91.81 (9)	N8—C11—H11	126.6
N5—Rh2—Rh1	91.81 (9)	C11—C12—N7	108.3 (4)
N10^ii—Rh2—Rh1	180.0	C11—C12—H12	125.9
C1—N1—C3	105.8 (4)	N7—C12—H12	125.9
C1—N1—Rh1	113.7 (3)	C13^i—N9—C13	119.1 (4)
C3—N1—Rh1	140.0 (3)	C13^i—N9—Rh1	120.5 (2)
N2—C1—N1	111.3 (4)	C13—N9—Rh1	120.5 (2)
N2—C1—C4	132.3 (4)	N9—C13—C14	120.8 (4)
N1—C1—C4	116.5 (4)	N9—C13—H13	119.6
C1—N2—C2	107.3 (4)	C14—C13—H13	119.6
C1—N2—H2N	126.4	N10—C14—C13	120.5 (4)
C2—N2—H2N	126.4	N10—C14—H14	119.8
C3—C2—N2	106.9 (4)	C13—C14—H14	119.8
C3—C2—H2	126.6	C14^i—N10—C14	118.3 (5)
N2—C2—H2	126.6	C14^i—N10—Rh2^iii	120.8 (2)
C2—C3—N1	108.8 (5)	C14—N10—Rh2^iii	120.8 (2)
C2—C3—H3	125.6	F6—Si1—F5	98.0 (7)
N1—C3—H3	125.6	F6—Si1—F1	166.1 (9)
C4—N3—C6	105.5 (3)	F5—Si1—F1	89.0 (7)
C4—N3—Rh1	114.0 (3)	F6—Si1—F4	85.2 (8)
C6—N3—Rh1	140.0 (3)	F5—Si1—F4	88.1 (5)
N3—C4—N4	110.8 (4)	F1—Si1—F4	107.2 (7)
N3—C4—C1	116.0 (4)	F6—Si1—F2	89.6 (8)
N4—C4—C1	133.2 (4)	F5—Si1—F2	93.5 (5)
C4—N4—C5	107.6 (4)	F1—Si1—F2	77.9 (7)
C4—N4—H4N	126.2	F4—Si1—F2	174.7 (6)
C5—N4—H4N	126.2	F6—Si1—F3	90.2 (7)
C6—C5—N4	106.8 (4)	F5—Si1—F3	170.9 (7)
C6—C5—H5	126.6	F1—Si1—F3	83.8 (6)
N4—C5—H5	126.6	F4—Si1—F3	88.8 (5)
C5—C6—N3	109.3 (4)	F2—Si1—F3	90.3 (5)
C5—C6—H6	125.3
N1—Rh1—Rh2—N7^i	−138.71 (14)	C1—C4—N4—C5	179.5 (5)
N1^i—Rh1—Rh2—N7^i	41.29 (14)	C4—N4—C5—C6	−0.9 (6)
N3—Rh1—Rh2—N7^i	142.02 (14)	N4—C5—C6—N3	0.8 (6)
N3^i—Rh1—Rh2—N7^i	−37.98 (14)	C4—N3—C6—C5	−0.4 (5)
N9—Rh1—Rh2—N7^i	−159 (100)	Rh1—N3—C6—C5	−170.7 (3)
N1—Rh1—Rh2—N7	41.29 (14)	N7^i—Rh2—N5—C7	−169.9 (3)
N1^i—Rh1—Rh2—N7	−138.71 (14)	N7—Rh2—N5—C7	5.6 (3)
N3—Rh1—Rh2—N7	−37.98 (14)	N5^i—Rh2—N5—C7	−82.5 (3)
N3^i—Rh1—Rh2—N7	142.02 (14)	N10^ii—Rh2—N5—C7	−82.5 (3)
N9—Rh1—Rh2—N7	21 (100)	Rh1—Rh2—N5—C7	97.5 (3)
N1—Rh1—Rh2—N5^i	142.05 (14)	N7^i—Rh2—N5—C9	−0.2 (4)
N1^i—Rh1—Rh2—N5^i	−37.95 (14)	N7—Rh2—N5—C9	175.2 (4)
N3—Rh1—Rh2—N5^i	62.78 (13)	N5^i—Rh2—N5—C9	87.1 (4)
N3^i—Rh1—Rh2—N5^i	−117.22 (13)	N10^ii—Rh2—N5—C9	87.1 (4)
N9—Rh1—Rh2—N5^i	122 (100)	Rh1—Rh2—N5—C9	−92.9 (4)
N1—Rh1—Rh2—N5	−37.95 (14)	C9—N5—C7—N6	0.7 (5)
N1^i—Rh1—Rh2—N5	142.05 (14)	Rh2—N5—C7—N6	173.8 (3)
N3—Rh1—Rh2—N5	−117.22 (13)	C9—N5—C7—C10	−178.9 (4)
N3^i—Rh1—Rh2—N5	62.78 (13)	Rh2—N5—C7—C10	−5.8 (5)
N9—Rh1—Rh2—N5	−58 (100)	N5—C7—N6—C8	−0.4 (6)
N1—Rh1—Rh2—N10^ii	153 (16)	C10—C7—N6—C8	179.1 (5)
N1^i—Rh1—Rh2—N10^ii	−27 (16)	C7—N6—C8—C9	−0.1 (6)
N3—Rh1—Rh2—N10^ii	74 (16)	N6—C8—C9—N5	0.6 (6)
