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Monocationic acetamidate-bridged dinuclear units are two-dimensionally connected by axially coordinating group 6 oxometallate ions in the structures [{M2(acam)4}2(M′O4)] (M = Rh, Ru; M′ = Cr, Mo, W; Hacam = acetamide). In these sheet structures, dinuclear units are connected to each other by NH...O hydrogen bonds. The sheets are also connected with NH...O hydrogen bonds. Amidate-bridged dirhodium units that have bulkier alkyl groups reacted with CrO42− or MoO42− give three-dimensional diamondoid structures [{Rh2(pram)4}2(CrO4)]·1.08H2O, [{Rh2(pram)4}2(MoO4)]·2.44H2O and [{Rh2(buam)4}2(MoO4)] (Hpram = propion­amide; Hbuam = butyramide). In these structures the NH group of the amidate ligands hydrogen bonds with O atoms in metallate ions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052519213024068/ry5054sup1.cif
Contains datablocks I, II, III, IV, V, VI, VII, VIII, IX, General

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IIsup3.hkl
Contains datablock fuma048_rhacammo4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IIIsup4.hkl
Contains datablock fuma052

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IVsup5.hkl
Contains datablock fuma079

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054Vsup6.hkl
Contains datablock V

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIsup7.hkl
Contains datablock fuma081

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIIsup8.hkl
Contains datablock fuma108

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054VIIIsup9.hkl
Contains datablock fuma138

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052519213024068/ry5054IXsup10.hkl
Contains datablock fuma187

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Portable Document Format (PDF) file https://doi.org/10.1107/S2052519213024068/ry5054sup11.pdf
Figures S1-2

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052519213024068/ry5054sup12.pdf
Tables S1-2

CCDC references: 969676; 969677; 969678; 969679; 969680; 969681; 969682; 969683; 969684

