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Monocationic acetamidate-bridged dinuclear units are two-dimensionally connected by axially coordinating group 6 oxometallate ions in the structures [{
M2(acam)
4}
2(
M′O
4)] (
M = Rh, Ru;
M′ = Cr, Mo, W; Hacam = acetamide). In these sheet structures, dinuclear units are connected to each other by NH
O hydrogen bonds. The sheets are also connected with NH
O hydrogen bonds. Amidate-bridged dirhodium units that have bulkier alkyl groups reacted with CrO
42− or MoO
42− give three-dimensional diamondoid structures [{Rh
2(pram)
4}
2(CrO
4)]·1.08H
2O, [{Rh
2(pram)
4}
2(MoO
4)]·2.44H
2O and [{Rh
2(buam)
4}
2(MoO
4)] (Hpram = propionamide; Hbuam = butyramide). In these structures the NH group of the amidate ligands hydrogen bonds with O atoms in metallate ions.
Supporting information
CCDC references: 969676; 969677; 969678; 969679; 969680; 969681; 969682; 969683; 969684
Crystal data, data collection and structure refinement details are summarized in Table 1.
S2. Results and discussion
top
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: ORTEPII (Johnson, 1976); software used to prepare material for publication: Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).
Crystal data top
C16H32CrN8O12Rh4 | Dx = 2.487 Mg m−3 |
Mr = 992.14 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/a | Cell parameters from 3335 reflections |
Hall symbol: -I 4ad | θ = 3.0–27.5° |
a = 9.4384 (7) Å | µ = 2.91 mm−1 |
c = 29.750 (3) Å | T = 296 K |
V = 2650.2 (4) Å3 | Prism, brown |
Z = 4 | 0.10 × 0.10 × 0.10 mm |
F(000) = 1936 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1528 independent reflections |
Radiation source: rotating-anode X-ray tube | 1383 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ω scans | h = −12→8 |
Absorption correction: integration (Higashi, 1999) | k = −8→12 |
Tmin = 0.759, Tmax = 0.806 | l = −36→38 |
10792 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + (0.019P)2 + 17.9794P] where P = (Fo2 + 2Fc2)/3 |
1528 reflections | (Δ/σ)max = 0.001 |
95 parameters | Δρmax = 0.49 e Å−3 |
0 restraints | Δρmin = −0.68 e Å−3 |
Crystal data top
C16H32CrN8O12Rh4 | Z = 4 |
Mr = 992.14 | Mo Kα radiation |
Tetragonal, I41/a | µ = 2.91 mm−1 |
a = 9.4384 (7) Å | T = 296 K |
c = 29.750 (3) Å | 0.10 × 0.10 × 0.10 mm |
V = 2650.2 (4) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1528 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1383 reflections with I > 2σ(I) |
Tmin = 0.759, Tmax = 0.806 | Rint = 0.060 |
10792 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + (0.019P)2 + 17.9794P] where P = (Fo2 + 2Fc2)/3 |
1528 reflections | Δρmax = 0.49 e Å−3 |
95 parameters | Δρmin = −0.68 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.37187 (4) | 0.25713 (4) | 0.168366 (13) | 0.01513 (13) | |
Cr1 | 0.0000 | 0.2500 | 0.1250 | 0.0196 (4) | |
O1 | 0.3838 (4) | 0.4047 (4) | 0.11961 (13) | 0.0209 (8) | |
O2 | 0.3833 (4) | 0.4134 (4) | 0.21563 (12) | 0.0222 (8) | |
O3 | 0.1381 (4) | 0.2767 (4) | 0.15810 (14) | 0.0317 (10) | |
N1 | 0.6231 (4) | 0.3963 (4) | 0.12405 (16) | 0.0197 (9) | |
H1 | 0.7024 | 0.4312 | 0.1151 | 0.024* | |
N2 | 0.6214 (4) | 0.3794 (4) | 0.21963 (15) | 0.0200 (10) | |
H2 | 0.6996 | 0.4019 | 0.2326 | 0.024* | |
C1 | 0.5065 (6) | 0.4488 (5) | 0.10727 (18) | 0.0196 (11) | |
C2 | 0.5085 (7) | 0.5616 (7) | 0.0717 (2) | 0.0369 (16) | |
H3 | 0.5025 | 0.5184 | 0.0426 | 0.055* | |
H4 | 0.5950 | 0.6147 | 0.0739 | 0.055* | |
H5 | 0.4293 | 0.6240 | 0.0759 | 0.055* | |
C3 | 0.5051 (6) | 0.4358 (5) | 0.23423 (19) | 0.0200 (11) | |
C4 | 0.5040 (7) | 0.5318 (7) | 0.2738 (2) | 0.0366 (15) | |
H6 | 0.4429 | 0.6109 | 0.2679 | 0.055* | |
H7 | 0.5984 | 0.5653 | 0.2795 | 0.055* | |
H8 | 0.4701 | 0.4812 | 0.2996 | 0.055* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0110 (2) | 0.0166 (2) | 0.0178 (2) | 0.00003 (14) | 0.00042 (15) | 0.00041 (15) |
Cr1 | 0.0142 (5) | 0.0142 (5) | 0.0304 (10) | 0.000 | 0.000 | 0.000 |
O1 | 0.0162 (18) | 0.0218 (19) | 0.025 (2) | 0.0002 (14) | 0.0003 (15) | 0.0075 (16) |
O2 | 0.0217 (19) | 0.0246 (19) | 0.020 (2) | 0.0023 (15) | 0.0014 (15) | −0.0051 (16) |
O3 | 0.0104 (17) | 0.044 (2) | 0.041 (3) | 0.0006 (16) | −0.0009 (17) | −0.0046 (19) |
N1 | 0.012 (2) | 0.023 (2) | 0.024 (3) | −0.0049 (16) | 0.0023 (17) | 0.0025 (18) |
N2 | 0.015 (2) | 0.023 (2) | 0.022 (3) | −0.0025 (17) | −0.0035 (17) | −0.0045 (18) |
C1 | 0.026 (3) | 0.012 (2) | 0.021 (3) | −0.001 (2) | 0.000 (2) | −0.002 (2) |
C2 | 0.031 (3) | 0.034 (3) | 0.046 (4) | 0.002 (3) | 0.004 (3) | 0.020 (3) |
C3 | 0.027 (3) | 0.014 (2) | 0.019 (3) | −0.001 (2) | 0.000 (2) | −0.001 (2) |
C4 | 0.052 (4) | 0.034 (3) | 0.025 (3) | 0.005 (3) | −0.003 (3) | −0.012 (3) |
Geometric parameters (Å, º) top
Rh1—N1i | 1.959 (4) | N2—C3 | 1.295 (6) |
Rh1—N2i | 1.998 (4) | N2—Rh1i | 1.998 (4) |
Rh1—O1 | 2.014 (4) | N2—H2 | 0.8600 |
Rh1—O2 | 2.041 (4) | C1—C2 | 1.501 (8) |
Rh1—O3 | 2.235 (4) | C2—H3 | 0.9600 |
Rh1—Rh1i | 2.4225 (8) | C2—H4 | 0.9600 |
Cr1—O3 | 1.653 (4) | C2—H5 | 0.9600 |
O1—C1 | 1.283 (6) | C3—C4 | 1.486 (8) |
O2—C3 | 1.294 (6) | C4—H6 | 0.9600 |
N1—C1 | 1.306 (7) | C4—H7 | 0.9600 |
N1—Rh1i | 1.959 (4) | C4—H8 | 0.9600 |
N1—H1 | 0.8600 | | |
| | | |
N1i—Rh1—N2i | 92.07 (18) | C1—N1—Rh1i | 123.9 (3) |
N1i—Rh1—O1 | 91.44 (17) | C1—N1—H1 | 118.0 |
N2i—Rh1—O1 | 173.79 (16) | Rh1i—N1—H1 | 118.0 |
N1i—Rh1—O2 | 175.39 (16) | C3—N2—Rh1i | 123.2 (4) |
N2i—Rh1—O2 | 86.48 (16) | C3—N2—H2 | 118.4 |
O1—Rh1—O2 | 89.63 (15) | Rh1i—N2—H2 | 118.4 |
N1i—Rh1—O3 | 89.60 (16) | O1—C1—N1 | 121.9 (5) |
N2i—Rh1—O3 | 100.89 (16) | O1—C1—C2 | 116.3 (5) |
O1—Rh1—O3 | 84.26 (15) | N1—C1—C2 | 121.8 (5) |
O2—Rh1—O3 | 94.97 (14) | C1—C2—H3 | 109.5 |
N1i—Rh1—Rh1i | 86.25 (12) | C1—C2—H4 | 109.5 |
N2i—Rh1—Rh1i | 86.13 (12) | H3—C2—H4 | 109.5 |
O1—Rh1—Rh1i | 88.99 (10) | C1—C2—H5 | 109.5 |
O2—Rh1—Rh1i | 89.29 (10) | H3—C2—H5 | 109.5 |
O3—Rh1—Rh1i | 171.99 (11) | H4—C2—H5 | 109.5 |
O3—Cr1—O3ii | 106.9 (3) | O2—C3—N2 | 122.9 (5) |
O3iii—Cr1—O3iv | 106.9 (3) | O2—C3—C4 | 115.6 (5) |
O3iii—Cr1—O3 | 110.79 (14) | N2—C3—C4 | 121.5 (5) |
O3iv—Cr1—O3 | 110.79 (14) | C3—C4—H6 | 109.5 |
O3iii—Cr1—O3ii | 110.79 (14) | C3—C4—H7 | 109.5 |
O3iv—Cr1—O3ii | 110.79 (14) | H6—C4—H7 | 109.5 |
C1—O1—Rh1 | 118.7 (3) | C3—C4—H8 | 109.5 |
C3—O2—Rh1 | 117.4 (3) | H6—C4—H8 | 109.5 |
Cr1—O3—Rh1 | 147.9 (2) | H7—C4—H8 | 109.5 |
| | | |
N1i—Rh1—O1—C1 | −90.8 (4) | N2i—Rh1—O3—Cr1 | −115.2 (5) |
O2—Rh1—O1—C1 | 84.7 (4) | O1—Rh1—O3—Cr1 | 68.4 (5) |
O3—Rh1—O1—C1 | 179.7 (4) | O2—Rh1—O3—Cr1 | 157.5 (4) |
Rh1i—Rh1—O1—C1 | −4.6 (4) | Rh1—O1—C1—N1 | 3.0 (7) |
N2i—Rh1—O2—C3 | 75.6 (4) | Rh1—O1—C1—C2 | −178.3 (4) |
O1—Rh1—O2—C3 | −99.6 (4) | Rh1i—N1—C1—O1 | 1.6 (7) |
O3—Rh1—O2—C3 | 176.2 (4) | Rh1i—N1—C1—C2 | −177.0 (4) |
Rh1i—Rh1—O2—C3 | −10.6 (4) | Rh1—O2—C3—N2 | 10.5 (7) |
O3iii—Cr1—O3—Rh1 | 28.9 (5) | Rh1—O2—C3—C4 | −169.6 (4) |
O3iv—Cr1—O3—Rh1 | −89.5 (6) | Rh1i—N2—C3—O2 | −3.0 (7) |
O3ii—Cr1—O3—Rh1 | 149.7 (5) | Rh1i—N2—C3—C4 | 177.1 (4) |
N1i—Rh1—O3—Cr1 | −23.1 (5) | | |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.38 | 3.076 (5) | 138 |
N2—H2···O2vi | 0.86 | 2.32 | 3.150 (5) | 162 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C16H32MoN8O12Rh4 | Dx = 2.535 Mg m−3 |
Mr = 1036.08 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/a | Cell parameters from 3061 reflections |
Hall symbol: -I 4ad | θ = 3.0–27.5° |
a = 9.5725 (8) Å | µ = 2.90 mm−1 |
c = 29.627 (3) Å | T = 296 K |
V = 2714.8 (4) Å3 | Block, brown |
Z = 4 | 0.10 × 0.10 × 0.06 mm |
F(000) = 2008 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1557 independent reflections |
Radiation source: rotating-anode X-ray tube | 1393 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.067 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = −9→12 |
Absorption correction: integration (Higashi, 1999) | k = −10→12 |
Tmin = 0.731, Tmax = 0.856 | l = −38→25 |
11116 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.30 | w = 1/[σ2(Fo2) + (0.0169P)2 + 35.6503P] where P = (Fo2 + 2Fc2)/3 |
1557 reflections | (Δ/σ)max = 0.001 |
95 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.71 e Å−3 |
Crystal data top
C16H32MoN8O12Rh4 | Z = 4 |
Mr = 1036.08 | Mo Kα radiation |
Tetragonal, I41/a | µ = 2.90 mm−1 |
a = 9.5725 (8) Å | T = 296 K |
c = 29.627 (3) Å | 0.10 × 0.10 × 0.06 mm |
V = 2714.8 (4) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1557 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1393 reflections with I > 2σ(I) |
Tmin = 0.731, Tmax = 0.856 | Rint = 0.067 |
11116 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.061 | 0 restraints |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.30 | w = 1/[σ2(Fo2) + (0.0169P)2 + 35.6503P] where P = (Fo2 + 2Fc2)/3 |
1557 reflections | Δρmax = 0.71 e Å−3 |
95 parameters | Δρmin = −0.71 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.37397 (6) | 0.25731 (6) | 0.169556 (17) | 0.01489 (15) | |
Mo1 | 0.0000 | 0.2500 | 0.1250 | 0.0182 (3) | |
N1 | 0.6215 (6) | 0.3964 (6) | 0.1251 (2) | 0.0208 (13) | |
H1 | 0.6997 | 0.4318 | 0.1164 | 0.025* | |
O1 | 0.3861 (5) | 0.4030 (5) | 0.12014 (16) | 0.0207 (11) | |
N2 | 0.6200 (6) | 0.3772 (6) | 0.22057 (19) | 0.0201 (14) | |
H2 | 0.6972 | 0.3986 | 0.2337 | 0.024* | |
O2 | 0.3849 (5) | 0.4127 (5) | 0.21626 (16) | 0.0226 (11) | |
O3 | 0.1446 (5) | 0.2760 (6) | 0.16062 (18) | 0.0324 (13) | |
C1 | 0.5065 (8) | 0.4472 (7) | 0.1082 (2) | 0.0203 (15) | |
C2 | 0.5094 (9) | 0.5599 (9) | 0.0729 (3) | 0.0321 (19) | |
H3 | 0.4964 | 0.5189 | 0.0436 | 0.048* | |
H4 | 0.5978 | 0.6071 | 0.0738 | 0.048* | |
H5 | 0.4357 | 0.6256 | 0.0786 | 0.048* | |
C3 | 0.5061 (9) | 0.4341 (8) | 0.2350 (2) | 0.0224 (16) | |
C4 | 0.5058 (10) | 0.5338 (9) | 0.2737 (2) | 0.037 (2) | |
H6 | 0.4398 | 0.5030 | 0.2960 | 0.056* | |
H7 | 0.4799 | 0.6251 | 0.2632 | 0.056* | |
H8 | 0.5973 | 0.5376 | 0.2869 | 0.056* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0098 (3) | 0.0162 (3) | 0.0187 (3) | −0.0001 (2) | 0.0000 (2) | −0.0001 (2) |
Mo1 | 0.0132 (4) | 0.0132 (4) | 0.0283 (6) | 0.000 | 0.000 | 0.000 |
N1 | 0.022 (3) | 0.021 (3) | 0.020 (3) | −0.001 (3) | 0.003 (2) | 0.004 (2) |
O1 | 0.017 (3) | 0.023 (3) | 0.022 (3) | 0.001 (2) | 0.000 (2) | 0.005 (2) |
N2 | 0.015 (3) | 0.023 (4) | 0.022 (3) | 0.000 (3) | −0.004 (2) | −0.004 (2) |
O2 | 0.022 (3) | 0.022 (3) | 0.024 (3) | 0.004 (2) | −0.001 (2) | −0.002 (2) |
O3 | 0.012 (3) | 0.045 (4) | 0.040 (3) | −0.001 (3) | −0.001 (2) | −0.002 (3) |
C1 | 0.023 (4) | 0.016 (4) | 0.022 (3) | −0.002 (3) | −0.001 (3) | 0.001 (3) |
C2 | 0.030 (5) | 0.028 (5) | 0.038 (4) | 0.001 (4) | 0.002 (4) | 0.013 (4) |
C3 | 0.031 (4) | 0.018 (4) | 0.018 (3) | −0.001 (3) | 0.000 (3) | 0.002 (3) |
C4 | 0.052 (6) | 0.034 (5) | 0.025 (4) | 0.008 (4) | −0.004 (4) | −0.013 (3) |
Geometric parameters (Å, º) top
Rh1—N1i | 1.975 (6) | N2—Rh1i | 1.986 (6) |
Rh1—N2i | 1.986 (6) | N2—H2 | 0.8600 |
Rh1—O1 | 2.026 (5) | O2—C3 | 1.303 (9) |
Rh1—O2 | 2.034 (5) | C1—C2 | 1.504 (10) |
Rh1—O3 | 2.219 (5) | C2—H3 | 0.9600 |
Rh1—Rh1i | 2.4170 (11) | C2—H4 | 0.9600 |
Mo1—O3 | 1.758 (5) | C2—H5 | 0.9600 |
N1—C1 | 1.303 (9) | C3—C4 | 1.492 (10) |
N1—Rh1i | 1.975 (6) | C4—H6 | 0.9600 |
N1—H1 | 0.8600 | C4—H7 | 0.9600 |
O1—C1 | 1.278 (9) | C4—H8 | 0.9600 |
N2—C3 | 1.292 (9) | | |
| | | |
N1i—Rh1—N2i | 91.4 (2) | C1—O1—Rh1 | 118.6 (4) |
N1i—Rh1—O1 | 91.7 (2) | C3—N2—Rh1i | 123.4 (5) |
N2i—Rh1—O1 | 174.1 (2) | C3—N2—H2 | 118.3 |
N1i—Rh1—O2 | 175.7 (2) | Rh1i—N2—H2 | 118.3 |
N2i—Rh1—O2 | 87.4 (2) | C3—O2—Rh1 | 116.8 (5) |
O1—Rh1—O2 | 89.1 (2) | Mo1—O3—Rh1 | 147.0 (3) |
N1i—Rh1—O3 | 90.1 (2) | O1—C1—N1 | 122.2 (6) |
N2i—Rh1—O3 | 99.9 (2) | O1—C1—C2 | 116.5 (7) |
O1—Rh1—O3 | 85.1 (2) | N1—C1—C2 | 121.3 (7) |
O2—Rh1—O3 | 94.2 (2) | C1—C2—H3 | 109.5 |
N1i—Rh1—Rh1i | 86.28 (18) | C1—C2—H4 | 109.5 |
N2i—Rh1—Rh1i | 86.20 (17) | H3—C2—H4 | 109.5 |
O1—Rh1—Rh1i | 89.01 (14) | C1—C2—H5 | 109.5 |
O2—Rh1—Rh1i | 89.48 (14) | H3—C2—H5 | 109.5 |
O3—Rh1—Rh1i | 173.02 (14) | H4—C2—H5 | 109.5 |
O3—Mo1—O3ii | 106.2 (3) | N2—C3—O2 | 122.9 (6) |
O3iii—Mo1—O3iv | 106.2 (3) | N2—C3—C4 | 121.8 (7) |
O3iii—Mo1—O3 | 111.12 (18) | O2—C3—C4 | 115.2 (7) |
O3iv—Mo1—O3 | 111.12 (18) | C3—C4—H6 | 109.5 |
O3iii—Mo1—O3ii | 111.12 (18) | C3—C4—H7 | 109.5 |
O3iv—Mo1—O3ii | 111.12 (18) | H6—C4—H7 | 109.5 |
C1—N1—Rh1i | 123.5 (5) | C3—C4—H8 | 109.5 |
C1—N1—H1 | 118.2 | H6—C4—H8 | 109.5 |
Rh1i—N1—H1 | 118.2 | H7—C4—H8 | 109.5 |
| | | |
N1i—Rh1—O1—C1 | −91.8 (5) | N2i—Rh1—O3—Mo1 | −117.0 (6) |
O2—Rh1—O1—C1 | 83.9 (5) | O1—Rh1—O3—Mo1 | 66.1 (6) |
O3—Rh1—O1—C1 | 178.2 (5) | O2—Rh1—O3—Mo1 | 154.9 (6) |
Rh1i—Rh1—O1—C1 | −5.6 (5) | Rh1—O1—C1—N1 | 3.6 (9) |
N2i—Rh1—O2—C3 | 75.2 (5) | Rh1—O1—C1—C2 | −177.4 (5) |
O1—Rh1—O2—C3 | −100.0 (5) | Rh1i—N1—C1—O1 | 1.8 (10) |
O3—Rh1—O2—C3 | 174.9 (5) | Rh1i—N1—C1—C2 | −177.2 (5) |
Rh1i—Rh1—O2—C3 | −11.0 (5) | Rh1i—N2—C3—O2 | −2.8 (10) |
O3iii—Mo1—O3—Rh1 | 31.1 (7) | Rh1i—N2—C3—C4 | 179.5 (6) |
O3iv—Mo1—O3—Rh1 | −87.0 (8) | Rh1—O2—C3—N2 | 10.7 (9) |
O3ii—Mo1—O3—Rh1 | 152.1 (7) | Rh1—O2—C3—C4 | −171.4 (5) |
N1i—Rh1—O3—Mo1 | −25.6 (6) | | |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.44 | 3.152 (8) | 140 |
N2—H2···O2vi | 0.86 | 2.33 | 3.170 (7) | 164 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C16H32N8O12Rh4W | Dx = 2.740 Mg m−3 |
Mr = 1123.99 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/a | Cell parameters from 2607 reflections |
Hall symbol: -I 4ad | θ = 3.0–27.5° |
a = 9.5905 (8) Å | µ = 6.65 mm−1 |
c = 29.625 (3) Å | T = 296 K |
V = 2724.8 (4) Å3 | Block, brown |
Z = 4 | 0.05 × 0.03 × 0.03 mm |
F(000) = 2136 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1566 independent reflections |
Radiation source: rotating-anode X-ray tube | 1265 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.080 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = −10→12 |
Absorption correction: integration (Higashi, 1999) | k = −12→10 |
Tmin = 0.672, Tmax = 0.801 | l = −24→38 |
11140 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.082 | H-atom parameters constrained |
S = 1.23 | w = 1/[σ2(Fo2) + (0.0229P)2 + 17.8895P] where P = (Fo2 + 2Fc2)/3 |
1566 reflections | (Δ/σ)max < 0.001 |
95 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.63 e Å−3 |
Crystal data top
C16H32N8O12Rh4W | Z = 4 |
Mr = 1123.99 | Mo Kα radiation |
Tetragonal, I41/a | µ = 6.65 mm−1 |
a = 9.5905 (8) Å | T = 296 K |
c = 29.625 (3) Å | 0.05 × 0.03 × 0.03 mm |
V = 2724.8 (4) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1566 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1265 reflections with I > 2σ(I) |
Tmin = 0.672, Tmax = 0.801 | Rint = 0.080 |
11140 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.050 | 0 restraints |
wR(F2) = 0.082 | H-atom parameters constrained |
S = 1.23 | w = 1/[σ2(Fo2) + (0.0229P)2 + 17.8895P] where P = (Fo2 + 2Fc2)/3 |
1566 reflections | Δρmax = 0.86 e Å−3 |
95 parameters | Δρmin = −0.63 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.37426 (6) | 0.25739 (6) | 0.16970 (2) | 0.01719 (17) | |
W1 | 0.0000 | 0.2500 | 0.1250 | 0.02068 (19) | |
N1 | 0.6203 (6) | 0.3954 (6) | 0.1256 (2) | 0.0210 (14) | |
H1 | 0.6985 | 0.4299 | 0.1167 | 0.025* | |
O1 | 0.3858 (5) | 0.4027 (5) | 0.11985 (19) | 0.0226 (12) | |
N2 | 0.6201 (6) | 0.3777 (6) | 0.2211 (2) | 0.0214 (16) | |
H2 | 0.6969 | 0.3987 | 0.2345 | 0.026* | |
O2 | 0.3856 (5) | 0.4126 (5) | 0.21632 (19) | 0.0240 (13) | |
O3 | 0.1451 (6) | 0.2770 (6) | 0.1608 (2) | 0.0323 (15) | |
C1 | 0.5056 (8) | 0.4483 (8) | 0.1086 (3) | 0.0212 (17) | |
C2 | 0.5087 (10) | 0.5597 (9) | 0.0729 (3) | 0.041 (3) | |
H3 | 0.4833 | 0.5199 | 0.0443 | 0.061* | |
H4 | 0.6009 | 0.5981 | 0.0710 | 0.061* | |
H5 | 0.4439 | 0.6321 | 0.0806 | 0.061* | |
C3 | 0.5058 (9) | 0.4346 (8) | 0.2351 (3) | 0.0223 (18) | |
C4 | 0.5073 (10) | 0.5344 (9) | 0.2743 (3) | 0.037 (2) | |
H6 | 0.5020 | 0.6283 | 0.2633 | 0.055* | |
H7 | 0.5921 | 0.5225 | 0.2911 | 0.055* | |
H8 | 0.4289 | 0.5159 | 0.2935 | 0.055* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0117 (3) | 0.0183 (3) | 0.0216 (4) | −0.0002 (2) | 0.0003 (3) | −0.0003 (3) |
W1 | 0.0148 (2) | 0.0148 (2) | 0.0324 (4) | 0.000 | 0.000 | 0.000 |
N1 | 0.015 (3) | 0.021 (3) | 0.027 (4) | −0.004 (2) | 0.000 (3) | −0.001 (3) |
O1 | 0.022 (3) | 0.023 (3) | 0.023 (3) | 0.001 (2) | −0.001 (2) | 0.009 (3) |
N2 | 0.013 (3) | 0.027 (4) | 0.025 (4) | 0.002 (3) | −0.006 (3) | −0.005 (3) |
O2 | 0.020 (3) | 0.020 (3) | 0.031 (4) | 0.003 (2) | 0.001 (3) | −0.002 (3) |
O3 | 0.013 (3) | 0.041 (4) | 0.043 (4) | 0.000 (2) | −0.002 (3) | −0.001 (3) |
C1 | 0.021 (4) | 0.020 (4) | 0.023 (5) | −0.001 (3) | 0.001 (4) | 0.002 (3) |
C2 | 0.037 (5) | 0.028 (5) | 0.057 (7) | 0.005 (4) | 0.008 (5) | 0.018 (5) |
C3 | 0.032 (5) | 0.020 (4) | 0.014 (4) | −0.005 (3) | 0.002 (4) | 0.003 (3) |
C4 | 0.048 (6) | 0.032 (5) | 0.030 (6) | −0.005 (4) | −0.005 (5) | −0.009 (4) |
Geometric parameters (Å, º) top
Rh1—N1i | 1.965 (7) | N2—Rh1i | 2.000 (6) |
Rh1—N2i | 2.000 (6) | N2—H2 | 0.8600 |
Rh1—O2 | 2.033 (5) | O2—C3 | 1.298 (9) |
Rh1—O1 | 2.034 (5) | C1—C2 | 1.504 (11) |
Rh1—O3 | 2.221 (5) | C2—H3 | 0.9600 |
Rh1—Rh1i | 2.4161 (11) | C2—H4 | 0.9600 |
W1—O3 | 1.770 (6) | C2—H5 | 0.9600 |
N1—C1 | 1.311 (9) | C3—C4 | 1.505 (10) |
N1—Rh1i | 1.965 (7) | C4—H6 | 0.9600 |
N1—H1 | 0.8600 | C4—H7 | 0.9600 |
O1—C1 | 1.273 (9) | C4—H8 | 0.9600 |
N2—C3 | 1.292 (9) | | |
| | | |
N1i—Rh1—N2i | 91.3 (3) | C1—O1—Rh1 | 118.3 (5) |
N1i—Rh1—O2 | 175.3 (2) | C3—N2—Rh1i | 122.7 (5) |
N2i—Rh1—O2 | 87.4 (2) | C3—N2—H2 | 118.6 |
N1i—Rh1—O1 | 91.5 (2) | Rh1i—N2—H2 | 118.6 |
N2i—Rh1—O1 | 174.5 (2) | C3—O2—Rh1 | 117.2 (5) |
O2—Rh1—O1 | 89.4 (2) | W1—O3—Rh1 | 146.8 (3) |
N1i—Rh1—O3 | 90.6 (2) | O1—C1—N1 | 121.7 (7) |
N2i—Rh1—O3 | 99.9 (2) | O1—C1—C2 | 116.5 (7) |
O2—Rh1—O3 | 94.1 (2) | N1—C1—C2 | 121.8 (7) |
O1—Rh1—O3 | 84.8 (2) | C1—C2—H3 | 109.5 |
N1i—Rh1—Rh1i | 85.98 (17) | C1—C2—H4 | 109.5 |
N2i—Rh1—Rh1i | 86.27 (17) | H3—C2—H4 | 109.5 |
O2—Rh1—Rh1i | 89.41 (14) | C1—C2—H5 | 109.5 |
O1—Rh1—Rh1i | 89.20 (14) | H3—C2—H5 | 109.5 |
O3—Rh1—Rh1i | 173.05 (16) | H4—C2—H5 | 109.5 |
O3—W1—O3ii | 106.3 (4) | N2—C3—O2 | 123.2 (7) |
O3iii—W1—O3iv | 106.3 (4) | N2—C3—C4 | 120.5 (8) |
O3iii—W1—O3 | 111.1 (2) | O2—C3—C4 | 116.3 (7) |
O3iv—W1—O3 | 111.1 (2) | C3—C4—H6 | 109.5 |
O3iii—W1—O3ii | 111.1 (2) | C3—C4—H7 | 109.5 |
O3iv—W1—O3ii | 111.1 (2) | H6—C4—H7 | 109.5 |
C1—N1—Rh1i | 124.4 (5) | C3—C4—H8 | 109.5 |
C1—N1—H1 | 117.8 | H6—C4—H8 | 109.5 |
Rh1i—N1—H1 | 117.8 | H7—C4—H8 | 109.5 |
| | | |
N1i—Rh1—O1—C1 | −93.0 (6) | N2i—Rh1—O3—W1 | −116.4 (6) |
O2—Rh1—O1—C1 | 82.4 (6) | O2—Rh1—O3—W1 | 155.5 (6) |
O3—Rh1—O1—C1 | 176.5 (6) | O1—Rh1—O3—W1 | 66.5 (6) |
Rh1i—Rh1—O1—C1 | −7.1 (6) | Rh1—O1—C1—N1 | 6.0 (10) |
N2i—Rh1—O2—C3 | 75.4 (5) | Rh1—O1—C1—C2 | −177.7 (6) |
O1—Rh1—O2—C3 | −100.1 (5) | Rh1i—N1—C1—O1 | −0.3 (11) |
O3—Rh1—O2—C3 | 175.1 (5) | Rh1i—N1—C1—C2 | −176.4 (6) |
Rh1i—Rh1—O2—C3 | −10.9 (5) | Rh1i—N2—C3—O2 | −2.0 (11) |
O3iii—W1—O3—Rh1 | 30.2 (6) | Rh1i—N2—C3—C4 | 179.3 (5) |
O3iv—W1—O3—Rh1 | −87.9 (7) | Rh1—O2—C3—N2 | 10.2 (10) |
O3ii—W1—O3—Rh1 | 151.1 (7) | Rh1—O2—C3—C4 | −171.0 (5) |
N1i—Rh1—O3—W1 | −24.9 (6) | | |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.47 | 3.174 (8) | 140 |
N2—H2···O2vi | 0.86 | 2.33 | 3.168 (8) | 165 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C16H32CrN8O12Ru4 | Dx = 2.442 Mg m−3 |
Mr = 984.78 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/a | Cell parameters from 3954 reflections |
Hall symbol: -I 4ad | θ = 3.0–27.5° |
a = 9.4232 (5) Å | µ = 2.67 mm−1 |
c = 30.168 (3) Å | T = 296 K |
V = 2678.9 (3) Å3 | Block, brown |
Z = 4 | 0.08 × 0.08 × 0.06 mm |
F(000) = 1920 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1539 independent reflections |
Radiation source: rotating-anode X-ray tube | 1475 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 4.0° |
ω scans | h = −11→12 |
Absorption correction: integration (Higashi, 1999) | k = −11→12 |
Tmin = 0.833, Tmax = 0.871 | l = −39→26 |
10957 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.33 | w = 1/[σ2(Fo2) + (0.0172P)2 + 12.7943P] where P = (Fo2 + 2Fc2)/3 |
1539 reflections | (Δ/σ)max < 0.001 |
95 parameters | Δρmax = 0.58 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
Crystal data top
C16H32CrN8O12Ru4 | Z = 4 |
Mr = 984.78 | Mo Kα radiation |
Tetragonal, I41/a | µ = 2.67 mm−1 |
a = 9.4232 (5) Å | T = 296 K |
c = 30.168 (3) Å | 0.08 × 0.08 × 0.06 mm |