N3^i—Rh1—Rh2—N10^ii	−106 (16)	C7—N5—C9—C8	−0.8 (5)
N9—Rh1—Rh2—N10^ii	133 (100)	Rh2—N5—C9—C8	−170.9 (4)
N1^i—Rh1—N1—C1	83.0 (3)	N7^i—Rh2—N7—C10	84.1 (3)
N3—Rh1—N1—C1	−6.3 (3)	N5^i—Rh2—N7—C10	171.8 (3)
N3^i—Rh1—N1—C1	171.1 (3)	N5—Rh2—N7—C10	−4.5 (3)
N9—Rh1—N1—C1	83.0 (3)	N10^ii—Rh2—N7—C10	84.1 (3)
Rh2—Rh1—N1—C1	−97.0 (3)	Rh1—Rh2—N7—C10	−95.9 (3)
N1^i—Rh1—N1—C3	−87.5 (5)	N7^i—Rh2—N7—C12	−89.4 (4)
N3—Rh1—N1—C3	−176.8 (5)	N5^i—Rh2—N7—C12	−1.6 (4)
N3^i—Rh1—N1—C3	0.6 (5)	N5—Rh2—N7—C12	−177.9 (4)
N9—Rh1—N1—C3	−87.5 (5)	N10^ii—Rh2—N7—C12	−89.3 (4)
Rh2—Rh1—N1—C3	92.5 (5)	Rh1—Rh2—N7—C12	90.6 (4)
C3—N1—C1—N2	−0.9 (5)	C12—N7—C10—N8	−1.1 (5)
Rh1—N1—C1—N2	−174.6 (3)	Rh2—N7—C10—N8	−176.7 (3)
C3—N1—C1—C4	178.7 (4)	C12—N7—C10—C7	178.4 (4)
Rh1—N1—C1—C4	5.0 (4)	Rh2—N7—C10—C7	2.9 (5)
N1—C1—N2—C2	0.6 (6)	N5—C7—C10—N7	2.0 (6)
C4—C1—N2—C2	−179.0 (5)	N6—C7—C10—N7	−177.5 (5)
C1—N2—C2—C3	0.0 (7)	N5—C7—C10—N8	−178.6 (5)
N2—C2—C3—N1	−0.6 (7)	N6—C7—C10—N8	1.9 (9)
C1—N1—C3—C2	0.9 (6)	N7—C10—N8—C11	0.6 (6)
Rh1—N1—C3—C2	171.9 (4)	C7—C10—N8—C11	−178.8 (5)
N1—Rh1—N3—C4	6.7 (3)	C10—N8—C11—C12	0.1 (6)
N1^i—Rh1—N3—C4	−167.3 (3)	N8—C11—C12—N7	−0.8 (6)
N3^i—Rh1—N3—C4	−80.6 (3)	C10—N7—C12—C11	1.2 (5)
N9—Rh1—N3—C4	−80.6 (3)	Rh2—N7—C12—C11	174.9 (4)
Rh2—Rh1—N3—C4	99.4 (3)	N1—Rh1—N9—C13^i	81.1 (3)
N1—Rh1—N3—C6	176.5 (4)	N1^i—Rh1—N9—C13^i	−98.9 (3)
N1^i—Rh1—N3—C6	2.5 (4)	N3—Rh1—N9—C13^i	160.3 (3)
N3^i—Rh1—N3—C6	89.2 (4)	N3^i—Rh1—N9—C13^i	−19.7 (3)
N9—Rh1—N3—C6	89.2 (4)	Rh2—Rh1—N9—C13^i	101 (100)
Rh2—Rh1—N3—C6	−90.8 (4)	N1—Rh1—N9—C13	−98.9 (3)
C6—N3—C4—N4	−0.2 (5)	N1^i—Rh1—N9—C13	81.1 (3)
Rh1—N3—C4—N4	173.0 (3)	N3—Rh1—N9—C13	−19.7 (3)
C6—N3—C4—C1	−179.3 (3)	N3^i—Rh1—N9—C13	160.3 (3)
Rh1—N3—C4—C1	−6.1 (4)	Rh2—Rh1—N9—C13	−79 (100)
N2—C1—C4—N3	−179.8 (5)	C13^i—N9—C13—C14	−0.5 (3)
N1—C1—C4—N3	0.7 (5)	Rh1—N9—C13—C14	179.5 (3)
N2—C1—C4—N4	1.4 (9)	N9—C13—C14—N10	1.0 (6)
N1—C1—C4—N4	−178.1 (4)	C13—C14—N10—C14^i	−0.5 (3)
N3—C4—N4—C5	0.7 (5)	C13—C14—N10—Rh2^iii	179.5 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···F4	0.86	1.83	2.619 (9)	153
N4—H4N···F5	0.86	2.09	2.903 (8)	157
N4—H4N···F4	0.86	2.56	3.219 (12)	135
N6—H6N···F2^vi	0.86	2.12	2.948 (12)	161
N6—H6N···F3^vi	0.86	2.30	2.963 (8)	134
N6—H6N···F1^vi	0.86	2.59	3.332 (17)	145
N8—H8N···F1^vi	0.86	2.38	3.161 (13)	152
N8—H8N···F3^vi	0.86	2.43	3.060 (12)	131

Symmetry code: (vi) −x+3/2, y−1/2, −z+1/2.