Experimental top

Refinement top

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

Results and discussion top

Computing details top

For all compounds, data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
(I) top
Crystal data top
C16H32CrN8O12Rh4Dx = 2.487 Mg m3
Mr = 992.14Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I41/aCell parameters from 3335 reflections
Hall symbol: -I 4adθ = 3.0–27.5°
a = 9.4384 (7) ŵ = 2.91 mm1
c = 29.750 (3) ÅT = 296 K
V = 2650.2 (4) Å3Prism, brown
Z = 40.10 × 0.10 × 0.10 mm
F(000) = 1936
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1528 independent reflections
Radiation source: rotating-anode X-ray tube1383 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.4°
ω scansh = 128
Absorption correction: integration
(Higashi, 1999)
k = 812
Tmin = 0.759, Tmax = 0.806l = 3638
10792 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.078H-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 parametersΔρmax = 0.49 e Å3
0 restraintsΔρmin = 0.68 e Å3
Crystal data top
C16H32CrN8O12Rh4Z = 4
Mr = 992.14Mo Kα radiation
Tetragonal, I41/aµ = 2.91 mm1
a = 9.4384 (7) ÅT = 296 K
c = 29.750 (3) Å0.10 × 0.10 × 0.10 mm
V = 2650.2 (4) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1528 independent reflections
Absorption correction: integration
(Higashi, 1999)
1383 reflections with I > 2σ(I)
Tmin = 0.759, Tmax = 0.806Rint = 0.060
10792 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.078H-atom parameters constrained
S = 1.28 w = 1/[σ2(Fo2) + (0.019P)2 + 17.9794P]
where P = (Fo2 + 2Fc2)/3
1528 reflectionsΔρmax = 0.49 e Å3
95 parametersΔρmin = 0.68 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rh10.37187 (4)0.25713 (4)0.168366 (13)0.01513 (13)
Cr10.00000.25000.12500.0196 (4)
O10.3838 (4)0.4047 (4)0.11961 (13)0.0209 (8)
O20.3833 (4)0.4134 (4)0.21563 (12)0.0222 (8)
O30.1381 (4)0.2767 (4)0.15810 (14)0.0317 (10)
N10.6231 (4)0.3963 (4)0.12405 (16)0.0197 (9)
H10.70240.43120.11510.024*
N20.6214 (4)0.3794 (4)0.21963 (15)0.0200 (10)
H20.69960.40190.23260.024*
C10.5065 (6)0.4488 (5)0.10727 (18)0.0196 (11)
C20.5085 (7)0.5616 (7)0.0717 (2)0.0369 (16)
H30.50250.51840.04260.055*
H40.59500.61470.07390.055*
H50.42930.62400.07590.055*
C30.5051 (6)0.4358 (5)0.23423 (19)0.0200 (11)
C40.5040 (7)0.5318 (7)0.2738 (2)0.0366 (15)
H60.44290.61090.26790.055*
H70.59840.56530.27950.055*
H80.47010.48120.29960.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0110 (2)0.0166 (2)0.0178 (2)0.00003 (14)0.00042 (15)0.00041 (15)
Cr10.0142 (5)0.0142 (5)0.0304 (10)0.0000.0000.000
O10.0162 (18)0.0218 (19)0.025 (2)0.0002 (14)0.0003 (15)0.0075 (16)
O20.0217 (19)0.0246 (19)0.020 (2)0.0023 (15)0.0014 (15)0.0051 (16)
O30.0104 (17)0.044 (2)0.041 (3)0.0006 (16)0.0009 (17)0.0046 (19)
N10.012 (2)0.023 (2)0.024 (3)0.0049 (16)0.0023 (17)0.0025 (18)
N20.015 (2)0.023 (2)0.022 (3)0.0025 (17)0.0035 (17)0.0045 (18)
C10.026 (3)0.012 (2)0.021 (3)0.001 (2)0.000 (2)0.002 (2)
C20.031 (3)0.034 (3)0.046 (4)0.002 (3)0.004 (3)0.020 (3)
C30.027 (3)0.014 (2)0.019 (3)0.001 (2)0.000 (2)0.001 (2)
C40.052 (4)0.034 (3)0.025 (3)0.005 (3)0.003 (3)0.012 (3)
Geometric parameters (Å, º) top
Rh1—N1i1.959 (4)N2—C31.295 (6)
Rh1—N2i1.998 (4)N2—Rh1i1.998 (4)
Rh1—O12.014 (4)N2—H20.8600
Rh1—O22.041 (4)C1—C21.501 (8)
Rh1—O32.235 (4)C2—H30.9600
Rh1—Rh1i2.4225 (8)C2—H40.9600
Cr1—O31.653 (4)C2—H50.9600
O1—C11.283 (6)C3—C41.486 (8)
O2—C31.294 (6)C4—H60.9600
N1—C11.306 (7)C4—H70.9600
N1—Rh1i1.959 (4)C4—H80.9600
N1—H10.8600
N1i—Rh1—N2i92.07 (18)C1—N1—Rh1i123.9 (3)
N1i—Rh1—O191.44 (17)C1—N1—H1118.0
N2i—Rh1—O1173.79 (16)Rh1i—N1—H1118.0
N1i—Rh1—O2175.39 (16)C3—N2—Rh1i123.2 (4)
N2i—Rh1—O286.48 (16)C3—N2—H2118.4
O1—Rh1—O289.63 (15)Rh1i—N2—H2118.4
N1i—Rh1—O389.60 (16)O1—C1—N1121.9 (5)
N2i—Rh1—O3100.89 (16)O1—C1—C2116.3 (5)
O1—Rh1—O384.26 (15)N1—C1—C2121.8 (5)