V = 2678.9 (3) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1539 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1475 reflections with I > 2σ(I) |
Tmin = 0.833, Tmax = 0.871 | Rint = 0.042 |
10957 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.33 | w = 1/[σ2(Fo2) + (0.0172P)2 + 12.7943P] where P = (Fo2 + 2Fc2)/3 |
1539 reflections | Δρmax = 0.58 e Å−3 |
95 parameters | Δρmin = −0.49 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Ru1 | 0.37778 (3) | 0.25660 (3) | 0.168745 (9) | 0.01376 (10) | |
Cr1 | 0.0000 | 0.2500 | 0.1250 | 0.0181 (3) | |
N1 | 0.6206 (4) | 0.3996 (4) | 0.12358 (11) | 0.0178 (7) | |
H1 | 0.7004 | 0.4339 | 0.1148 | 0.021* | |
O1 | 0.3823 (3) | 0.4060 (3) | 0.11980 (9) | 0.0197 (6) | |
N2 | 0.6197 (4) | 0.3832 (4) | 0.22004 (10) | 0.0192 (7) | |
H2 | 0.6987 | 0.4069 | 0.2322 | 0.023* | |
O2 | 0.3820 (3) | 0.4137 (3) | 0.21617 (9) | 0.0209 (6) | |
O3 | 0.1409 (3) | 0.2678 (4) | 0.15736 (10) | 0.0294 (7) | |
C1 | 0.5040 (5) | 0.4513 (4) | 0.10698 (12) | 0.0191 (8) | |
C2 | 0.5045 (6) | 0.5629 (5) | 0.07182 (16) | 0.0341 (11) | |
H3 | 0.4811 | 0.5207 | 0.0438 | 0.051* | |
H4 | 0.5971 | 0.6051 | 0.0701 | 0.051* | |
H5 | 0.4358 | 0.6345 | 0.0790 | 0.051* | |
C3 | 0.5028 (5) | 0.4379 (4) | 0.23502 (12) | 0.0192 (8) | |
C4 | 0.5009 (6) | 0.5324 (6) | 0.27483 (14) | 0.0361 (12) | |
H6 | 0.4575 | 0.6213 | 0.2673 | 0.054* | |
H7 | 0.5964 | 0.5488 | 0.2847 | 0.054* | |
H8 | 0.4477 | 0.4879 | 0.2981 | 0.054* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru1 | 0.01003 (17) | 0.01556 (18) | 0.01570 (15) | −0.00014 (12) | 0.00020 (11) | 0.00047 (11) |
Cr1 | 0.0143 (4) | 0.0143 (4) | 0.0256 (6) | 0.000 | 0.000 | 0.000 |
N1 | 0.0126 (17) | 0.0202 (18) | 0.0205 (15) | −0.0044 (14) | 0.0027 (13) | 0.0008 (13) |
O1 | 0.0158 (15) | 0.0220 (16) | 0.0213 (14) | 0.0003 (12) | 0.0001 (11) | 0.0059 (11) |
N2 | 0.0149 (18) | 0.0215 (19) | 0.0211 (17) | −0.0020 (15) | −0.0042 (13) | −0.0060 (13) |
O2 | 0.0199 (15) | 0.0224 (16) | 0.0205 (14) | 0.0025 (12) | −0.0004 (11) | −0.0047 (11) |
O3 | 0.0090 (15) | 0.042 (2) | 0.0368 (16) | 0.0006 (14) | −0.0018 (12) | −0.0023 (15) |
C1 | 0.024 (2) | 0.017 (2) | 0.0165 (17) | −0.0008 (17) | 0.0021 (16) | −0.0010 (15) |
C2 | 0.031 (3) | 0.029 (3) | 0.042 (3) | 0.001 (2) | 0.002 (2) | 0.019 (2) |
C3 | 0.026 (2) | 0.014 (2) | 0.0168 (18) | −0.0002 (18) | 0.0004 (16) | −0.0005 (14) |
C4 | 0.046 (3) | 0.037 (3) | 0.025 (2) | 0.006 (2) | −0.003 (2) | −0.016 (2) |
Geometric parameters (Å, º) top
Ru1—N1i | 2.006 (3) | N2—Ru1i | 2.032 (3) |
Ru1—N2i | 2.033 (3) | N2—H2 | 0.8600 |
Ru1—O1 | 2.041 (3) | O2—C3 | 1.293 (5) |
Ru1—O2 | 2.059 (3) | C1—C2 | 1.493 (6) |
Ru1—O3 | 2.261 (3) | C2—H3 | 0.9600 |
Ru1—Ru1i | 2.3068 (6) | C2—H4 | 0.9600 |
Cr1—O3 | 1.657 (3) | C2—H5 | 0.9600 |
N1—C1 | 1.302 (5) | C3—C4 | 1.495 (6) |
N1—Ru1i | 2.006 (3) | C4—H6 | 0.9600 |
N1—H1 | 0.8600 | C4—H7 | 0.9600 |
O1—C1 | 1.283 (5) | C4—H8 | 0.9600 |
N2—C3 | 1.298 (5) | | |
| | | |
N1i—Ru1—N2i | 92.38 (14) | C1—O1—Ru1 | 117.8 (3) |
N1i—Ru1—O1 | 90.84 (13) | C3—N2—Ru1i | 122.2 (3) |
N2i—Ru1—O1 | 176.27 (13) | C3—N2—H2 | 118.9 |
N1i—Ru1—O2 | 178.04 (13) | Ru1i—N2—H2 | 118.9 |
N2i—Ru1—O2 | 86.38 (13) | C3—O2—Ru1 | 116.7 (2) |
O1—Ru1—O2 | 90.36 (12) | Cr1—O3—Ru1 | 151.18 (18) |
N1i—Ru1—O3 | 86.48 (13) | O1—C1—N1 | 120.9 (4) |
N2i—Ru1—O3 | 99.07 (13) | O1—C1—C2 | 116.8 (4) |
O1—Ru1—O3 | 83.00 (12) | N1—C1—C2 | 122.3 (4) |
O2—Ru1—O3 | 95.21 (12) | C1—C2—H3 | 109.5 |
N1i—Ru1—Ru1i | 87.30 (10) | C1—C2—H4 | 109.5 |
N2i—Ru1—Ru1i | 87.32 (10) | H3—C2—H4 | 109.5 |
O1—Ru1—Ru1i | 90.95 (8) | C1—C2—H5 | 109.5 |
O2—Ru1—Ru1i | 91.13 (8) | H3—C2—H5 | 109.5 |
O3—Ru1—Ru1i | 171.26 (8) | H4—C2—H5 | 109.5 |
O3ii—Cr1—O3 | 107.8 (2) | O2—C3—N2 | 121.6 (3) |
O3iii—Cr1—O3iv | 107.8 (2) | O2—C3—C4 | 116.6 (4) |
O3iii—Cr1—O3ii | 110.32 (11) | N2—C3—C4 | 121.8 (4) |
O3iv—Cr1—O3ii | 110.32 (11) | C3—C4—H6 | 109.5 |
O3iii—Cr1—O3 | 110.32 (11) | C3—C4—H7 | 109.5 |
O3iv—Cr1—O3 | 110.32 (11) | H6—C4—H7 | 109.5 |
C1—N1—Ru1i | 122.8 (3) | C3—C4—H8 | 109.5 |
C1—N1—H1 | 118.6 | H6—C4—H8 | 109.5 |
Ru1i—N1—H1 | 118.6 | H7—C4—H8 | 109.5 |
| | | |
N1i—Ru1—O1—C1 | −91.7 (3) | N2i—Ru1—O3—Cr1 | −122.3 (4) |
O2—Ru1—O1—C1 | 86.8 (3) | O1—Ru1—O3—Cr1 | 60.8 (4) |
O3—Ru1—O1—C1 | −178.0 (3) | O2—Ru1—O3—Cr1 | 150.6 (4) |
Ru1i—Ru1—O1—C1 | −4.3 (3) | Ru1—O1—C1—N1 | 2.5 (5) |
O1—Ru1—O2—C3 | −101.3 (3) | Ru1—O1—C1—C2 | −178.7 (3) |
O3—Ru1—O2—C3 | 175.7 (3) | Ru1i—N1—C1—O1 | 1.7 (5) |
Ru1i—Ru1—O2—C3 | −10.4 (3) | Ru1i—N1—C1—C2 | −177.1 (3) |
O3iii—Cr1—O3—Ru1 | 38.8 (5) | Ru1—O2—C3—N2 | 10.9 (5) |
O3iv—Cr1—O3—Ru1 | −80.2 (5) | Ru1—O2—C3—C4 | −169.3 (3) |
O3ii—Cr1—O3—Ru1 | 159.3 (5) | Ru1i—N2—C3—O2 | −4.7 (6) |
N1i—Ru1—O3—Cr1 | −30.4 (4) | Ru1i—N2—C3—C4 | 175.5 (3) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.35 | 3.046 (4) | 138 |
N2—H2···O2vi | 0.86 | 2.33 | 3.146 (4) | 159 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C16H32MoN8O12Ru4 | Dx = 2.503 Mg m−3 |
Mr = 1028.72 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/a | Cell parameters from 2775 reflections |
Hall symbol: -I 4ad | θ = 3.3–27.5° |
a = 9.5504 (5) Å | µ = 2.68 mm−1 |
c = 29.933 (3) Å | T = 296 K |
V = 2730.2 (3) Å3 | Prism, dark brown |
Z = 4 | 0.30 × 0.10 × 0.10 mm |
F(000) = 1992 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1568 independent reflections |
Radiation source: rotating-anode X-ray tube | 1156 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.112 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −12→7 |
Absorption correction: integration (Higashi, 1999) | k = −12→12 |
Tmin = 0.844, Tmax = 0.931 | l = −37→38 |
10984 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0349P)2] where P = (Fo2 + 2Fc2)/3 |
1568 reflections | (Δ/σ)max < 0.001 |
96 parameters | Δρmax = 0.99 e Å−3 |
0 restraints | Δρmin = −0.84 e Å−3 |
Crystal data top
C16H32MoN8O12Ru4 | Z = 4 |
Mr = 1028.72 | Mo Kα radiation |
Tetragonal, I41/a | µ = 2.68 mm−1 |
a = 9.5504 (5) Å | T = 296 K |
c = 29.933 (3) Å | 0.30 × 0.10 × 0.10 mm |
V = 2730.2 (3) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1568 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1156 reflections with I > 2σ(I) |
Tmin = 0.844, Tmax = 0.931 | Rint = 0.112 |
10984 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.056 | 0 restraints |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.99 e Å−3 |
1568 reflections | Δρmin = −0.84 e Å−3 |
96 parameters | |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Ru1 | 0.37996 (6) | 0.25615 (12) | 0.16978 (2) | 0.0232 (2) | |
Mo1 | 0.0000 | 0.2500 | 0.1250 | 0.0256 (4) | |
N1 | 0.6181 (9) | 0.3999 (9) | 0.1245 (3) | 0.025 (2) | |
H1 | 0.6968 | 0.4344 | 0.1158 | 0.030* | |
O1 | 0.3847 (8) | 0.4052 (7) | 0.1199 (3) | 0.029 (2) | |
N2 | 0.6181 (9) | 0.3819 (9) | 0.2209 (3) | 0.026 (2) | |
H2 | 0.6960 | 0.4037 | 0.2335 | 0.031* | |
O2 | 0.3830 (7) | 0.4111 (7) | 0.2169 (3) | 0.030 (2) | |
O3 | 0.1471 (5) | 0.2672 (9) | 0.1605 (2) | 0.0404 (19) | |
C1 | 0.5042 (15) | 0.4504 (7) | 0.1078 (3) | 0.0249 (18) | |
C2 | 0.5035 (16) | 0.5587 (9) | 0.0716 (3) | 0.045 (3) | |
H3 | 0.4754 | 0.5162 | 0.0439 | 0.068* | |
H4 | 0.5957 | 0.5974 | 0.0684 | 0.068* | |
H5 | 0.4389 | 0.6319 | 0.0792 | 0.068* | |
C3 | 0.5029 (15) | 0.4391 (7) | 0.2353 (3) | 0.0258 (19) | |
C4 | 0.5023 (17) | 0.5361 (9) | 0.2753 (3) | 0.046 (3) | |
H6 | 0.5966 | 0.5505 | 0.2854 | 0.070* | |
H7 | 0.4480 | 0.4950 | 0.2989 | 0.070* | |
H8 | 0.4619 | 0.6243 | 0.2669 | 0.070* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru1 | 0.0153 (3) | 0.0226 (4) | 0.0317 (4) | 0.0006 (4) | 0.0002 (3) | −0.0008 (5) |
Mo1 | 0.0174 (4) | 0.0174 (4) | 0.0420 (10) | 0.000 | 0.000 | 0.000 |
N1 | 0.012 (4) | 0.030 (5) | 0.033 (7) | 0.003 (4) | 0.008 (4) | −0.003 (4) |
O1 | 0.022 (4) | 0.024 (4) | 0.039 (6) | 0.003 (3) | 0.000 (4) | 0.013 (4) |
N2 | 0.022 (5) | 0.033 (5) | 0.023 (6) | −0.002 (4) | −0.007 (4) | −0.009 (4) |
O2 | 0.019 (4) | 0.026 (4) | 0.043 (6) | 0.001 (3) | 0.005 (4) | −0.008 (4) |
O3 | 0.006 (3) | 0.053 (5) | 0.063 (5) | −0.003 (3) | 0.000 (3) | 0.002 (5) |
C1 | 0.030 (4) | 0.015 (4) | 0.029 (5) | −0.010 (6) | 0.004 (7) | −0.002 (3) |
C2 | 0.047 (6) | 0.036 (5) | 0.053 (7) | −0.012 (7) | −0.004 (9) | 0.023 (5) |
C3 | 0.033 (4) | 0.014 (4) | 0.030 (5) | −0.007 (6) | −0.006 (7) | 0.008 (3) |
C4 | 0.060 (6) | 0.041 (5) | 0.038 (6) | 0.005 (8) | −0.015 (10) | −0.013 (5) |
Geometric parameters (Å, º) top
Ru1—N1i | 2.015 (9) | N2—Ru1i | 2.019 (9) |
Ru1—N2i | 2.020 (9) | N2—H2 | 0.8600 |
Ru1—O2 | 2.045 (7) | O2—C3 | 1.299 (13) |
Ru1—O1 | 2.063 (7) | C1—C2 | 1.499 (10) |
Ru1—O3 | 2.244 (5) | C2—H3 | 0.9600 |
Ru1—Ru1i | 2.2958 (12) | C2—H4 | 0.9600 |
Mo1—O3 | 1.769 (6) | C2—H5 | 0.9600 |
N1—C1 | 1.290 (14) | C3—C4 | 1.512 (11) |
N1—Ru1i | 2.015 (9) | C4—H6 | 0.9600 |
N1—H1 | 0.8600 | C4—H7 | 0.9600 |
O1—C1 | 1.272 (13) | C4—H8 | 0.9600 |
N2—C3 | 1.302 (14) | | |
| | | |
N1i—Ru1—N2i | 91.5 (4) | C1—O1—Ru1 | 117.4 (6) |
N1i—Ru1—O2 | 178.1 (3) | C3—N2—Ru1i | 122.2 (7) |
N2i—Ru1—O2 | 87.1 (3) | C3—N2—H2 | 118.9 |
N1i—Ru1—O1 | 91.3 (2) | Ru1i—N2—H2 | 118.9 |
N2i—Ru1—O1 | 176.6 (3) | C3—O2—Ru1 | 117.0 (6) |
O2—Ru1—O1 | 90.0 (3) | Mo1—O3—Ru1 | 149.0 (4) |
N1i—Ru1—O3 | 87.7 (3) | O1—C1—N1 | 121.3 (7) |
N2i—Ru1—O3 | 97.7 (3) | O1—C1—C2 | 115.8 (12) |
O2—Ru1—O3 | 93.8 (3) | N1—C1—C2 | 122.8 (12) |
O1—Ru1—O3 | 84.2 (3) | C1—C2—H3 | 109.5 |
N1i—Ru1—Ru1i | 87.3 (2) | C1—C2—H4 | 109.5 |
N2i—Ru1—Ru1i | 87.6 (2) | H3—C2—H4 | 109.5 |
O2—Ru1—Ru1i | 91.3 (2) | C1—C2—H5 | 109.5 |
O1—Ru1—Ru1i | 90.8 (2) | H3—C2—H5 | 109.5 |
O3—Ru1—Ru1i | 172.86 (18) | H4—C2—H5 | 109.5 |
O3ii—Mo1—O3 | 106.2 (4) | O2—C3—N2 | 121.2 (7) |
O3ii—Mo1—O3iii | 111.1 (2) | O2—C3—C4 | 117.3 (12) |
O3—Mo1—O3iii | 111.1 (2) | N2—C3—C4 | 121.5 (12) |
O3ii—Mo1—O3iv | 111.1 (2) | C3—C4—H6 | 109.5 |
O3—Mo1—O3iv | 111.1 (2) | C3—C4—H7 | 109.5 |
O3iii—Mo1—O3iv | 106.2 (4) | H6—C4—H7 | 109.5 |
C1—N1—Ru1i | 123.0 (7) | C3—C4—H8 | 109.5 |
C1—N1—H1 | 118.5 | H6—C4—H8 | 109.5 |
Ru1i—N1—H1 | 118.5 | H7—C4—H8 | 109.5 |
| | | |
N1i—Ru1—O1—C1 | −92.6 (7) | N2i—Ru1—O3—Mo1 | −124.2 (9) |
O2—Ru1—O1—C1 | 86.0 (7) | O2—Ru1—O3—Mo1 | 148.3 (9) |
O3—Ru1—O1—C1 | 179.8 (7) | O1—Ru1—O3—Mo1 | 58.7 (9) |
Ru1i—Ru1—O1—C1 | −5.3 (6) | Ru1—O1—C1—N1 | 3.4 (10) |
N2i—Ru1—O2—C3 | 78.8 (7) | Ru1—O1—C1—C2 | −179.9 (6) |
O1—Ru1—O2—C3 | −99.4 (6) | Ru1i—N1—C1—O1 | 1.3 (11) |
O3—Ru1—O2—C3 | 176.4 (6) | Ru1i—N1—C1—C2 | −175.2 (7) |
Ru1i—Ru1—O2—C3 | −8.7 (6) | Ru1—O2—C3—N2 | 7.4 (10) |
O3ii—Mo1—O3—Ru1 | 161.6 (11) | Ru1—O2—C3—C4 | −170.3 (6) |
O3iii—Mo1—O3—Ru1 | 40.6 (11) | Ru1i—N2—C3—O2 | −1.0 (11) |
O3iv—Mo1—O3—Ru1 | −77.4 (11) | Ru1i—N2—C3—C4 | 176.6 (6) |
N1i—Ru1—O3—Mo1 | −32.9 (9) | | |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.42 | 3.122 (8) | 140 |
N2—H2···O2vi | 0.86 | 2.32 | 3.154 (8) | 162 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C16H32N8O12Ru4W | Dx = 2.703 Mg m−3 |
Mr = 1116.63 | Mo Kα radiation, λ = 0.71070 Å |
Tetragonal, I41/a | Cell parameters from 3975 reflections |
Hall symbol: -I 4ad | θ = 3.3–27.5° |
a = 9.5668 (7) Å | µ = 6.40 mm−1 |
c = 29.980 (3) Å | T = 296 K |
V = 2743.9 (4) Å3 | Block, brown |
Z = 4 | 0.06 × 0.06 × 0.04 mm |
F(000) = 2120 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1580 independent reflections |
Graphite monochromator | 1543 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.050 |
ω scans | θmax = 27.5°, θmin = 3.3° |
Absorption correction: integration (Higashi, 1999) | h = −12→9 |
Tmin = 0.621, Tmax = 0.831 | k = −12→11 |
10895 measured reflections | l = −25→38 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (0.0074P)2 + 37.8978P] where P = (Fo2 + 2Fc2)/3 |
1580 reflections | (Δ/σ)max < 0.001 |
96 parameters | Δρmax = 0.64 e Å−3 |
0 restraints | Δρmin = −0.80 e Å−3 |
Crystal data top
C16H32N8O12Ru4W | Z = 4 |
Mr = 1116.63 | Mo Kα radiation |
Tetragonal, I41/a | µ = 6.40 mm−1 |
a = 9.5668 (7) Å | T = 296 K |
c = 29.980 (3) Å | 0.06 × 0.06 × 0.04 mm |
V = 2743.9 (4) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 1580 independent reflections |
Absorption correction: integration (Higashi, 1999) | 1543 reflections with I > 2σ(I) |
Tmin = 0.621, Tmax = 0.831 | Rint = 0.050 |
10895 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (0.0074P)2 + 37.8978P] where P = (Fo2 + 2Fc2)/3 |
1580 reflections | Δρmax = 0.64 e Å−3 |
96 parameters | Δρmin = −0.80 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Ru1 | 0.38025 (5) | 0.25719 (9) | 0.169932 (17) | 0.01477 (13) | |
W1 | 0.0000 | 0.2500 | 0.1250 | 0.01743 (13) | |
N1 | 0.6186 (9) | 0.3999 (9) | 0.1249 (2) | 0.0190 (18) | |
H1 | 0.6973 | 0.4350 | 0.1167 | 0.023* | |
O1 | 0.3841 (8) | 0.4045 (7) | 0.1206 (2) | 0.0216 (16) | |
N2 | 0.6175 (9) | 0.3831 (8) | 0.2217 (2) | 0.0195 (15) | |
H2 | 0.6952 | 0.4053 | 0.2343 | 0.023* | |
O2 | 0.3834 (8) | 0.4120 (7) | 0.2171 (2) | 0.0242 (15) | |
O3 | 0.1485 (5) | 0.2698 (8) | 0.16017 (19) | 0.0287 (15) | |
C1 | 0.5063 (12) | 0.4500 (6) | 0.1078 (2) | 0.0168 (13) | |
C2 | 0.5002 (16) | 0.5611 (8) | 0.0723 (3) | 0.039 (2) | |
H3 | 0.4658 | 0.5212 | 0.0451 | 0.059* | |
H4 | 0.5922 | 0.5983 | 0.0675 | 0.059* | |
H5 | 0.4388 | 0.6347 | 0.0818 | 0.059* | |
C3 | 0.5032 (14) | 0.4390 (6) | 0.2361 (2) | 0.0210 (13) | |
C4 | 0.5062 (18) | 0.5369 (8) | 0.2744 (3) | 0.0368 (19) | |
H6 | 0.4533 | 0.4982 | 0.2987 | 0.055* | |
H7 | 0.4661 | 0.6247 | 0.2657 | 0.055* | |
H8 | 0.6012 | 0.5511 | 0.2837 | 0.055* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru1 | 0.0100 (2) | 0.0167 (3) | 0.0177 (3) | 0.0002 (3) | 0.00008 (18) | −0.0003 (4) |
W1 | 0.01293 (16) | 0.01293 (16) | 0.0264 (3) | 0.000 | 0.000 | 0.000 |
N1 | 0.013 (4) | 0.021 (4) | 0.023 (5) | 0.000 (3) | −0.001 (3) | −0.004 (3) |
O1 | 0.017 (3) | 0.023 (4) | 0.025 (4) | −0.001 (3) | −0.003 (3) | 0.010 (3) |
N2 | 0.012 (3) | 0.026 (4) | 0.020 (4) | −0.003 (3) | −0.006 (3) | −0.006 (3) |
O2 | 0.027 (3) | 0.027 (3) | 0.019 (3) | 0.004 (3) | 0.000 (3) | 0.001 (3) |
O3 | 0.008 (2) | 0.038 (4) | 0.040 (3) | 0.001 (2) | 0.000 (2) | −0.003 (3) |
C1 | 0.019 (3) | 0.014 (3) | 0.018 (3) | −0.003 (4) | 0.002 (5) | 0.004 (2) |
C2 | 0.037 (4) | 0.036 (4) | 0.045 (5) | −0.006 (7) | −0.005 (8) | 0.024 (4) |
C3 | 0.026 (3) | 0.017 (3) | 0.019 (3) | 0.003 (5) | 0.002 (6) | 0.001 (2) |
C4 | 0.047 (5) | 0.038 (4) | 0.026 (4) | 0.007 (6) | 0.000 (7) | −0.017 (3) |
Geometric parameters (Å, º) top
Ru1—N1i | 2.021 (8) | N2—Ru1i | 2.053 (7) |
Ru1—N2i | 2.053 (7) | N2—H2 | 0.8600 |
Ru1—O1 | 2.043 (6) | O2—C3 | 1.305 (14) |
Ru1—O2 | 2.048 (7) | C1—C2 | 1.505 (9) |
Ru1—O3 | 2.239 (5) | C2—H3 | 0.9600 |
Ru1—Ru1i | 2.2954 (9) | C2—H4 | 0.9600 |
W1—O3 | 1.780 (5) | C2—H5 | 0.9600 |
N1—C1 | 1.282 (14) | C3—C4 | 1.483 (9) |
N1—Ru1i | 2.021 (8) | C4—H6 | 0.9600 |
N1—H1 | 0.8600 | C4—H7 | 0.9600 |
O1—C1 | 1.305 (13) | C4—H8 | 0.9600 |
N2—C3 | 1.291 (14) | | |
| | | |
N1i—Ru1—O1 | 91.7 (2) | C1—O1—Ru1 | 117.3 (5) |
N1i—Ru1—O2 | 177.9 (3) | C3—N2—Ru1i | 122.1 (6) |
O1—Ru1—O2 | 90.0 (3) | C3—N2—H2 | 119.0 |
N1i—Ru1—N2i | 91.1 (3) | Ru1i—N2—H2 | 119.0 |
O1—Ru1—N2i | 176.7 (3) | C3—O2—Ru1 | 117.1 (6) |
O2—Ru1—N2i | 87.1 (2) | W1—O3—Ru1 | 149.6 (3) |
N1i—Ru1—O3 | 87.6 (3) | N1—C1—O1 | 120.6 (6) |
O1—Ru1—O3 | 83.5 (3) | N1—C1—C2 | 125.3 (11) |
O2—Ru1—O3 | 93.8 (3) | O1—C1—C2 | 114.1 (10) |
N2i—Ru1—O3 | 98.3 (3) | C1—C2—H3 | 109.5 |
N1i—Ru1—Ru1i | 87.1 (2) | C1—C2—H4 | 109.5 |
O1—Ru1—Ru1i | 91.3 (2) | H3—C2—H4 | 109.5 |
O2—Ru1—Ru1i | 91.7 (2) | C1—C2—H5 | 109.5 |
N2i—Ru1—Ru1i | 87.2 (2) | H3—C2—H5 | 109.5 |
O3—Ru1—Ru1i | 172.48 (15) | H4—C2—H5 | 109.5 |
O3—W1—O3ii | 107.3 (4) | N2—C3—O2 | 121.2 (6) |
O3iii—W1—O3iv | 107.3 (4) | N2—C3—C4 | 120.2 (11) |
O3iii—W1—O3 | 110.56 (18) | O2—C3—C4 | 118.6 (11) |
O3iv—W1—O3 | 110.56 (18) | C3—C4—H6 | 109.5 |
O3iii—W1—O3ii | 110.56 (18) | C3—C4—H7 | 109.5 |
O3iv—W1—O3ii | 110.56 (18) | H6—C4—H7 | 109.5 |
C1—N1—Ru1i | 123.3 (7) | C3—C4—H8 | 109.5 |
C1—N1—H1 | 118.4 | H6—C4—H8 | 109.5 |
Ru1i—N1—H1 | 118.4 | H7—C4—H8 | 109.5 |
| | | |
N1i—Ru1—O1—C1 | −92.1 (6) | O1—Ru1—O3—W1 | 61.2 (8) |
O2—Ru1—O1—C1 | 86.7 (6) | O2—Ru1—O3—W1 | 150.8 (8) |
O3—Ru1—O1—C1 | −179.5 (6) | N2i—Ru1—O3—W1 | −121.6 (8) |
Ru1i—Ru1—O1—C1 | −5.0 (6) | Ru1i—N1—C1—O1 | 3.1 (9) |
O1—Ru1—O2—C3 | −100.5 (6) | Ru1i—N1—C1—C2 | −176.4 (6) |
N2i—Ru1—O2—C3 | 77.9 (6) | Ru1—O1—C1—N1 | 2.1 (8) |
O3—Ru1—O2—C3 | 176.0 (5) | Ru1—O1—C1—C2 | −178.4 (5) |
Ru1i—Ru1—O2—C3 | −9.2 (5) | Ru1i—N2—C3—O2 | −2.2 (10) |
O3iii—W1—O3—Ru1 | 38.0 (9) | Ru1i—N2—C3—C4 | 178.3 (5) |
O3iv—W1—O3—Ru1 | −80.7 (10) | Ru1—O2—C3—N2 | 8.5 (9) |
O3ii—W1—O3—Ru1 | 158.7 (10) | Ru1—O2—C3—C4 | −172.1 (5) |
N1i—Ru1—O3—W1 | −30.8 (8) | | |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4; (iv) −y+1/4, x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1v | 0.86 | 2.40 | 3.122 (7) | 141 |
N2—H2···O2vi | 0.86 | 2.32 | 3.147 (7) | 163 |
Symmetry codes: (v) −y+5/4, x+1/4, −z+1/4; (vi) x+1/2, y, −z+1/2. |
Crystal data top
C24H48CrN8O12Rh4·1.08(H2O) | Z = 2 |
Mr = 1123.76 | F(000) = 1116 |
Triclinic, P1 | Dx = 1.758 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
a = 12.978 (2) Å | Cell parameters from 4246 reflections |
b = 13.576 (3) Å | θ = 3.1–27.5° |
c = 14.498 (3) Å | µ = 1.83 mm−1 |
α = 112.405 (5)° | T = 296 K |
β = 101.362 (4)° | Prism, brown |
γ = 106.816 (5)° | 0.30 × 0.10 × 0.10 mm |
V = 2120.1 (8) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 9650 independent reflections |
Graphite monochromator | 6828 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.065 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: integration (Higashi, 1999) | h = −16→16 |
Tmin = 0.843, Tmax = 0.945 | k = −16→17 |
17505 measured reflections | l = −18→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.089 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.133 | H-atom parameters constrained |
S = 1.17 | w = 1/[σ2(Fo2) + (0.P)2 + 19.3981P] where P = (Fo2 + 2Fc2)/3 |
9650 reflections | (Δ/σ)max < 0.001 |
588 parameters | Δρmax = 0.88 e Å−3 |
394 restraints | Δρmin = −0.93 e Å−3 |
Crystal data top
C24H48CrN8O12Rh4·1.08(H2O) | γ = 106.816 (5)° |
Mr = 1123.76 | V = 2120.1 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.978 (2) Å | Mo Kα radiation |
b = 13.576 (3) Å | µ = 1.83 mm−1 |
c = 14.498 (3) Å | T = 296 K |
α = 112.405 (5)° | 0.30 × 0.10 × 0.10 mm |
β = 101.362 (4)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 9650 independent reflections |
Absorption correction: integration (Higashi, 1999) | 6828 reflections with I > 2σ(I) |
Tmin = 0.843, Tmax = 0.945 | Rint = 0.065 |
17505 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.089 | 394 restraints |
wR(F2) = 0.133 | H-atom parameters constrained |
S = 1.17 | w = 1/[σ2(Fo2) + (0.P)2 + 19.3981P] where P = (Fo2 + 2Fc2)/3 |
9650 reflections | Δρmax = 0.88 e Å−3 |
588 parameters | Δρmin = −0.93 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.90911 (6) | 0.43100 (6) | 0.48748 (6) | 0.01574 (17) | |
Rh2 | 0.53889 (6) | 0.44323 (6) | 0.44196 (6) | 0.01450 (17) | |
Rh3 | 0.50903 (6) | 0.05012 (6) | 0.44729 (6) | 0.01919 (18) | |
Rh4 | 0.56458 (6) | 0.05915 (7) | 0.09075 (6) | 0.0230 (2) | |
N1 | 0.9308 (6) | 0.3172 (7) | 0.3670 (7) | 0.032 (2) | |
H1 | 0.8808 | 0.2464 | 0.3337 | 0.039* | |
O1 | 1.1015 (5) | 0.4457 (6) | 0.3861 (5) | 0.0312 (18) | |
N2 | 0.8427 (6) | 0.4852 (7) | 0.3932 (7) | 0.029 (2) | |
H2 | 0.7691 | 0.4565 | 0.3662 | 0.035* | |
O2 | 1.0107 (5) | 0.6132 (7) | 0.4103 (6) | 0.042 (2) | |
N3 | 0.6313 (6) | 0.4490 (6) | 0.5726 (6) | 0.0205 (18) | |
H3 | 0.6772 | 0.4141 | 0.5667 | 0.025* | |
O3 | 0.5550 (5) | 0.5493 (5) | 0.6828 (5) | 0.0210 (15) | |
N4 | 0.4072 (6) | 0.3062 (6) | 0.4161 (6) | 0.0216 (18) | |
H4 | 0.4027 | 0.2386 | 0.3748 | 0.026* | |
O4 | 0.3329 (5) | 0.4074 (5) | 0.5260 (5) | 0.0210 (15) | |
N5 | 0.4804 (6) | 0.1701 (6) | 0.5566 (6) | 0.0226 (18) | |
H5 | 0.4798 | 0.2297 | 0.5489 | 0.027* | |
O5 | 0.4655 (5) | 0.0813 (6) | 0.6600 (5) | 0.0251 (16) | |
N6 | 0.6741 (6) | 0.1250 (6) | 0.5316 (6) | 0.0183 (17) | |
H6 | 0.7182 | 0.1721 | 0.5158 | 0.022* | |
O6 | 0.6629 (5) | 0.0369 (6) | 0.6365 (5) | 0.0258 (16) | |
N7 | 0.4821 (7) | 0.1631 (7) | 0.1004 (6) | 0.032 (2) | |
H7 | 0.5047 | 0.2251 | 0.1597 | 0.038* | |
O7 | 0.3547 (6) | 0.0515 (6) | −0.0683 (5) | 0.0345 (19) | |
N8 | 0.4510 (7) | −0.0406 (7) | 0.1252 (7) | 0.037 (2) | |
H8 | 0.4666 | −0.0282 | 0.1901 | 0.045* | |
O8 | 0.3234 (6) | −0.1515 (6) | −0.0456 (5) | 0.036 (2) | |
