Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052519213024068/ry5054sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IIIsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IVsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054Vsup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIsup7.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIIsup8.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIIIsup9.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IXsup10.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052519213024068/ry5054sup11.pdf | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052519213024068/ry5054sup12.pdf |
CCDC references: 969676; 969677; 969678; 969679; 969680; 969681; 969682; 969683; 969684
Crystal data, data collection and structure refinement details are summarized in Table 1.
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).
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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 |
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 |
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 |
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. |
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* |
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) |
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. |
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. |
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 |
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 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 |
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)° |
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 |
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 |
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. |
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) |
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) |
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. |
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. |
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 |
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 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 |
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)° |
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 |
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 |
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. |
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) |
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) |
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. |
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. |
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 |
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 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 |
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)° |
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 |
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 |
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. |
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* |
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) |
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. |
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 |
Computer programs: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001), CrystalClear, SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976), Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).
Rh1—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. |
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. |
Rh1—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. |
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. |
Rh1—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. |
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. |
Ru1—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. |
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. |
Ru1—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. |
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. |
Ru1—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. |
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. |
Rh1—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. |
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. |
Rh1—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. |
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. |
Rh1—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. |
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. |