O2—Rh1—O394.97 (14)C1—C2—H3109.5
N1i—Rh1—Rh1i86.25 (12)C1—C2—H4109.5
N2i—Rh1—Rh1i86.13 (12)H3—C2—H4109.5
O1—Rh1—Rh1i88.99 (10)C1—C2—H5109.5
O2—Rh1—Rh1i89.29 (10)H3—C2—H5109.5
O3—Rh1—Rh1i171.99 (11)H4—C2—H5109.5
O3—Cr1—O3ii106.9 (3)O2—C3—N2122.9 (5)
O3iii—Cr1—O3iv106.9 (3)O2—C3—C4115.6 (5)
O3iii—Cr1—O3110.79 (14)N2—C3—C4121.5 (5)
O3iv—Cr1—O3110.79 (14)C3—C4—H6109.5
O3iii—Cr1—O3ii110.79 (14)C3—C4—H7109.5
O3iv—Cr1—O3ii110.79 (14)H6—C4—H7109.5
C1—O1—Rh1118.7 (3)C3—C4—H8109.5
C3—O2—Rh1117.4 (3)H6—C4—H8109.5
Cr1—O3—Rh1147.9 (2)H7—C4—H8109.5
N1i—Rh1—O1—C190.8 (4)N2i—Rh1—O3—Cr1115.2 (5)
O2—Rh1—O1—C184.7 (4)O1—Rh1—O3—Cr168.4 (5)
O3—Rh1—O1—C1179.7 (4)O2—Rh1—O3—Cr1157.5 (4)
Rh1i—Rh1—O1—C14.6 (4)Rh1—O1—C1—N13.0 (7)
N2i—Rh1—O2—C375.6 (4)Rh1—O1—C1—C2178.3 (4)
O1—Rh1—O2—C399.6 (4)Rh1i—N1—C1—O11.6 (7)
O3—Rh1—O2—C3176.2 (4)Rh1i—N1—C1—C2177.0 (4)
Rh1i—Rh1—O2—C310.6 (4)Rh1—O2—C3—N210.5 (7)
O3iii—Cr1—O3—Rh128.9 (5)Rh1—O2—C3—C4169.6 (4)
O3iv—Cr1—O3—Rh189.5 (6)Rh1i—N2—C3—O23.0 (7)
O3ii—Cr1—O3—Rh1149.7 (5)Rh1i—N2—C3—C4177.1 (4)
N1i—Rh1—O3—Cr123.1 (5)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.383.076 (5)138
N2—H2···O2vi0.862.323.150 (5)162
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(II) top
Crystal data top
C16H32MoN8O12Rh4Dx = 2.535 Mg m3
Mr = 1036.08Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I41/aCell parameters from 3061 reflections
Hall symbol: -I 4adθ = 3.0–27.5°
a = 9.5725 (8) ŵ = 2.90 mm1
c = 29.627 (3) ÅT = 296 K
V = 2714.8 (4) Å3Block, brown
Z = 40.10 × 0.10 × 0.06 mm
F(000) = 2008
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1557 independent reflections
Radiation source: rotating-anode X-ray tube1393 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 912
Absorption correction: integration
(Higashi, 1999)
k = 1012
Tmin = 0.731, Tmax = 0.856l = 3825
11116 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-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 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.71 e Å3
Crystal data top
C16H32MoN8O12Rh4Z = 4
Mr = 1036.08Mo Kα radiation
Tetragonal, I41/aµ = 2.90 mm1
a = 9.5725 (8) ÅT = 296 K
c = 29.627 (3) Å0.10 × 0.10 × 0.06 mm
V = 2714.8 (4) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1557 independent reflections
Absorption correction: integration
(Higashi, 1999)
1393 reflections with I > 2σ(I)
Tmin = 0.731, Tmax = 0.856Rint = 0.067
11116 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0610 restraints
wR(F2) = 0.091H-atom parameters constrained
S = 1.30 w = 1/[σ2(Fo2) + (0.0169P)2 + 35.6503P]
where P = (Fo2 + 2Fc2)/3
1557 reflectionsΔρmax = 0.71 e Å3
95 parametersΔρmin = 0.71 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rh10.37397 (6)0.25731 (6)0.169556 (17)0.01489 (15)
Mo10.00000.25000.12500.0182 (3)
N10.6215 (6)0.3964 (6)0.1251 (2)0.0208 (13)
H10.69970.43180.11640.025*
O10.3861 (5)0.4030 (5)0.12014 (16)0.0207 (11)
N20.6200 (6)0.3772 (6)0.22057 (19)0.0201 (14)
H20.69720.39860.23370.024*
O20.3849 (5)0.4127 (5)0.21626 (16)0.0226 (11)
O30.1446 (5)0.2760 (6)0.16062 (18)0.0324 (13)
C10.5065 (8)0.4472 (7)0.1082 (2)0.0203 (15)
C20.5094 (9)0.5599 (9)0.0729 (3)0.0321 (19)
H30.49640.51890.04360.048*
H40.59780.60710.07380.048*
H50.43570.62560.07860.048*
C30.5061 (9)0.4341 (8)0.2350 (2)0.0224 (16)
C40.5058 (10)0.5338 (9)0.2737 (2)0.037 (2)
H60.43980.50300.29600.056*
H70.47990.62510.26320.056*
H80.59730.53760.28690.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0098 (3)0.0162 (3)0.0187 (3)0.0001 (2)0.0000 (2)0.0001 (2)
Mo10.0132 (4)0.0132 (4)0.0283 (6)0.0000.0000.000
N10.022 (3)0.021 (3)0.020 (3)0.001 (3)0.003 (2)0.004 (2)
O10.017 (3)0.023 (3)0.022 (3)0.001 (2)0.000 (2)0.005 (2)
N20.015 (3)0.023 (4)0.022 (3)0.000 (3)0.004 (2)0.004 (2)
O20.022 (3)0.022 (3)0.024 (3)0.004 (2)0.001 (2)0.002 (2)
O30.012 (3)0.045 (4)0.040 (3)0.001 (3)0.001 (2)0.002 (3)