Cr1 | 0.63841 (11) | 0.23545 (12) | 0.35111 (11) | 0.0143 (3) | |
O9 | 0.7442 (5) | 0.3007 (5) | 0.4669 (5) | 0.0165 (14) | |
O10 | 0.6020 (5) | 0.3353 (5) | 0.3297 (4) | 0.0155 (13) | |
O11 | 0.5248 (5) | 0.1421 (5) | 0.3528 (5) | 0.0186 (14) | |
O12 | 0.6823 (5) | 0.1681 (5) | 0.2567 (5) | 0.0207 (15) | |
O13 | 0.7441 (12) | −0.0304 (13) | 0.2723 (13) | 0.056 (7) | 0.55 (2) |
O14 | 0.9443 (17) | 0.1153 (18) | 0.4449 (18) | 0.094 (11) | 0.53 (3) |
C1 | 1.0184 (8) | 0.3451 (9) | 0.3358 (8) | 0.035 (3) | |
C2A | 1.024 (2) | 0.273 (2) | 0.2267 (17) | 0.027 (7) | 0.51 (6) |
H9A | 1.0128 | 0.3105 | 0.1830 | 0.032* | 0.51 (6) |
H10A | 1.1004 | 0.2735 | 0.2374 | 0.032* | 0.51 (6) |
C3A | 0.939 (2) | 0.150 (2) | 0.167 (2) | 0.032 (6) | 0.51 (6) |
H11A | 0.9405 | 0.1142 | 0.2129 | 0.047* | 0.51 (6) |
H12A | 0.9591 | 0.1081 | 0.1076 | 0.047* | 0.51 (6) |
H13A | 0.8640 | 0.1469 | 0.1414 | 0.047* | 0.51 (6) |
C2B | 1.031 (2) | 0.247 (2) | 0.247 (2) | 0.026 (7) | 0.49 (6) |
H9B | 1.0257 | 0.2624 | 0.1872 | 0.031* | 0.49 (6) |
H10 | 1.1086 | 0.2517 | 0.2730 | 0.031* | 0.49 (6) |
C3B | 0.951 (3) | 0.124 (2) | 0.207 (3) | 0.052 (10) | 0.49 (6) |
H11B | 0.9707 | 0.0974 | 0.2579 | 0.079* | 0.49 (6) |
H12B | 0.9559 | 0.0752 | 0.1408 | 0.079* | 0.49 (6) |
H13B | 0.8737 | 0.1189 | 0.1953 | 0.079* | 0.49 (6) |
C4 | 0.8988 (9) | 0.5597 (11) | 0.3677 (10) | 0.048 (3) | |
C5A | 0.8450 (15) | 0.579 (2) | 0.2769 (16) | 0.069 (7) | 0.820 (19) |
H14A | 0.8610 | 0.6608 | 0.3042 | 0.083* | 0.820 (19) |
H15A | 0.8824 | 0.5590 | 0.2249 | 0.083* | 0.820 (19) |
C6A | 0.7181 (11) | 0.5109 (16) | 0.2210 (14) | 0.070 (6) | 0.820 (19) |
H16A | 0.7009 | 0.4292 | 0.1911 | 0.105* | 0.820 (19) |
H17A | 0.6926 | 0.5293 | 0.1653 | 0.105* | 0.820 (19) |
H18A | 0.6794 | 0.5309 | 0.2709 | 0.105* | 0.820 (19) |
C5B | 0.838 (8) | 0.619 (7) | 0.322 (5) | 0.042 (11) | 0.180 (19) |
H14B | 0.7603 | 0.6007 | 0.3238 | 0.051* | 0.180 (19) |
H15B | 0.8802 | 0.7031 | 0.3575 | 0.051* | 0.180 (19) |
C6B | 0.840 (6) | 0.562 (6) | 0.212 (5) | 0.048 (13) | 0.180 (19) |
H16B | 0.8394 | 0.6119 | 0.1796 | 0.072* | 0.180 (19) |
H17B | 0.7739 | 0.4895 | 0.1697 | 0.072* | 0.180 (19) |
H18B | 0.9084 | 0.5470 | 0.2148 | 0.072* | 0.180 (19) |
C7 | 0.6260 (8) | 0.5024 (8) | 0.6660 (7) | 0.020 (2) | |
C8 | 0.7040 (8) | 0.5119 (9) | 0.7649 (7) | 0.026 (2) | |
H19 | 0.6586 | 0.4979 | 0.8079 | 0.032* | |
H20 | 0.7618 | 0.5910 | 0.8062 | 0.032* | |
C9 | 0.7651 (9) | 0.4285 (10) | 0.7446 (8) | 0.033 (3) | |
H21 | 0.7090 | 0.3496 | 0.7050 | 0.050* | |
H22 | 0.8114 | 0.4401 | 0.8114 | 0.050* | |
H23 | 0.8132 | 0.4435 | 0.7048 | 0.050* | |
C10 | 0.3270 (7) | 0.3103 (8) | 0.4566 (8) | 0.022 (2) | |
C11 | 0.2268 (8) | 0.2021 (9) | 0.4277 (9) | 0.045 (3) | |
H24A | 0.2535 | 0.1408 | 0.4207 | 0.054* | 0.513 (18) |
H25A | 0.1728 | 0.1782 | 0.3587 | 0.054* | 0.513 (18) |
H24B | 0.1642 | 0.2231 | 0.4423 | 0.054* | 0.487 (18) |
H25B | 0.2482 | 0.1689 | 0.4731 | 0.054* | 0.487 (18) |
C12A | 0.1629 (16) | 0.2140 (17) | 0.5080 (16) | 0.037 (6) | 0.513 (18) |
H26A | 0.2177 | 0.2574 | 0.5791 | 0.055* | 0.513 (18) |
H27A | 0.1165 | 0.1380 | 0.4963 | 0.055* | 0.513 (18) |
H28A | 0.1147 | 0.2539 | 0.4986 | 0.055* | 0.513 (18) |
C12B | 0.1832 (16) | 0.1083 (16) | 0.3108 (16) | 0.037 (6) | 0.487 (18) |
H26B | 0.1822 | 0.1444 | 0.2654 | 0.056* | 0.487 (18) |
H27B | 0.1070 | 0.0538 | 0.2929 | 0.056* | 0.487 (18) |
H28B | 0.2333 | 0.0681 | 0.3013 | 0.056* | 0.487 (18) |
C13 | 0.4623 (8) | 0.1632 (8) | 0.6399 (8) | 0.023 (2) | |
C14 | 0.4364 (10) | 0.2569 (10) | 0.7208 (9) | 0.040 (3) | |
H29A | 0.4485 | 0.3209 | 0.7038 | 0.048* | 0.611 (19) |
H30A | 0.3559 | 0.2241 | 0.7119 | 0.048* | 0.611 (19) |
H29B | 0.4978 | 0.2993 | 0.7894 | 0.048* | 0.389 (19) |
H30B | 0.4260 | 0.3114 | 0.6958 | 0.048* | 0.389 (19) |
C15A | 0.508 (2) | 0.306 (2) | 0.8378 (15) | 0.070 (8) | 0.611 (19) |
H31A | 0.4934 | 0.3709 | 0.8806 | 0.105* | 0.611 (19) |
H32A | 0.5876 | 0.3304 | 0.8466 | 0.105* | 0.611 (19) |
H33A | 0.4862 | 0.2465 | 0.8595 | 0.105* | 0.611 (19) |
C15B | 0.324 (2) | 0.186 (2) | 0.728 (3) | 0.047 (8) | 0.389 (19) |
H31B | 0.2613 | 0.1615 | 0.6653 | 0.070* | 0.389 (19) |
H32B | 0.3122 | 0.2340 | 0.7896 | 0.070* | 0.389 (19) |
H33B | 0.3300 | 0.1194 | 0.7328 | 0.070* | 0.389 (19) |
C16 | 0.7218 (7) | 0.1087 (8) | 0.6096 (7) | 0.019 (2) | |
C17 | 0.8469 (8) | 0.1746 (10) | 0.6714 (8) | 0.033 (3) | |
H34A | 0.8654 | 0.1683 | 0.7365 | 0.040* | 0.57 (2) |
H35A | 0.8693 | 0.2562 | 0.6898 | 0.040* | 0.57 (2) |
H34B | 0.8555 | 0.2364 | 0.7384 | 0.040* | 0.43 (2) |
H35B | 0.8807 | 0.2116 | 0.6328 | 0.040* | 0.43 (2) |
C18A | 0.9106 (16) | 0.1202 (19) | 0.599 (2) | 0.060 (8) | 0.57 (2) |
H36A | 0.9883 | 0.1434 | 0.6420 | 0.091* | 0.57 (2) |
H37A | 0.9106 | 0.1467 | 0.5466 | 0.091* | 0.57 (2) |
H38A | 0.8722 | 0.0369 | 0.5645 | 0.091* | 0.57 (2) |
C18B | 0.9183 (19) | 0.111 (2) | 0.697 (2) | 0.050 (10) | 0.43 (2) |
H36B | 0.8860 | 0.0723 | 0.7340 | 0.076* | 0.43 (2) |
H37B | 0.9956 | 0.1664 | 0.7409 | 0.076* | 0.43 (2) |
H38B | 0.9186 | 0.0552 | 0.6320 | 0.076* | 0.43 (2) |
C19 | 0.3968 (9) | 0.1434 (9) | 0.0235 (9) | 0.038 (3) | |
C20A | 0.350 (3) | 0.234 (3) | 0.033 (5) | 0.055 (11) | 0.52 (6) |
H39A | 0.3776 | 0.2918 | 0.1067 | 0.066* | 0.52 (6) |
H40A | 0.3784 | 0.2729 | −0.0067 | 0.066* | 0.52 (6) |
C21A | 0.221 (3) | 0.186 (4) | −0.008 (5) | 0.10 (2) | 0.52 (6) |
H41A | 0.1907 | 0.1041 | −0.0311 | 0.149* | 0.52 (6) |
H42A | 0.1955 | 0.1998 | −0.0674 | 0.149* | 0.52 (6) |
H43A | 0.1949 | 0.2240 | 0.0471 | 0.149* | 0.52 (6) |
C20B | 0.326 (3) | 0.214 (3) | 0.044 (5) | 0.042 (8) | 0.48 (6) |
H39B | 0.3734 | 0.2897 | 0.1057 | 0.051* | 0.48 (6) |
H40B | 0.3035 | 0.2276 | −0.0165 | 0.051* | 0.48 (6) |
C21B | 0.222 (4) | 0.157 (3) | 0.063 (6) | 0.099 (19) | 0.48 (6) |
H41B | 0.1731 | 0.0845 | 0.0014 | 0.149* | 0.48 (6) |
H42B | 0.1810 | 0.2069 | 0.0781 | 0.149* | 0.48 (6) |
H43B | 0.2440 | 0.1435 | 0.1230 | 0.149* | 0.48 (6) |
C22 | 0.3524 (9) | −0.1252 (9) | 0.0542 (8) | 0.036 (3) | |
C23A | 0.257 (3) | −0.174 (3) | 0.092 (3) | 0.047 (10) | 0.40 (2) |
H44A | 0.2039 | −0.1359 | 0.0912 | 0.056* | 0.40 (2) |
H45A | 0.2885 | −0.1625 | 0.1632 | 0.056* | 0.40 (2) |
C23B | 0.286 (3) | −0.211 (5) | 0.087 (5) | 0.046 (9) | 0.37 (3) |
H44B | 0.3052 | −0.1748 | 0.1636 | 0.056* | 0.37 (3) |
H45B | 0.3055 | −0.2785 | 0.0656 | 0.056* | 0.37 (3) |
C23C | 0.265 (6) | −0.197 (10) | 0.085 (11) | 0.042 (10) | 0.23 (3) |
H44C | 0.2983 | −0.1816 | 0.1575 | 0.050* | 0.23 (3) |
H45C | 0.2389 | −0.2792 | 0.0380 | 0.050* | 0.23 (3) |
C24A | 0.195 (3) | −0.308 (2) | 0.008 (2) | 0.044 (7) | 0.40 (2) |
H46A | 0.2488 | −0.3439 | 0.0107 | 0.065* | 0.40 (2) |
H47A | 0.1662 | −0.3172 | −0.0618 | 0.065* | 0.40 (2) |
H48A | 0.1323 | −0.3452 | 0.0261 | 0.065* | 0.40 (2) |
C24B | 0.153 (3) | −0.249 (4) | 0.029 (3) | 0.066 (11) | 0.37 (3) |
H46B | 0.1421 | −0.1847 | 0.0215 | 0.098* | 0.37 (3) |
H47B | 0.1103 | −0.2703 | 0.0696 | 0.098* | 0.37 (3) |
H48B | 0.1277 | −0.3138 | −0.0408 | 0.098* | 0.37 (3) |
C24C | 0.160 (4) | −0.158 (6) | 0.074 (5) | 0.058 (13) | 0.23 (3) |
H46C | 0.1884 | −0.0748 | 0.1160 | 0.087* | 0.23 (3) |
H47C | 0.1055 | −0.1955 | 0.0983 | 0.087* | 0.23 (3) |
H48C | 0.1242 | −0.1790 | 0.0006 | 0.087* | 0.23 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0116 (3) | 0.0149 (4) | 0.0192 (4) | 0.0032 (3) | 0.0050 (3) | 0.0083 (3) |
Rh2 | 0.0154 (3) | 0.0142 (4) | 0.0152 (4) | 0.0070 (3) | 0.0069 (3) | 0.0066 (3) |
Rh3 | 0.0164 (4) | 0.0183 (4) | 0.0217 (4) | 0.0025 (3) | 0.0032 (3) | 0.0131 (3) |
Rh4 | 0.0212 (4) | 0.0181 (4) | 0.0162 (4) | 0.0019 (3) | 0.0070 (3) | −0.0007 (3) |
N1 | 0.013 (4) | 0.011 (4) | 0.051 (6) | −0.004 (3) | 0.010 (4) | 0.000 (4) |
O1 | 0.013 (3) | 0.035 (4) | 0.023 (4) | 0.002 (3) | 0.006 (3) | −0.003 (3) |
N2 | 0.010 (4) | 0.040 (5) | 0.040 (5) | 0.002 (4) | 0.008 (4) | 0.027 (5) |
O2 | 0.017 (4) | 0.056 (5) | 0.060 (5) | 0.000 (3) | 0.004 (4) | 0.049 (5) |
N3 | 0.024 (4) | 0.026 (4) | 0.018 (4) | 0.020 (4) | 0.009 (3) | 0.008 (4) |
O3 | 0.027 (3) | 0.027 (4) | 0.013 (3) | 0.015 (3) | 0.007 (3) | 0.010 (3) |
N4 | 0.019 (4) | 0.014 (4) | 0.026 (4) | 0.008 (3) | 0.012 (3) | 0.001 (3) |
O4 | 0.019 (3) | 0.023 (4) | 0.028 (4) | 0.011 (3) | 0.015 (3) | 0.013 (3) |
N5 | 0.027 (4) | 0.018 (4) | 0.034 (5) | 0.015 (4) | 0.013 (4) | 0.018 (4) |
O5 | 0.032 (4) | 0.023 (4) | 0.024 (4) | 0.007 (3) | 0.012 (3) | 0.016 (3) |
N6 | 0.010 (3) | 0.020 (4) | 0.021 (4) | −0.001 (3) | 0.003 (3) | 0.013 (3) |
O6 | 0.023 (3) | 0.028 (4) | 0.028 (4) | 0.008 (3) | 0.004 (3) | 0.019 (3) |
N7 | 0.026 (4) | 0.029 (5) | 0.018 (4) | 0.007 (4) | −0.005 (4) | −0.003 (4) |
O7 | 0.030 (4) | 0.033 (4) | 0.018 (4) | 0.008 (3) | 0.004 (3) | −0.004 (3) |
N8 | 0.037 (5) | 0.031 (5) | 0.018 (5) | −0.004 (4) | 0.003 (4) | 0.003 (4) |
O8 | 0.029 (4) | 0.031 (4) | 0.018 (4) | −0.009 (3) | 0.007 (3) | −0.003 (3) |
Cr1 | 0.0130 (7) | 0.0121 (7) | 0.0153 (7) | 0.0037 (6) | 0.0052 (6) | 0.0048 (6) |
O9 | 0.011 (3) | 0.019 (3) | 0.020 (3) | 0.004 (3) | 0.007 (3) | 0.010 (3) |
O10 | 0.015 (3) | 0.014 (3) | 0.014 (3) | 0.005 (2) | 0.004 (2) | 0.003 (3) |
O11 | 0.016 (3) | 0.017 (3) | 0.020 (3) | 0.005 (3) | 0.005 (3) | 0.009 (3) |
O12 | 0.018 (3) | 0.015 (3) | 0.020 (3) | 0.009 (3) | 0.007 (3) | −0.002 (3) |
O13 | 0.042 (10) | 0.057 (11) | 0.079 (14) | 0.020 (8) | 0.028 (9) | 0.038 (10) |
O14 | 0.093 (17) | 0.086 (17) | 0.11 (2) | 0.037 (13) | 0.018 (14) | 0.059 (15) |
C1 | 0.015 (5) | 0.029 (5) | 0.028 (6) | 0.000 (4) | 0.003 (4) | −0.009 (4) |
C2A | 0.021 (10) | 0.029 (10) | 0.031 (11) | 0.015 (8) | 0.010 (9) | 0.010 (8) |
C3A | 0.030 (7) | 0.031 (6) | 0.031 (7) | 0.017 (5) | 0.016 (5) | 0.007 (4) |
C2B | 0.025 (11) | 0.022 (10) | 0.009 (10) | 0.004 (9) | −0.006 (8) | −0.003 (8) |
C3B | 0.056 (17) | 0.023 (9) | 0.05 (2) | 0.005 (11) | 0.010 (15) | 0.000 (12) |
C4 | 0.025 (6) | 0.064 (8) | 0.065 (8) | 0.010 (5) | −0.002 (5) | 0.051 (7) |
C5A | 0.028 (7) | 0.099 (14) | 0.089 (15) | −0.003 (9) | −0.002 (10) | 0.085 (13) |
C6A | 0.028 (7) | 0.112 (15) | 0.087 (13) | 0.011 (8) | 0.003 (7) | 0.086 (12) |
C5B | 0.031 (18) | 0.048 (18) | 0.063 (18) | 0.012 (14) | 0.009 (15) | 0.047 (15) |
C6B | 0.03 (2) | 0.06 (2) | 0.058 (16) | 0.003 (18) | 0.002 (17) | 0.047 (18) |
C7 | 0.023 (5) | 0.020 (5) | 0.014 (5) | 0.006 (4) | 0.004 (4) | 0.007 (4) |
C8 | 0.033 (5) | 0.042 (6) | 0.020 (5) | 0.025 (5) | 0.011 (4) | 0.022 (5) |
C9 | 0.039 (6) | 0.048 (7) | 0.022 (5) | 0.025 (5) | 0.011 (5) | 0.020 (5) |
C10 | 0.015 (4) | 0.021 (5) | 0.031 (6) | 0.009 (4) | 0.011 (4) | 0.012 (4) |
C11 | 0.022 (5) | 0.016 (5) | 0.071 (8) | −0.005 (4) | 0.017 (5) | 0.004 (5) |
C12A | 0.024 (10) | 0.029 (12) | 0.049 (13) | −0.003 (8) | 0.006 (9) | 0.025 (10) |
C12B | 0.019 (10) | 0.018 (9) | 0.066 (12) | 0.007 (8) | 0.002 (10) | 0.017 (8) |
C13 | 0.022 (5) | 0.017 (5) | 0.035 (5) | 0.011 (4) | 0.012 (4) | 0.015 (4) |
C14 | 0.057 (7) | 0.042 (7) | 0.045 (6) | 0.034 (6) | 0.034 (6) | 0.026 (5) |
C15A | 0.11 (2) | 0.065 (16) | 0.038 (8) | 0.043 (15) | 0.035 (11) | 0.022 (10) |
C15B | 0.066 (15) | 0.037 (15) | 0.068 (19) | 0.043 (11) | 0.049 (14) | 0.025 (13) |
C16 | 0.016 (4) | 0.018 (5) | 0.017 (5) | 0.003 (4) | 0.002 (4) | 0.007 (4) |
C17 | 0.022 (5) | 0.044 (7) | 0.028 (6) | 0.001 (4) | −0.001 (4) | 0.025 (5) |
C18A | 0.026 (9) | 0.060 (15) | 0.10 (2) | 0.020 (10) | 0.026 (11) | 0.041 (14) |
C18B | 0.029 (11) | 0.028 (13) | 0.06 (2) | −0.009 (10) | −0.027 (13) | 0.024 (14) |
C19 | 0.039 (6) | 0.025 (6) | 0.033 (6) | 0.012 (5) | 0.007 (5) | −0.001 (5) |
C20A | 0.062 (14) | 0.035 (13) | 0.032 (18) | 0.028 (12) | −0.009 (15) | −0.011 (12) |
C21A | 0.065 (14) | 0.07 (2) | 0.11 (3) | 0.044 (15) | 0.00 (2) | −0.01 (2) |
C20B | 0.046 (13) | 0.044 (14) | 0.019 (13) | 0.027 (10) | 0.010 (10) | −0.008 (11) |
C21B | 0.069 (19) | 0.06 (2) | 0.15 (4) | 0.032 (16) | 0.07 (2) | 0.02 (2) |
C22 | 0.035 (6) | 0.033 (6) | 0.025 (6) | 0.000 (5) | 0.014 (5) | 0.006 (5) |
C23A | 0.029 (13) | 0.046 (12) | 0.043 (14) | −0.004 (13) | 0.016 (11) | 0.013 (11) |
C23B | 0.049 (13) | 0.039 (16) | 0.025 (13) | −0.005 (14) | 0.028 (13) | −0.001 (12) |
C23C | 0.038 (16) | 0.036 (18) | 0.033 (17) | −0.001 (13) | 0.022 (15) | 0.005 (15) |
C24A | 0.045 (8) | 0.043 (7) | 0.042 (8) | 0.008 (4) | 0.018 (5) | 0.024 (5) |
C24B | 0.050 (11) | 0.060 (18) | 0.057 (16) | −0.001 (10) | 0.031 (12) | 0.009 (13) |
C24C | 0.043 (13) | 0.06 (2) | 0.06 (2) | 0.012 (14) | 0.031 (15) | 0.026 (15) |
Geometric parameters (Å, º) top
Rh1—N1 | 1.976 (8) | C8—C9 | 1.534 (13) |
Rh1—N2 | 1.956 (8) | C8—H19 | 0.9700 |
Rh1—O1i | 2.019 (7) | C8—H20 | 0.9700 |
Rh1—O2i | 2.017 (7) | C9—H21 | 0.9600 |
Rh1—O9 | 2.226 (5) | C9—H22 | 0.9600 |
Rh1—Rh1i | 2.4071 (14) | C9—H23 | 0.9600 |
Rh2—N3 | 1.992 (7) | C10—C11 | 1.495 (12) |
Rh2—N4 | 1.975 (7) | C11—C12B | 1.541 (18) |
Rh2—O3ii | 2.027 (6) | C11—C12A | 1.545 (18) |
Rh2—O4ii | 2.030 (6) | C11—H24A | 0.9700 |
Rh2—O10 | 2.207 (6) | C11—H25A | 0.9700 |
Rh2—Rh2ii | 2.4122 (15) | C11—H24B | 0.9700 |
Rh3—N5 | 1.980 (8) | C11—H25B | 0.9700 |
Rh3—N6 | 1.969 (6) | C12A—H26A | 0.9600 |
Rh3—O5iii | 2.034 (7) | C12A—H27A | 0.9600 |
Rh3—O6iii | 2.040 (6) | C12A—H28A | 0.9600 |
Rh3—O11 | 2.179 (6) | C12B—H26B | 0.9600 |
Rh3—Rh3iii | 2.4053 (15) | C12B—H27B | 0.9600 |
Rh4—N7 | 1.985 (9) | C12B—H28B | 0.9600 |
Rh4—N8 | 1.977 (9) | C13—C14 | 1.540 (14) |
Rh4—O7iv | 2.033 (7) | C14—C15A | 1.530 (19) |
Rh4—O8iv | 2.016 (7) | C14—C15B | 1.54 (2) |
Rh4—O12 | 2.201 (6) | C14—H29A | 0.9700 |
Rh4—Rh4iv | 2.4076 (15) | C14—H30A | 0.9700 |
N1—C1 | 1.313 (12) | C14—H29B | 0.9700 |
N1—H1 | 0.8600 | C14—H30B | 0.9700 |
O1—C1 | 1.280 (11) | C15A—H31A | 0.9600 |
N2—C4 | 1.286 (13) | C15A—H32A | 0.9600 |
N2—H2 | 0.8600 | C15A—H33A | 0.9600 |
O2—C4 | 1.309 (12) | C15B—H31B | 0.9600 |
N3—C7 | 1.296 (11) | C15B—H32B | 0.9600 |
N3—H3 | 0.8600 | C15B—H33B | 0.9600 |
O3—C7 | 1.275 (11) | C16—C17 | 1.488 (12) |
N4—C10 | 1.297 (11) | C17—C18B | 1.52 (2) |
N4—H4 | 0.8600 | C17—C18A | 1.56 (2) |
O4—C10 | 1.286 (11) | C17—H34A | 0.9700 |
N5—C13 | 1.306 (12) | C17—H35A | 0.9700 |
N5—H5 | 0.8600 | C17—H34B | 0.9700 |
O5—C13 | 1.262 (11) | C17—H35B | 0.9700 |
N6—C16 | 1.306 (11) | C18A—H36A | 0.9600 |
N6—H6 | 0.8600 | C18A—H37A | 0.9600 |
O6—C16 | 1.290 (11) | C18A—H38A | 0.9600 |
N7—C19 | 1.286 (13) | C18B—H36B | 0.9600 |
N7—H7 | 0.8600 | C18B—H37B | 0.9600 |
O7—C19 | 1.296 (11) | C18B—H38B | 0.9600 |
N8—C22 | 1.322 (12) | C19—C20B | 1.50 (2) |
N8—H8 | 0.8600 | C19—C20A | 1.50 (2) |
O8—C22 | 1.294 (12) | C20A—C21A | 1.50 (3) |
Cr1—O12 | 1.639 (6) | C20A—H39A | 0.9700 |
Cr1—O11 | 1.654 (6) | C20A—H40A | 0.9700 |
Cr1—O9 | 1.656 (6) | C21A—H41A | 0.9600 |
Cr1—O10 | 1.670 (6) | C21A—H42A | 0.9600 |
C1—C2B | 1.540 (18) | C21A—H43A | 0.9600 |
C1—C2A | 1.541 (18) | C20B—C21B | 1.49 (3) |
C2A—C3A | 1.485 (19) | C20B—H39B | 0.9700 |
C2A—H9A | 0.9700 | C20B—H40B | 0.9700 |
C2A—H10A | 0.9700 | C21B—H41B | 0.9600 |
C3A—H11A | 0.9600 | C21B—H42B | 0.9600 |
C3A—H12A | 0.9600 | C21B—H43B | 0.9600 |
C3A—H13A | 0.9600 | C22—C23C | 1.53 (2) |
C2B—C3B | 1.49 (2) | C22—C23B | 1.53 (2) |
C2B—H9B | 0.9700 | C22—C23A | 1.526 (19) |
C2B—H10 | 0.9700 | C23A—C24A | 1.59 (4) |
C3B—H11B | 0.9600 | C23A—H44A | 0.9700 |
C3B—H12B | 0.9600 | C23A—H45A | 0.9700 |
C3B—H13B | 0.9600 | C23B—C24B | 1.59 (4) |
C4—C5A | 1.511 (16) | C23B—H44B | 0.9700 |
C4—C5B | 1.51 (2) | C23B—H45B | 0.9700 |
C5A—C6A | 1.50 (2) | C23C—C24C | 1.59 (4) |
C5A—H14A | 0.9700 | C23C—H44C | 0.9700 |
C5A—H15A | 0.9700 | C23C—H45C | 0.9700 |
C6A—H16A | 0.9600 | C24A—H46A | 0.9600 |
C6A—H17A | 0.9600 | C24A—H47A | 0.9600 |
C6A—H18A | 0.9600 | C24A—H48A | 0.9600 |
C5B—C6B | 1.51 (3) | C24B—H46B | 0.9600 |
C5B—H14B | 0.9700 | C24B—H47B | 0.9600 |
C5B—H15B | 0.9700 | C24B—H48B | 0.9600 |
C6B—H16B | 0.9600 | C24C—H46C | 0.9600 |
C6B—H17B | 0.9600 | C24C—H47C | 0.9600 |
C6B—H18B | 0.9600 | C24C—H48C | 0.9600 |
C7—C8 | 1.521 (12) | | |
| | | |
N2—Rh1—N1 | 89.6 (4) | C9—C8—H19 | 108.4 |
N2—Rh1—O2i | 175.4 (3) | C7—C8—H20 | 108.4 |
N1—Rh1—O2i | 91.5 (4) | C9—C8—H20 | 108.4 |
N2—Rh1—O1i | 91.1 (3) | H19—C8—H20 | 107.5 |
N1—Rh1—O1i | 176.1 (3) | C8—C9—H21 | 109.5 |
O2i—Rh1—O1i | 87.5 (3) | C8—C9—H22 | 109.5 |
N2—Rh1—O9 | 96.6 (3) | H21—C9—H22 | 109.5 |
N1—Rh1—O9 | 93.0 (3) | C8—C9—H23 | 109.5 |
O2i—Rh1—O9 | 87.8 (2) | H21—C9—H23 | 109.5 |
O1i—Rh1—O9 | 90.8 (2) | H22—C9—H23 | 109.5 |
N2—Rh1—Rh1i | 85.3 (2) | O4—C10—N4 | 121.1 (8) |
N1—Rh1—Rh1i | 86.5 (2) | O4—C10—C11 | 117.6 (8) |
O2i—Rh1—Rh1i | 90.29 (18) | N4—C10—C11 | 121.2 (9) |
O1i—Rh1—Rh1i | 89.67 (18) | C10—C11—C12B | 114.8 (11) |
O9—Rh1—Rh1i | 178.04 (17) | C10—C11—C12A | 114.8 (10) |
N4—Rh2—N3 | 92.0 (3) | C12B—C11—C12A | 128.0 (12) |
N4—Rh2—O3ii | 90.0 (3) | C10—C11—H24A | 108.6 |
N3—Rh2—O3ii | 175.1 (3) | C12A—C11—H24A | 108.6 |
N4—Rh2—O4ii | 175.1 (3) | C10—C11—H25A | 108.6 |
N3—Rh2—O4ii | 88.8 (3) | C12A—C11—H25A | 108.6 |
O3ii—Rh2—O4ii | 88.8 (3) | H24A—C11—H25A | 107.5 |
N4—Rh2—O10 | 92.6 (3) | C10—C11—H24B | 108.6 |
N3—Rh2—O10 | 97.0 (3) | C12B—C11—H24B | 108.6 |
O3ii—Rh2—O10 | 87.3 (2) | C10—C11—H25B | 108.6 |
O4ii—Rh2—O10 | 92.1 (2) | C12B—C11—H25B | 108.6 |
N4—Rh2—Rh2ii | 85.8 (2) | H24B—C11—H25B | 107.6 |
N3—Rh2—Rh2ii | 85.2 (2) | C11—C12A—H26A | 109.5 |
O3ii—Rh2—Rh2ii | 90.50 (18) | C11—C12A—H27A | 109.5 |
O4ii—Rh2—Rh2ii | 89.47 (18) | H26A—C12A—H27A | 109.5 |
O10—Rh2—Rh2ii | 177.28 (15) | C11—C12A—H28A | 109.5 |
N6—Rh3—N5 | 90.8 (3) | H26A—C12A—H28A | 109.5 |
N6—Rh3—O5iii | 89.8 (3) | H27A—C12A—H28A | 109.5 |
N5—Rh3—O5iii | 175.6 (3) | C11—C12B—H26B | 109.5 |
N6—Rh3—O6iii | 175.7 (3) | C11—C12B—H27B | 109.5 |
N5—Rh3—O6iii | 90.3 (3) | H26B—C12B—H27B | 109.5 |
O5iii—Rh3—O6iii | 88.7 (3) | C11—C12B—H28B | 109.5 |
N6—Rh3—O11 | 94.3 (3) | H26B—C12B—H28B | 109.5 |
N5—Rh3—O11 | 93.3 (3) | H27B—C12B—H28B | 109.5 |
O5iii—Rh3—O11 | 91.0 (2) | O5—C13—N5 | 123.0 (9) |
O6iii—Rh3—O11 | 89.8 (2) | O5—C13—C14 | 115.8 (9) |
N6—Rh3—Rh3iii | 85.8 (2) | N5—C13—C14 | 121.2 (9) |
N5—Rh3—Rh3iii | 86.2 (2) | C15A—C14—C13 | 115.9 (12) |
O5iii—Rh3—Rh3iii | 89.51 (19) | C15B—C14—C13 | 103.5 (13) |
O6iii—Rh3—Rh3iii | 90.12 (19) | C15A—C14—H29A | 108.3 |
O11—Rh3—Rh3iii | 179.44 (18) | C13—C14—H29A | 108.3 |
N8—Rh4—N7 | 91.9 (4) | C15A—C14—H30A | 108.3 |
N8—Rh4—O8iv | 176.1 (3) | C13—C14—H30A | 108.3 |
N7—Rh4—O8iv | 89.7 (3) | H29A—C14—H30A | 107.4 |
N8—Rh4—O7iv | 89.8 (4) | C15B—C14—H29B | 111.1 |
N7—Rh4—O7iv | 175.5 (3) | C13—C14—H29B | 111.1 |
O8iv—Rh4—O7iv | 88.4 (3) | C15B—C14—H30B | 111.1 |
N8—Rh4—O12 | 94.1 (3) | C13—C14—H30B | 111.1 |
N7—Rh4—O12 | 93.7 (3) | H30A—C14—H30B | 92.3 |
O8iv—Rh4—O12 | 89.4 (2) | H29B—C14—H30B | 109.0 |
O7iv—Rh4—O12 | 90.4 (2) | C14—C15A—H31A | 109.5 |
N8—Rh4—Rh4iv | 85.9 (2) | C14—C15A—H32A | 109.5 |
N7—Rh4—Rh4iv | 85.9 (2) | H31A—C15A—H32A | 109.5 |
O8iv—Rh4—Rh4iv | 90.58 (19) | C14—C15A—H33A | 109.5 |
O7iv—Rh4—Rh4iv | 89.97 (18) | H31A—C15A—H33A | 109.5 |
O12—Rh4—Rh4iv | 179.67 (18) | H32A—C15A—H33A | 109.5 |
C1—N1—Rh1 | 122.7 (6) | C14—C15B—H31B | 109.5 |
C1—N1—H1 | 118.6 | C14—C15B—H32B | 109.5 |
Rh1—N1—H1 | 118.6 | H31B—C15B—H32B | 109.5 |
C1—O1—Rh1i | 118.1 (6) | C14—C15B—H33B | 109.5 |
C4—N2—Rh1 | 126.2 (7) | H31B—C15B—H33B | 109.5 |
C4—N2—H2 | 116.9 | H32B—C15B—H33B | 109.5 |
Rh1—N2—H2 | 116.9 | O6—C16—N6 | 121.7 (8) |
C4—O2—Rh1i | 117.2 (7) | O6—C16—C17 | 117.9 (8) |
C7—N3—Rh2 | 123.6 (6) | N6—C16—C17 | 120.4 (8) |
C7—N3—H3 | 118.2 | C16—C17—C18B | 119.7 (12) |
Rh2—N3—H3 | 118.2 | C16—C17—C18A | 106.9 (11) |
C7—O3—Rh2ii | 116.6 (6) | C16—C17—H34A | 110.3 |
C10—N4—Rh2 | 124.9 (6) | C18A—C17—H34A | 110.3 |
C10—N4—H4 | 117.5 | C16—C17—H35A | 110.3 |
Rh2—N4—H4 | 117.5 | C18A—C17—H35A | 110.3 |
C10—O4—Rh2ii | 118.4 (6) | H34A—C17—H35A | 108.6 |
C13—N5—Rh3 | 123.2 (7) | C16—C17—H34B | 107.4 |
C13—N5—H5 | 118.4 | C18B—C17—H34B | 107.4 |
Rh3—N5—H5 | 118.4 | C16—C17—H35B | 107.4 |
C13—O5—Rh3iii | 118.0 (6) | C18B—C17—H35B | 107.4 |
C16—N6—Rh3 | 125.0 (6) | H34B—C17—H35B | 106.9 |
C16—N6—H6 | 117.5 | C17—C18A—H36A | 109.5 |
Rh3—N6—H6 | 117.5 | C17—C18A—H37A | 109.5 |
C16—O6—Rh3iii | 117.3 (6) | H36A—C18A—H37A | 109.5 |
C19—N7—Rh4 | 124.0 (7) | C17—C18A—H38A | 109.5 |
C19—N7—H7 | 118.0 | H36A—C18A—H38A | 109.5 |
Rh4—N7—H7 | 118.0 | H37A—C18A—H38A | 109.5 |
C19—O7—Rh4iv | 117.1 (7) | C17—C18B—H36B | 109.5 |
C22—N8—Rh4 | 123.7 (8) | C17—C18B—H37B | 109.5 |
C22—N8—H8 | 118.1 | H36B—C18B—H37B | 109.5 |
Rh4—N8—H8 | 118.1 | C17—C18B—H38B | 109.5 |
C22—O8—Rh4iv | 117.6 (6) | H36B—C18B—H38B | 109.5 |