C10.023 (4)0.016 (4)0.022 (3)0.002 (3)0.001 (3)0.001 (3)
C20.030 (5)0.028 (5)0.038 (4)0.001 (4)0.002 (4)0.013 (4)
C30.031 (4)0.018 (4)0.018 (3)0.001 (3)0.000 (3)0.002 (3)
C40.052 (6)0.034 (5)0.025 (4)0.008 (4)0.004 (4)0.013 (3)
Geometric parameters (Å, º) top
Rh1—N1i1.975 (6)N2—Rh1i1.986 (6)
Rh1—N2i1.986 (6)N2—H20.8600
Rh1—O12.026 (5)O2—C31.303 (9)
Rh1—O22.034 (5)C1—C21.504 (10)
Rh1—O32.219 (5)C2—H30.9600
Rh1—Rh1i2.4170 (11)C2—H40.9600
Mo1—O31.758 (5)C2—H50.9600
N1—C11.303 (9)C3—C41.492 (10)
N1—Rh1i1.975 (6)C4—H60.9600
N1—H10.8600C4—H70.9600
O1—C11.278 (9)C4—H80.9600
N2—C31.292 (9)
N1i—Rh1—N2i91.4 (2)C1—O1—Rh1118.6 (4)
N1i—Rh1—O191.7 (2)C3—N2—Rh1i123.4 (5)
N2i—Rh1—O1174.1 (2)C3—N2—H2118.3
N1i—Rh1—O2175.7 (2)Rh1i—N2—H2118.3
N2i—Rh1—O287.4 (2)C3—O2—Rh1116.8 (5)
O1—Rh1—O289.1 (2)Mo1—O3—Rh1147.0 (3)
N1i—Rh1—O390.1 (2)O1—C1—N1122.2 (6)
N2i—Rh1—O399.9 (2)O1—C1—C2116.5 (7)
O1—Rh1—O385.1 (2)N1—C1—C2121.3 (7)
O2—Rh1—O394.2 (2)C1—C2—H3109.5
N1i—Rh1—Rh1i86.28 (18)C1—C2—H4109.5
N2i—Rh1—Rh1i86.20 (17)H3—C2—H4109.5
O1—Rh1—Rh1i89.01 (14)C1—C2—H5109.5
O2—Rh1—Rh1i89.48 (14)H3—C2—H5109.5
O3—Rh1—Rh1i173.02 (14)H4—C2—H5109.5
O3—Mo1—O3ii106.2 (3)N2—C3—O2122.9 (6)
O3iii—Mo1—O3iv106.2 (3)N2—C3—C4121.8 (7)
O3iii—Mo1—O3111.12 (18)O2—C3—C4115.2 (7)
O3iv—Mo1—O3111.12 (18)C3—C4—H6109.5
O3iii—Mo1—O3ii111.12 (18)C3—C4—H7109.5
O3iv—Mo1—O3ii111.12 (18)H6—C4—H7109.5
C1—N1—Rh1i123.5 (5)C3—C4—H8109.5
C1—N1—H1118.2H6—C4—H8109.5
Rh1i—N1—H1118.2H7—C4—H8109.5
N1i—Rh1—O1—C191.8 (5)N2i—Rh1—O3—Mo1117.0 (6)
O2—Rh1—O1—C183.9 (5)O1—Rh1—O3—Mo166.1 (6)
O3—Rh1—O1—C1178.2 (5)O2—Rh1—O3—Mo1154.9 (6)
Rh1i—Rh1—O1—C15.6 (5)Rh1—O1—C1—N13.6 (9)
N2i—Rh1—O2—C375.2 (5)Rh1—O1—C1—C2177.4 (5)
O1—Rh1—O2—C3100.0 (5)Rh1i—N1—C1—O11.8 (10)
O3—Rh1—O2—C3174.9 (5)Rh1i—N1—C1—C2177.2 (5)
Rh1i—Rh1—O2—C311.0 (5)Rh1i—N2—C3—O22.8 (10)
O3iii—Mo1—O3—Rh131.1 (7)Rh1i—N2—C3—C4179.5 (6)
O3iv—Mo1—O3—Rh187.0 (8)Rh1—O2—C3—N210.7 (9)
O3ii—Mo1—O3—Rh1152.1 (7)Rh1—O2—C3—C4171.4 (5)
N1i—Rh1—O3—Mo125.6 (6)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.443.152 (8)140
N2—H2···O2vi0.862.333.170 (7)164
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(III) top
Crystal data top
C16H32N8O12Rh4WDx = 2.740 Mg m3
Mr = 1123.99Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I41/aCell parameters from 2607 reflections
Hall symbol: -I 4adθ = 3.0–27.5°
a = 9.5905 (8) ŵ = 6.65 mm1
c = 29.625 (3) ÅT = 296 K
V = 2724.8 (4) Å3Block, brown
Z = 40.05 × 0.03 × 0.03 mm
F(000) = 2136
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1566 independent reflections
Radiation source: rotating-anode X-ray tube1265 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.080
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 1012
Absorption correction: integration
(Higashi, 1999)
k = 1210
Tmin = 0.672, Tmax = 0.801l = 2438
11140 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H-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 parametersΔρmax = 0.86 e Å3
0 restraintsΔρmin = 0.63 e Å3
Crystal data top
C16H32N8O12Rh4WZ = 4
Mr = 1123.99Mo Kα radiation
Tetragonal, I41/aµ = 6.65 mm1
a = 9.5905 (8) ÅT = 296 K
c = 29.625 (3) Å0.05 × 0.03 × 0.03 mm
V = 2724.8 (4) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1566 independent reflections
Absorption correction: integration
(Higashi, 1999)
1265 reflections with I > 2σ(I)
Tmin = 0.672, Tmax = 0.801Rint = 0.080
11140 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0500 restraints
wR(F2) = 0.082H-atom parameters constrained
S = 1.23 w = 1/[σ2(Fo2) + (0.0229P)2 + 17.8895P]
where P = (Fo2 + 2Fc2)/3
1566 reflectionsΔρmax = 0.86 e Å3
95 parametersΔρmin = 0.63 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rh10.37426 (6)0.25739 (6)0.16970 (2)0.01719 (17)
W10.00000.25000.12500.02068 (19)
N10.6203 (6)0.3954 (6)0.1256 (2)0.0210 (14)
H10.69850.42990.11670.025*
O10.3858 (5)0.4027 (5)0.11985 (19)0.0226 (12)
N20.6201 (6)0.3777 (6)0.2211 (2)0.0214 (16)
H20.69690.39870.23450.026*
O20.3856 (5)0.4126 (5)0.21632 (19)0.0240 (13)
O30.1451 (6)0.2770 (6)0.1608 (2)0.0323 (15)
C10.5056 (8)0.4483 (8)0.1086 (3)0.0212 (17)
C20.5087 (10)0.5597 (9)0.0729 (3)0.041 (3)
H30.48330.51990.04430.061*
H40.60090.59810.07100.061*
H50.44390.63210.08060.061*
C30.5058 (9)0.4346 (8)0.2351 (3)0.0223 (18)
C40.5073 (10)0.5344 (9)0.2743 (3)0.037 (2)
H60.50200.62830.26330.055*
H70.59210.52250.29110.055*
H80.42890.51590.29350.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0117 (3)0.0183 (3)0.0216 (4)0.0002 (2)0.0003 (3)0.0003 (3)
W10.0148 (2)0.0148 (2)0.0324 (4)0.0000.0000.000
N10.015 (3)0.021 (3)0.027 (4)0.004 (2)0.000 (3)0.001 (3)
O10.022 (3)0.023 (3)0.023 (3)0.001 (2)0.001 (2)0.009 (3)
N20.013 (3)0.027 (4)0.025 (4)0.002 (3)0.006 (3)0.005 (3)
O20.020 (3)0.020 (3)0.031 (4)0.003 (2)0.001 (3)0.002 (3)
O30.013 (3)0.041 (4)0.043 (4)0.000 (2)0.002 (3)0.001 (3)
C10.021 (4)0.020 (4)0.023 (5)0.001 (3)0.001 (4)0.002 (3)
C20.037 (5)0.028 (5)0.057 (7)0.005 (4)0.008 (5)0.018 (5)
C30.032 (5)0.020 (4)0.014 (4)0.005 (3)0.002 (4)0.003 (3)
C40.048 (6)0.032 (5)0.030 (6)0.005 (4)0.005 (5)0.009 (4)
Geometric parameters (Å, º) top
Rh1—N1i1.965 (7)N2—Rh1i2.000 (6)
Rh1—N2i2.000 (6)N2—H20.8600
Rh1—O22.033 (5)O2—C31.298 (9)
Rh1—O12.034 (5)C1—C21.504 (11)
Rh1—O32.221 (5)C2—H30.9600
Rh1—Rh1i2.4161 (11)C2—H40.9600
W1—O31.770 (6)C2—H50.9600
N1—C11.311 (9)C3—C41.505 (10)
N1—Rh1i1.965 (7)C4—H60.9600
N1—H10.8600C4—H70.9600
O1—C11.273 (9)C4—H80.9600
N2—C31.292 (9)
N1i—Rh1—N2i91.3 (3)C1—O1—Rh1118.3 (5)
N1i—Rh1—O2175.3 (2)C3—N2—Rh1i122.7 (5)
N2i—Rh1—O287.4 (2)C3—N2—H2118.6
N1i—Rh1—O191.5 (2)Rh1i—N2—H2118.6
N2i—Rh1—O1174.5 (2)C3—O2—Rh1117.2 (5)
O2—Rh1—O189.4 (2)W1—O3—Rh1146.8 (3)
N1i—Rh1—O390.6 (2)O1—C1—N1121.7 (7)
N2i—Rh1—O399.9 (2)O1—C1—C2116.5 (7)
O2—Rh1—O394.1 (2)N1—C1—C2121.8 (7)
O1—Rh1—O384.8 (2)C1—C2—H3109.5
N1i—Rh1—Rh1i85.98 (17)C1—C2—H4109.5
N2i—Rh1—Rh1i86.27 (17)H3—C2—H4109.5
O2—Rh1—Rh1i89.41 (14)C1—C2—H5109.5
O1—Rh1—Rh1i89.20 (14)H3—C2—H5109.5
O3—Rh1—Rh1i173.05 (16)H4—C2—H5109.5
O3—W1—O3ii106.3 (4)N2—C3—O2123.2 (7)
O3iii—W1—O3iv106.3 (4)N2—C3—C4120.5 (8)
O3iii—W1—O3111.1 (2)O2—C3—C4116.3 (7)
O3iv—W1—O3111.1 (2)C3—C4—H6109.5
O3iii—W1—O3ii111.1 (2)C3—C4—H7109.5
O3iv—W1—O3ii111.1 (2)H6—C4—H7109.5
C1—N1—Rh1i124.4 (5)C3—C4—H8109.5
C1—N1—H1117.8H6—C4—H8109.5
Rh1i—N1—H1117.8H7—C4—H8109.5
N1i—Rh1—O1—C193.0 (6)N2i—Rh1—O3—W1116.4 (6)
O2—Rh1—O1—C182.4 (6)O2—Rh1—O3—W1155.5 (6)
O3—Rh1—O1—C1176.5 (6)O1—Rh1—O3—W166.5 (6)
Rh1i—Rh1—O1—C17.1 (6)Rh1—O1—C1—N16.0 (10)
N2i—Rh1—O2—C375.4 (5)Rh1—O1—C1—C2177.7 (6)
O1—Rh1—O2—C3100.1 (5)Rh1i—N1—C1—O10.3 (11)
O3—Rh1—O2—C3175.1 (5)Rh1i—N1—C1—C2176.4 (6)
Rh1i—Rh1—O2—C310.9 (5)Rh1i—N2—C3—O22.0 (11)
O3iii—W1—O3—Rh130.2 (6)Rh1i—N2—C3—C4179.3 (5)
O3iv—W1—O3—Rh187.9 (7)Rh1—O2—C3—N210.2 (10)
O3ii—W1—O3—Rh1151.1 (7)Rh1—O2—C3—C4171.0 (5)
N1i—Rh1—O3—W124.9 (6)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.473.174 (8)140
N2—H2···O2vi0.862.333.168 (8)165
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(IV) top
Crystal data top
C16H32CrN8O12Ru4Dx = 2.442 Mg m3
Mr = 984.78Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I41/aCell parameters from 3954 reflections
Hall symbol: -I 4adθ = 3.0–27.5°
a = 9.4232 (5) ŵ = 2.67 mm1
c = 30.168 (3) ÅT = 296 K
V = 2678.9 (3) Å3Block, brown
Z = 40.08 × 0.08 × 0.06 mm
F(000) = 1920
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1539 independent reflections
Radiation source: rotating-anode X-ray tube1475 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 4.0°
ω scansh = 1112
Absorption correction: integration
(Higashi, 1999)
k = 1112
Tmin = 0.833, Tmax = 0.871l = 3926
10957 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H-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 parametersΔρmax = 0.58 e Å3