O9—Cr1—O10 | 109.2 (3) | H37B—C18B—H38B | 109.5 |
O11—Cr1—O9 | 110.1 (3) | N7—C19—O7 | 122.8 (10) |
O12—Cr1—O9 | 108.9 (3) | N7—C19—C20B | 120 (2) |
O11—Cr1—O10 | 108.4 (3) | O7—C19—C20B | 116 (2) |
O12—Cr1—O10 | 109.8 (3) | N7—C19—C20A | 121 (2) |
O12—Cr1—O11 | 110.4 (3) | O7—C19—C20A | 116 (2) |
Cr1—O9—Rh1 | 118.1 (3) | C21A—C20A—C19 | 114 (2) |
Cr1—O10—Rh2 | 119.7 (3) | C21A—C20A—H39A | 108.8 |
Cr1—O11—Rh3 | 131.4 (3) | C19—C20A—H39A | 108.8 |
Cr1—O12—Rh4 | 121.1 (3) | C21A—C20A—H40A | 108.8 |
O1—C1—N1 | 122.8 (9) | C19—C20A—H40A | 108.8 |
O1—C1—C2B | 118.5 (13) | H39A—C20A—H40A | 107.7 |
N1—C1—C2B | 117.8 (14) | C20A—C21A—H41A | 109.5 |
O1—C1—C2A | 111.4 (13) | C20A—C21A—H42A | 109.5 |
N1—C1—C2A | 124.9 (12) | H41A—C21A—H42A | 109.5 |
C3A—C2A—C1 | 115.9 (18) | C20A—C21A—H43A | 109.5 |
C3A—C2A—H9A | 108.3 | H41A—C21A—H43A | 109.5 |
C1—C2A—H9A | 108.3 | H42A—C21A—H43A | 109.5 |
C3A—C2A—H10A | 108.3 | C21B—C20B—C19 | 113 (3) |
C1—C2A—H10A | 108.3 | C21B—C20B—H39B | 109.1 |
H9A—C2A—H10A | 107.4 | C19—C20B—H39B | 109.1 |
C2A—C3A—H11A | 109.5 | C21B—C20B—H40B | 109.1 |
C2A—C3A—H12A | 109.5 | C19—C20B—H40B | 109.1 |
H11A—C3A—H12A | 109.5 | H39B—C20B—H40B | 107.8 |
C2A—C3A—H13A | 109.5 | C20B—C21B—H41B | 109.5 |
H11A—C3A—H13A | 109.5 | C20B—C21B—H42B | 109.5 |
H12A—C3A—H13A | 109.5 | H41B—C21B—H42B | 109.5 |
C3B—C2B—C1 | 119 (2) | C20B—C21B—H43B | 109.5 |
C3B—C2B—H9B | 107.5 | H41B—C21B—H43B | 109.5 |
C1—C2B—H9B | 107.5 | H42B—C21B—H43B | 109.5 |
C3B—C2B—H10 | 107.5 | O8—C22—N8 | 122.1 (10) |
C1—C2B—H10 | 107.5 | O8—C22—C23C | 116 (5) |
H9B—C2B—H10 | 107.0 | N8—C22—C23C | 122 (5) |
C2B—C3B—H11B | 109.5 | O8—C22—C23B | 119 (3) |
C2B—C3B—H12B | 109.5 | N8—C22—C23B | 117 (2) |
H11B—C3B—H12B | 109.5 | O8—C22—C23A | 117 (2) |
C2B—C3B—H13B | 109.5 | N8—C22—C23A | 119.4 (19) |
H11B—C3B—H13B | 109.5 | C22—C23A—C24A | 104 (2) |
H12B—C3B—H13B | 109.5 | C22—C23A—H44A | 110.9 |
N2—C4—O2 | 121.0 (10) | C24A—C23A—H44A | 110.9 |
N2—C4—C5A | 123.4 (11) | C22—C23A—H45A | 110.9 |
O2—C4—C5A | 115.0 (12) | C24A—C23A—H45A | 110.9 |
N2—C4—C5B | 119 (4) | H44A—C23A—H45A | 108.9 |
O2—C4—C5B | 116 (4) | C22—C23B—C24B | 107 (3) |
C6A—C5A—C4 | 116.1 (14) | C22—C23B—H44B | 110.4 |
C6A—C5A—H14A | 108.3 | C24B—C23B—H44B | 110.4 |
C4—C5A—H14A | 108.3 | C22—C23B—H45B | 110.4 |
C6A—C5A—H15A | 108.3 | C24B—C23B—H45B | 110.4 |
C4—C5A—H15A | 108.3 | H44B—C23B—H45B | 108.6 |
H14A—C5A—H15A | 107.4 | C22—C23C—C24C | 106 (4) |
C5A—C6A—H16A | 109.5 | C22—C23C—H44C | 110.5 |
C5A—C6A—H17A | 109.5 | C24C—C23C—H44C | 110.5 |
H16A—C6A—H17A | 109.5 | C22—C23C—H45C | 110.5 |
C5A—C6A—H18A | 109.5 | C24C—C23C—H45C | 110.5 |
H16A—C6A—H18A | 109.5 | H44C—C23C—H45C | 108.7 |
H17A—C6A—H18A | 109.5 | C23A—C24A—H46A | 109.5 |
C6B—C5B—C4 | 97 (4) | C23A—C24A—H47A | 109.5 |
C6B—C5B—H14B | 112.4 | H46A—C24A—H47A | 109.5 |
C4—C5B—H14B | 112.4 | C23A—C24A—H48A | 109.5 |
C6B—C5B—H15B | 112.4 | H46A—C24A—H48A | 109.5 |
C4—C5B—H15B | 112.4 | H47A—C24A—H48A | 109.5 |
H14B—C5B—H15B | 110.0 | C23B—C24B—H46B | 109.5 |
C5B—C6B—H16B | 109.5 | C23B—C24B—H47B | 109.5 |
C5B—C6B—H17B | 109.5 | H46B—C24B—H47B | 109.5 |
H16B—C6B—H17B | 109.5 | C23B—C24B—H48B | 109.5 |
C5B—C6B—H18B | 109.5 | H46B—C24B—H48B | 109.5 |
H16B—C6B—H18B | 109.5 | H47B—C24B—H48B | 109.5 |
H17B—C6B—H18B | 109.5 | C23C—C24C—H46C | 109.5 |
O3—C7—N3 | 123.6 (8) | C23C—C24C—H47C | 109.5 |
O3—C7—C8 | 114.4 (8) | H46C—C24C—H47C | 109.5 |
N3—C7—C8 | 122.0 (9) | C23C—C24C—H48C | 109.5 |
C7—C8—C9 | 115.5 (8) | H46C—C24C—H48C | 109.5 |
C7—C8—H19 | 108.4 | H47C—C24C—H48C | 109.5 |
| | | |
N2—Rh1—N1—C1 | 81.6 (9) | N1—C1—C2B—C3B | −5 (3) |
O2i—Rh1—N1—C1 | −93.9 (9) | C2A—C1—C2B—C3B | −120 (6) |
O9—Rh1—N1—C1 | 178.2 (9) | Rh1—N2—C4—O2 | −4.3 (19) |
Rh1i—Rh1—N1—C1 | −3.7 (9) | Rh1—N2—C4—C5A | 166.1 (14) |
N1—Rh1—N2—C4 | −83.1 (11) | Rh1—N2—C4—C5B | −162 (3) |
O1i—Rh1—N2—C4 | 93.0 (11) | Rh1i—O2—C4—N2 | 2.3 (17) |
O9—Rh1—N2—C4 | −176.1 (11) | Rh1i—O2—C4—C5A | −168.9 (13) |
Rh1i—Rh1—N2—C4 | 3.4 (11) | Rh1i—O2—C4—C5B | 160 (3) |
N4—Rh2—N3—C7 | −86.1 (8) | N2—C4—C5A—C6A | 4 (3) |
O4ii—Rh2—N3—C7 | 89.1 (8) | O2—C4—C5A—C6A | 175.3 (16) |
O10—Rh2—N3—C7 | −178.9 (7) | C5B—C4—C5A—C6A | −86 (9) |
Rh2ii—Rh2—N3—C7 | −0.5 (7) | N2—C4—C5B—C6B | −111 (5) |
N3—Rh2—N4—C10 | 86.8 (8) | O2—C4—C5B—C6B | 90 (5) |
O3ii—Rh2—N4—C10 | −88.7 (8) | C5A—C4—C5B—C6B | −5 (5) |
O10—Rh2—N4—C10 | −176.0 (8) | Rh2ii—O3—C7—N3 | −8.0 (12) |
Rh2ii—Rh2—N4—C10 | 1.8 (8) | Rh2ii—O3—C7—C8 | 173.1 (6) |
N6—Rh3—N5—C13 | −86.1 (7) | Rh2—N3—C7—O3 | 5.5 (13) |
O6iii—Rh3—N5—C13 | 89.8 (7) | Rh2—N3—C7—C8 | −175.6 (7) |
O11—Rh3—N5—C13 | 179.6 (7) | O3—C7—C8—C9 | 163.2 (9) |
Rh3iii—Rh3—N5—C13 | −0.3 (7) | N3—C7—C8—C9 | −15.7 (14) |
N5—Rh3—N6—C16 | 83.8 (8) | Rh2ii—O4—C10—N4 | 7.1 (12) |
O5iii—Rh3—N6—C16 | −91.9 (8) | Rh2ii—O4—C10—C11 | −175.2 (7) |
O11—Rh3—N6—C16 | 177.1 (8) | Rh2—N4—C10—O4 | −6.0 (14) |
Rh3iii—Rh3—N6—C16 | −2.4 (8) | Rh2—N4—C10—C11 | 176.5 (8) |
N8—Rh4—N7—C19 | −84.6 (10) | O4—C10—C11—C12B | 145.9 (12) |
O8iv—Rh4—N7—C19 | 91.8 (9) | N4—C10—C11—C12B | −36.5 (16) |
O12—Rh4—N7—C19 | −178.9 (9) | O4—C10—C11—C12A | −18.1 (16) |
Rh4iv—Rh4—N7—C19 | 1.2 (9) | N4—C10—C11—C12A | 159.6 (12) |
N7—Rh4—N8—C22 | 83.4 (10) | Rh3iii—O5—C13—N5 | −3.6 (12) |
O7iv—Rh4—N8—C22 | −92.4 (10) | Rh3iii—O5—C13—C14 | 176.9 (6) |
O12—Rh4—N8—C22 | 177.2 (9) | Rh3—N5—C13—O5 | 2.6 (13) |
Rh4iv—Rh4—N8—C22 | −2.4 (9) | Rh3—N5—C13—C14 | −177.9 (7) |
O12—Cr1—O9—Rh1 | 58.5 (4) | O5—C13—C14—C15A | 48.9 (16) |
O11—Cr1—O9—Rh1 | 179.7 (3) | N5—C13—C14—C15A | −130.7 (14) |
O10—Cr1—O9—Rh1 | −61.3 (4) | O5—C13—C14—C15B | −53.7 (17) |
N2—Rh1—O9—Cr1 | 31.2 (4) | N5—C13—C14—C15B | 126.8 (16) |
N1—Rh1—O9—Cr1 | −58.8 (4) | Rh3iii—O6—C16—N6 | −0.4 (12) |
O2i—Rh1—O9—Cr1 | −150.2 (4) | Rh3iii—O6—C16—C17 | 178.8 (7) |
O1i—Rh1—O9—Cr1 | 122.4 (4) | Rh3—N6—C16—O6 | 2.2 (13) |
O12—Cr1—O10—Rh2 | −179.9 (3) | Rh3—N6—C16—C17 | −176.9 (7) |
O11—Cr1—O10—Rh2 | 59.3 (4) | O6—C16—C17—C18B | 46 (2) |
O9—Cr1—O10—Rh2 | −60.6 (4) | N6—C16—C17—C18B | −134.9 (18) |
N4—Rh2—O10—Cr1 | −60.2 (4) | O6—C16—C17—C18A | 106.3 (14) |
N3—Rh2—O10—Cr1 | 32.2 (4) | N6—C16—C17—C18A | −74.5 (15) |
O3ii—Rh2—O10—Cr1 | −150.1 (3) | Rh4—N7—C19—O7 | 1.2 (17) |
O4ii—Rh2—O10—Cr1 | 121.2 (3) | Rh4—N7—C19—C20B | 169 (2) |
O12—Cr1—O11—Rh3 | 95.8 (5) | Rh4—N7—C19—C20A | −172 (3) |
O9—Cr1—O11—Rh3 | −24.4 (5) | Rh4iv—O7—C19—N7 | −3.4 (15) |
O10—Cr1—O11—Rh3 | −143.8 (4) | Rh4iv—O7—C19—C20B | −171 (2) |
N6—Rh3—O11—Cr1 | 2.9 (5) | Rh4iv—O7—C19—C20A | 170 (2) |
N5—Rh3—O11—Cr1 | 94.0 (5) | N7—C19—C20A—C21A | −137 (4) |
O5iii—Rh3—O11—Cr1 | −87.0 (5) | O7—C19—C20A—C21A | 49 (5) |
O6iii—Rh3—O11—Cr1 | −175.7 (5) | C20B—C19—C20A—C21A | −44 (11) |
O11—Cr1—O12—Rh4 | 54.6 (5) | N7—C19—C20B—C21B | −95 (5) |
O9—Cr1—O12—Rh4 | 175.6 (3) | O7—C19—C20B—C21B | 73 (5) |
O10—Cr1—O12—Rh4 | −65.0 (4) | C20A—C19—C20B—C21B | 168 (18) |
N8—Rh4—O12—Cr1 | −55.7 (5) | Rh4iv—O8—C22—N8 | 0.5 (15) |
N7—Rh4—O12—Cr1 | 36.4 (5) | Rh4iv—O8—C22—C23C | 180 (4) |
O8iv—Rh4—O12—Cr1 | 126.1 (4) | Rh4iv—O8—C22—C23B | −164 (2) |
O7iv—Rh4—O12—Cr1 | −145.5 (4) | Rh4iv—O8—C22—C23A | 165 (2) |
Rh1i—O1—C1—N1 | −4.5 (15) | Rh4—N8—C22—O8 | 1.7 (17) |
Rh1i—O1—C1—C2B | −173.2 (18) | Rh4—N8—C22—C23C | −177 (4) |
Rh1i—O1—C1—C2A | 165.0 (16) | Rh4—N8—C22—C23B | 167 (2) |
Rh1—N1—C1—O1 | 6.0 (16) | Rh4—N8—C22—C23A | −163 (2) |
Rh1—N1—C1—C2B | 174.7 (17) | O8—C22—C23A—C24A | 49 (4) |
Rh1—N1—C1—C2A | −162.1 (19) | N8—C22—C23A—C24A | −145 (2) |
O1—C1—C2A—C3A | 173.2 (18) | O8—C22—C23B—C24B | −48 (5) |
N1—C1—C2A—C3A | −18 (3) | N8—C22—C23B—C24B | 146 (3) |
C2B—C1—C2A—C3A | 59 (4) | O8—C22—C23C—C24C | −71 (9) |
O1—C1—C2B—C3B | 165 (2) | N8—C22—C23C—C24C | 109 (6) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O12 | 0.86 | 2.32 | 2.963 (9) | 132 |
N2—H2···O10 | 0.86 | 2.12 | 2.917 (9) | 153 |
N3—H3···O9 | 0.86 | 2.19 | 2.965 (9) | 150 |
N4—H4···O11 | 0.86 | 2.33 | 3.015 (10) | 137 |
N5—H5···N4 | 0.86 | 2.66 | 3.404 (11) | 146 |
N6—H6···O9 | 0.86 | 2.09 | 2.860 (9) | 149 |
N7—H7···O10 | 0.86 | 2.19 | 2.978 (9) | 153 |
N8—H8···O11 | 0.86 | 2.37 | 3.016 (10) | 132 |
N8—H8···O5iii | 0.86 | 2.61 | 3.392 (11) | 151 |
Symmetry code: (iii) −x+1, −y, −z+1. |
Crystal data top
C24H48MoN8O12Rh4·2.44(OH2) | Z = 2 |
Mr = 1191.52 | F(000) = 1180 |
Triclinic, P1 | Dx = 1.815 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
a = 12.952 (4) Å | Cell parameters from 6964 reflections |
b = 13.849 (5) Å | θ = 3.1–27.5° |
c = 14.679 (5) Å | µ = 1.83 mm−1 |
α = 112.460 (2)° | T = 223 K |
β = 99.574 (2)° | Block, brown |
γ = 108.472 (3)° | 0.50 × 0.30 × 0.20 mm |
V = 2180.4 (13) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 9884 independent reflections |
Graphite monochromator | 8783 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.030 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: integration (Higashi, 1999) | h = −10→16 |
Tmin = 0.581, Tmax = 0.859 | k = −17→17 |
17845 measured reflections | l = −19→17 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0235P)2 + 3.5108P] where P = (Fo2 + 2Fc2)/3 |
9884 reflections | (Δ/σ)max = 0.001 |
543 parameters | Δρmax = 0.72 e Å−3 |
178 restraints | Δρmin = −0.84 e Å−3 |
Crystal data top
C24H48MoN8O12Rh4·2.44(OH2) | γ = 108.472 (3)° |
Mr = 1191.52 | V = 2180.4 (13) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.952 (4) Å | Mo Kα radiation |
b = 13.849 (5) Å | µ = 1.83 mm−1 |
c = 14.679 (5) Å | T = 223 K |
α = 112.460 (2)° | 0.50 × 0.30 × 0.20 mm |
β = 99.574 (2)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 9884 independent reflections |
Absorption correction: integration (Higashi, 1999) | 8783 reflections with I > 2σ(I) |
Tmin = 0.581, Tmax = 0.859 | Rint = 0.030 |
17845 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.036 | 178 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.72 e Å−3 |
9884 reflections | Δρmin = −0.84 e Å−3 |
543 parameters | |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.96536 (2) | 0.03178 (3) | 0.44022 (2) | 0.02026 (7) | |
Rh2 | 0.93213 (2) | 0.40664 (2) | 0.48075 (2) | 0.02081 (7) | |
Rh3 | 0.57970 (2) | 0.04872 (3) | 0.07975 (2) | 0.02054 (7) | |
Rh4 | 0.55655 (2) | −0.00010 (2) | 0.44237 (2) | 0.01812 (7) | |
N1 | 0.8188 (3) | −0.1028 (3) | 0.3925 (3) | 0.0260 (7) | |
H1 | 0.7611 | −0.1126 | 0.3448 | 0.031* | |
O1 | 0.8775 (2) | −0.1655 (2) | 0.5049 (2) | 0.0284 (6) | |
N2 | 0.9303 (3) | 0.1340 (3) | 0.5567 (2) | 0.0248 (7) | |
H2 | 0.8995 | 0.1776 | 0.5457 | 0.030* | |
O2 | 0.9859 (2) | 0.0700 (3) | 0.6692 (2) | 0.0292 (6) | |
N3 | 0.8766 (3) | 0.3867 (3) | 0.3379 (3) | 0.0276 (7) | |
H3 | 0.8172 | 0.3235 | 0.2928 | 0.033* | |
O3 | 1.0050 (2) | 0.5602 (2) | 0.3692 (2) | 0.0290 (6) | |
N4 | 1.0517 (3) | 0.3537 (3) | 0.4450 (3) | 0.0277 (7) | |
H4 | 1.0382 | 0.2826 | 0.4292 | 0.033* | |
O4 | 1.1814 (2) | 0.5266 (2) | 0.4753 (2) | 0.0305 (6) | |
N5 | 0.5087 (3) | 0.1573 (3) | 0.1341 (3) | 0.0303 (8) | |
H5 | 0.5429 | 0.2133 | 0.1974 | 0.036* | |
O5 | 0.3553 (3) | 0.0656 (3) | −0.0139 (2) | 0.0368 (7) | |
N6 | 0.4856 (3) | −0.0595 (3) | 0.1213 (2) | 0.0278 (7) | |
H6 | 0.5140 | −0.0524 | 0.1827 | 0.033* | |
O6 | 0.3326 (2) | −0.1535 (3) | −0.0264 (2) | 0.0324 (7) | |
N7 | 0.6541 (3) | −0.0370 (3) | 0.5314 (3) | 0.0240 (7) | |
H7 | 0.7145 | −0.0437 | 0.5164 | 0.029* | |
O7 | 0.5501 (2) | −0.0394 (2) | 0.6407 (2) | 0.0274 (6) | |
N8 | 0.6433 (3) | 0.1648 (3) | 0.5391 (2) | 0.0228 (6) | |
H8 | 0.6987 | 0.2040 | 0.5239 | 0.027* | |
O8 | 0.5434 (2) | 0.1708 (2) | 0.6529 (2) | 0.0264 (6) | |
Mo1 | 0.76942 (2) | 0.11035 (3) | 0.33011 (2) | 0.01589 (7) | |
O9 | 0.8928 (2) | 0.0823 (2) | 0.3257 (2) | 0.0268 (6) | |
O10 | 0.8080 (2) | 0.2355 (2) | 0.4486 (2) | 0.0226 (5) | |
O11 | 0.7270 (2) | 0.1361 (2) | 0.2252 (2) | 0.0239 (6) | |
O12 | 0.6568 (2) | −0.0043 (2) | 0.3284 (2) | 0.0215 (5) | |
O13 | 0.5799 (3) | 0.2864 (4) | 0.3722 (3) | 0.0672 (11) | |
O14 | 0.8897 (8) | −0.0055 (14) | 0.1111 (6) | 0.221 (11) | 0.74 (2) |
O15 | 1.0649 (16) | 0.153 (2) | 0.0531 (18) | 0.249 (17) | 0.50 (3) |
O16 | 0.897 (2) | 0.149 (3) | 0.092 (3) | 0.13 (2) | 0.196 (17) |
C1 | 0.8021 (3) | −0.1784 (4) | 0.4275 (3) | 0.0267 (8) | |
C2 | 0.6908 (4) | −0.2856 (4) | 0.3772 (4) | 0.0424 (11) | |
H9 | 0.6612 | −0.2963 | 0.4315 | 0.051* | |
H10 | 0.6335 | −0.2765 | 0.3324 | 0.051* | |
C3 | 0.7077 (6) | −0.3900 (6) | 0.3133 (6) | 0.084 (2) | |
H11 | 0.7675 | −0.3969 | 0.3566 | 0.126* | |
H12 | 0.7305 | −0.3826 | 0.2557 | 0.126* | |
H13 | 0.6362 | −0.4580 | 0.2862 | 0.126* | |
C4 | 0.9512 (3) | 0.1391 (3) | 0.6491 (3) | 0.0256 (8) | |
C5 | 0.9325 (4) | 0.2274 (4) | 0.7360 (4) | 0.0405 (11) | |
H14 | 0.8548 | 0.1923 | 0.7381 | 0.049* | |
H15 | 0.9367 | 0.2911 | 0.7205 | 0.049* | |
C6 | 1.0187 (6) | 0.2749 (5) | 0.8422 (4) | 0.0650 (17) | |
H16 | 1.0961 | 0.3085 | 0.8406 | 0.097* | |
H17 | 1.0114 | 0.2133 | 0.8605 | 0.097* | |
H18 | 1.0041 | 0.3334 | 0.8937 | 0.097* | |
C7 | 0.9226 (3) | 0.4611 (3) | 0.3067 (3) | 0.0271 (8) | |
C8 | 0.8835 (4) | 0.4327 (4) | 0.1936 (3) | 0.0436 (12) | |
H19 | 0.8135 | 0.3608 | 0.1561 | 0.052* | |
H20 | 0.8644 | 0.4937 | 0.1880 | 0.052* | |
C9 | 0.9726 (6) | 0.4202 (7) | 0.1435 (5) | 0.092 (3) | |
H21 | 0.9844 | 0.3534 | 0.1404 | 0.138* | |
H22 | 1.0444 | 0.4884 | 0.1840 | 0.138* | |
H23 | 0.9471 | 0.4106 | 0.0734 | 0.138* | |
C10 | 1.1490 (3) | 0.4171 (4) | 0.4432 (3) | 0.0299 (9) | |
C11 | 1.2278 (4) | 0.3663 (4) | 0.4005 (5) | 0.0478 (12) | |
H24A | 1.2090 | 0.2930 | 0.4025 | 0.057* | 0.610 (11) |
H25A | 1.2106 | 0.3492 | 0.3270 | 0.057* | 0.610 (11) |
H24B | 1.3041 | 0.4277 | 0.4215 | 0.057* | 0.390 (11) |
H25B | 1.2365 | 0.3145 | 0.4287 | 0.057* | 0.390 (11) |
C12A | 1.3546 (7) | 0.4375 (7) | 0.4541 (8) | 0.056 (3) | 0.610 (11) |
H26A | 1.3742 | 0.5129 | 0.4580 | 0.084* | 0.610 (11) |
H27A | 1.3963 | 0.4001 | 0.4151 | 0.084* | 0.610 (11) |
H28A | 1.3755 | 0.4455 | 0.5241 | 0.084* | 0.610 (11) |
C12B | 1.1805 (17) | 0.3039 (18) | 0.2887 (12) | 0.097 (7) | 0.390 (11) |
H26B | 1.1669 | 0.3541 | 0.2615 | 0.145* | 0.390 (11) |
H27B | 1.1083 | 0.2389 | 0.2683 | 0.145* | 0.390 (11) |
H28B | 1.2342 | 0.2764 | 0.2609 | 0.145* | 0.390 (11) |
C13 | 0.4130 (4) | 0.1480 (4) | 0.0786 (3) | 0.0366 (10) | |
C14A | 0.3707 (11) | 0.2417 (11) | 0.1198 (8) | 0.063 (3) | 0.84 (2) |
H29A | 0.2901 | 0.2063 | 0.1152 | 0.075* | 0.84 (2) |
H30A | 0.4160 | 0.2936 | 0.1935 | 0.075* | 0.84 (2) |
C15A | 0.3792 (19) | 0.3085 (12) | 0.0627 (11) | 0.144 (7) | 0.84 (2) |
H31A | 0.3483 | 0.2568 | −0.0117 | 0.216* | 0.84 (2) |
H32A | 0.4594 | 0.3588 | 0.0811 | 0.216* | 0.84 (2) |
H33A | 0.3356 | 0.3543 | 0.0808 | 0.216* | 0.84 (2) |
C14B | 0.357 (4) | 0.225 (4) | 0.131 (3) | 0.040 (8) | 0.16 (2) |
H29B | 0.3198 | 0.1948 | 0.1733 | 0.048* | 0.16 (2) |
H30B | 0.4184 | 0.3014 | 0.1792 | 0.048* | 0.16 (2) |
C15B | 0.272 (7) | 0.238 (6) | 0.064 (5) | 0.13 (2) | 0.16 (2) |
H31B | 0.2289 | 0.2716 | 0.1036 | 0.189* | 0.16 (2) |
H32B | 0.2204 | 0.1636 | 0.0061 | 0.189* | 0.16 (2) |
H33B | 0.3115 | 0.2883 | 0.0373 | 0.189* | 0.16 (2) |
C16 | 0.3832 (4) | −0.1410 (4) | 0.0623 (3) | 0.0321 (9) | |
C17 | 0.3223 (4) | −0.2285 (5) | 0.0946 (4) | 0.0539 (15) | |
H34 | 0.3462 | −0.1932 | 0.1709 | 0.065* | |
H35 | 0.2390 | −0.2526 | 0.0682 | 0.065* | |
C18 | 0.3484 (7) | −0.3315 (6) | 0.0540 (6) | 0.084 (2) | |
H36 | 0.4291 | −0.3097 | 0.0875 | 0.126* | |
H37 | 0.3321 | −0.3621 | −0.0208 | 0.126* | |
H38 | 0.3010 | −0.3897 | 0.0689 | 0.126* | |
C19 | 0.6352 (3) | −0.0519 (3) | 0.6104 (3) | 0.0265 (8) | |
C20A | 0.7079 (5) | −0.0899 (8) | 0.6683 (7) | 0.0379 (15) | 0.943 (10) |
H39A | 0.6635 | −0.1709 | 0.6487 | 0.045* | 0.943 (10) |
H40A | 0.7759 | −0.0846 | 0.6460 | 0.045* | 0.943 (10) |
C21A | 0.7474 (5) | −0.0209 (6) | 0.7854 (4) | 0.0575 (19) | 0.943 (10) |
H41A | 0.6808 | −0.0270 | 0.8086 | 0.086* | 0.943 (10) |
H42A | 0.7936 | 0.0591 | 0.8060 | 0.086* | 0.943 (10) |
H43A | 0.7932 | −0.0504 | 0.8171 | 0.086* | 0.943 (10) |
C20B | 0.732 (6) | −0.067 (16) | 0.668 (13) | 0.040 (13) | 0.057 (10) |
H39B | 0.7628 | −0.1120 | 0.6201 | 0.048* | 0.057 (10) |
H40B | 0.7947 | 0.0074 | 0.7194 | 0.048* | 0.057 (10) |
C21B | 0.672 (8) | −0.131 (9) | 0.721 (8) | 0.045 (14) | 0.057 (10) |
H41B | 0.6064 | −0.2010 | 0.6682 | 0.068* | 0.057 (10) |
H42B | 0.6451 | −0.0831 | 0.7696 | 0.068* | 0.057 (10) |
H43B | 0.7249 | −0.1503 | 0.7575 | 0.068* | 0.057 (10) |
C22 | 0.6242 (3) | 0.2204 (3) | 0.6245 (3) | 0.0246 (8) | |
C23 | 0.6999 (4) | 0.3472 (3) | 0.6949 (3) | 0.0340 (9) | |
H44A | 0.7507 | 0.3563 | 0.7579 | 0.041* | 0.91 (3) |
H45A | 0.7486 | 0.3767 | 0.6588 | 0.041* | 0.91 (3) |
H44B | 0.7205 | 0.3626 | 0.7680 | 0.041* | 0.09 (3) |
H45B | 0.7711 | 0.3694 | 0.6781 | 0.041* | 0.09 (3) |
C24A | 0.6327 (6) | 0.4177 (5) | 0.7263 (11) | 0.051 (3) | 0.91 (3) |
H46A | 0.5882 | 0.3925 | 0.7664 | 0.076* | 0.91 (3) |
H47A | 0.5810 | 0.4080 | 0.6644 | 0.076* | 0.91 (3) |
H48A | 0.6853 | 0.4981 | 0.7686 | 0.076* | 0.91 (3) |
C24B | 0.635 (7) | 0.416 (6) | 0.679 (9) | 0.055 (15) | 0.09 (3) |
H46B | 0.6895 | 0.4916 | 0.6950 | 0.083* | 0.09 (3) |
H47B | 0.5891 | 0.4235 | 0.7252 | 0.083* | 0.09 (3) |
H48B | 0.5850 | 0.3767 | 0.6073 | 0.083* | 0.09 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.01803 (14) | 0.02761 (16) | 0.02194 (15) | 0.01231 (12) | 0.00773 (11) | 0.01530 (13) |
Rh2 | 0.01839 (14) | 0.01624 (14) | 0.02128 (15) | 0.00054 (11) | 0.00243 (11) | 0.00951 (12) |
Rh3 | 0.01777 (14) | 0.02307 (15) | 0.01422 (14) | 0.00418 (12) | −0.00010 (11) | 0.00807 (12) |
Rh4 | 0.01614 (13) | 0.01826 (14) | 0.01854 (14) | 0.00455 (11) | 0.00782 (11) | 0.00843 (12) |
N1 | 0.0195 (15) | 0.0321 (18) | 0.0287 (18) | 0.0115 (14) | 0.0059 (13) | 0.0166 (16) |
O1 | 0.0220 (13) | 0.0330 (16) | 0.0354 (16) | 0.0114 (12) | 0.0081 (12) | 0.0216 (14) |
N2 | 0.0244 (16) | 0.0343 (19) | 0.0255 (17) | 0.0183 (15) | 0.0096 (14) | 0.0179 (15) |
O2 | 0.0354 (15) | 0.0385 (17) | 0.0274 (15) | 0.0230 (14) | 0.0163 (13) | 0.0198 (14) |
N3 | 0.0231 (16) | 0.0190 (16) | 0.0258 (18) | −0.0029 (13) | −0.0020 (14) | 0.0098 (14) |
O3 | 0.0305 (15) | 0.0205 (14) | 0.0218 (14) | −0.0026 (12) | −0.0002 (12) | 0.0106 (12) |
N4 | 0.0241 (16) | 0.0191 (16) | 0.038 (2) | 0.0045 (14) | 0.0084 (15) | 0.0163 (16) |
O4 | 0.0246 (14) | 0.0264 (15) | 0.0401 (17) | 0.0078 (12) | 0.0129 (13) | 0.0167 (14) |
N5 | 0.0321 (18) | 0.0299 (19) | 0.0199 (17) | 0.0128 (16) | 0.0034 (14) | 0.0051 (15) |
O5 | 0.0337 (16) | 0.0414 (18) | 0.0312 (17) | 0.0185 (15) | 0.0048 (13) | 0.0131 (15) |
N6 | 0.0274 (17) | 0.0303 (18) | 0.0173 (16) | 0.0030 (15) | 0.0000 (13) | 0.0132 (15) |
O6 | 0.0250 (14) | 0.0372 (17) | 0.0208 (14) | −0.0009 (13) | −0.0030 (11) | 0.0153 (13) |
N7 | 0.0205 (15) | 0.0303 (18) | 0.0276 (17) | 0.0126 (14) | 0.0124 (13) | 0.0161 (15) |
O7 | 0.0247 (14) | 0.0382 (16) | 0.0260 (15) | 0.0142 (13) | 0.0116 (12) | 0.0190 (13) |
N8 | 0.0224 (15) | 0.0210 (16) | 0.0224 (16) | 0.0042 (13) | 0.0104 (13) | 0.0103 (14) |
O8 | 0.0264 (14) | 0.0224 (14) | 0.0235 (14) | 0.0041 (11) | 0.0123 (11) | 0.0073 (12) |
Mo1 | 0.01268 (13) | 0.01782 (15) | 0.01501 (15) | 0.00316 (12) | 0.00231 (11) | 0.00905 (12) |
O9 | 0.0208 (13) | 0.0411 (17) | 0.0304 (15) | 0.0157 (13) | 0.0117 (12) | 0.0245 (14) |
O10 | 0.0191 (12) | 0.0193 (13) | 0.0201 (13) | −0.0010 (10) | 0.0030 (10) | 0.0090 (11) |
O11 | 0.0183 (12) | 0.0244 (14) | 0.0212 (13) | 0.0019 (11) | −0.0012 (10) | 0.0120 (12) |
O12 | 0.0201 (12) | 0.0190 (13) | 0.0210 (13) | 0.0039 (11) | 0.0062 (10) | 0.0086 (11) |
O13 | 0.054 (2) | 0.081 (3) | 0.055 (3) | 0.028 (2) | 0.010 (2) | 0.024 (2) |
O14 | 0.112 (8) | 0.45 (3) | 0.060 (6) | 0.165 (12) | 0.032 (5) | 0.040 (9) |
O15 | 0.147 (18) | 0.39 (4) | 0.24 (3) | 0.08 (2) | 0.115 (17) | 0.17 (3) |
O16 | 0.058 (18) | 0.12 (3) | 0.25 (5) | 0.038 (18) | 0.09 (2) | 0.10 (3) |
C1 | 0.0207 (18) | 0.032 (2) | 0.032 (2) | 0.0141 (17) | 0.0099 (16) | 0.0162 (19) |
C2 | 0.031 (2) | 0.038 (3) | 0.052 (3) | 0.008 (2) | 0.006 (2) | 0.025 (2) |
C3 | 0.074 (5) | 0.051 (4) | 0.087 (5) | 0.010 (4) | 0.007 (4) | 0.015 (4) |
C4 | 0.0206 (18) | 0.031 (2) | 0.032 (2) | 0.0132 (17) | 0.0112 (16) | 0.0171 (18) |
C5 | 0.051 (3) | 0.047 (3) | 0.034 (3) | 0.029 (2) | 0.020 (2) | 0.018 (2) |
C6 | 0.096 (5) | 0.059 (4) | 0.029 (3) | 0.039 (4) | 0.013 (3) | 0.009 (3) |
C7 | 0.027 (2) | 0.025 (2) | 0.024 (2) | 0.0043 (17) | 0.0031 (16) | 0.0133 (17) |
C8 | 0.046 (3) | 0.037 (3) | 0.023 (2) | −0.006 (2) | −0.002 (2) | 0.015 (2) |