0 restraintsΔρmin = 0.49 e Å3
Crystal data top
C16H32CrN8O12Ru4Z = 4
Mr = 984.78Mo Kα radiation
Tetragonal, I41/aµ = 2.67 mm1
a = 9.4232 (5) ÅT = 296 K
c = 30.168 (3) Å0.08 × 0.08 × 0.06 mm
V = 2678.9 (3) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1539 independent reflections
Absorption correction: integration
(Higashi, 1999)
1475 reflections with I > 2σ(I)
Tmin = 0.833, Tmax = 0.871Rint = 0.042
10957 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.066H-atom parameters constrained
S = 1.33 w = 1/[σ2(Fo2) + (0.0172P)2 + 12.7943P]
where P = (Fo2 + 2Fc2)/3
1539 reflectionsΔρmax = 0.58 e Å3
95 parametersΔρmin = 0.49 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.37778 (3)0.25660 (3)0.168745 (9)0.01376 (10)
Cr10.00000.25000.12500.0181 (3)
N10.6206 (4)0.3996 (4)0.12358 (11)0.0178 (7)
H10.70040.43390.11480.021*
O10.3823 (3)0.4060 (3)0.11980 (9)0.0197 (6)
N20.6197 (4)0.3832 (4)0.22004 (10)0.0192 (7)
H20.69870.40690.23220.023*
O20.3820 (3)0.4137 (3)0.21617 (9)0.0209 (6)
O30.1409 (3)0.2678 (4)0.15736 (10)0.0294 (7)
C10.5040 (5)0.4513 (4)0.10698 (12)0.0191 (8)
C20.5045 (6)0.5629 (5)0.07182 (16)0.0341 (11)
H30.48110.52070.04380.051*
H40.59710.60510.07010.051*
H50.43580.63450.07900.051*
C30.5028 (5)0.4379 (4)0.23502 (12)0.0192 (8)
C40.5009 (6)0.5324 (6)0.27483 (14)0.0361 (12)
H60.45750.62130.26730.054*
H70.59640.54880.28470.054*
H80.44770.48790.29810.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01003 (17)0.01556 (18)0.01570 (15)0.00014 (12)0.00020 (11)0.00047 (11)
Cr10.0143 (4)0.0143 (4)0.0256 (6)0.0000.0000.000
N10.0126 (17)0.0202 (18)0.0205 (15)0.0044 (14)0.0027 (13)0.0008 (13)
O10.0158 (15)0.0220 (16)0.0213 (14)0.0003 (12)0.0001 (11)0.0059 (11)
N20.0149 (18)0.0215 (19)0.0211 (17)0.0020 (15)0.0042 (13)0.0060 (13)
O20.0199 (15)0.0224 (16)0.0205 (14)0.0025 (12)0.0004 (11)0.0047 (11)
O30.0090 (15)0.042 (2)0.0368 (16)0.0006 (14)0.0018 (12)0.0023 (15)
C10.024 (2)0.017 (2)0.0165 (17)0.0008 (17)0.0021 (16)0.0010 (15)
C20.031 (3)0.029 (3)0.042 (3)0.001 (2)0.002 (2)0.019 (2)
C30.026 (2)0.014 (2)0.0168 (18)0.0002 (18)0.0004 (16)0.0005 (14)
C40.046 (3)0.037 (3)0.025 (2)0.006 (2)0.003 (2)0.016 (2)
Geometric parameters (Å, º) top
Ru1—N1i2.006 (3)N2—Ru1i2.032 (3)
Ru1—N2i2.033 (3)N2—H20.8600
Ru1—O12.041 (3)O2—C31.293 (5)
Ru1—O22.059 (3)C1—C21.493 (6)
Ru1—O32.261 (3)C2—H30.9600
Ru1—Ru1i2.3068 (6)C2—H40.9600
Cr1—O31.657 (3)C2—H50.9600
N1—C11.302 (5)C3—C41.495 (6)
N1—Ru1i2.006 (3)C4—H60.9600
N1—H10.8600C4—H70.9600
O1—C11.283 (5)C4—H80.9600
N2—C31.298 (5)
N1i—Ru1—N2i92.38 (14)C1—O1—Ru1117.8 (3)
N1i—Ru1—O190.84 (13)C3—N2—Ru1i122.2 (3)
N2i—Ru1—O1176.27 (13)C3—N2—H2118.9
N1i—Ru1—O2178.04 (13)Ru1i—N2—H2118.9
N2i—Ru1—O286.38 (13)C3—O2—Ru1116.7 (2)
O1—Ru1—O290.36 (12)Cr1—O3—Ru1151.18 (18)
N1i—Ru1—O386.48 (13)O1—C1—N1120.9 (4)
N2i—Ru1—O399.07 (13)O1—C1—C2116.8 (4)
O1—Ru1—O383.00 (12)N1—C1—C2122.3 (4)
O2—Ru1—O395.21 (12)C1—C2—H3109.5
N1i—Ru1—Ru1i87.30 (10)C1—C2—H4109.5
N2i—Ru1—Ru1i87.32 (10)H3—C2—H4109.5
O1—Ru1—Ru1i90.95 (8)C1—C2—H5109.5
O2—Ru1—Ru1i91.13 (8)H3—C2—H5109.5
O3—Ru1—Ru1i171.26 (8)H4—C2—H5109.5
O3ii—Cr1—O3107.8 (2)O2—C3—N2121.6 (3)
O3iii—Cr1—O3iv107.8 (2)O2—C3—C4116.6 (4)
O3iii—Cr1—O3ii110.32 (11)N2—C3—C4121.8 (4)
O3iv—Cr1—O3ii110.32 (11)C3—C4—H6109.5
O3iii—Cr1—O3110.32 (11)C3—C4—H7109.5
O3iv—Cr1—O3110.32 (11)H6—C4—H7109.5
C1—N1—Ru1i122.8 (3)C3—C4—H8109.5
C1—N1—H1118.6H6—C4—H8109.5
Ru1i—N1—H1118.6H7—C4—H8109.5
N1i—Ru1—O1—C191.7 (3)N2i—Ru1—O3—Cr1122.3 (4)
O2—Ru1—O1—C186.8 (3)O1—Ru1—O3—Cr160.8 (4)
O3—Ru1—O1—C1178.0 (3)O2—Ru1—O3—Cr1150.6 (4)
Ru1i—Ru1—O1—C14.3 (3)Ru1—O1—C1—N12.5 (5)
O1—Ru1—O2—C3101.3 (3)Ru1—O1—C1—C2178.7 (3)
O3—Ru1—O2—C3175.7 (3)Ru1i—N1—C1—O11.7 (5)
Ru1i—Ru1—O2—C310.4 (3)Ru1i—N1—C1—C2177.1 (3)
O3iii—Cr1—O3—Ru138.8 (5)Ru1—O2—C3—N210.9 (5)
O3iv—Cr1—O3—Ru180.2 (5)Ru1—O2—C3—C4169.3 (3)