C9 | 0.066 (4) | 0.121 (7) | 0.032 (3) | 0.001 (4) | 0.016 (3) | 0.011 (4) |
C10 | 0.028 (2) | 0.029 (2) | 0.036 (2) | 0.0097 (18) | 0.0114 (18) | 0.019 (2) |
C11 | 0.043 (3) | 0.038 (3) | 0.075 (4) | 0.021 (2) | 0.033 (3) | 0.030 (3) |
C12A | 0.040 (4) | 0.047 (5) | 0.109 (8) | 0.027 (4) | 0.041 (5) | 0.050 (6) |
C12B | 0.099 (15) | 0.114 (17) | 0.073 (8) | 0.062 (14) | 0.057 (10) | 0.014 (11) |
C13 | 0.042 (2) | 0.037 (2) | 0.029 (2) | 0.022 (2) | 0.008 (2) | 0.012 (2) |
C14A | 0.080 (7) | 0.073 (7) | 0.047 (5) | 0.059 (7) | 0.020 (4) | 0.018 (4) |
C15A | 0.268 (19) | 0.116 (10) | 0.157 (11) | 0.152 (12) | 0.121 (12) | 0.089 (8) |
C14B | 0.037 (14) | 0.023 (13) | 0.061 (17) | 0.010 (10) | 0.029 (11) | 0.019 (12) |
C15B | 0.14 (3) | 0.11 (3) | 0.13 (3) | 0.10 (2) | 0.00 (2) | 0.03 (2) |
C16 | 0.031 (2) | 0.037 (2) | 0.021 (2) | 0.0038 (19) | 0.0026 (17) | 0.0164 (19) |
C17 | 0.045 (3) | 0.053 (3) | 0.035 (3) | −0.014 (2) | −0.009 (2) | 0.029 (3) |
C18 | 0.106 (6) | 0.059 (4) | 0.078 (5) | 0.015 (4) | 0.006 (4) | 0.049 (4) |
C19 | 0.0238 (19) | 0.030 (2) | 0.032 (2) | 0.0147 (17) | 0.0123 (17) | 0.0158 (18) |
C20A | 0.034 (3) | 0.059 (5) | 0.051 (3) | 0.029 (3) | 0.026 (3) | 0.042 (3) |
C21A | 0.055 (4) | 0.096 (5) | 0.048 (3) | 0.043 (4) | 0.020 (3) | 0.050 (4) |
C20B | 0.04 (2) | 0.06 (2) | 0.04 (2) | 0.023 (18) | 0.009 (19) | 0.039 (17) |
C21B | 0.06 (3) | 0.07 (3) | 0.06 (3) | 0.05 (3) | 0.04 (2) | 0.05 (2) |
C22 | 0.0276 (19) | 0.0234 (19) | 0.026 (2) | 0.0104 (16) | 0.0106 (16) | 0.0142 (17) |
C23 | 0.033 (2) | 0.023 (2) | 0.032 (2) | 0.0017 (18) | 0.0123 (19) | 0.0064 (19) |
C24A | 0.057 (4) | 0.021 (3) | 0.063 (6) | 0.011 (2) | 0.027 (3) | 0.011 (3) |
C24B | 0.06 (2) | 0.039 (19) | 0.05 (2) | 0.018 (15) | 0.015 (15) | 0.019 (16) |
Geometric parameters (Å, º) top
Rh1—N1 | 1.971 (3) | C8—C9 | 1.488 (8) |
Rh1—N2 | 1.987 (3) | C8—H19 | 0.9800 |
Rh1—O1i | 2.036 (3) | C8—H20 | 0.9800 |
Rh1—O2i | 2.034 (3) | C9—H21 | 0.9700 |
Rh1—O9 | 2.233 (2) | C9—H22 | 0.9700 |
Rh1—Rh1i | 2.4117 (8) | C9—H23 | 0.9700 |
Rh2—N3 | 1.980 (3) | C10—C11 | 1.504 (6) |
Rh2—N4 | 1.977 (3) | C11—C12B | 1.435 (14) |
Rh2—O3ii | 2.030 (3) | C11—C12A | 1.497 (9) |
Rh2—O4ii | 2.039 (3) | C11—H24A | 0.9800 |
Rh2—O10 | 2.214 (3) | C11—H25A | 0.9800 |
Rh2—Rh2ii | 2.4019 (9) | C11—H24B | 0.9800 |
Rh3—N5 | 1.986 (3) | C11—H25B | 0.9800 |
Rh3—N6 | 1.972 (3) | C12A—H26A | 0.9700 |
Rh3—O5iii | 2.025 (3) | C12A—H27A | 0.9700 |
Rh3—O6iii | 2.032 (3) | C12A—H28A | 0.9700 |
Rh3—O11 | 2.207 (2) | C12B—H26B | 0.9700 |
Rh3—Rh3iii | 2.4037 (8) | C12B—H27B | 0.9700 |
Rh4—N7 | 1.983 (3) | C12B—H28B | 0.9700 |
Rh4—N8 | 1.965 (3) | C13—C14B | 1.516 (18) |
Rh4—O7iv | 2.031 (3) | C13—C14A | 1.520 (7) |
Rh4—O8iv | 2.038 (3) | C14A—C15A | 1.459 (13) |
Rh4—O12 | 2.277 (3) | C14A—H29A | 0.9800 |
Rh4—Rh4iv | 2.4148 (8) | C14A—H30A | 0.9800 |
N1—C1 | 1.309 (5) | C15A—H31A | 0.9700 |
N1—H1 | 0.8700 | C15A—H32A | 0.9700 |
O1—C1 | 1.281 (4) | C15A—H33A | 0.9700 |
N2—C4 | 1.308 (5) | C14B—C15B | 1.46 (2) |
N2—H2 | 0.8700 | C14B—H29B | 0.9800 |
O2—C4 | 1.284 (4) | C14B—H30B | 0.9800 |
N3—C7 | 1.301 (5) | C15B—H31B | 0.9700 |
N3—H3 | 0.8700 | C15B—H32B | 0.9700 |
O3—C7 | 1.284 (5) | C15B—H33B | 0.9700 |
N4—C10 | 1.298 (5) | C16—C17 | 1.508 (6) |
N4—H4 | 0.8700 | C17—C18 | 1.492 (9) |
O4—C10 | 1.296 (5) | C17—H34 | 0.9800 |
N5—C13 | 1.304 (5) | C17—H35 | 0.9800 |
N5—H5 | 0.8700 | C18—H36 | 0.9700 |
O5—C13 | 1.282 (5) | C18—H37 | 0.9700 |
N6—C16 | 1.306 (5) | C18—H38 | 0.9700 |
N6—H6 | 0.8700 | C19—C20A | 1.508 (6) |
O6—C16 | 1.276 (4) | C19—C20B | 1.51 (2) |
N7—C19 | 1.301 (5) | C20A—C21A | 1.508 (10) |
N7—H7 | 0.8700 | C20A—H39A | 0.9800 |
O7—C19 | 1.292 (4) | C20A—H40A | 0.9800 |
N8—C22 | 1.308 (5) | C21A—H41A | 0.9700 |
N8—H8 | 0.8700 | C21A—H42A | 0.9700 |
O8—C22 | 1.284 (5) | C21A—H43A | 0.9700 |
Mo1—O11 | 1.750 (2) | C20B—C21B | 1.51 (2) |
Mo1—O9 | 1.766 (2) | C20B—H39B | 0.9800 |
Mo1—O12 | 1.771 (3) | C20B—H40B | 0.9800 |
Mo1—O10 | 1.772 (3) | C21B—H41B | 0.9700 |
C1—C2 | 1.510 (6) | C21B—H42B | 0.9700 |
C2—C3 | 1.500 (8) | C21B—H43B | 0.9700 |
C2—H9 | 0.9800 | C22—C23 | 1.517 (6) |
C2—H10 | 0.9800 | C23—C24A | 1.501 (7) |
C3—H11 | 0.9700 | C23—C24B | 1.51 (2) |
C3—H12 | 0.9700 | C23—H44A | 0.9800 |
C3—H13 | 0.9700 | C23—H45A | 0.9800 |
C4—C5 | 1.510 (6) | C23—H44B | 0.9800 |
C5—C6 | 1.510 (7) | C23—H45B | 0.9800 |
C5—H14 | 0.9800 | C24A—H46A | 0.9700 |
C5—H15 | 0.9800 | C24A—H47A | 0.9700 |
C6—H16 | 0.9700 | C24A—H48A | 0.9700 |
C6—H17 | 0.9700 | C24B—H46B | 0.9700 |
C6—H18 | 0.9700 | C24B—H47B | 0.9700 |
C7—C8 | 1.504 (6) | C24B—H48B | 0.9700 |
| | | |
N1—Rh1—N2 | 94.51 (14) | C9—C8—H20 | 109.1 |
N1—Rh1—O2i | 88.21 (13) | C7—C8—H20 | 109.1 |
N2—Rh1—O2i | 174.84 (11) | H19—C8—H20 | 107.8 |
N1—Rh1—O1i | 175.65 (11) | C8—C9—H21 | 109.5 |
N2—Rh1—O1i | 86.26 (13) | C8—C9—H22 | 109.5 |
O2i—Rh1—O1i | 90.70 (12) | H21—C9—H22 | 109.5 |
N1—Rh1—O9 | 91.66 (11) | C8—C9—H23 | 109.5 |
N2—Rh1—O9 | 94.46 (11) | H21—C9—H23 | 109.5 |
O2i—Rh1—O9 | 89.84 (10) | H22—C9—H23 | 109.5 |
O1i—Rh1—O9 | 92.55 (10) | O4—C10—N4 | 121.8 (4) |
N1—Rh1—Rh1i | 85.39 (9) | O4—C10—C11 | 116.7 (4) |
N2—Rh1—Rh1i | 86.14 (9) | N4—C10—C11 | 121.5 (4) |
O2i—Rh1—Rh1i | 89.71 (8) | C12B—C11—C10 | 109.5 (8) |
O1i—Rh1—Rh1i | 90.39 (7) | C12A—C11—C10 | 117.0 (5) |
O9—Rh1—Rh1i | 177.03 (7) | C12A—C11—H24A | 108.0 |
N4—Rh2—N3 | 90.09 (14) | C10—C11—H24A | 108.0 |
N4—Rh2—O3ii | 90.80 (13) | C12A—C11—H25A | 108.0 |
N3—Rh2—O3ii | 175.78 (12) | C10—C11—H25A | 108.0 |
N4—Rh2—O4ii | 175.64 (13) | H24A—C11—H25A | 107.3 |
N3—Rh2—O4ii | 91.35 (13) | C12B—C11—H24B | 109.8 |
O3ii—Rh2—O4ii | 87.47 (12) | C10—C11—H24B | 109.8 |
N4—Rh2—O10 | 94.50 (12) | C12B—C11—H25B | 109.8 |
N3—Rh2—O10 | 95.81 (11) | C10—C11—H25B | 109.8 |
O3ii—Rh2—O10 | 88.23 (10) | H24B—C11—H25B | 108.2 |
O4ii—Rh2—O10 | 89.44 (11) | C11—C12A—H26A | 109.5 |
N4—Rh2—Rh2ii | 85.71 (10) | C11—C12A—H27A | 109.5 |
N3—Rh2—Rh2ii | 85.29 (9) | H26A—C12A—H27A | 109.5 |
O3ii—Rh2—Rh2ii | 90.66 (8) | C11—C12A—H28A | 109.5 |
O4ii—Rh2—Rh2ii | 90.31 (8) | H26A—C12A—H28A | 109.5 |
O10—Rh2—Rh2ii | 178.87 (7) | H27A—C12A—H28A | 109.5 |
N6—Rh3—N5 | 92.05 (15) | C11—C12B—H26B | 109.5 |
N6—Rh3—O5iii | 88.86 (14) | C11—C12B—H27B | 109.5 |
N5—Rh3—O5iii | 175.88 (12) | H26B—C12B—H27B | 109.5 |
N6—Rh3—O6iii | 175.75 (12) | C11—C12B—H28B | 109.5 |
N5—Rh3—O6iii | 88.12 (14) | H26B—C12B—H28B | 109.5 |
O5iii—Rh3—O6iii | 90.68 (13) | H27B—C12B—H28B | 109.5 |
N6—Rh3—O11 | 93.74 (11) | O5—C13—N5 | 122.5 (4) |
N5—Rh3—O11 | 94.04 (12) | O5—C13—C14B | 118 (2) |
O5iii—Rh3—O11 | 89.91 (11) | N5—C13—C14B | 118.8 (19) |
O6iii—Rh3—O11 | 90.49 (10) | O5—C13—C14A | 117.3 (5) |
N6—Rh3—Rh3iii | 86.15 (9) | N5—C13—C14A | 120.0 (6) |
N5—Rh3—Rh3iii | 86.83 (10) | C15A—C14A—C13 | 112.9 (7) |
O5iii—Rh3—Rh3iii | 89.22 (9) | C15A—C14A—H29A | 109.0 |
O6iii—Rh3—Rh3iii | 89.61 (8) | C13—C14A—H29A | 109.0 |
O11—Rh3—Rh3iii | 179.13 (7) | C15A—C14A—H30A | 109.0 |
N8—Rh4—N7 | 90.44 (13) | C13—C14A—H30A | 109.0 |
N8—Rh4—O7iv | 88.66 (12) | H29A—C14A—H30A | 107.8 |
N7—Rh4—O7iv | 175.56 (12) | C14A—C15A—H31A | 109.5 |
N8—Rh4—O8iv | 175.50 (11) | C14A—C15A—H32A | 109.5 |
N7—Rh4—O8iv | 90.52 (13) | H31A—C15A—H32A | 109.5 |
O7iv—Rh4—O8iv | 90.05 (11) | C14A—C15A—H33A | 109.5 |
N8—Rh4—O12 | 96.02 (11) | H31A—C15A—H33A | 109.5 |
N7—Rh4—O12 | 96.51 (11) | H32A—C15A—H33A | 109.5 |
O7iv—Rh4—O12 | 87.91 (10) | C15B—C14B—C13 | 117 (3) |
O8iv—Rh4—O12 | 88.23 (10) | C15B—C14B—H29B | 108.0 |
N8—Rh4—Rh4iv | 85.49 (9) | C13—C14B—H29B | 108.0 |
N7—Rh4—Rh4iv | 85.07 (9) | C15B—C14B—H30B | 108.0 |
O7iv—Rh4—Rh4iv | 90.53 (8) | C13—C14B—H30B | 108.0 |
O8iv—Rh4—Rh4iv | 90.22 (8) | H29B—C14B—H30B | 107.2 |
O12—Rh4—Rh4iv | 177.80 (6) | C14B—C15B—H31B | 109.5 |
C1—N1—Rh1 | 124.7 (3) | C14B—C15B—H32B | 109.5 |
C1—N1—H1 | 117.6 | H31B—C15B—H32B | 109.5 |
Rh1—N1—H1 | 117.6 | C14B—C15B—H33B | 109.5 |
C1—O1—Rh1i | 116.7 (2) | H31B—C15B—H33B | 109.5 |
C4—N2—Rh1 | 123.4 (3) | H32B—C15B—H33B | 109.5 |
C4—N2—H2 | 118.3 | O6—C16—N6 | 122.0 (4) |
Rh1—N2—H2 | 118.3 | O6—C16—C17 | 117.1 (4) |
C4—O2—Rh1i | 117.6 (2) | N6—C16—C17 | 120.8 (3) |
C7—N3—Rh2 | 124.7 (3) | C18—C17—C16 | 111.7 (5) |
C7—N3—H3 | 117.7 | C18—C17—H34 | 109.3 |
Rh2—N3—H3 | 117.7 | C16—C17—H34 | 109.3 |
C7—O3—Rh2ii | 116.9 (2) | C18—C17—H35 | 109.3 |
C10—N4—Rh2 | 124.9 (3) | C16—C17—H35 | 109.3 |
C10—N4—H4 | 117.6 | H34—C17—H35 | 108.0 |
Rh2—N4—H4 | 117.6 | C17—C18—H36 | 109.5 |
C10—O4—Rh2ii | 117.0 (2) | C17—C18—H37 | 109.5 |
C13—N5—Rh3 | 122.7 (3) | H36—C18—H37 | 109.5 |
C13—N5—H5 | 118.7 | C17—C18—H38 | 109.5 |
Rh3—N5—H5 | 118.7 | H36—C18—H38 | 109.5 |
C13—O5—Rh3iii | 118.7 (3) | H37—C18—H38 | 109.5 |
C16—N6—Rh3 | 124.0 (3) | O7—C19—N7 | 121.6 (3) |
C16—N6—H6 | 118.0 | O7—C19—C20A | 116.4 (4) |
Rh3—N6—H6 | 118.0 | N7—C19—C20A | 122.0 (4) |
C16—O6—Rh3iii | 118.1 (3) | O7—C19—C20B | 126 (5) |
C19—N7—Rh4 | 125.4 (3) | N7—C19—C20B | 112 (4) |
C19—N7—H7 | 117.3 | C21A—C20A—C19 | 114.2 (6) |
Rh4—N7—H7 | 117.3 | C21A—C20A—H39A | 108.7 |
C19—O7—Rh4iv | 117.4 (2) | C19—C20A—H39A | 108.7 |
C22—N8—Rh4 | 125.1 (3) | C21A—C20A—H40A | 108.7 |
C22—N8—H8 | 117.5 | C19—C20A—H40A | 108.7 |
Rh4—N8—H8 | 117.5 | H39A—C20A—H40A | 107.6 |
C22—O8—Rh4iv | 116.9 (2) | C20A—C21A—H41A | 109.5 |
O9—Mo1—O10 | 107.90 (13) | C20A—C21A—H42A | 109.5 |
O11—Mo1—O9 | 108.53 (12) | H41A—C21A—H42A | 109.5 |
O9—Mo1—O12 | 111.38 (12) | C20A—C21A—H43A | 109.5 |
O11—Mo1—O10 | 109.17 (12) | H41A—C21A—H43A | 109.5 |
O12—Mo1—O10 | 108.12 (12) | H42A—C21A—H43A | 109.5 |
O11—Mo1—O12 | 111.64 (12) | C21B—C20B—C19 | 102 (4) |
Mo1—O9—Rh1 | 119.29 (13) | C21B—C20B—H39B | 111.5 |
Mo1—O10—Rh2 | 122.07 (13) | C19—C20B—H39B | 111.5 |
Mo1—O11—Rh3 | 136.57 (14) | C21B—C20B—H40B | 111.5 |
Mo1—O12—Rh4 | 129.21 (13) | C19—C20B—H40B | 111.5 |
O1—C1—N1 | 122.4 (4) | H39B—C20B—H40B | 109.3 |
O1—C1—C2 | 117.2 (4) | C20B—C21B—H41B | 109.5 |
N1—C1—C2 | 120.4 (4) | C20B—C21B—H42B | 109.5 |
C3—C2—C1 | 111.4 (4) | H41B—C21B—H42B | 109.5 |
C3—C2—H9 | 109.3 | C20B—C21B—H43B | 109.5 |
C1—C2—H9 | 109.3 | H41B—C21B—H43B | 109.5 |
C3—C2—H10 | 109.3 | H42B—C21B—H43B | 109.5 |
C1—C2—H10 | 109.3 | O8—C22—N8 | 122.3 (4) |
H9—C2—H10 | 108.0 | O8—C22—C23 | 117.6 (3) |
C2—C3—H11 | 109.5 | N8—C22—C23 | 120.1 (3) |
C2—C3—H12 | 109.5 | C24A—C23—C22 | 113.2 (4) |
H11—C3—H12 | 109.5 | C24B—C23—C22 | 109 (3) |
C2—C3—H13 | 109.5 | C24A—C23—H44A | 108.9 |
H11—C3—H13 | 109.5 | C22—C23—H44A | 108.9 |
H12—C3—H13 | 109.5 | C24A—C23—H45A | 108.9 |
O2—C4—N2 | 122.4 (4) | C22—C23—H45A | 108.9 |
O2—C4—C5 | 117.8 (3) | H44A—C23—H45A | 107.7 |
N2—C4—C5 | 119.8 (3) | C24B—C23—H44B | 109.9 |
C4—C5—C6 | 113.7 (4) | C22—C23—H44B | 109.9 |
C4—C5—H14 | 108.8 | C24A—C23—H45B | 127.0 |
C6—C5—H14 | 108.8 | C24B—C23—H45B | 109.9 |
C4—C5—H15 | 108.8 | C22—C23—H45B | 109.9 |
C6—C5—H15 | 108.8 | H44B—C23—H45B | 108.3 |
H14—C5—H15 | 107.7 | C23—C24A—H46A | 109.5 |
C5—C6—H16 | 109.5 | C23—C24A—H47A | 109.5 |
C5—C6—H17 | 109.5 | H46A—C24A—H47A | 109.5 |
H16—C6—H17 | 109.5 | C23—C24A—H48A | 109.5 |
C5—C6—H18 | 109.5 | H46A—C24A—H48A | 109.5 |
H16—C6—H18 | 109.5 | H47A—C24A—H48A | 109.5 |
H17—C6—H18 | 109.5 | C23—C24B—H46B | 109.5 |
O3—C7—N3 | 122.3 (4) | C23—C24B—H47B | 109.5 |
O3—C7—C8 | 116.8 (3) | H46B—C24B—H47B | 109.5 |
N3—C7—C8 | 120.9 (4) | C23—C24B—H48B | 109.5 |
C9—C8—C7 | 112.5 (4) | H46B—C24B—H48B | 109.5 |
C9—C8—H19 | 109.1 | H47B—C24B—H48B | 109.5 |
C7—C8—H19 | 109.1 | | |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y, −z; (iv) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O12 | 0.87 | 2.36 | 3.049 (4) | 136 |
N2—H2···O10 | 0.87 | 2.24 | 3.048 (4) | 156 |
N3—H3···O11 | 0.87 | 2.19 | 2.970 (4) | 148 |
N4—H4···O9 | 0.87 | 2.46 | 3.210 (4) | 144 |
N4—H4···O1i | 0.87 | 2.59 | 3.307 (4) | 140 |
N5—H5···O13 | 0.87 | 2.27 | 3.061 (5) | 152 |
N6—H6···O12 | 0.87 | 2.29 | 3.107 (4) | 156 |
N7—H7···N1 | 0.87 | 2.49 | 3.286 (5) | 153 |
N8—H8···O10 | 0.87 | 1.98 | 2.808 (4) | 159 |
Symmetry code: (i) −x+2, −y, −z+1. |
Crystal data top
C32H64MoN8O12Rh4 | Z = 4 |
Mr = 1260.49 | F(000) = 2520 |
Triclinic, P1 | Dx = 1.811 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
a = 15.567 (4) Å | Cell parameters from 8708 reflections |
b = 15.778 (4) Å | θ = 3.2–27.5° |
c = 19.221 (5) Å | µ = 1.72 mm−1 |
α = 87.720 (6)° | T = 118 K |
β = 89.872 (6)° | Block, brown |
γ = 78.448 (5)° | 0.10 × 0.10 × 0.10 mm |
V = 4621.6 (19) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 21025 independent reflections |
Graphite monochromator | 13532 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.066 |
ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: integration NUMABS (Higashi, 1999) | h = −20→15 |
Tmin = 0.804, Tmax = 0.902 | k = −20→19 |
38498 measured reflections | l = −24→24 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.062 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.104 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0273P)2] where P = (Fo2 + 2Fc2)/3 |
21025 reflections | (Δ/σ)max = 0.002 |
1043 parameters | Δρmax = 1.09 e Å−3 |
33 restraints | Δρmin = −0.96 e Å−3 |
Crystal data top
C32H64MoN8O12Rh4 | γ = 78.448 (5)° |
Mr = 1260.49 | V = 4621.6 (19) Å3 |
Triclinic, P1 | Z = 4 |
a = 15.567 (4) Å | Mo Kα radiation |
b = 15.778 (4) Å | µ = 1.72 mm−1 |
c = 19.221 (5) Å | T = 118 K |
α = 87.720 (6)° | 0.10 × 0.10 × 0.10 mm |
β = 89.872 (6)° | |
Data collection top
Rigaku/MSC Mercury CCD diffractometer | 21025 independent reflections |
Absorption correction: integration NUMABS (Higashi, 1999) | 13532 reflections with I > 2σ(I) |
Tmin = 0.804, Tmax = 0.902 | Rint = 0.066 |
38498 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.062 | 33 restraints |
wR(F2) = 0.104 | H-atom parameters constrained |
S = 1.02 | Δρmax = 1.09 e Å−3 |
21025 reflections | Δρmin = −0.96 e Å−3 |
1043 parameters | |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.15014 (4) | 0.27528 (3) | 0.24126 (3) | 0.01180 (13) | |
Rh2 | 0.30164 (4) | 0.24005 (3) | 0.27786 (3) | 0.01195 (13) | |
Rh3 | −0.22217 (4) | 0.26759 (3) | 0.19721 (3) | 0.01093 (13) | |
Rh4 | −0.31888 (4) | 0.24687 (3) | 0.29173 (3) | 0.01124 (13) | |
Rh5 | 0.01650 (4) | 0.42438 (3) | 0.01760 (3) | 0.01075 (13) | |
Rh6 | 0.00771 (4) | 0.04862 (3) | 0.04559 (3) | 0.01138 (13) | |
Rh7 | 0.47703 (4) | 0.07599 (3) | 0.48433 (3) | 0.01132 (13) | |
Rh8 | 0.48546 (4) | 0.45860 (3) | 0.45154 (3) | 0.01110 (13) | |
Mo1 | −0.01569 (4) | 0.24969 (4) | 0.12292 (3) | 0.00904 (14) | |
Mo2 | 0.48237 (4) | 0.25815 (4) | 0.37689 (3) | 0.00942 (14) | |
N1 | 0.1959 (4) | 0.2876 (3) | 0.1462 (3) | 0.0121 (13) | |
H1 | 0.1584 | 0.3089 | 0.1126 | 0.015* | |
O1 | 0.3393 (3) | 0.2473 (3) | 0.1772 (2) | 0.0188 (12) | |
N2 | 0.1612 (4) | 0.1497 (3) | 0.2299 (3) | 0.0158 (14) | |
H2 | 0.1149 | 0.1315 | 0.2151 | 0.019* | |
O2 | 0.3037 (3) | 0.1117 (3) | 0.2648 (2) | 0.0134 (11) | |
O3 | 0.1127 (3) | 0.2604 (3) | 0.3421 (2) | 0.0159 (12) | |
N3 | 0.2563 (4) | 0.2244 (3) | 0.3733 (3) | 0.0163 (14) | |
H3 | 0.2947 | 0.2100 | 0.4074 | 0.020* | |
O4 | 0.1454 (3) | 0.4022 (3) | 0.2573 (2) | 0.0131 (11) | |
N4 | 0.2893 (4) | 0.3662 (3) | 0.2885 (3) | 0.0137 (13) | |
H4 | 0.3365 | 0.3853 | 0.3000 | 0.016* | |
N5 | −0.1500 (4) | 0.3063 (3) | 0.2694 (3) | 0.0121 (13) | |
H5 | −0.1037 | 0.3264 | 0.2555 | 0.015* | |
O5 | −0.2353 (3) | 0.2809 (3) | 0.3616 (2) | 0.0151 (11) | |
N6 | −0.1628 (4) | 0.1451 (3) | 0.2156 (3) | 0.0123 (13) | |
H6 | −0.1173 | 0.1234 | 0.1902 | 0.015* | |
O6 | −0.2542 (3) | 0.1210 (3) | 0.3037 (2) | 0.0168 (12) | |
O7 | −0.3048 (3) | 0.2295 (3) | 0.1284 (2) | 0.0136 (11) | |
N7 | −0.3963 (4) | 0.2165 (3) | 0.2187 (3) | 0.0152 (14) | |
H7 | −0.4459 | 0.2023 | 0.2321 | 0.018* | |
O8 | −0.2920 (3) | 0.3904 (3) | 0.1805 (2) | 0.0159 (11) | |
N8 | −0.3748 (4) | 0.3708 (3) | 0.2749 (3) | 0.0148 (14) | |
H8 | −0.4145 | 0.3951 | 0.3044 | 0.018* | |
N9 | 0.0137 (4) | 0.4651 (3) | 0.1139 (3) | 0.0145 (14) | |
H9 | 0.0281 | 0.4258 | 0.1480 | 0.017* | |
O9 | −0.0224 (3) | 0.6090 (3) | 0.0836 (2) | 0.0165 (12) | |
N10 | −0.1112 (4) | 0.4322 (3) | 0.0197 (3) | 0.0122 (13) | |
H10 | −0.1306 | 0.3845 | 0.0297 | 0.015* | |
O10 | −0.1459 (3) | 0.5761 (3) | −0.0113 (2) | 0.0147 (11) | |
N11 | 0.0212 (4) | 0.1332 (3) | −0.0316 (3) | 0.0146 (14) | |
H11 | 0.0327 | 0.1834 | −0.0207 | 0.018* | |
O11 | 0.0018 (3) | 0.0454 (3) | −0.1186 (2) | 0.0177 (12) | |
N12 | −0.1215 (4) | 0.0849 (3) | 0.0402 (3) | 0.0157 (14) | |
H12 | −0.1472 | 0.1258 | 0.0675 | 0.019* | |
O12 | −0.1398 (3) | −0.0055 (3) | −0.0462 (2) | 0.0172 (12) | |
N13 | 0.6032 (4) | 0.0730 (3) | 0.4719 (3) | 0.0162 (14) | |
H13 | 0.6183 | 0.1224 | 0.4599 | 0.019* | |
O13 | 0.6505 (3) | −0.0701 (3) | 0.4982 (2) | 0.0166 (12) | |
N14 | 0.4653 (4) | 0.0390 (4) | 0.3883 (3) | 0.0158 (14) | |
H14 | 0.4453 | 0.0788 | 0.3557 | 0.019* | |
O14 | 0.5127 (3) | −0.1048 (3) | 0.4145 (2) | 0.0154 (11) | |
N15 | 0.5999 (4) | 0.3821 (3) | 0.4743 (3) | 0.0148 (13) | |
H15 | 0.6192 | 0.3391 | 0.4468 | 0.018* | |
O15 | 0.6276 (3) | 0.4547 (3) | 0.5685 (2) | 0.0142 (11) | |
N16 | 0.4262 (4) | 0.3943 (3) | 0.5200 (3) | 0.0159 (14) | |
H16 | 0.4008 | 0.3537 | 0.5043 | 0.019* | |
O16 | 0.4523 (3) | 0.4674 (3) | 0.6131 (2) | 0.0158 (11) | |
O17 | 0.0127 (3) | 0.3003 (3) | 0.1975 (2) | 0.0100 (11) | |
O18 | −0.1295 (3) | 0.2798 (3) | 0.1083 (2) | 0.0154 (11) | |
O19 | 0.0410 (3) | 0.2836 (3) | 0.0504 (2) | 0.0126 (11) | |
O20 | 0.0140 (3) | 0.1358 (3) | 0.1353 (2) | 0.0135 (11) | |
O21 | 0.4453 (3) | 0.2106 (3) | 0.3036 (2) | 0.0125 (11) | |
O22 | 0.5981 (3) | 0.2283 (3) | 0.3832 (2) | 0.0107 (11) | |
O23 | 0.4360 (3) | 0.2196 (3) | 0.4528 (2) | 0.0128 (11) | |
O24 | 0.4537 (3) | 0.3724 (3) | 0.3676 (2) | 0.0122 (11) | |
C1 | 0.2783 (5) | 0.2659 (4) | 0.1305 (4) | 0.0131 (16) | |
C2 | 0.3060 (5) | 0.2549 (4) | 0.0561 (3) | 0.0161 (17) | |
H2A | 0.3619 | 0.2747 | 0.0485 | 0.019* | 0.37 (3) |
H2B | 0.2610 | 0.2901 | 0.0248 | 0.019* | 0.37 (3) |
H2C | 0.3549 | 0.2853 | 0.0469 | 0.019* | 0.63 (3) |
H2D | 0.2564 | 0.2822 | 0.0253 | 0.019* | 0.63 (3) |
C3A | 0.336 (3) | 0.1583 (10) | 0.0380 (15) | 0.039 (13)* | 0.37 (3) |
H3A | 0.3000 | 0.1195 | 0.0602 | 0.047* | 0.37 (3) |
H3B | 0.3991 | 0.1351 | 0.0455 | 0.047* | 0.37 (3) |
C4A | 0.310 (4) | 0.185 (4) | −0.0404 (19) | 0.18 (2)* | 0.37 (3) |
H4A | 0.3236 | 0.1333 | −0.0685 | 0.272* | 0.37 (3) |
H4B | 0.3437 | 0.2274 | −0.0576 | 0.272* | 0.37 (3) |
H4C | 0.2474 | 0.2097 | −0.0437 | 0.272* | 0.37 (3) |
C3B | 0.3177 (19) | 0.1586 (8) | 0.0398 (8) | 0.046 (9)* | 0.63 (3) |
H3C | 0.2602 | 0.1409 | 0.0423 | 0.056* | 0.63 (3) |
H3D | 0.3571 | 0.1231 | 0.0749 | 0.056* | 0.63 (3) |
C4B | 0.3573 (9) | 0.1421 (8) | −0.0343 (6) | 0.024 (5)* | 0.63 (3) |
H4D | 0.3631 | 0.0808 | −0.0442 | 0.036* | 0.63 (3) |
H4E | 0.4151 | 0.1577 | −0.0362 | 0.036* | 0.63 (3) |
H4F | 0.3184 | 0.1775 | −0.0690 | 0.036* | 0.63 (3) |
C5 | 0.2322 (5) | 0.0921 (4) | 0.2427 (3) | 0.0149 (16) | |
C6 | 0.2304 (5) | −0.0017 (4) | 0.2345 (4) | 0.0218 (19) | |
H6A | 0.2886 | −0.0322 | 0.2186 | 0.026* | |
H6B | 0.1867 | −0.0068 | 0.1984 | 0.026* | |
C7 | 0.2075 (6) | −0.0452 (5) | 0.3027 (5) | 0.039 (2) | |
H7A | 0.2160 | −0.1084 | 0.2968 | 0.047* | |
H7B | 0.2482 | −0.0356 | 0.3397 | 0.047* | |
C8 | 0.1139 (7) | −0.0111 (6) | 0.3253 (5) | 0.065 (4) | |
H8A | 0.1068 | 0.0502 | 0.3358 | 0.097* | |
H8B | 0.1010 | −0.0440 | 0.3670 | 0.097* | |
H8C | 0.0735 | −0.0174 | 0.2877 | 0.097* | |
C9 | 0.1734 (5) | 0.2340 (4) | 0.3888 (4) | 0.0142 (16) | |
C10 | 0.1432 (5) | 0.2152 (4) | 0.4611 (3) | 0.0200 (18) | |
H10A | 0.1946 | 0.1850 | 0.4889 | 0.024* | |
H10B | 0.1019 | 0.1753 | 0.4583 | 0.024* | |
C11 | 0.0986 (5) | 0.2948 (5) | 0.4994 (4) | 0.0252 (19) | |
H11A | 0.0538 | 0.3312 | 0.4686 | 0.030* | |
H11B | 0.1426 | 0.3296 | 0.5111 | 0.030* | |
C12 | 0.0548 (6) | 0.2683 (6) | 0.5666 (4) | 0.051 (3) | |
H12A | 0.0128 | 0.2323 | 0.5551 | 0.077* | |
H12B | 0.0241 | 0.3204 | 0.5891 | 0.077* | |
H12C | 0.0998 | 0.2355 | 0.5983 | 0.077* | |
C13 | 0.2157 (5) | 0.4239 (4) | 0.2795 (3) | 0.0123 (16) | |
C14 | 0.2089 (5) | 0.5174 (4) | 0.2971 (4) | 0.0182 (17) | |
H14A | 0.1939 | 0.5548 | 0.2545 | 0.022* | |
H14B | 0.2664 | 0.5257 | 0.3145 | 0.022* | |
C15 | 0.1398 (5) | 0.5440 (5) | 0.3519 (4) | 0.0253 (19) | |
H15A | 0.1371 | 0.6055 | 0.3620 | 0.030* | |
H15B | 0.0820 | 0.5389 | 0.3331 | 0.030* | |
C16 | 0.1574 (5) | 0.4898 (5) | 0.4189 (4) | 0.031 (2) | |
H16A | 0.1501 | 0.4307 | 0.4109 | 0.046* | |
H16B | 0.1160 | 0.5151 | 0.4545 | 0.046* | |
H16C | 0.2175 | 0.4886 | 0.4347 | 0.046* | |
C17 | −0.1660 (5) | 0.3042 (4) | 0.3368 (4) | 0.0124 (16) | |
C18 | −0.1044 (5) | 0.3297 (4) | 0.3862 (4) | 0.0151 (16) | |
H18A | −0.0452 | 0.2939 | 0.3793 | 0.018* | |
H18B | −0.1228 | 0.3176 | 0.4343 | 0.018* | |
C19 | −0.0991 (5) | 0.4258 (4) | 0.3778 (4) | 0.0242 (19) | |
H19A | −0.0585 | 0.4393 | 0.4133 | 0.029* | |
H19B | −0.0749 | 0.4367 | 0.3314 | 0.029* | |
C20 | −0.1883 (6) | 0.4857 (5) | 0.3851 (4) | 0.035 (2) | |
H20A | −0.2282 | 0.4740 | 0.3490 | 0.052* | |
H20B | −0.1815 | 0.5461 | 0.3800 | 0.052* | |
H20C | −0.2124 | 0.4755 | 0.4312 | 0.052* | |
C21 | −0.1890 (5) | 0.0954 (4) | 0.2642 (4) | 0.0151 (16) | |
C22 | −0.1449 (4) | 0.0016 (4) | 0.2717 (4) | 0.0163 (17) | |
H22A | −0.1188 | −0.0103 | 0.3189 | 0.020* | |
H22B | −0.0968 | −0.0105 | 0.2375 | 0.020* | |
C23 | −0.2082 (5) | −0.0582 (5) | 0.2605 (4) | 0.0238 (19) | |
H23A | −0.1771 | −0.1190 | 0.2685 | 0.029* | |
H23B | −0.2561 | −0.0464 | 0.2949 | 0.029* | |
C24 | −0.2471 (5) | −0.0469 (5) | 0.1878 (4) | 0.030 (2) | |
H24A | −0.2762 | 0.0136 | 0.1791 | 0.045* | |
H24B | −0.2900 | −0.0842 | 0.1836 | 0.045* | |
H24C | −0.2003 | −0.0629 | 0.1537 | 0.045* | |
C25 | −0.3789 (5) | 0.2161 (4) | 0.1524 (4) | 0.0151 (17) | |
C26 | −0.4452 (5) | 0.2036 (5) | 0.0992 (4) | 0.0197 (17) | |
H26A | −0.5030 | 0.2077 | 0.1219 | 0.024* | |
H26B | −0.4279 | 0.1450 | 0.0808 | 0.024* | |
C27 | −0.4536 (5) | 0.2703 (4) | 0.0391 (4) | 0.0231 (19) | |
H27A | −0.3961 | 0.2654 | 0.0158 | 0.028* | |
H27B | −0.4960 | 0.2578 | 0.0046 | 0.028* | |
C28 | −0.4836 (5) | 0.3619 (5) | 0.0625 (4) | 0.036 (2) | |
H28A | −0.5346 | 0.3646 | 0.0928 | 0.055* | |
H28B | −0.4996 | 0.4011 | 0.0216 | 0.055* | |
H28C | −0.4360 | 0.3793 | 0.0880 | 0.055* | |
C29 | −0.3550 (4) | 0.4178 (4) | 0.2218 (4) | 0.0125 (16) | |
C30 | −0.4052 (5) | 0.5086 (4) | 0.2064 (4) | 0.0181 (17) | |
H30A | −0.3944 | 0.5246 | 0.1573 | 0.022* | |
H30B | −0.3808 | 0.5482 | 0.2359 | 0.022* | |
C31 | −0.5042 (5) | 0.5246 (5) | 0.2176 (4) | 0.030 (2) | |
H31A | −0.5299 | 0.4849 | 0.1890 | 0.036* | |
H31B | −0.5164 | 0.5121 | 0.2671 | 0.036* | |
C32 | −0.5465 (6) | 0.6178 (5) | 0.1975 (5) | 0.047 (3) | |
H32A | −0.5239 | 0.6569 | 0.2278 | 0.071* | |
H32B | −0.6102 | 0.6259 | 0.2028 | 0.071* | |
H32C | −0.5327 | 0.6307 | 0.1489 | 0.071* | |
C33 | −0.0079 (5) | 0.5462 (4) | 0.1305 (4) | 0.0158 (17) | |
C34 | −0.0208 (5) | 0.5706 (4) | 0.2046 (3) | 0.0186 (17) | |
H34A | 0.0209 | 0.6077 | 0.2164 | 0.022* | |
H34B | −0.0075 | 0.5175 | 0.2351 | 0.022* | |
C35 | −0.1120 (6) | 0.6177 (5) | 0.2187 (5) | 0.043 (3) | |
H35A | −0.1173 | 0.6296 | 0.2689 | 0.051* | |
H35B | −0.1227 | 0.6741 | 0.1924 | 0.051* | |
C36 | −0.1791 (6) | 0.5702 (6) | 0.1998 (4) | 0.048 (3) | |
H36A | −0.1843 | 0.5706 | 0.1490 | 0.072* | |
H36B | −0.2355 | 0.5977 | 0.2196 | 0.072* | |
H36C | −0.1628 | 0.5102 | 0.2182 | 0.072* | |
C37 | −0.1693 (4) | 0.5035 (4) | 0.0074 (3) | 0.0118 (16) | |
C38 | −0.2654 (4) | 0.5023 (4) | 0.0133 (4) | 0.0167 (17) | |
H38A | −0.2758 | 0.4713 | 0.0573 | 0.020* | |
H38B | −0.2990 | 0.5625 | 0.0150 | 0.020* | |
C39 | −0.2982 (5) | 0.4590 (5) | −0.0467 (4) | 0.029 (2) | |
H39A | −0.3620 | 0.4623 | −0.0413 | 0.035* | |
H39B | −0.2693 | 0.3970 | −0.0449 | 0.035* | |
C40 | −0.2818 (5) | 0.4983 (5) | −0.1173 (4) | 0.039 (2) | |
H40A | −0.3171 | 0.5571 | −0.1224 | 0.058* | |
H40B | −0.2980 | 0.4628 | −0.1539 | 0.058* | |
H40C | −0.2195 | 0.5006 | −0.1215 | 0.058* | |
C41 | 0.0141 (5) | 0.1185 (4) | −0.0968 (4) | 0.0179 (17) | |
C42 | 0.0173 (5) | 0.1888 (4) | −0.1528 (4) | 0.0243 (19) | |
H42A | 0.0599 | 0.1655 | −0.1891 | 0.029* | |
H42B | 0.0373 | 0.2379 | −0.1319 | 0.029* | |
C43 | −0.0739 (7) | 0.2208 (5) | −0.1862 (5) | 0.045 (3) | |
H43A | −0.0984 | 0.1703 | −0.1993 | 0.054* | |
H43B | −0.0680 | 0.2557 | −0.2293 | 0.054* | |
C44 | −0.1379 (6) | 0.2762 (6) | −0.1363 (5) | 0.061 (3) | |
H44A | −0.1443 | 0.2417 | −0.0938 | 0.091* | |
H44B | −0.1951 | 0.2949 | −0.1590 | 0.091* | |
H44C | −0.1146 | 0.3271 | −0.1243 | 0.091* | |
C45 | −0.1710 (5) | 0.0517 (4) | −0.0014 (4) | 0.0170 (17) | |
C46 | −0.2690 (5) | 0.0767 (5) | 0.0048 (4) | 0.027 (2) | |
H46A | −0.2835 | 0.1339 | 0.0260 | 0.033* | |
H46B | −0.2887 | 0.0344 | 0.0375 | 0.033* | |
C47 | −0.3215 (5) | 0.0814 (5) | −0.0620 (4) | 0.029 (2) | |
H47A | −0.3847 | 0.0892 | −0.0510 | 0.035* | |
H47B | −0.3040 | 0.0265 | −0.0863 | 0.035* | |
C48 | −0.3060 (6) | 0.1571 (5) | −0.1098 (4) | 0.038 (2) | |
H48A | −0.3192 | 0.2109 | −0.0846 | 0.057* | |
H48B | −0.3443 | 0.1624 | −0.1508 | 0.057* | |
H48C | −0.2447 | 0.1465 | −0.1247 | 0.057* | |
C49 | 0.6670 (5) | 0.0051 (5) | 0.4795 (4) | 0.0193 (18) | |
C50 | 0.7610 (5) | 0.0086 (4) | 0.4671 (4) | 0.027 (2) | |
H50A | 0.7756 | −0.0074 | 0.4186 | 0.032* | |
H50B | 0.7977 | −0.0356 | 0.4982 | 0.032* | |
C51 | 0.7858 (5) | 0.0951 (5) | 0.4784 (4) | 0.032 (2) | |
H51A | 0.7705 | 0.1124 | 0.5265 | 0.039* | |
H51B | 0.7512 | 0.1394 | 0.4461 | 0.039* | |
C52 | 0.8827 (5) | 0.0931 (5) | 0.4669 (4) | 0.037 (2) | |
H52A | 0.9174 | 0.0476 | 0.4973 | 0.055* | |
H52B | 0.8960 | 0.1492 | 0.4778 | 0.055* | |
H52C | 0.8973 | 0.0810 | 0.4182 | 0.055* | |
C53 | 0.4860 (5) | −0.0428 (5) | 0.3705 (4) | 0.0185 (18) | |
C54 | 0.4773 (5) | −0.0641 (4) | 0.2961 (3) | 0.0175 (17) | |
H54A | 0.4143 | −0.0591 | 0.2852 | 0.021* | |
H54B | 0.5066 | −0.1251 | 0.2903 | 0.021* | |
C55 | 0.5158 (5) | −0.0071 (5) | 0.2437 (4) | 0.027 (2) | |
H55A | 0.5787 | −0.0112 | 0.2547 | 0.032* | |
H55B | 0.4857 | 0.0539 | 0.2483 | 0.032* | |
C56 | 0.5069 (6) | −0.0327 (5) | 0.1685 (4) | 0.035 (2) | |
H56A | 0.5439 | −0.0898 | 0.1619 | 0.052* | |
H56B | 0.5256 | 0.0102 | 0.1367 | 0.052* | |
H56C | 0.4456 | −0.0348 | 0.1589 | 0.052* | |
C57 | 0.6482 (5) | 0.3915 (4) | 0.5274 (4) | 0.0144 (16) | |
C58 | 0.7278 (5) | 0.3247 (4) | 0.5464 (4) | 0.0212 (18) | |
H58A | 0.7798 | 0.3521 | 0.5459 | 0.025* | |
H58B | 0.7369 | 0.2796 | 0.5113 | 0.025* | |
C59 | 0.7196 (5) | 0.2826 (4) | 0.6181 (4) | 0.0234 (19) | |
H59A | 0.7160 | 0.3270 | 0.6535 | 0.028* | |
H59B | 0.7731 | 0.2380 | 0.6280 | 0.028* | |
C60 | 0.6395 (5) | 0.2407 (5) | 0.6247 (4) | 0.037 (2) | |
H60A | 0.5861 | 0.2848 | 0.6164 | 0.055* | |
H60B | 0.6379 | 0.2143 | 0.6715 | 0.055* | |
H60C | 0.6430 | 0.1960 | 0.5902 | 0.055* | |
C61 | 0.4215 (4) | 0.4070 (4) | 0.5865 (4) | 0.0128 (16) | |
C62 | 0.3811 (5) | 0.3497 (4) | 0.6357 (4) | 0.0176 (17) | |
H62A | 0.4280 | 0.3164 | 0.6664 | 0.021* | |
H62B | 0.3389 | 0.3870 | 0.6656 | 0.021* | |
C63 | 0.3344 (5) | 0.2868 (4) | 0.6026 (4) | 0.0219 (18) | |
H63A | 0.3766 | 0.2472 | 0.5742 | 0.026* | |
H63B | 0.2881 | 0.3192 | 0.5710 | 0.026* | |
C64 | 0.2926 (5) | 0.2329 (5) | 0.6566 (4) | 0.034 (2) | |
H64A | 0.3382 | 0.1999 | 0.6876 | 0.050* | |
H64B | 0.2632 | 0.1929 | 0.6325 | 0.050* | |
H64C | 0.2495 | 0.2716 | 0.6840 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0091 (3) | 0.0128 (3) | 0.0133 (3) | −0.0019 (2) | −0.0012 (2) | 0.0005 (2) |
Rh2 | 0.0089 (3) | 0.0133 (3) | 0.0134 (3) | −0.0018 (2) | −0.0008 (2) | 0.0006 (2) |
Rh3 | 0.0098 (3) | 0.0125 (3) | 0.0110 (3) | −0.0032 (2) | 0.0015 (2) | −0.0010 (2) |
Rh4 | 0.0105 (3) | 0.0129 (3) | 0.0108 (3) | −0.0036 (2) | 0.0017 (2) | −0.0008 (2) |
Rh5 | 0.0114 (3) | 0.0098 (3) | 0.0111 (3) | −0.0024 (2) | 0.0002 (2) | 0.0004 (2) |
Rh6 | 0.0128 (3) | 0.0104 (3) | 0.0115 (3) | −0.0031 (2) | 0.0000 (2) | −0.0034 (2) |
Rh7 | 0.0123 (3) | 0.0088 (3) | 0.0124 (3) | −0.0012 (2) | 0.0002 (2) | 0.0006 (2) |
Rh8 | 0.0120 (3) | 0.0110 (3) | 0.0107 (3) | −0.0031 (2) | 0.0003 (2) | −0.0017 (2) |
Mo1 | 0.0091 (3) | 0.0092 (3) | 0.0094 (3) | −0.0030 (2) | 0.0004 (3) | −0.0012 (3) |
Mo2 | 0.0088 (3) | 0.0095 (3) | 0.0102 (3) | −0.0025 (2) | 0.0001 (3) | −0.0003 (3) |
N1 | 0.009 (3) | 0.008 (3) | 0.019 (3) | −0.003 (2) | −0.007 (3) | −0.002 (3) |
O1 | 0.011 (3) | 0.033 (3) | 0.013 (3) | −0.008 (2) | −0.002 (2) | 0.007 (2) |
N2 | 0.010 (3) | 0.016 (3) | 0.021 (3) | −0.001 (3) | 0.000 (3) | 0.005 (3) |
O2 | 0.014 (3) | 0.012 (2) | 0.014 (3) | −0.004 (2) | −0.001 (2) | −0.002 (2) |
O3 | 0.013 (3) | 0.020 (3) | 0.014 (3) | −0.003 (2) | −0.003 (2) | 0.003 (2) |
N3 | 0.010 (3) | 0.023 (3) | 0.015 (3) | 0.000 (3) | −0.004 (3) | 0.001 (3) |
O4 | 0.011 (3) | 0.011 (2) | 0.017 (3) | −0.001 (2) | −0.002 (2) | −0.002 (2) |
N4 | 0.013 (3) | 0.015 (3) | 0.014 (3) | −0.004 (3) | 0.000 (3) | −0.005 (3) |
N5 | 0.013 (3) | 0.016 (3) | 0.011 (3) | −0.012 (3) | 0.002 (3) | −0.006 (3) |
O5 | 0.016 (3) | 0.021 (3) | 0.010 (3) | −0.005 (2) | −0.003 (2) | −0.003 (2) |
N6 | 0.014 (3) | 0.010 (3) | 0.014 (3) | −0.004 (2) | 0.006 (3) | −0.005 (3) |
O6 | 0.015 (3) | 0.015 (3) | 0.017 (3) | 0.003 (2) | 0.004 (2) | 0.001 (2) |
O7 | 0.010 (3) | 0.016 (3) | 0.016 (3) | −0.007 (2) | 0.003 (2) | 0.000 (2) |
N7 | 0.009 (3) | 0.023 (3) | 0.015 (3) | −0.004 (3) | 0.004 (3) | −0.005 (3) |
O8 | 0.017 (3) | 0.014 (3) | 0.016 (3) | 0.000 (2) | 0.001 (2) | −0.003 (2) |
N8 | 0.010 (3) | 0.016 (3) | 0.016 (3) | 0.003 (2) | 0.007 (2) | −0.004 (2) |
N9 | 0.019 (4) | 0.010 (3) | 0.014 (3) | −0.003 (3) | 0.000 (3) | 0.003 (3) |
O9 | 0.026 (3) | 0.008 (2) | 0.015 (3) | −0.002 (2) | −0.001 (2) | 0.002 (2) |
N10 | 0.012 (3) | 0.009 (3) | 0.014 (3) | −0.001 (2) | 0.001 (3) | 0.005 (3) |
O10 | 0.012 (3) | 0.015 (3) | 0.017 (3) | −0.002 (2) | −0.001 (2) | 0.004 (2) |
N11 | 0.019 (4) | 0.010 (3) | 0.016 (3) | −0.004 (3) | 0.006 (3) | −0.003 (3) |
O11 | 0.023 (3) | 0.014 (3) | 0.016 (3) | −0.005 (2) | 0.000 (2) | 0.000 (2) |
N12 | 0.015 (4) | 0.014 (3) | 0.019 (3) | −0.002 (3) | 0.000 (3) | −0.008 (3) |
O12 | 0.015 (3) | 0.011 (2) | 0.026 (3) | −0.002 (2) | −0.002 (2) | −0.008 (2) |
N13 | 0.012 (3) | 0.012 (3) | 0.025 (4) | −0.002 (3) | 0.003 (3) | 0.001 (3) |
O13 | 0.014 (3) | 0.018 (3) | 0.017 (3) | −0.002 (2) | 0.000 (2) | 0.003 (2) |
N14 | 0.022 (4) | 0.015 (3) | 0.010 (3) | −0.005 (3) | 0.000 (3) | 0.003 (3) |
O14 | 0.019 (3) | 0.012 (2) | 0.012 (3) | 0.002 (2) | −0.004 (2) | 0.003 (2) |
N15 | 0.018 (4) | 0.014 (3) | 0.014 (3) | −0.008 (3) | 0.001 (3) | −0.006 (3) |
O15 | 0.013 (3) | 0.014 (2) | 0.016 (3) | −0.001 (2) | −0.002 (2) | −0.004 (2) |
N16 | 0.021 (4) | 0.015 (3) | 0.013 (3) | −0.007 (3) | −0.001 (3) | 0.001 (3) |
O16 | 0.018 (3) | 0.015 (3) | 0.016 (3) | −0.006 (2) | 0.002 (2) | 0.001 (2) |
O17 | 0.009 (3) | 0.013 (2) | 0.009 (2) | −0.004 (2) | 0.001 (2) | 0.001 (2) |
O18 | 0.009 (3) | 0.020 (3) | 0.017 (3) | −0.004 (2) | 0.000 (2) | −0.001 (2) |
O19 | 0.011 (3) | 0.013 (2) | 0.015 (3) | −0.005 (2) | −0.003 (2) | −0.001 (2) |
O20 | 0.013 (3) | 0.014 (2) | 0.013 (3) | −0.001 (2) | 0.000 (2) | 0.002 (2) |
O21 | 0.007 (3) | 0.012 (2) | 0.018 (3) | −0.001 (2) | 0.001 (2) | −0.001 (2) |
O22 | 0.010 (3) | 0.012 (2) | 0.010 (2) | −0.001 (2) | 0.003 (2) | 0.000 (2) |
O23 | 0.015 (3) | 0.012 (2) | 0.012 (3) | −0.004 (2) | 0.004 (2) | −0.002 (2) |
O24 | 0.014 (3) | 0.007 (2) | 0.015 (3) | −0.001 (2) | 0.000 (2) | −0.001 (2) |
C1 | 0.011 (4) | 0.009 (3) | 0.019 (4) | −0.002 (3) | 0.002 (3) | −0.001 (3) |
C2 | 0.014 (4) | 0.024 (4) | 0.014 (4) | −0.012 (3) | −0.002 (3) | −0.001 (3) |
C5 | 0.019 (4) | 0.015 (4) | 0.010 (4) | −0.002 (3) | −0.001 (3) | −0.004 (3) |
C6 | 0.022 (5) | 0.008 (4) | 0.034 (5) | 0.001 (3) | −0.012 (4) | −0.003 (3) |
C7 | 0.040 (6) | 0.024 (5) | 0.054 (6) | −0.011 (4) | −0.002 (5) | 0.013 (5) |
C8 | 0.061 (8) | 0.062 (7) | 0.073 (8) | −0.020 (6) | 0.026 (6) | 0.029 (6) |
C9 | 0.015 (4) | 0.014 (4) | 0.013 (4) | −0.001 (3) | 0.000 (3) | −0.005 (3) |
C10 | 0.026 (5) | 0.020 (4) | 0.011 (4) | 0.003 (3) | 0.006 (3) | 0.001 (3) |
C11 | 0.020 (5) | 0.033 (5) | 0.019 (4) | 0.003 (4) | 0.002 (4) | −0.002 (4) |
C12 | 0.043 (7) | 0.080 (7) | 0.024 (5) | 0.001 (6) | 0.015 (5) | −0.006 (5) |
C13 | 0.020 (4) | 0.007 (3) | 0.010 (4) | −0.003 (3) | −0.003 (3) | −0.001 (3) |
C14 | 0.023 (5) | 0.013 (4) | 0.018 (4) | −0.003 (3) | −0.005 (3) | 0.002 (3) |
C15 | 0.018 (5) | 0.034 (5) | 0.025 (5) | −0.006 (4) | −0.005 (4) | −0.014 (4) |
C16 | 0.041 (6) | 0.027 (5) | 0.029 (5) | −0.016 (4) | 0.010 (4) | −0.010 (4) |
C17 | 0.012 (4) | 0.006 (3) | 0.020 (4) | −0.003 (3) | 0.008 (3) | −0.005 (3) |
C18 | 0.018 (4) | 0.013 (4) | 0.015 (4) | −0.002 (3) | −0.002 (3) | −0.006 (3) |
C19 | 0.021 (5) | 0.030 (4) | 0.026 (5) | −0.013 (4) | −0.007 (4) | −0.004 (4) |
C20 | 0.052 (6) | 0.016 (4) | 0.032 (5) | 0.003 (4) | −0.004 (5) | −0.002 (4) |
C21 | 0.013 (4) | 0.017 (4) | 0.015 (4) | −0.003 (3) | −0.006 (3) | −0.001 (3) |
C22 | 0.012 (4) | 0.020 (4) | 0.014 (4) | 0.004 (3) | 0.005 (3) | −0.001 (3) |
C23 | 0.022 (5) | 0.024 (4) | 0.027 (5) | −0.011 (4) | 0.009 (4) | −0.001 (4) |
C24 | 0.024 (5) | 0.037 (5) | 0.032 (5) | −0.010 (4) | 0.007 (4) | −0.016 (4) |
C25 | 0.013 (4) | 0.018 (4) | 0.011 (4) | 0.003 (3) | 0.003 (3) | 0.004 (3) |
C26 | 0.012 (4) | 0.031 (4) | 0.019 (4) | −0.011 (3) | −0.001 (3) | −0.009 (4) |
C27 | 0.018 (5) | 0.027 (4) | 0.024 (4) | −0.003 (3) | −0.002 (4) | −0.001 (4) |
C28 | 0.029 (5) | 0.033 (5) | 0.048 (6) | −0.012 (4) | −0.011 (5) | 0.009 (5) |
C29 | 0.009 (4) | 0.012 (4) | 0.016 (4) | −0.001 (3) | −0.004 (3) | 0.001 (3) |
C30 | 0.018 (4) | 0.018 (4) | 0.017 (4) | −0.002 (3) | 0.007 (3) | −0.001 (3) |
C31 | 0.022 (5) | 0.029 (5) | 0.033 (5) | 0.008 (4) | −0.005 (4) | 0.000 (4) |
C32 | 0.043 (6) | 0.021 (5) | 0.071 (7) | 0.013 (4) | −0.012 (6) | −0.013 (5) |
C33 | 0.013 (4) | 0.013 (4) | 0.021 (4) | −0.002 (3) | 0.003 (3) | 0.002 (3) |
C34 | 0.028 (4) | 0.021 (4) | 0.010 (4) | −0.010 (3) | −0.002 (3) | −0.009 (3) |
C35 | 0.050 (7) | 0.040 (6) | 0.040 (6) | −0.014 (5) | 0.010 (5) | 0.005 (5) |
C36 | 0.056 (7) | 0.065 (7) | 0.029 (5) | −0.028 (6) | 0.023 (5) | −0.011 (5) |
C37 | 0.009 (4) | 0.021 (4) | 0.006 (3) | −0.004 (3) | 0.000 (3) | 0.003 (3) |
C38 | 0.007 (4) | 0.016 (4) | 0.026 (4) | −0.002 (3) | 0.000 (3) | 0.007 (3) |
C39 | 0.017 (5) | 0.036 (5) | 0.037 (5) | −0.010 (4) | −0.002 (4) | 0.000 (4) |
C40 | 0.019 (5) | 0.055 (6) | 0.044 (6) | −0.011 (4) | −0.004 (4) | −0.010 (5) |
C41 | 0.015 (4) | 0.014 (4) | 0.025 (4) | −0.003 (3) | 0.007 (3) | −0.005 (3) |
C42 | 0.035 (5) | 0.015 (4) | 0.023 (5) | −0.007 (4) | 0.010 (4) | 0.001 (3) |
C43 | 0.079 (8) | 0.022 (5) | 0.041 (6) | −0.029 (5) | −0.020 (6) | 0.009 (4) |
C44 | 0.036 (7) | 0.042 (6) | 0.099 (9) | 0.005 (5) | 0.004 (6) | 0.011 (6) |
C45 | 0.021 (5) | 0.016 (4) | 0.014 (4) | −0.002 (3) | 0.001 (3) | 0.003 (3) |
C46 | 0.027 (5) | 0.029 (5) | 0.025 (5) | 0.000 (4) | 0.011 (4) | −0.014 (4) |
C47 | 0.028 (5) | 0.026 (4) | 0.031 (5) | 0.001 (4) | −0.007 (4) | −0.009 (4) |
C48 | 0.036 (6) | 0.030 (5) | 0.046 (6) | −0.002 (4) | −0.008 (5) | −0.009 (4) |
C49 | 0.019 (5) | 0.020 (4) | 0.019 (4) | −0.004 (3) | 0.003 (3) | −0.002 (3) |
C50 | 0.017 (5) | 0.008 (4) | 0.053 (6) | 0.000 (3) | 0.012 (4) | 0.006 (4) |
C51 | 0.024 (5) | 0.037 (5) | 0.037 (5) | −0.009 (4) | 0.002 (4) | −0.005 (4) |
C52 | 0.034 (6) | 0.040 (5) | 0.042 (6) | −0.022 (4) | 0.003 (5) | −0.011 (4) |
C53 | 0.015 (4) | 0.022 (4) | 0.020 (4) | −0.007 (3) | 0.000 (3) | −0.002 (4) |
C54 | 0.017 (4) | 0.018 (4) | 0.018 (4) | −0.004 (3) | 0.001 (3) | −0.004 (3) |
C55 | 0.034 (5) | 0.030 (5) | 0.021 (4) | −0.013 (4) | 0.006 (4) | −0.007 (4) |
C56 | 0.041 (6) | 0.039 (5) | 0.024 (5) | −0.008 (4) | 0.011 (4) | −0.007 (4) |
C57 | 0.012 (4) | 0.011 (3) | 0.023 (4) | −0.009 (3) | 0.002 (3) | 0.002 (3) |
C58 | 0.022 (5) | 0.012 (4) | 0.028 (5) | −0.001 (3) | −0.003 (4) | −0.001 (3) |
C59 | 0.023 (5) | 0.014 (4) | 0.030 (5) | 0.005 (3) | −0.001 (4) | 0.001 (3) |
C60 | 0.027 (5) | 0.041 (5) | 0.041 (6) | −0.007 (4) | 0.007 (4) | 0.014 (5) |
C61 | 0.005 (4) | 0.015 (4) | 0.018 (4) | 0.000 (3) | −0.001 (3) | −0.011 (3) |
C62 | 0.019 (4) | 0.018 (4) | 0.016 (4) | −0.004 (3) | 0.007 (3) | 0.001 (3) |
C63 | 0.023 (5) | 0.018 (4) | 0.025 (4) | −0.005 (3) | 0.011 (4) | −0.004 (3) |
C64 | 0.035 (6) | 0.029 (5) | 0.043 (6) | −0.021 (4) | 0.009 (4) | −0.003 (4) |
Geometric parameters (Å, º) top
Rh1—N2 | 1.975 (5) | C9—C10 | 1.503 (9) |
Rh1—N1 | 1.977 (6) | C10—C11 | 1.524 (10) |
Rh1—O4 | 2.024 (4) | C10—H10A | 0.9900 |
Rh1—O3 | 2.041 (4) | C10—H10B | 0.9900 |
Rh1—O17 | 2.254 (4) | C11—C12 | 1.541 (9) |
Rh1—Rh2 | 2.4119 (9) | C11—H11A | 0.9900 |
Rh2—N4 | 1.980 (5) | C11—H11B | 0.9900 |
Rh2—N3 | 1.988 (6) | C12—H12A | 0.9800 |
Rh2—O1 | 2.025 (5) | C12—H12B | 0.9800 |
Rh2—O2 | 2.044 (4) | C12—H12C | 0.9800 |
Rh2—O21 | 2.243 (4) | C13—C14 | 1.510 (9) |
Rh3—N5 | 1.978 (5) | C14—C15 | 1.513 (9) |
Rh3—N6 | 1.986 (5) | C14—H14A | 0.9900 |
Rh3—O8 | 2.036 (4) | C14—H14B | 0.9900 |
Rh3—O7 | 2.036 (5) | C15—C16 | 1.511 (9) |
Rh3—O18 | 2.261 (4) | C15—H15A | 0.9900 |
Rh3—Rh4 | 2.4108 (9) | C15—H15B | 0.9900 |
Rh4—N7 | 1.987 (6) | C16—H16A | 0.9800 |
Rh4—N8 | 1.988 (5) | C16—H16B | 0.9800 |
Rh4—O5 | 2.031 (5) | C16—H16C | 0.9800 |
Rh4—O6 | 2.043 (4) | C17—C18 | 1.473 (9) |
Rh4—O22i | 2.225 (4) | C18—C19 | 1.536 (9) |
Rh5—N10 | 1.968 (5) | C18—H18A | 0.9900 |
Rh5—N9 | 1.981 (6) | C18—H18B | 0.9900 |
Rh5—O10ii | 2.017 (5) | C19—C20 | 1.524 (10) |
Rh5—O9ii | 2.032 (5) | C19—H19A | 0.9900 |
Rh5—O19 | 2.242 (4) | C19—H19B | 0.9900 |
Rh5—Rh5ii | 2.4080 (11) | C20—H20A | 0.9800 |
Rh6—N12 | 1.980 (6) | C20—H20B | 0.9800 |
Rh6—N11 | 1.995 (5) | C20—H20C | 0.9800 |
Rh6—O11iii | 2.027 (4) | C21—C22 | 1.503 (9) |
Rh6—O12iii | 2.032 (5) | C22—C23 | 1.516 (9) |
Rh6—O20 | 2.262 (5) | C22—H22A | 0.9900 |
Rh6—Rh6iii | 2.4179 (12) | C22—H22B | 0.9900 |
Rh7—N13 | 1.969 (6) | C23—C24 | 1.513 (10) |
Rh7—N14 | 1.978 (6) | C23—H23A | 0.9900 |
Rh7—O14iv | 2.028 (5) | C23—H23B | 0.9900 |
Rh7—O13iv | 2.033 (5) | C24—H24A | 0.9800 |
Rh7—O23 | 2.285 (4) | C24—H24B | 0.9800 |
Rh7—Rh7iv | 2.4134 (11) | C24—H24C | 0.9800 |
Rh8—N16 | 1.968 (5) | C25—C26 | 1.501 (9) |
Rh8—N15 | 1.981 (5) | C26—C27 | 1.519 (8) |
Rh8—O15v | 2.028 (4) | C26—H26A | 0.9900 |
Rh8—O16v | 2.044 (4) | C26—H26B | 0.9900 |
Rh8—O24 | 2.269 (5) | C27—C28 | 1.512 (10) |
Rh8—Rh8v | 2.4118 (12) | C27—H27A | 0.9900 |
Mo1—O18 | 1.760 (4) | C27—H27B | 0.9900 |
Mo1—O17 | 1.768 (5) | C28—H28A | 0.9800 |
Mo1—O19 | 1.770 (4) | C28—H28B | 0.9800 |
Mo1—O20 | 1.770 (4) | C28—H28C | 0.9800 |
Mo2—O23 | 1.766 (4) | C29—C30 | 1.507 (8) |
Mo2—O24 | 1.769 (4) | C30—C31 | 1.527 (10) |
Mo2—O21 | 1.772 (5) | C30—H30A | 0.9900 |
Mo2—O22 | 1.772 (4) | C30—H30B | 0.9900 |
N1—C1 | 1.298 (8) | C31—C32 | 1.521 (9) |
N1—H1 | 0.8800 | C31—H31A | 0.9900 |
O1—C1 | 1.291 (8) | C31—H31B | 0.9900 |
N2—C5 | 1.300 (8) | C32—H32A | 0.9800 |
N2—H2 | 0.8800 | C32—H32B | 0.9800 |
O2—C5 | 1.291 (8) | C32—H32C | 0.9800 |
O3—C9 | 1.300 (7) | C33—C34 | 1.492 (9) |
N3—C9 | 1.304 (8) | C34—C35 | 1.495 (10) |
N3—H3 | 0.8800 | C34—H34A | 0.9900 |
O4—C13 | 1.290 (8) | C34—H34B | 0.9900 |
N4—C13 | 1.319 (8) | C35—C36 | 1.457 (11) |
N4—H4 | 0.8800 | C35—H35A | 0.9900 |
N5—C17 | 1.320 (8) | C35—H35B | 0.9900 |
N5—H5 | 0.8800 | C36—H36A | 0.9800 |
O5—C17 | 1.293 (7) | C36—H36B | 0.9800 |
N6—C21 | 1.312 (7) | C36—H36C | 0.9800 |
N6—H6 | 0.8800 | C37—C38 | 1.505 (9) |
O6—C21 | 1.275 (8) | C38—C39 | 1.503 (10) |
O7—C25 | 1.294 (8) | C38—H38A | 0.9900 |
N7—C25 | 1.302 (8) | C38—H38B | 0.9900 |
N7—H7 | 0.8800 | C39—C40 | 1.513 (9) |
O8—C29 | 1.279 (8) | C39—H39A | 0.9900 |
N8—C29 | 1.309 (7) | C39—H39B | 0.9900 |
N8—H8 | 0.8800 | C40—H40A | 0.9800 |
N9—C33 | 1.309 (8) | C40—H40B | 0.9800 |
N9—H9 | 0.8800 | C40—H40C | 0.9800 |
O9—C33 | 1.299 (7) | C41—C42 | 1.523 (8) |
O9—Rh5ii | 2.032 (5) | C42—C43 | 1.542 (11) |
N10—C37 | 1.308 (8) | C42—H42A | 0.9900 |
N10—H10 | 0.8800 | C42—H42B | 0.9900 |
O10—C37 | 1.306 (7) | C43—C44 | 1.546 (12) |
O10—Rh5ii | 2.017 (5) | C43—H43A | 0.9900 |
N11—C41 | 1.291 (9) | C43—H43B | 0.9900 |
N11—H11 | 0.8800 | C44—H44A | 0.9800 |
O11—C41 | 1.292 (8) | C44—H44B | 0.9800 |
O11—Rh6iii | 2.027 (4) | C44—H44C | 0.9800 |
N12—C45 | 1.305 (9) | C45—C46 | 1.504 (10) |
N12—H12 | 0.8800 | C46—C47 | 1.515 (10) |
O12—C45 | 1.294 (8) | C46—H46A | 0.9900 |
O12—Rh6iii | 2.032 (5) | C46—H46B | 0.9900 |
N13—C49 | 1.311 (8) | C47—C48 | 1.535 (9) |
N13—H13 | 0.8800 | C47—H47A | 0.9900 |
O13—C49 | 1.299 (7) | C47—H47B | 0.9900 |
O13—Rh7iv | 2.033 (5) | C48—H48A | 0.9800 |
N14—C53 | 1.325 (9) | C48—H48B | 0.9800 |
N14—H14 | 0.8800 | C48—H48C | 0.9800 |
O14—C53 | 1.271 (7) | C49—C50 | 1.494 (10) |
O14—Rh7iv | 2.028 (5) | C50—C51 | 1.515 (10) |
N15—C57 | 1.300 (8) | C50—H50A | 0.9900 |
N15—H15 | 0.8800 | C50—H50B | 0.9900 |
O15—C57 | 1.286 (8) | C51—C52 | 1.518 (10) |