O3ii—Cr1—O3—Ru1159.3 (5)Ru1i—N2—C3—O24.7 (6)
N1i—Ru1—O3—Cr130.4 (4)Ru1i—N2—C3—C4175.5 (3)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.353.046 (4)138
N2—H2···O2vi0.862.333.146 (4)159
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(V) top
Crystal data top
C16H32MoN8O12Ru4Dx = 2.503 Mg m3
Mr = 1028.72Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I41/aCell parameters from 2775 reflections
Hall symbol: -I 4adθ = 3.3–27.5°
a = 9.5504 (5) ŵ = 2.68 mm1
c = 29.933 (3) ÅT = 296 K
V = 2730.2 (3) Å3Prism, dark brown
Z = 40.30 × 0.10 × 0.10 mm
F(000) = 1992
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1568 independent reflections
Radiation source: rotating-anode X-ray tube1156 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.112
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = 127
Absorption correction: integration
(Higashi, 1999)
k = 1212
Tmin = 0.844, Tmax = 0.931l = 3738
10984 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.056Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-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 parametersΔρmax = 0.99 e Å3
0 restraintsΔρmin = 0.84 e Å3
Crystal data top
C16H32MoN8O12Ru4Z = 4
Mr = 1028.72Mo Kα radiation
Tetragonal, I41/aµ = 2.68 mm1
a = 9.5504 (5) ÅT = 296 K
c = 29.933 (3) Å0.30 × 0.10 × 0.10 mm
V = 2730.2 (3) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1568 independent reflections
Absorption correction: integration
(Higashi, 1999)
1156 reflections with I > 2σ(I)
Tmin = 0.844, Tmax = 0.931Rint = 0.112
10984 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0560 restraints
wR(F2) = 0.105H-atom parameters constrained
S = 1.02Δρmax = 0.99 e Å3
1568 reflectionsΔρmin = 0.84 e Å3
96 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.37996 (6)0.25615 (12)0.16978 (2)0.0232 (2)
Mo10.00000.25000.12500.0256 (4)
N10.6181 (9)0.3999 (9)0.1245 (3)0.025 (2)
H10.69680.43440.11580.030*
O10.3847 (8)0.4052 (7)0.1199 (3)0.029 (2)
N20.6181 (9)0.3819 (9)0.2209 (3)0.026 (2)
H20.69600.40370.23350.031*
O20.3830 (7)0.4111 (7)0.2169 (3)0.030 (2)
O30.1471 (5)0.2672 (9)0.1605 (2)0.0404 (19)
C10.5042 (15)0.4504 (7)0.1078 (3)0.0249 (18)
C20.5035 (16)0.5587 (9)0.0716 (3)0.045 (3)
H30.47540.51620.04390.068*
H40.59570.59740.06840.068*
H50.43890.63190.07920.068*
C30.5029 (15)0.4391 (7)0.2353 (3)0.0258 (19)
C40.5023 (17)0.5361 (9)0.2753 (3)0.046 (3)
H60.59660.55050.28540.070*
H70.44800.49500.29890.070*
H80.46190.62430.26690.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0153 (3)0.0226 (4)0.0317 (4)0.0006 (4)0.0002 (3)0.0008 (5)
Mo10.0174 (4)0.0174 (4)0.0420 (10)0.0000.0000.000
N10.012 (4)0.030 (5)0.033 (7)0.003 (4)0.008 (4)0.003 (4)
O10.022 (4)0.024 (4)0.039 (6)0.003 (3)0.000 (4)0.013 (4)
N20.022 (5)0.033 (5)0.023 (6)0.002 (4)0.007 (4)0.009 (4)
O20.019 (4)0.026 (4)0.043 (6)0.001 (3)0.005 (4)0.008 (4)
O30.006 (3)0.053 (5)0.063 (5)0.003 (3)0.000 (3)0.002 (5)
C10.030 (4)0.015 (4)0.029 (5)0.010 (6)0.004 (7)0.002 (3)
C20.047 (6)0.036 (5)0.053 (7)0.012 (7)0.004 (9)0.023 (5)
C30.033 (4)0.014 (4)0.030 (5)0.007 (6)0.006 (7)0.008 (3)
C40.060 (6)0.041 (5)0.038 (6)0.005 (8)0.015 (10)0.013 (5)
Geometric parameters (Å, º) top
Ru1—N1i2.015 (9)N2—Ru1i2.019 (9)
Ru1—N2i2.020 (9)N2—H20.8600
Ru1—O22.045 (7)O2—C31.299 (13)
Ru1—O12.063 (7)C1—C21.499 (10)
Ru1—O32.244 (5)C2—H30.9600
Ru1—Ru1i2.2958 (12)C2—H40.9600
Mo1—O31.769 (6)C2—H50.9600
N1—C11.290 (14)C3—C41.512 (11)
N1—Ru1i2.015 (9)C4—H60.9600
N1—H10.8600C4—H70.9600
O1—C11.272 (13)C4—H80.9600
N2—C31.302 (14)
N1i—Ru1—N2i91.5 (4)C1—O1—Ru1117.4 (6)
N1i—Ru1—O2178.1 (3)C3—N2—Ru1i122.2 (7)
N2i—Ru1—O287.1 (3)C3—N2—H2118.9
N1i—Ru1—O191.3 (2)Ru1i—N2—H2118.9
N2i—Ru1—O1176.6 (3)C3—O2—Ru1117.0 (6)
O2—Ru1—O190.0 (3)Mo1—O3—Ru1149.0 (4)
N1i—Ru1—O387.7 (3)O1—C1—N1121.3 (7)
N2i—Ru1—O397.7 (3)O1—C1—C2115.8 (12)