O15—Rh8v | 2.028 (4) | C51—H51A | 0.9900 |
N16—C61 | 1.302 (8) | C51—H51B | 0.9900 |
N16—H16 | 0.8800 | C52—H52A | 0.9800 |
O16—C61 | 1.273 (8) | C52—H52B | 0.9800 |
O16—Rh8v | 2.044 (4) | C52—H52C | 0.9800 |
O22—Rh4vi | 2.225 (4) | C53—C54 | 1.495 (10) |
C1—C2 | 1.500 (9) | C54—C55 | 1.524 (8) |
C2—C3B | 1.539 (12) | C54—H54A | 0.9900 |
C2—C3A | 1.555 (16) | C54—H54B | 0.9900 |
C2—H2A | 0.9900 | C55—C56 | 1.530 (10) |
C2—H2B | 0.9900 | C55—H55A | 0.9900 |
C2—H2C | 0.9900 | C55—H55B | 0.9900 |
C2—H2D | 0.9900 | C56—H56A | 0.9800 |
C3A—C4A | 1.577 (17) | C56—H56B | 0.9800 |
C3A—H3A | 0.9900 | C56—H56C | 0.9800 |
C3A—H3B | 0.9900 | C57—C58 | 1.493 (9) |
C4A—H4A | 0.9800 | C58—C59 | 1.522 (9) |
C4A—H4B | 0.9800 | C58—H58A | 0.9900 |
C4A—H4C | 0.9800 | C58—H58B | 0.9900 |
C3B—C4B | 1.561 (14) | C59—C60 | 1.528 (10) |
C3B—H3C | 0.9900 | C59—H59A | 0.9900 |
C3B—H3D | 0.9900 | C59—H59B | 0.9900 |
C4B—H4D | 0.9800 | C60—H60A | 0.9800 |
C4B—H4E | 0.9800 | C60—H60B | 0.9800 |
C4B—H4F | 0.9800 | C60—H60C | 0.9800 |
C5—C6 | 1.501 (9) | C61—C62 | 1.505 (8) |
C6—C7 | 1.529 (9) | C62—C63 | 1.502 (9) |
C6—H6A | 0.9900 | C62—H62A | 0.9900 |
C6—H6B | 0.9900 | C62—H62B | 0.9900 |
C7—C8 | 1.518 (11) | C63—C64 | 1.541 (8) |
C7—H7A | 0.9900 | C63—H63A | 0.9900 |
C7—H7B | 0.9900 | C63—H63B | 0.9900 |
C8—H8A | 0.9800 | C64—H64A | 0.9800 |
C8—H8B | 0.9800 | C64—H64B | 0.9800 |
C8—H8C | 0.9800 | C64—H64C | 0.9800 |
| | | |
N2—Rh1—N1 | 89.9 (2) | C12—C11—H11A | 109.5 |
N2—Rh1—O4 | 176.3 (2) | C10—C11—H11B | 109.5 |
N1—Rh1—O4 | 91.24 (19) | C12—C11—H11B | 109.5 |
N2—Rh1—O3 | 89.8 (2) | H11A—C11—H11B | 108.1 |
N1—Rh1—O3 | 175.6 (2) | C11—C12—H12A | 109.5 |
O4—Rh1—O3 | 88.74 (18) | C11—C12—H12B | 109.5 |
N2—Rh1—O17 | 90.5 (2) | H12A—C12—H12B | 109.5 |
N1—Rh1—O17 | 89.55 (19) | C11—C12—H12C | 109.5 |
O4—Rh1—O17 | 92.95 (17) | H12A—C12—H12C | 109.5 |
O3—Rh1—O17 | 94.84 (17) | H12B—C12—H12C | 109.5 |
N2—Rh1—Rh2 | 85.82 (17) | O4—C13—N4 | 121.3 (6) |
N1—Rh1—Rh2 | 85.98 (16) | O4—C13—C14 | 116.9 (6) |
O4—Rh1—Rh2 | 90.78 (13) | N4—C13—C14 | 121.8 (6) |
O3—Rh1—Rh2 | 89.63 (13) | C13—C14—C15 | 111.2 (6) |
O17—Rh1—Rh2 | 174.23 (12) | C13—C14—H14A | 109.4 |
N4—Rh2—N3 | 91.6 (2) | C15—C14—H14A | 109.4 |
N4—Rh2—O1 | 92.9 (2) | C13—C14—H14B | 109.4 |
N3—Rh2—O1 | 173.7 (2) | C15—C14—H14B | 109.4 |
N4—Rh2—O2 | 175.3 (2) | H14A—C14—H14B | 108.0 |
N3—Rh2—O2 | 87.8 (2) | C16—C15—C14 | 113.0 (6) |
O1—Rh2—O2 | 87.36 (19) | C16—C15—H15A | 109.0 |
N4—Rh2—O21 | 94.0 (2) | C14—C15—H15A | 109.0 |
N3—Rh2—O21 | 98.1 (2) | C16—C15—H15B | 109.0 |
O1—Rh2—O21 | 85.88 (17) | C14—C15—H15B | 109.0 |
O2—Rh2—O21 | 90.72 (17) | H15A—C15—H15B | 107.8 |
N4—Rh2—Rh1 | 85.14 (17) | C15—C16—H16A | 109.5 |
N3—Rh2—Rh1 | 86.23 (16) | C15—C16—H16B | 109.5 |
O1—Rh2—Rh1 | 89.82 (13) | H16A—C16—H16B | 109.5 |
O2—Rh2—Rh1 | 90.14 (13) | C15—C16—H16C | 109.5 |
O21—Rh2—Rh1 | 175.57 (11) | H16A—C16—H16C | 109.5 |
N5—Rh3—N6 | 91.0 (2) | H16B—C16—H16C | 109.5 |
N5—Rh3—O8 | 91.2 (2) | O5—C17—N5 | 121.9 (7) |
N6—Rh3—O8 | 175.5 (2) | O5—C17—C18 | 118.2 (6) |
N5—Rh3—O7 | 175.3 (2) | N5—C17—C18 | 120.0 (6) |
N6—Rh3—O7 | 90.2 (2) | C17—C18—C19 | 113.0 (5) |
O8—Rh3—O7 | 87.23 (18) | C17—C18—H18A | 109.0 |
N5—Rh3—O18 | 95.7 (2) | C19—C18—H18A | 109.0 |
N6—Rh3—O18 | 90.46 (19) | C17—C18—H18B | 109.0 |
O8—Rh3—O18 | 93.22 (17) | C19—C18—H18B | 109.0 |
O7—Rh3—O18 | 88.82 (17) | H18A—C18—H18B | 107.8 |
N5—Rh3—Rh4 | 85.23 (16) | C20—C19—C18 | 112.5 (6) |
N6—Rh3—Rh4 | 86.84 (16) | C20—C19—H19A | 109.1 |
O8—Rh3—Rh4 | 89.44 (13) | C18—C19—H19A | 109.1 |
O7—Rh3—Rh4 | 90.35 (13) | C20—C19—H19B | 109.1 |
O18—Rh3—Rh4 | 177.17 (12) | C18—C19—H19B | 109.1 |
N7—Rh4—N8 | 88.9 (2) | H19A—C19—H19B | 107.8 |
N7—Rh4—O5 | 176.4 (2) | C19—C20—H20A | 109.5 |
N8—Rh4—O5 | 90.1 (2) | C19—C20—H20B | 109.5 |
N7—Rh4—O6 | 91.4 (2) | H20A—C20—H20B | 109.5 |
N8—Rh4—O6 | 175.6 (2) | C19—C20—H20C | 109.5 |
O5—Rh4—O6 | 89.36 (18) | H20A—C20—H20C | 109.5 |
N7—Rh4—O22i | 97.7 (2) | H20B—C20—H20C | 109.5 |
N8—Rh4—O22i | 94.35 (19) | O6—C21—N6 | 123.4 (6) |
O5—Rh4—O22i | 85.80 (17) | O6—C21—C22 | 117.0 (6) |
O6—Rh4—O22i | 89.99 (16) | N6—C21—C22 | 119.5 (7) |
N7—Rh4—Rh3 | 85.56 (16) | C21—C22—C23 | 112.1 (6) |
N8—Rh4—Rh3 | 86.33 (16) | C21—C22—H22A | 109.2 |
O5—Rh4—Rh3 | 90.94 (13) | C23—C22—H22A | 109.2 |
O6—Rh4—Rh3 | 89.29 (13) | C21—C22—H22B | 109.2 |
O22i—Rh4—Rh3 | 176.67 (12) | C23—C22—H22B | 109.2 |
N10—Rh5—N9 | 90.2 (2) | H22A—C22—H22B | 107.9 |
N10—Rh5—O10ii | 176.06 (17) | C24—C23—C22 | 112.1 (6) |
N9—Rh5—O10ii | 90.8 (2) | C24—C23—H23A | 109.2 |
N10—Rh5—O9ii | 91.7 (2) | C22—C23—H23A | 109.2 |
N9—Rh5—O9ii | 175.65 (19) | C24—C23—H23B | 109.2 |
O10ii—Rh5—O9ii | 87.09 (19) | C22—C23—H23B | 109.2 |
N10—Rh5—O19 | 91.50 (18) | H23A—C23—H23B | 107.9 |
N9—Rh5—O19 | 94.56 (19) | C23—C24—H24A | 109.5 |
O10ii—Rh5—O19 | 92.23 (16) | C23—C24—H24B | 109.5 |
O9ii—Rh5—O19 | 89.31 (16) | H24A—C24—H24B | 109.5 |
N10—Rh5—Rh5ii | 86.02 (14) | C23—C24—H24C | 109.5 |
N9—Rh5—Rh5ii | 85.53 (15) | H24A—C24—H24C | 109.5 |
O10ii—Rh5—Rh5ii | 90.25 (12) | H24B—C24—H24C | 109.5 |
O9ii—Rh5—Rh5ii | 90.69 (12) | O7—C25—N7 | 122.1 (7) |
O19—Rh5—Rh5ii | 177.52 (12) | O7—C25—C26 | 116.2 (6) |
N12—Rh6—N11 | 90.8 (2) | N7—C25—C26 | 121.7 (6) |
N12—Rh6—O11iii | 91.2 (2) | C25—C26—C27 | 112.3 (6) |
N11—Rh6—O11iii | 175.2 (2) | C25—C26—H26A | 109.1 |
N12—Rh6—O12iii | 176.1 (2) | C27—C26—H26A | 109.1 |
N11—Rh6—O12iii | 89.1 (2) | C25—C26—H26B | 109.1 |
O11iii—Rh6—O12iii | 88.61 (18) | C27—C26—H26B | 109.1 |
N12—Rh6—O20 | 91.3 (2) | H26A—C26—H26B | 107.9 |
N11—Rh6—O20 | 97.7 (2) | C28—C27—C26 | 112.5 (6) |
O11iii—Rh6—O20 | 86.63 (17) | C28—C27—H27A | 109.1 |
O12iii—Rh6—O20 | 92.51 (18) | C26—C27—H27A | 109.1 |
N12—Rh6—Rh6iii | 85.80 (18) | C28—C27—H27B | 109.1 |
N11—Rh6—Rh6iii | 85.57 (18) | C26—C27—H27B | 109.1 |
O11iii—Rh6—Rh6iii | 90.17 (15) | H27A—C27—H27B | 107.8 |
O12iii—Rh6—Rh6iii | 90.34 (14) | C27—C28—H28A | 109.5 |
O20—Rh6—Rh6iii | 175.65 (12) | C27—C28—H28B | 109.5 |
N13—Rh7—N14 | 91.7 (2) | H28A—C28—H28B | 109.5 |
N13—Rh7—O14iv | 89.9 (2) | C27—C28—H28C | 109.5 |
N14—Rh7—O14iv | 175.50 (19) | H28A—C28—H28C | 109.5 |
N13—Rh7—O13iv | 175.40 (18) | H28B—C28—H28C | 109.5 |
N14—Rh7—O13iv | 89.4 (2) | O8—C29—N8 | 122.6 (6) |
O14iv—Rh7—O13iv | 88.61 (19) | O8—C29—C30 | 115.9 (5) |
N13—Rh7—O23 | 94.36 (19) | N8—C29—C30 | 121.5 (6) |
N14—Rh7—O23 | 93.09 (19) | C29—C30—C31 | 116.6 (6) |
O14iv—Rh7—O23 | 90.96 (16) | C29—C30—H30A | 108.2 |
O13iv—Rh7—O23 | 90.03 (17) | C31—C30—H30A | 108.2 |
N13—Rh7—Rh7iv | 84.59 (15) | C29—C30—H30B | 108.2 |
N14—Rh7—Rh7iv | 86.16 (15) | C31—C30—H30B | 108.2 |
O14iv—Rh7—Rh7iv | 89.84 (12) | H30A—C30—H30B | 107.3 |
O13iv—Rh7—Rh7iv | 91.04 (12) | C32—C31—C30 | 110.8 (6) |
O23—Rh7—Rh7iv | 178.68 (12) | C32—C31—H31A | 109.5 |
N16—Rh8—N15 | 90.9 (2) | C30—C31—H31A | 109.5 |
N16—Rh8—O15v | 91.2 (2) | C32—C31—H31B | 109.5 |
N15—Rh8—O15v | 175.1 (2) | C30—C31—H31B | 109.5 |
N16—Rh8—O16v | 175.1 (2) | H31A—C31—H31B | 108.1 |
N15—Rh8—O16v | 89.54 (19) | C31—C32—H32A | 109.5 |
O15v—Rh8—O16v | 88.03 (18) | C31—C32—H32B | 109.5 |
N16—Rh8—O24 | 89.2 (2) | H32A—C32—H32B | 109.5 |
N15—Rh8—O24 | 93.3 (2) | C31—C32—H32C | 109.5 |
O15v—Rh8—O24 | 91.09 (17) | H32A—C32—H32C | 109.5 |
O16v—Rh8—O24 | 95.60 (17) | H32B—C32—H32C | 109.5 |
N16—Rh8—Rh8v | 85.60 (18) | O9—C33—N9 | 121.9 (7) |
N15—Rh8—Rh8v | 85.89 (17) | O9—C33—C34 | 116.8 (6) |
O15v—Rh8—Rh8v | 89.87 (14) | N9—C33—C34 | 121.2 (6) |
O16v—Rh8—Rh8v | 89.59 (14) | C33—C34—C35 | 112.6 (6) |
O24—Rh8—Rh8v | 174.75 (10) | C33—C34—H34A | 109.1 |
O18—Mo1—O17 | 109.4 (2) | C35—C34—H34A | 109.1 |
O18—Mo1—O19 | 109.70 (19) | C33—C34—H34B | 109.1 |
O17—Mo1—O19 | 108.7 (2) | C35—C34—H34B | 109.1 |
O18—Mo1—O20 | 109.4 (2) | H34A—C34—H34B | 107.8 |
O17—Mo1—O20 | 109.97 (19) | C36—C35—C34 | 113.4 (8) |
O19—Mo1—O20 | 109.6 (2) | C36—C35—H35A | 108.9 |
O23—Mo2—O24 | 111.3 (2) | C34—C35—H35A | 108.9 |
O23—Mo2—O21 | 108.8 (2) | C36—C35—H35B | 108.9 |
O24—Mo2—O21 | 110.12 (19) | C34—C35—H35B | 108.9 |
O23—Mo2—O22 | 108.86 (19) | H35A—C35—H35B | 107.7 |
O24—Mo2—O22 | 108.0 (2) | C35—C36—H36A | 109.5 |
O21—Mo2—O22 | 109.7 (2) | C35—C36—H36B | 109.5 |
C1—N1—Rh1 | 123.4 (5) | H36A—C36—H36B | 109.5 |
C1—N1—H1 | 118.3 | C35—C36—H36C | 109.5 |
Rh1—N1—H1 | 118.3 | H36A—C36—H36C | 109.5 |
C1—O1—Rh2 | 117.4 (4) | H36B—C36—H36C | 109.5 |
C5—N2—Rh1 | 124.5 (5) | O10—C37—N10 | 121.5 (6) |
C5—N2—H2 | 117.7 | O10—C37—C38 | 118.7 (6) |
Rh1—N2—H2 | 117.7 | N10—C37—C38 | 119.8 (6) |
C5—O2—Rh2 | 116.7 (4) | C39—C38—C37 | 112.1 (6) |
C9—O3—Rh1 | 118.2 (4) | C39—C38—H38A | 109.2 |
C9—N3—Rh2 | 124.4 (5) | C37—C38—H38A | 109.2 |
C9—N3—H3 | 117.8 | C39—C38—H38B | 109.2 |
Rh2—N3—H3 | 117.8 | C37—C38—H38B | 109.2 |
C13—O4—Rh1 | 117.6 (4) | H38A—C38—H38B | 107.9 |
C13—N4—Rh2 | 125.0 (5) | C38—C39—C40 | 113.9 (6) |
C13—N4—H4 | 117.5 | C38—C39—H39A | 108.8 |
Rh2—N4—H4 | 117.5 | C40—C39—H39A | 108.8 |
C17—N5—Rh3 | 124.9 (5) | C38—C39—H39B | 108.8 |
C17—N5—H5 | 117.6 | C40—C39—H39B | 108.8 |
Rh3—N5—H5 | 117.6 | H39A—C39—H39B | 107.7 |
C17—O5—Rh4 | 116.9 (4) | C39—C40—H40A | 109.5 |
C21—N6—Rh3 | 122.5 (5) | C39—C40—H40B | 109.5 |
C21—N6—H6 | 118.7 | H40A—C40—H40B | 109.5 |
Rh3—N6—H6 | 118.7 | C39—C40—H40C | 109.5 |
C21—O6—Rh4 | 117.9 (4) | H40A—C40—H40C | 109.5 |
C25—O7—Rh3 | 117.0 (4) | H40B—C40—H40C | 109.5 |
C25—N7—Rh4 | 124.5 (5) | N11—C41—O11 | 123.1 (6) |
C25—N7—H7 | 117.7 | N11—C41—C42 | 121.0 (7) |
Rh4—N7—H7 | 117.7 | O11—C41—C42 | 115.9 (7) |
C29—O8—Rh3 | 118.2 (4) | C41—C42—C43 | 110.5 (6) |
C29—N8—Rh4 | 123.0 (5) | C41—C42—H42A | 109.5 |
C29—N8—H8 | 118.5 | C43—C42—H42A | 109.5 |
Rh4—N8—H8 | 118.5 | C41—C42—H42B | 109.5 |
C33—N9—Rh5 | 124.6 (5) | C43—C42—H42B | 109.5 |
C33—N9—H9 | 117.7 | H42A—C42—H42B | 108.1 |
Rh5—N9—H9 | 117.7 | C42—C43—C44 | 111.7 (8) |
C33—O9—Rh5ii | 117.0 (4) | C42—C43—H43A | 109.3 |
C37—N10—Rh5 | 124.5 (5) | C44—C43—H43A | 109.3 |
C37—N10—H10 | 117.8 | C42—C43—H43B | 109.3 |
Rh5—N10—H10 | 117.8 | C44—C43—H43B | 109.3 |
C37—O10—Rh5ii | 117.6 (4) | H43A—C43—H43B | 107.9 |
C41—N11—Rh6 | 123.8 (5) | C43—C44—H44A | 109.5 |
C41—N11—H11 | 118.1 | C43—C44—H44B | 109.5 |
Rh6—N11—H11 | 118.1 | H44A—C44—H44B | 109.5 |
C41—O11—Rh6iii | 117.3 (4) | C43—C44—H44C | 109.5 |
C45—N12—Rh6 | 123.9 (5) | H44A—C44—H44C | 109.5 |
C45—N12—H12 | 118.0 | H44B—C44—H44C | 109.5 |
Rh6—N12—H12 | 118.0 | O12—C45—N12 | 123.1 (7) |
C45—O12—Rh6iii | 116.8 (5) | O12—C45—C46 | 117.5 (7) |
C49—N13—Rh7 | 126.8 (5) | N12—C45—C46 | 119.3 (7) |
C49—N13—H13 | 116.6 | C45—C46—C47 | 116.6 (6) |
Rh7—N13—H13 | 116.6 | C45—C46—H46A | 108.1 |
C49—O13—Rh7iv | 117.0 (4) | C47—C46—H46A | 108.1 |
C53—N14—Rh7 | 123.2 (5) | C45—C46—H46B | 108.1 |
C53—N14—H14 | 118.4 | C47—C46—H46B | 108.1 |
Rh7—N14—H14 | 118.4 | H46A—C46—H46B | 107.3 |
C53—O14—Rh7iv | 118.1 (5) | C46—C47—C48 | 110.6 (7) |
C57—N15—Rh8 | 123.9 (5) | C46—C47—H47A | 109.5 |
C57—N15—H15 | 118.0 | C48—C47—H47A | 109.5 |
Rh8—N15—H15 | 118.0 | C46—C47—H47B | 109.5 |
C57—O15—Rh8v | 117.7 (4) | C48—C47—H47B | 109.5 |
C61—N16—Rh8 | 125.3 (5) | H47A—C47—H47B | 108.1 |
C61—N16—H16 | 117.4 | C47—C48—H48A | 109.5 |
Rh8—N16—H16 | 117.4 | C47—C48—H48B | 109.5 |
C61—O16—Rh8v | 117.9 (4) | H48A—C48—H48B | 109.5 |
Mo1—O17—Rh1 | 122.7 (2) | C47—C48—H48C | 109.5 |
Mo1—O18—Rh3 | 119.2 (2) | H48A—C48—H48C | 109.5 |
Mo1—O19—Rh5 | 119.4 (2) | H48B—C48—H48C | 109.5 |
Mo1—O20—Rh6 | 120.5 (2) | O13—C49—N13 | 120.5 (7) |
Mo2—O21—Rh2 | 118.9 (2) | O13—C49—C50 | 116.5 (6) |
Mo2—O22—Rh4vi | 120.3 (2) | N13—C49—C50 | 123.0 (6) |
Mo2—O23—Rh7 | 118.2 (2) | C49—C50—C51 | 115.7 (6) |
Mo2—O24—Rh8 | 121.6 (2) | C49—C50—H50A | 108.3 |
O1—C1—N1 | 122.6 (6) | C51—C50—H50A | 108.3 |
O1—C1—C2 | 116.8 (6) | C49—C50—H50B | 108.3 |
N1—C1—C2 | 120.4 (6) | C51—C50—H50B | 108.3 |
C1—C2—C3B | 108.7 (7) | H50A—C50—H50B | 107.4 |
C1—C2—C3A | 112.8 (13) | C50—C51—C52 | 112.7 (7) |
C3B—C2—C3A | 10 (2) | C50—C51—H51A | 109.0 |
C1—C2—H2A | 109.9 | C52—C51—H51A | 109.0 |
C3B—C2—H2A | 109.9 | C50—C51—H51B | 109.0 |
C3A—C2—H2A | 99.5 | C52—C51—H51B | 109.0 |
C1—C2—H2B | 109.9 | H51A—C51—H51B | 107.8 |
C3B—C2—H2B | 109.9 | C51—C52—H52A | 109.5 |
C3A—C2—H2B | 115.7 | C51—C52—H52B | 109.5 |
H2A—C2—H2B | 108.3 | H52A—C52—H52B | 109.5 |
C1—C2—H2C | 109.0 | C51—C52—H52C | 109.5 |
C3B—C2—H2C | 119.3 | H52A—C52—H52C | 109.5 |
C3A—C2—H2C | 109.0 | H52B—C52—H52C | 109.5 |
H2A—C2—H2C | 10.6 | O14—C53—N14 | 122.6 (7) |
H2B—C2—H2C | 99.4 | O14—C53—C54 | 118.2 (6) |
C1—C2—H2D | 109.0 | N14—C53—C54 | 119.3 (6) |
C3B—C2—H2D | 102.4 | C53—C54—C55 | 114.8 (6) |
C3A—C2—H2D | 109.0 | C53—C54—H54A | 108.6 |
H2A—C2—H2D | 116.3 | C55—C54—H54A | 108.6 |
H2B—C2—H2D | 9.0 | C53—C54—H54B | 108.6 |
H2C—C2—H2D | 107.8 | C55—C54—H54B | 108.6 |
C2—C3A—C4A | 89 (3) | H54A—C54—H54B | 107.6 |
C2—C3A—H3A | 113.8 | C54—C55—C56 | 112.7 (6) |
C4A—C3A—H3A | 113.8 | C54—C55—H55A | 109.1 |
C2—C3A—H3B | 113.8 | C56—C55—H55A | 109.1 |
C4A—C3A—H3B | 113.8 | C54—C55—H55B | 109.1 |
H3A—C3A—H3B | 111.1 | C56—C55—H55B | 109.1 |
C3A—C4A—H4A | 109.5 | H55A—C55—H55B | 107.8 |
C3A—C4A—H4B | 109.5 | C55—C56—H56A | 109.5 |
H4A—C4A—H4B | 109.5 | C55—C56—H56B | 109.5 |
C3A—C4A—H4C | 109.5 | H56A—C56—H56B | 109.5 |
H4A—C4A—H4C | 109.5 | C55—C56—H56C | 109.5 |
H4B—C4A—H4C | 109.5 | H56A—C56—H56C | 109.5 |
C2—C3B—C4B | 110.6 (11) | H56B—C56—H56C | 109.5 |
C2—C3B—H3C | 109.5 | O15—C57—N15 | 122.5 (6) |
C4B—C3B—H3C | 109.5 | O15—C57—C58 | 116.7 (7) |
C2—C3B—H3D | 109.5 | N15—C57—C58 | 120.6 (7) |
C4B—C3B—H3D | 109.5 | C57—C58—C59 | 111.8 (6) |
H3C—C3B—H3D | 108.1 | C57—C58—H58A | 109.3 |
C3B—C4B—H4D | 109.5 | C59—C58—H58A | 109.3 |
C3B—C4B—H4E | 109.5 | C57—C58—H58B | 109.3 |
H4D—C4B—H4E | 109.5 | C59—C58—H58B | 109.3 |
C3B—C4B—H4F | 109.5 | H58A—C58—H58B | 107.9 |
H4D—C4B—H4F | 109.5 | C58—C59—C60 | 113.1 (6) |
H4E—C4B—H4F | 109.5 | C58—C59—H59A | 109.0 |
O2—C5—N2 | 122.8 (6) | C60—C59—H59A | 109.0 |
O2—C5—C6 | 118.2 (6) | C58—C59—H59B | 109.0 |
N2—C5—C6 | 118.9 (7) | C60—C59—H59B | 109.0 |
C5—C6—C7 | 111.9 (6) | H59A—C59—H59B | 107.8 |
C5—C6—H6A | 109.2 | C59—C60—H60A | 109.5 |
C7—C6—H6A | 109.2 | C59—C60—H60B | 109.5 |
C5—C6—H6B | 109.2 | H60A—C60—H60B | 109.5 |
C7—C6—H6B | 109.2 | C59—C60—H60C | 109.5 |
H6A—C6—H6B | 107.9 | H60A—C60—H60C | 109.5 |
C8—C7—C6 | 112.6 (6) | H60B—C60—H60C | 109.5 |
C8—C7—H7A | 109.1 | O16—C61—N16 | 121.6 (6) |
C6—C7—H7A | 109.1 | O16—C61—C62 | 117.0 (6) |
C8—C7—H7B | 109.1 | N16—C61—C62 | 121.4 (6) |
C6—C7—H7B | 109.1 | C63—C62—C61 | 116.1 (6) |
H7A—C7—H7B | 107.8 | C63—C62—H62A | 108.3 |
C7—C8—H8A | 109.5 | C61—C62—H62A | 108.3 |
C7—C8—H8B | 109.5 | C63—C62—H62B | 108.3 |
H8A—C8—H8B | 109.5 | C61—C62—H62B | 108.3 |
C7—C8—H8C | 109.5 | H62A—C62—H62B | 107.4 |
H8A—C8—H8C | 109.5 | C62—C63—C64 | 112.6 (6) |
H8B—C8—H8C | 109.5 | C62—C63—H63A | 109.1 |
O3—C9—N3 | 121.3 (6) | C64—C63—H63A | 109.1 |
O3—C9—C10 | 116.8 (6) | C62—C63—H63B | 109.1 |
N3—C9—C10 | 121.9 (6) | C64—C63—H63B | 109.1 |
C9—C10—C11 | 114.7 (5) | H63A—C63—H63B | 107.8 |
C9—C10—H10A | 108.6 | C63—C64—H64A | 109.5 |
C11—C10—H10A | 108.6 | C63—C64—H64B | 109.5 |
C9—C10—H10B | 108.6 | H64A—C64—H64B | 109.5 |
C11—C10—H10B | 108.6 | C63—C64—H64C | 109.5 |
H10A—C10—H10B | 107.6 | H64A—C64—H64C | 109.5 |
C10—C11—C12 | 110.8 (6) | H64B—C64—H64C | 109.5 |
C10—C11—H11A | 109.5 | | |
| | | |
N2—Rh1—Rh2—N4 | 179.7 (2) | N2—Rh1—O17—Mo1 | −44.2 (3) |
N1—Rh1—Rh2—N4 | 89.5 (2) | N1—Rh1—O17—Mo1 | 45.7 (3) |
O4—Rh1—Rh2—N4 | −1.7 (2) | O4—Rh1—O17—Mo1 | 137.0 (2) |
O3—Rh1—Rh2—N4 | −90.4 (2) | O3—Rh1—O17—Mo1 | −134.1 (2) |
O17—Rh1—Rh2—N4 | 128.7 (10) | Rh2—Rh1—O17—Mo1 | 6.7 (12) |
N2—Rh1—Rh2—N3 | −88.3 (2) | O17—Mo1—O18—Rh3 | −50.3 (3) |
N1—Rh1—Rh2—N3 | −178.5 (2) | O19—Mo1—O18—Rh3 | −169.6 (2) |
O4—Rh1—Rh2—N3 | 90.3 (2) | O20—Mo1—O18—Rh3 | 70.2 (3) |
O3—Rh1—Rh2—N3 | 1.5 (2) | N5—Rh3—O18—Mo1 | 38.8 (3) |
O17—Rh1—Rh2—N3 | −139.4 (10) | N6—Rh3—O18—Mo1 | −52.2 (3) |
N2—Rh1—Rh2—O1 | 86.8 (2) | O8—Rh3—O18—Mo1 | 130.4 (3) |
N1—Rh1—Rh2—O1 | −3.4 (2) | O7—Rh3—O18—Mo1 | −142.5 (3) |
O4—Rh1—Rh2—O1 | −94.58 (19) | Rh4—Rh3—O18—Mo1 | −70 (3) |
O3—Rh1—Rh2—O1 | 176.69 (19) | O18—Mo1—O19—Rh5 | 58.3 (3) |
O17—Rh1—Rh2—O1 | 35.8 (10) | O17—Mo1—O19—Rh5 | −61.4 (3) |
N2—Rh1—Rh2—O2 | −0.5 (2) | O20—Mo1—O19—Rh5 | 178.4 (2) |
N1—Rh1—Rh2—O2 | −90.75 (19) | N10—Rh5—O19—Mo1 | −49.2 (3) |
O4—Rh1—Rh2—O2 | 178.07 (17) | N9—Rh5—O19—Mo1 | 41.1 (3) |
O3—Rh1—Rh2—O2 | 89.33 (18) | O10ii—Rh5—O19—Mo1 | 132.0 (3) |
O17—Rh1—Rh2—O2 | −51.6 (10) | O9ii—Rh5—O19—Mo1 | −140.9 (3) |
N2—Rh1—Rh2—O21 | 100.8 (16) | Rh5ii—Rh5—O19—Mo1 | −51 (3) |
N1—Rh1—Rh2—O21 | 10.5 (16) | O18—Mo1—O20—Rh6 | 69.3 (3) |
O4—Rh1—Rh2—O21 | −80.7 (16) | O17—Mo1—O20—Rh6 | −170.5 (2) |
O3—Rh1—Rh2—O21 | −169.4 (16) | O19—Mo1—O20—Rh6 | −51.0 (3) |
O17—Rh1—Rh2—O21 | 49.7 (18) | N12—Rh6—O20—Mo1 | −65.9 (3) |
N5—Rh3—Rh4—N7 | 175.9 (2) | N11—Rh6—O20—Mo1 | 25.1 (3) |
N6—Rh3—Rh4—N7 | −92.8 (2) | O11iii—Rh6—O20—Mo1 | −157.0 (3) |
O8—Rh3—Rh4—N7 | 84.7 (2) | O12iii—Rh6—O20—Mo1 | 114.6 (3) |
O7—Rh3—Rh4—N7 | −2.56 (19) | Rh6iii—Rh6—O20—Mo1 | −114.4 (13) |
O18—Rh3—Rh4—N7 | −75 (2) | O23—Mo2—O21—Rh2 | 63.5 (3) |
N5—Rh3—Rh4—N8 | 86.8 (2) | O24—Mo2—O21—Rh2 | −58.7 (3) |
N6—Rh3—Rh4—N8 | 178.1 (2) | O22—Mo2—O21—Rh2 | −177.47 (19) |
O8—Rh3—Rh4—N8 | −4.5 (2) | N4—Rh2—O21—Mo2 | 46.6 (3) |
O7—Rh3—Rh4—N8 | −91.7 (2) | N3—Rh2—O21—Mo2 | −45.6 (3) |
O18—Rh3—Rh4—N8 | −165 (2) | O1—Rh2—O21—Mo2 | 139.2 (2) |
N5—Rh3—Rh4—O5 | −3.25 (19) | O2—Rh2—O21—Mo2 | −133.5 (2) |
N6—Rh3—Rh4—O5 | 88.0 (2) | Rh1—Rh2—O21—Mo2 | 125.2 (15) |
O8—Rh3—Rh4—O5 | −94.52 (19) | O23—Mo2—O22—Rh4vi | 170.7 (2) |
O7—Rh3—Rh4—O5 | 178.25 (17) | O24—Mo2—O22—Rh4vi | −68.3 (3) |
O18—Rh3—Rh4—O5 | 105 (2) | O21—Mo2—O22—Rh4vi | 51.7 (3) |
N5—Rh3—Rh4—O6 | −92.6 (2) | O24—Mo2—O23—Rh7 | −172.4 (2) |
N6—Rh3—Rh4—O6 | −1.3 (2) | O21—Mo2—O23—Rh7 | 66.1 (3) |
O8—Rh3—Rh4—O6 | 176.13 (19) | O22—Mo2—O23—Rh7 | −53.4 (3) |
O7—Rh3—Rh4—O6 | 88.90 (18) | N13—Rh7—O23—Mo2 | 47.0 (3) |
O18—Rh3—Rh4—O6 | 16 (2) | N14—Rh7—O23—Mo2 | −45.0 (3) |
N5—Rh3—Rh4—O22i | −15.1 (19) | O14iv—Rh7—O23—Mo2 | 137.0 (3) |
N6—Rh3—Rh4—O22i | 76.2 (19) | O13iv—Rh7—O23—Mo2 | −134.4 (3) |
O8—Rh3—Rh4—O22i | −106.4 (19) | Rh7iv—Rh7—O23—Mo2 | 10 (6) |
O7—Rh3—Rh4—O22i | 166.4 (19) | O23—Mo2—O24—Rh8 | 57.4 (3) |
O18—Rh3—Rh4—O22i | 94 (3) | O21—Mo2—O24—Rh8 | 178.2 (2) |
N2—Rh1—N1—C1 | −77.4 (5) | O22—Mo2—O24—Rh8 | −62.1 (3) |
O4—Rh1—N1—C1 | 99.1 (5) | N16—Rh8—O24—Mo2 | −53.4 (3) |
O3—Rh1—N1—C1 | 9 (3) | N15—Rh8—O24—Mo2 | 37.4 (3) |
O17—Rh1—N1—C1 | −167.9 (5) | O15v—Rh8—O24—Mo2 | −144.6 (3) |
Rh2—Rh1—N1—C1 | 8.4 (5) | O16v—Rh8—O24—Mo2 | 127.3 (3) |
N4—Rh2—O1—C1 | −85.3 (5) | Rh8v—Rh8—O24—Mo2 | −44.0 (14) |
N3—Rh2—O1—C1 | 51 (2) | Rh2—O1—C1—N1 | 6.5 (8) |
O2—Rh2—O1—C1 | 90.0 (5) | Rh2—O1—C1—C2 | −168.9 (4) |
O21—Rh2—O1—C1 | −179.1 (5) | Rh1—N1—C1—O1 | −11.3 (9) |
Rh1—Rh2—O1—C1 | −0.2 (5) | Rh1—N1—C1—C2 | 164.0 (4) |
N1—Rh1—N2—C5 | 86.3 (6) | O1—C1—C2—C3B | 80.6 (13) |
O4—Rh1—N2—C5 | −22 (4) | N1—C1—C2—C3B | −94.9 (13) |
O3—Rh1—N2—C5 | −89.3 (6) | O1—C1—C2—C3A | 70 (2) |
O17—Rh1—N2—C5 | 175.9 (6) | N1—C1—C2—C3A | −105 (2) |
Rh2—Rh1—N2—C5 | 0.4 (5) | C1—C2—C3A—C4A | 154 (3) |
N4—Rh2—O2—C5 | 4 (3) | C3B—C2—C3A—C4A | 85 (9) |
N3—Rh2—O2—C5 | 87.1 (5) | C1—C2—C3B—C4B | −173.2 (14) |
O1—Rh2—O2—C5 | −89.0 (5) | C3A—C2—C3B—C4B | −59 (8) |
O21—Rh2—O2—C5 | −174.8 (5) | Rh2—O2—C5—N2 | −0.8 (9) |
Rh1—Rh2—O2—C5 | 0.8 (5) | Rh2—O2—C5—C6 | −178.2 (5) |
N2—Rh1—O3—C9 | 81.6 (5) | Rh1—N2—C5—O2 | 0.2 (10) |
N1—Rh1—O3—C9 | −5 (3) | Rh1—N2—C5—C6 | 177.5 (5) |
O4—Rh1—O3—C9 | −95.0 (5) | O2—C5—C6—C7 | 85.5 (8) |
O17—Rh1—O3—C9 | 172.1 (5) | N2—C5—C6—C7 | −92.0 (8) |
Rh2—Rh1—O3—C9 | −4.3 (5) | C5—C6—C7—C8 | 67.3 (9) |
N4—Rh2—N3—C9 | 85.8 (6) | Rh1—O3—C9—N3 | 5.9 (9) |
O1—Rh2—N3—C9 | −50 (2) | Rh1—O3—C9—C10 | −174.0 (4) |
O2—Rh2—N3—C9 | −89.5 (6) | Rh2—N3—C9—O3 | −4.3 (10) |
O21—Rh2—N3—C9 | −180.0 (6) | Rh2—N3—C9—C10 | 175.6 (5) |
Rh1—Rh2—N3—C9 | 0.7 (5) | O3—C9—C10—C11 | −69.5 (9) |
N2—Rh1—O4—C13 | 22 (3) | N3—C9—C10—C11 | 110.6 (8) |
N1—Rh1—O4—C13 | −86.1 (5) | C9—C10—C11—C12 | 169.3 (7) |
O3—Rh1—O4—C13 | 89.5 (5) | Rh1—O4—C13—N4 | 3.1 (8) |
O17—Rh1—O4—C13 | −175.7 (5) | Rh1—O4—C13—C14 | −174.9 (4) |
Rh2—Rh1—O4—C13 | −0.1 (5) | Rh2—N4—C13—O4 | −5.5 (9) |
N3—Rh2—N4—C13 | −81.9 (6) | Rh2—N4—C13—C14 | 172.3 (4) |
O1—Rh2—N4—C13 | 93.8 (5) | O4—C13—C14—C15 | 57.9 (8) |
O2—Rh2—N4—C13 | 1 (3) | N4—C13—C14—C15 | −120.1 (7) |
O21—Rh2—N4—C13 | 179.9 (5) | C13—C14—C15—C16 | 58.8 (8) |
Rh1—Rh2—N4—C13 | 4.2 (5) | Rh4—O5—C17—N5 | 0.2 (8) |
N6—Rh3—N5—C17 | −81.7 (5) | Rh4—O5—C17—C18 | 179.7 (4) |
O8—Rh3—N5—C17 | 94.4 (5) | Rh3—N5—C17—O5 | −4.4 (9) |
O7—Rh3—N5—C17 | 24 (3) | Rh3—N5—C17—C18 | 176.1 (4) |
O18—Rh3—N5—C17 | −172.3 (5) | O5—C17—C18—C19 | −114.1 (7) |
Rh4—Rh3—N5—C17 | 5.0 (5) | N5—C17—C18—C19 | 65.4 (8) |
N7—Rh4—O5—C17 | −10 (4) | C17—C18—C19—C20 | 56.7 (8) |
N8—Rh4—O5—C17 | −83.6 (5) | Rh4—O6—C21—N6 | −1.5 (9) |
O6—Rh4—O5—C17 | 92.0 (5) | Rh4—O6—C21—C22 | −177.4 (5) |
O22i—Rh4—O5—C17 | −178.0 (5) | Rh3—N6—C21—O6 | −0.1 (10) |
Rh3—Rh4—O5—C17 | 2.7 (4) | Rh3—N6—C21—C22 | 175.7 (5) |
N5—Rh3—N6—C21 | 86.4 (6) | O6—C21—C22—C23 | 57.2 (8) |
O8—Rh3—N6—C21 | −33 (3) | N6—C21—C22—C23 | −118.8 (7) |
O7—Rh3—N6—C21 | −89.1 (6) | C21—C22—C23—C24 | 61.9 (8) |
O18—Rh3—N6—C21 | −177.9 (6) | Rh3—O7—C25—N7 | −8.1 (8) |
Rh4—Rh3—N6—C21 | 1.3 (5) | Rh3—O7—C25—C26 | 169.5 (4) |
N7—Rh4—O6—C21 | 87.4 (5) | Rh4—N7—C25—O7 | 5.4 (9) |
N8—Rh4—O6—C21 | −6 (3) | Rh4—N7—C25—C26 | −172.0 (5) |
O5—Rh4—O6—C21 | −89.1 (5) | O7—C25—C26—C27 | −45.7 (9) |
O22i—Rh4—O6—C21 | −174.9 (5) | N7—C25—C26—C27 | 131.8 (7) |
Rh3—Rh4—O6—C21 | 1.9 (5) | C25—C26—C27—C28 | −61.2 (9) |
N5—Rh3—O7—C25 | −12 (2) | Rh3—O8—C29—N8 | 1.5 (9) |
N6—Rh3—O7—C25 | 93.0 (5) | Rh3—O8—C29—C30 | −179.2 (5) |
O8—Rh3—O7—C25 | −83.3 (5) | Rh4—N8—C29—O8 | −7.3 (10) |
O18—Rh3—O7—C25 | −176.6 (5) | Rh4—N8—C29—C30 | 173.5 (5) |
Rh4—Rh3—O7—C25 | 6.1 (4) | O8—C29—C30—C31 | 141.9 (7) |
N8—Rh4—N7—C25 | 86.1 (6) | N8—C29—C30—C31 | −38.8 (10) |
O5—Rh4—N7—C25 | 13 (4) | C29—C30—C31—C32 | −177.9 (7) |
O6—Rh4—N7—C25 | −89.5 (5) | Rh5ii—O9—C33—N9 | 3.3 (9) |
O22i—Rh4—N7—C25 | −179.7 (5) | Rh5ii—O9—C33—C34 | −174.3 (5) |
Rh3—Rh4—N7—C25 | −0.3 (5) | Rh5—N9—C33—O9 | −6.3 (10) |
N5—Rh3—O8—C29 | −82.1 (5) | Rh5—N9—C33—C34 | 171.1 (5) |
N6—Rh3—O8—C29 | 38 (3) | O9—C33—C34—C35 | 59.1 (9) |
O7—Rh3—O8—C29 | 93.5 (5) | N9—C33—C34—C35 | −118.4 (8) |
O18—Rh3—O8—C29 | −177.8 (5) | C33—C34—C35—C36 | 55.9 (9) |
Rh4—Rh3—O8—C29 | 3.2 (5) | Rh5ii—O10—C37—N10 | −1.8 (9) |
N7—Rh4—N8—C29 | −78.1 (6) | Rh5ii—O10—C37—C38 | 179.3 (5) |
O5—Rh4—N8—C29 | 98.4 (6) | Rh5—N10—C37—O10 | 3.5 (9) |
O6—Rh4—N8—C29 | 15 (3) | Rh5—N10—C37—C38 | −177.6 (5) |
O22i—Rh4—N8—C29 | −175.8 (6) | O10—C37—C38—C39 | 104.9 (8) |
Rh3—Rh4—N8—C29 | 7.5 (5) | N10—C37—C38—C39 | −74.0 (8) |
N10—Rh5—N9—C33 | −81.0 (6) | C37—C38—C39—C40 | −56.1 (8) |
O10ii—Rh5—N9—C33 | 95.2 (6) | Rh6—N11—C41—O11 | −3.6 (10) |
O9ii—Rh5—N9—C33 | 35 (3) | Rh6—N11—C41—C42 | 174.6 (5) |
O19—Rh5—N9—C33 | −172.5 (6) | Rh6iii—O11—C41—N11 | 0.6 (9) |
Rh5ii—Rh5—N9—C33 | 5.0 (6) | Rh6iii—O11—C41—C42 | −177.7 (5) |
N9—Rh5—N10—C37 | 82.6 (6) | N11—C41—C42—C43 | −109.2 (8) |
O10ii—Rh5—N10—C37 | −22 (4) | O11—C41—C42—C43 | 69.2 (9) |
O9ii—Rh5—N10—C37 | −93.4 (6) | C41—C42—C43—C44 | 72.2 (8) |
O19—Rh5—N10—C37 | 177.2 (6) | Rh6iii—O12—C45—N12 | 3.6 (8) |
Rh5ii—Rh5—N10—C37 | −2.9 (5) | Rh6iii—O12—C45—C46 | −172.9 (4) |
N12—Rh6—N11—C41 | −82.0 (6) | Rh6—N12—C45—O12 | −3.7 (9) |
O11iii—Rh6—N11—C41 | 32 (3) | Rh6—N12—C45—C46 | 172.8 (4) |
O12iii—Rh6—N11—C41 | 94.2 (6) | O12—C45—C46—C47 | −36.8 (9) |
O20—Rh6—N11—C41 | −173.4 (6) | N12—C45—C46—C47 | 146.5 (7) |
Rh6iii—Rh6—N11—C41 | 3.8 (6) | C45—C46—C47—C48 | −68.0 (9) |
N11—Rh6—N12—C45 | 87.1 (5) | Rh7iv—O13—C49—N13 | −0.7 (9) |
O11iii—Rh6—N12—C45 | −88.5 (5) | Rh7iv—O13—C49—C50 | 179.8 (5) |
O12iii—Rh6—N12—C45 | −1 (3) | Rh7—N13—C49—O13 | −1.2 (10) |
O20—Rh6—N12—C45 | −175.2 (5) | Rh7—N13—C49—C50 | 178.3 (6) |
Rh6iii—Rh6—N12—C45 | 1.6 (5) | O13—C49—C50—C51 | −152.7 (7) |
N14—Rh7—N13—C49 | −84.1 (6) | N13—C49—C50—C51 | 27.7 (11) |
O14iv—Rh7—N13—C49 | 91.7 (6) | C49—C50—C51—C52 | 178.3 (7) |
O13iv—Rh7—N13—C49 | 20 (3) | Rh7iv—O14—C53—N14 | 0.3 (9) |
O23—Rh7—N13—C49 | −177.3 (6) | Rh7iv—O14—C53—C54 | −179.2 (5) |
Rh7iv—Rh7—N13—C49 | 1.9 (6) | Rh7—N14—C53—O14 | 2.3 (10) |
N13—Rh7—N14—C53 | 81.5 (6) | Rh7—N14—C53—C54 | −178.2 (5) |
O14iv—Rh7—N14—C53 | −30 (3) | O14—C53—C54—C55 | −133.7 (7) |
O13iv—Rh7—N14—C53 | −94.0 (6) | N14—C53—C54—C55 | 46.8 (9) |
O23—Rh7—N14—C53 | 176.0 (6) | C53—C54—C55—C56 | 178.8 (6) |
Rh7iv—Rh7—N14—C53 | −2.9 (6) | Rh8v—O15—C57—N15 | 0.4 (8) |
N16—Rh8—N15—C57 | −81.7 (5) | Rh8v—O15—C57—C58 | −175.3 (4) |
O15v—Rh8—N15—C57 | 33 (3) | Rh8—N15—C57—O15 | −3.4 (9) |
O16v—Rh8—N15—C57 | 93.4 (5) | Rh8—N15—C57—C58 | 172.0 (5) |
O24—Rh8—N15—C57 | −171.0 (5) | O15—C57—C58—C59 | 58.8 (8) |
Rh8v—Rh8—N15—C57 | 3.8 (5) | N15—C57—C58—C59 | −117.0 (7) |
N15—Rh8—N16—C61 | 83.3 (6) | C57—C58—C59—C60 | 57.3 (9) |
O15v—Rh8—N16—C61 | −92.3 (6) | Rh8v—O16—C61—N16 | −2.6 (8) |
O16v—Rh8—N16—C61 | −12 (3) | Rh8v—O16—C61—C62 | 176.1 (4) |
O24—Rh8—N16—C61 | 176.6 (6) | Rh8—N16—C61—O16 | 3.8 (9) |
Rh8v—Rh8—N16—C61 | −2.5 (5) | Rh8—N16—C61—C62 | −174.9 (5) |
O18—Mo1—O17—Rh1 | 176.1 (2) | O16—C61—C62—C63 | 172.0 (6) |
O19—Mo1—O17—Rh1 | −64.0 (3) | N16—C61—C62—C63 | −9.3 (10) |
O20—Mo1—O17—Rh1 | 56.0 (3) | C61—C62—C63—C64 | −178.1 (6) |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z; (iii) −x, −y, −z; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+1; (vi) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O19 | 0.88 | 2.30 | 3.049 (7) | 144 |
N1—H1···O10ii | 0.88 | 2.59 | 3.294 (6) | 138 |
N2—H2···O20 | 0.88 | 2.19 | 2.976 (7) | 149 |
N3—H3···O23 | 0.88 | 2.40 | 3.177 (7) | 147 |
N4—H4···O24 | 0.88 | 2.21 | 3.001 (7) | 149 |
N5—H5···O17 | 0.88 | 2.10 | 2.868 (7) | 145 |
N6—H6···O20 | 0.88 | 2.34 | 3.133 (7) | 151 |
N7—H7···O21i | 0.88 | 2.17 | 2.969 (7) | 151 |
N8—H8···O24i | 0.88 | 2.46 | 3.203 (7) | 142 |
N9—H9···O17 | 0.88 | 2.22 | 3.004 (6) | 148 |
N10—H10···O18 | 0.88 | 2.19 | 2.950 (6) | 144 |
N11—H11···O19 | 0.88 | 2.15 | 2.967 (7) | 154 |
N12—H12···O18 | 0.88 | 2.65 | 3.370 (8) | 140 |
N13—H13···O22 | 0.88 | 2.16 | 2.916 (6) | 144 |
N14—H14···O21 | 0.88 | 2.27 | 3.064 (6) | 150 |
N15—H15···O22 | 0.88 | 2.25 | 3.053 (7) | 152 |
N16—H16···O23 | 0.88 | 2.34 | 3.067 (7) | 140 |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z. |
Experimental details
| (I) | (II) | (III) | (IV) |
Crystal data |
Chemical formula | C16H32CrN8O12Rh4 | C16H32MoN8O12Rh4 | C16H32N8O12Rh4W | C16H32CrN8O12Ru4 |
Mr | 992.14 | 1036.08 | 1123.99 | 984.78 |
Crystal system, space group | Tetragonal, I41/a | Tetragonal, I41/a | Tetragonal, I41/a | Tetragonal, I41/a |
Temperature (K) | 296 | 296 | 296 | 296 |
a, b, c (Å) | 9.4384 (7), 9.4384 (7), 29.750 (3) | 9.5725 (8), 9.5725 (8), 29.627 (3) | 9.5905 (8), 9.5905 (8), 29.625 (3) | 9.4232 (5), 9.4232 (5), 30.168 (3) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 2650.2 (4) | 2714.8 (4) | 2724.8 (4) | 2678.9 (3) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.91 | 2.90 | 6.65 | 2.67 |
Crystal size (mm) | 0.10 × 0.10 × 0.10 | 0.10 × 0.10 × 0.06 | 0.05 × 0.03 × 0.03 | 0.08 × 0.08 × 0.06 |
|
Data collection |
Diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer |
Absorption correction | Integration (Higashi, 1999) | Integration (Higashi, 1999) | Integration (Higashi, 1999) | Integration (Higashi, 1999) |
Tmin, Tmax | 0.759, 0.806 | 0.731, 0.856 | 0.672, 0.801 | 0.833, 0.871 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10792, 1528, 1383 | 11116, 1557, 1393 | 11140, 1566, 1265 | 10957, 1539, 1475 |
Rint | 0.060 | 0.067 | 0.080 | 0.042 |
(sin θ/λ)max (Å−1) | 0.649 | 0.649 | 0.649 | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.078, 1.28 | 0.061, 0.091, 1.30 | 0.050, 0.082, 1.23 | 0.038, 0.066, 1.33 |
No. of reflections | 1528 | 1557 | 1566 | 1539 |
No. of parameters | 95 | 95 | 95 | 95 |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.019P)2 + 17.9794P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0169P)2 + 35.6503P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0229P)2 + 17.8895P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0172P)2 + 12.7943P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.49, −0.68 | 0.71, −0.71 | 0.86, −0.63 | 0.58, −0.49 |
| (V) | (VI) | (VII) | (VIII) |
Crystal data |
Chemical formula | C16H32MoN8O12Ru4 | C16H32N8O12Ru4W | C24H48CrN8O12Rh4·1.08(H2O) | C24H48MoN8O12Rh4·2.44(OH2) |
Mr | 1028.72 | 1116.63 | 1123.76 | 1191.52 |
Crystal system, space group | Tetragonal, I41/a | Tetragonal, I41/a | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 296 | 296 | 296 | 223 |
a, b, c (Å) | 9.5504 (5), 9.5504 (5), 29.933 (3) | 9.5668 (7), 9.5668 (7), 29.980 (3) | 12.978 (2), 13.576 (3), 14.498 (3) | 12.952 (4), 13.849 (5), 14.679 (5) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 112.405 (5), 101.362 (4), 106.816 (5) | 112.460 (2), 99.574 (2), 108.472 (3) |
V (Å3) | 2730.2 (3) | 2743.9 (4) | 2120.1 (8) | 2180.4 (13) |
Z | 4 | 4 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.68 | 6.40 | 1.83 | 1.83 |
Crystal size (mm) | 0.30 × 0.10 × 0.10 | 0.06 × 0.06 × 0.04 | 0.30 × 0.10 × 0.10 | 0.50 × 0.30 × 0.20 |
|
Data collection |
Diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer | Rigaku/MSC Mercury CCD diffractometer |
Absorption correction | Integration (Higashi, 1999) | Integration (Higashi, 1999) | Integration (Higashi, 1999) | Integration (Higashi, 1999) |
Tmin, Tmax | 0.844, 0.931 | 0.621, 0.831 | 0.843, 0.945 | 0.581, 0.859 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10984, 1568, 1156 | 10895, 1580, 1543 | 17505, 9650, 6828 | 17845, 9884, 8783 |
Rint | 0.112 | 0.050 | 0.065 | 0.030 |
(sin θ/λ)max (Å−1) | 0.649 | 0.649 | 0.649 | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.056, 0.105, 1.02 | 0.040, 0.069, 1.26 | 0.089, 0.133, 1.17 | 0.036, 0.078, 1.09 |
No. of reflections | 1568 | 1580 | 9650 | 9884 |
No. of parameters | 96 | 96 | 588 | 543 |
No. of restraints | 0 | 0 | 394 | 178 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.0349P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0074P)2 + 37.8978P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.P)2 + 19.3981P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0235P)2 + 3.5108P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 0.99, −0.84 | 0.64, −0.80 | 0.88, −0.93 | 0.72, −0.84 |
| (IX) |
Crystal data |
Chemical formula | C32H64MoN8O12Rh4 |
Mr | 1260.49 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 118 |
a, b, c (Å) | 15.567 (4), 15.778 (4), 19.221 (5) |
α, β, γ (°) | 87.720 (6), 89.872 (6), 78.448 (5) |
V (Å3) | 4621.6 (19) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.72 |
Crystal size (mm) | 0.10 × 0.10 × 0.10 |
|
Data collection |
Diffractometer | Rigaku/MSC Mercury CCD diffractometer |
Absorption correction | Integration NUMABS (Higashi, 1999) |
Tmin, Tmax | 0.804, 0.902 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 38498, 21025, 13532 |
Rint | 0.066 |
(sin θ/λ)max (Å−1) | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.062, 0.104, 1.02 |
No. of reflections | 21025 |
No. of parameters | 1043 |
No. of restraints | 33 |
H-atom treatment | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.0273P)2] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 1.09, −0.96 |
Selected geometric parameters (Å, º) for (I) topRh1—N1i | 1.959 (4) | Rh1—O3 | 2.235 (4) |
Rh1—N2i | 1.998 (4) | Rh1—Rh1i | 2.4225 (8) |
Rh1—O1 | 2.014 (4) | Cr1—O3 | 1.653 (4) |
Rh1—O2 | 2.041 (4) | | |
| | | |
O3—Rh1—Rh1i | 171.99 (11) | O3iii—Cr1—O3 | 110.79 (14) |
O3—Cr1—O3ii | 106.9 (3) | Cr1—O3—Rh1 | 147.9 (2) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.38 | 3.076 (5) | 137.8 |
N2—H2···O2v | 0.86 | 2.32 | 3.150 (5) | 162.0 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (II) topRh1—N1i | 1.975 (6) | Rh1—O3 | 2.219 (5) |
Rh1—N2i | 1.986 (6) | Rh1—Rh1i | 2.4170 (11) |
Rh1—O1 | 2.026 (5) | Mo1—O3 | 1.758 (5) |
Rh1—O2 | 2.034 (5) | | |
| | | |
O3—Rh1—Rh1i | 173.02 (14) | O3iii—Mo1—O3 | 111.12 (18) |
O3—Mo1—O3ii | 106.2 (3) | Mo1—O3—Rh1 | 147.0 (3) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (II) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.44 | 3.152 (8) | 140.2 |
N2—H2···O2v | 0.86 | 2.33 | 3.170 (7) | 164.4 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (III) topRh1—N1i | 1.965 (7) | Rh1—O3 | 2.221 (5) |
Rh1—N2i | 2.000 (6) | Rh1—Rh1i | 2.4161 (11) |
Rh1—O2 | 2.033 (5) | W1—O3 | 1.770 (6) |
Rh1—O1 | 2.034 (5) | | |
| | | |
O3—Rh1—Rh1i | 173.05 (16) | O3iii—W1—O3 | 111.1 (2) |
O3—W1—O3ii | 106.3 (4) | W1—O3—Rh1 | 146.8 (3) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (III) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.47 | 3.174 (8) | 139.7 |
N2—H2···O2v | 0.86 | 2.33 | 3.168 (8) | 165.3 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (IV) topRu1—N1i | 2.006 (3) | Ru1—O3 | 2.261 (3) |
Ru1—N2i | 2.033 (3) | Ru1—Ru1i | 2.3068 (6) |
Ru1—O1 | 2.041 (3) | Cr1—O3 | 1.657 (3) |
Ru1—O2 | 2.059 (3) | | |
| | | |
O3—Ru1—Ru1i | 171.26 (8) | O3iii—Cr1—O3 | 110.32 (11) |
O3ii—Cr1—O3 | 107.8 (2) | Cr1—O3—Ru1 | 151.18 (18) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.35 | 3.046 (4) | 137.7 |
N2—H2···O2v | 0.86 | 2.33 | 3.146 (4) | 159.4 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (V) topRu1—N1i | 2.015 (9) | Ru1—O3 | 2.244 (5) |
Ru1—N2i | 2.020 (9) | Ru1—Ru1i | 2.2958 (12) |
Ru1—O2 | 2.045 (7) | Mo1—O3 | 1.769 (6) |
Ru1—O1 | 2.063 (7) | | |
| | | |
O3—Ru1—Ru1i | 172.86 (18) | O3—Mo1—O3iii | 111.1 (2) |
O3ii—Mo1—O3 | 106.2 (4) | Mo1—O3—Ru1 | 149.0 (4) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (V) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.42 | 3.122 (8) | 139.6 |
N2—H2···O2v | 0.86 | 2.32 | 3.154 (8) | 162.4 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (VI) topRu1—N1i | 2.021 (8) | Ru1—O3 | 2.239 (5) |
Ru1—N2i | 2.053 (7) | Ru1—Ru1i | 2.2954 (9) |
Ru1—O1 | 2.043 (6) | W1—O3 | 1.780 (5) |
Ru1—O2 | 2.048 (7) | | |
| | | |
O3—Ru1—Ru1i | 172.48 (15) | O3iii—W1—O3 | 110.56 (18) |
O3—W1—O3ii | 107.3 (4) | W1—O3—Ru1 | 149.6 (3) |
Symmetry codes: (i) −x+1, −y+1/2, z; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |
Hydrogen-bond geometry (Å, º) for (VI) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O1iv | 0.86 | 2.40 | 3.122 (7) | 141.3 |
N2—H2···O2v | 0.86 | 2.32 | 3.147 (7) | 162.6 |
Symmetry codes: (iv) −y+5/4, x+1/4, −z+1/4; (v) x+1/2, y, −z+1/2. |
Selected geometric parameters (Å, º) for (VII) topRh1—N1 | 1.976 (8) | Rh3—N5 | 1.980 (8) |
Rh1—N2 | 1.956 (8) | Rh3—N6 | 1.969 (6) |
Rh1—O1i | 2.019 (7) | Rh3—O5iii | 2.034 (7) |
Rh1—O2i | 2.017 (7) | Rh3—O6iii | 2.040 (6) |
Rh1—O9 | 2.226 (5) | Rh3—O11 | 2.179 (6) |
Rh1—Rh1i | 2.4071 (14) | Rh3—Rh3iii | 2.4053 (15) |
Rh2—N3 | 1.992 (7) | Rh4—N7 | 1.985 (9) |
Rh2—N4 | 1.975 (7) | Rh4—N8 | 1.977 (9) |
Rh2—O3ii | 2.027 (6) | Rh4—O7iv | 2.033 (7) |
Rh2—O4ii | 2.030 (6) | Rh4—O8iv | 2.016 (7) |
Rh2—O10 | 2.207 (6) | Rh4—O12 | 2.201 (6) |
Rh2—Rh2ii | 2.4122 (15) | Rh4—Rh4iv | 2.4076 (15) |
| | | |
O9—Rh1—Rh1i | 178.04 (17) | O11—Cr1—O10 | 108.4 (3) |
O10—Rh2—Rh2ii | 177.28 (15) | O12—Cr1—O10 | 109.8 (3) |
O11—Rh3—Rh3iii | 179.44 (18) | O12—Cr1—O11 | 110.4 (3) |
O12—Rh4—Rh4iv | 179.67 (18) | Cr1—O9—Rh1 | 118.1 (3) |
O9—Cr1—O10 | 109.2 (3) | Cr1—O10—Rh2 | 119.7 (3) |
O11—Cr1—O9 | 110.1 (3) | Cr1—O11—Rh3 | 131.4 (3) |
O12—Cr1—O9 | 108.9 (3) | Cr1—O12—Rh4 | 121.1 (3) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) for (VII) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O12 | 0.86 | 2.32 | 2.963 (9) | 131.5 |
N2—H2···O10 | 0.86 | 2.12 | 2.917 (9) | 153.2 |
N3—H3···O9 | 0.86 | 2.19 | 2.965 (9) | 149.9 |
N4—H4···O11 | 0.86 | 2.33 | 3.015 (10) | 137.3 |
N5—H5···N4 | 0.86 | 2.66 | 3.404 (11) | 146.3 |
N6—H6···O9 | 0.86 | 2.09 | 2.860 (9) | 149.0 |
N7—H7···O10 | 0.86 | 2.19 | 2.978 (9) | 153.1 |
N8—H8···O11 | 0.86 | 2.37 | 3.016 (10) | 132.4 |
N8—H8···O5iii | 0.86 | 2.61 | 3.392 (11) | 151.3 |
Symmetry code: (iii) −x+1, −y, −z+1. |
Selected geometric parameters (Å, º) for (VIII) topRh1—N1 | 1.971 (3) | Rh3—N5 | 1.986 (3) |
Rh1—N2 | 1.987 (3) | Rh3—N6 | 1.972 (3) |
Rh1—O1i | 2.036 (3) | Rh3—O5iii | 2.025 (3) |
Rh1—O2i | 2.034 (3) | Rh3—O6iii | 2.032 (3) |
Rh1—O9 | 2.233 (2) | Rh3—O11 | 2.207 (2) |
Rh1—Rh1i | 2.4117 (8) | Rh3—Rh3iii | 2.4037 (8) |
Rh2—N3 | 1.980 (3) | Rh4—N7 | 1.983 (3) |
Rh2—N4 | 1.977 (3) | Rh4—N8 | 1.965 (3) |
Rh2—O3ii | 2.030 (3) | Rh4—O7iv | 2.031 (3) |
Rh2—O4ii | 2.039 (3) | Rh4—O8iv | 2.038 (3) |
Rh2—O10 | 2.214 (3) | Rh4—O12 | 2.277 (3) |
Rh2—Rh2ii | 2.4019 (9) | Rh4—Rh4iv | 2.4148 (8) |
| | | |
O9—Rh1—Rh1i | 177.03 (7) | O11—Mo1—O10 | 109.17 (12) |
O10—Rh2—Rh2ii | 178.87 (7) | O12—Mo1—O10 | 108.12 (12) |
O11—Rh3—Rh3iii | 179.13 (7) | O11—Mo1—O12 | 111.64 (12) |
O12—Rh4—Rh4iv | 177.80 (6) | Mo1—O9—Rh1 | 119.29 (13) |
O9—Mo1—O10 | 107.90 (13) | Mo1—O10—Rh2 | 122.07 (13) |
O11—Mo1—O9 | 108.53 (12) | Mo1—O11—Rh3 | 136.57 (14) |
O9—Mo1—O12 | 111.38 (12) | Mo1—O12—Rh4 | 129.21 (13) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y, −z; (iv) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) for (VIII) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O12 | 0.87 | 2.36 | 3.049 (4) | 135.8 |
N2—H2···O10 | 0.87 | 2.24 | 3.048 (4) | 155.5 |
N3—H3···O11 | 0.87 | 2.19 | 2.970 (4) | 148.4 |
N4—H4···O9 | 0.87 | 2.46 | 3.210 (4) | 144.2 |
N4—H4···O1i | 0.87 | 2.59 | 3.307 (4) | 139.8 |
N5—H5···O13 | 0.87 | 2.27 | 3.061 (5) | 152.0 |
N6—H6···O12 | 0.87 | 2.29 | 3.107 (4) | 156.0 |
N7—H7···N1 | 0.87 | 2.49 | 3.286 (5) | 153.1 |
N8—H8···O10 | 0.87 | 1.98 | 2.808 (4) | 158.9 |
Symmetry code: (i) −x+2, −y, −z+1. |
Selected geometric parameters (Å, º) for (IX) topRh1—N2 | 1.975 (5) | Rh5—Rh5ii | 2.4080 (11) |
Rh1—N1 | 1.977 (6) | Rh6—N12 | 1.980 (6) |
Rh1—O4 | 2.024 (4) | Rh6—N11 | 1.995 (5) |
Rh1—O3 | 2.041 (4) | Rh6—O11iii | 2.027 (4) |
Rh1—O17 | 2.254 (4) | Rh6—O12iii | 2.032 (5) |
Rh1—Rh2 | 2.4119 (9) | Rh6—O20 | 2.262 (5) |
Rh2—N4 | 1.980 (5) | Rh6—Rh6iii | 2.4179 (12) |
Rh2—N3 | 1.988 (6) | Rh7—N13 | 1.969 (6) |
Rh2—O1 | 2.025 (5) | Rh7—N14 | 1.978 (6) |
Rh2—O2 | 2.044 (4) | Rh7—O14iv | 2.028 (5) |
Rh2—O21 | 2.243 (4) | Rh7—O13iv | 2.033 (5) |
Rh3—N5 | 1.978 (5) | Rh7—O23 | 2.285 (4) |
Rh3—N6 | 1.986 (5) | Rh7—Rh7iv | 2.4134 (11) |
Rh3—O8 | 2.036 (4) | Rh8—N16 | 1.968 (5) |
Rh3—O7 | 2.036 (5) | Rh8—N15 | 1.981 (5) |
Rh3—O18 | 2.261 (4) | Rh8—O15v | 2.028 (4) |
Rh3—Rh4 | 2.4108 (9) | Rh8—O16v | 2.044 (4) |
Rh4—N7 | 1.987 (6) | Rh8—O24 | 2.269 (5) |
Rh4—N8 | 1.988 (5) | Rh8—Rh8v | 2.4118 (12) |
Rh4—O5 | 2.031 (5) | Mo1—O18 | 1.760 (4) |
Rh4—O6 | 2.043 (4) | Mo1—O17 | 1.768 (5) |
Rh4—O22i | 2.225 (4) | Mo1—O19 | 1.770 (4) |
Rh5—N10 | 1.968 (5) | Mo1—O20 | 1.770 (4) |
Rh5—N9 | 1.981 (6) | Mo2—O23 | 1.766 (4) |
Rh5—O10ii | 2.017 (5) | Mo2—O24 | 1.769 (4) |
Rh5—O9ii | 2.032 (5) | Mo2—O21 | 1.772 (5) |
Rh5—O19 | 2.242 (4) | Mo2—O22 | 1.772 (4) |
| | | |
O17—Rh1—Rh2 | 174.23 (12) | O23—Mo2—O24 | 111.3 (2) |
O21—Rh2—Rh1 | 175.57 (11) | O23—Mo2—O21 | 108.8 (2) |
O18—Rh3—Rh4 | 177.17 (12) | O24—Mo2—O21 | 110.12 (19) |
O22i—Rh4—Rh3 | 176.67 (12) | O23—Mo2—O22 | 108.86 (19) |
O19—Rh5—Rh5ii | 177.52 (12) | O24—Mo2—O22 | 108.0 (2) |
O20—Rh6—Rh6iii | 175.65 (12) | O21—Mo2—O22 | 109.7 (2) |
O23—Rh7—Rh7iv | 178.68 (12) | Mo1—O17—Rh1 | 122.7 (2) |
O24—Rh8—Rh8v | 174.75 (10) | Mo1—O18—Rh3 | 119.2 (2) |
O18—Mo1—O17 | 109.4 (2) | Mo1—O19—Rh5 | 119.4 (2) |
O18—Mo1—O19 | 109.70 (19) | Mo1—O20—Rh6 | 120.5 (2) |
O17—Mo1—O19 | 108.7 (2) | Mo2—O21—Rh2 | 118.9 (2) |
O18—Mo1—O20 | 109.4 (2) | Mo2—O22—Rh4vi | 120.3 (2) |
O17—Mo1—O20 | 109.97 (19) | Mo2—O23—Rh7 | 118.2 (2) |
O19—Mo1—O20 | 109.6 (2) | Mo2—O24—Rh8 | 121.6 (2) |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z; (iii) −x, −y, −z; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+1; (vi) x+1, y, z. |
Hydrogen-bond geometry (Å, º) for (IX) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O19 | 0.88 | 2.30 | 3.049 (7) | 143.6 |
N1—H1···O10ii | 0.88 | 2.59 | 3.294 (6) | 137.6 |
N2—H2···O20 | 0.88 | 2.19 | 2.976 (7) | 149.0 |
N3—H3···O23 | 0.88 | 2.40 | 3.177 (7) | 146.9 |
N4—H4···O24 | 0.88 | 2.21 | 3.001 (7) | 148.8 |
N5—H5···O17 | 0.88 | 2.10 | 2.868 (7) | 144.9 |
N6—H6···O20 | 0.88 | 2.34 | 3.133 (7) | 150.6 |
N7—H7···O21i | 0.88 | 2.17 | 2.969 (7) | 151.3 |
N8—H8···O24i | 0.88 | 2.46 | 3.203 (7) | 142.3 |
N9—H9···O17 | 0.88 | 2.22 | 3.004 (6) | 148.3 |
N10—H10···O18 | 0.88 | 2.19 | 2.950 (6) | 144.3 |
N11—H11···O19 | 0.88 | 2.15 | 2.967 (7) | 153.6 |
N12—H12···O18 | 0.88 | 2.65 | 3.370 (8) | 139.9 |
N13—H13···O22 | 0.88 | 2.16 | 2.916 (6) | 143.9 |
N14—H14···O21 | 0.88 | 2.27 | 3.064 (6) | 149.8 |
N15—H15···O22 | 0.88 | 2.25 | 3.053 (7) | 151.5 |
N16—H16···O23 | 0.88 | 2.34 | 3.067 (7) | 140.4 |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z. |
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