O2—Ru1—O393.8 (3)N1—C1—C2122.8 (12)
O1—Ru1—O384.2 (3)C1—C2—H3109.5
N1i—Ru1—Ru1i87.3 (2)C1—C2—H4109.5
N2i—Ru1—Ru1i87.6 (2)H3—C2—H4109.5
O2—Ru1—Ru1i91.3 (2)C1—C2—H5109.5
O1—Ru1—Ru1i90.8 (2)H3—C2—H5109.5
O3—Ru1—Ru1i172.86 (18)H4—C2—H5109.5
O3ii—Mo1—O3106.2 (4)O2—C3—N2121.2 (7)
O3ii—Mo1—O3iii111.1 (2)O2—C3—C4117.3 (12)
O3—Mo1—O3iii111.1 (2)N2—C3—C4121.5 (12)
O3ii—Mo1—O3iv111.1 (2)C3—C4—H6109.5
O3—Mo1—O3iv111.1 (2)C3—C4—H7109.5
O3iii—Mo1—O3iv106.2 (4)H6—C4—H7109.5
C1—N1—Ru1i123.0 (7)C3—C4—H8109.5
C1—N1—H1118.5H6—C4—H8109.5
Ru1i—N1—H1118.5H7—C4—H8109.5
N1i—Ru1—O1—C192.6 (7)N2i—Ru1—O3—Mo1124.2 (9)
O2—Ru1—O1—C186.0 (7)O2—Ru1—O3—Mo1148.3 (9)
O3—Ru1—O1—C1179.8 (7)O1—Ru1—O3—Mo158.7 (9)
Ru1i—Ru1—O1—C15.3 (6)Ru1—O1—C1—N13.4 (10)
N2i—Ru1—O2—C378.8 (7)Ru1—O1—C1—C2179.9 (6)
O1—Ru1—O2—C399.4 (6)Ru1i—N1—C1—O11.3 (11)
O3—Ru1—O2—C3176.4 (6)Ru1i—N1—C1—C2175.2 (7)
Ru1i—Ru1—O2—C38.7 (6)Ru1—O2—C3—N27.4 (10)
O3ii—Mo1—O3—Ru1161.6 (11)Ru1—O2—C3—C4170.3 (6)
O3iii—Mo1—O3—Ru140.6 (11)Ru1i—N2—C3—O21.0 (11)
O3iv—Mo1—O3—Ru177.4 (11)Ru1i—N2—C3—C4176.6 (6)
N1i—Ru1—O3—Mo132.9 (9)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.423.122 (8)140
N2—H2···O2vi0.862.323.154 (8)162
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(VI) top
Crystal data top
C16H32N8O12Ru4WDx = 2.703 Mg m3
Mr = 1116.63Mo Kα radiation, λ = 0.71070 Å
Tetragonal, I41/aCell parameters from 3975 reflections
Hall symbol: -I 4adθ = 3.3–27.5°
a = 9.5668 (7) ŵ = 6.40 mm1
c = 29.980 (3) ÅT = 296 K
V = 2743.9 (4) Å3Block, brown
Z = 40.06 × 0.06 × 0.04 mm
F(000) = 2120
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1580 independent reflections
Graphite monochromator1543 reflections with I > 2σ(I)
Detector resolution: 14.62 pixels mm-1Rint = 0.050
ω scansθmax = 27.5°, θmin = 3.3°
Absorption correction: integration
(Higashi, 1999)
h = 129
Tmin = 0.621, Tmax = 0.831k = 1211
10895 measured reflectionsl = 2538
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-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 parametersΔρmax = 0.64 e Å3
0 restraintsΔρmin = 0.80 e Å3
Crystal data top
C16H32N8O12Ru4WZ = 4
Mr = 1116.63Mo Kα radiation
Tetragonal, I41/aµ = 6.40 mm1
a = 9.5668 (7) ÅT = 296 K
c = 29.980 (3) Å0.06 × 0.06 × 0.04 mm
V = 2743.9 (4) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
1580 independent reflections
Absorption correction: integration
(Higashi, 1999)
1543 reflections with I > 2σ(I)
Tmin = 0.621, Tmax = 0.831Rint = 0.050
10895 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.069H-atom parameters constrained
S = 1.26 w = 1/[σ2(Fo2) + (0.0074P)2 + 37.8978P]
where P = (Fo2 + 2Fc2)/3
1580 reflectionsΔρmax = 0.64 e Å3
96 parametersΔρmin = 0.80 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.38025 (5)0.25719 (9)0.169932 (17)0.01477 (13)
W10.00000.25000.12500.01743 (13)
N10.6186 (9)0.3999 (9)0.1249 (2)0.0190 (18)
H10.69730.43500.11670.023*
O10.3841 (8)0.4045 (7)0.1206 (2)0.0216 (16)
N20.6175 (9)0.3831 (8)0.2217 (2)0.0195 (15)
H20.69520.40530.23430.023*
O20.3834 (8)0.4120 (7)0.2171 (2)0.0242 (15)
O30.1485 (5)0.2698 (8)0.16017 (19)0.0287 (15)
C10.5063 (12)0.4500 (6)0.1078 (2)0.0168 (13)
C20.5002 (16)0.5611 (8)0.0723 (3)0.039 (2)
H30.46580.52120.04510.059*
H40.59220.59830.06750.059*
H50.43880.63470.08180.059*
C30.5032 (14)0.4390 (6)0.2361 (2)0.0210 (13)
C40.5062 (18)0.5369 (8)0.2744 (3)0.0368 (19)
H60.45330.49820.29870.055*
H70.46610.62470.26570.055*
H80.60120.55110.28370.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0100 (2)0.0167 (3)0.0177 (3)0.0002 (3)0.00008 (18)0.0003 (4)
W10.01293 (16)0.01293 (16)0.0264 (3)0.0000.0000.000
N10.013 (4)0.021 (4)0.023 (5)0.000 (3)0.001 (3)0.004 (3)
O10.017 (3)0.023 (4)0.025 (4)0.001 (3)0.003 (3)0.010 (3)
N20.012 (3)0.026 (4)0.020 (4)0.003 (3)0.006 (3)0.006 (3)
O20.027 (3)0.027 (3)0.019 (3)0.004 (3)0.000 (3)0.001 (3)
O30.008 (2)0.038 (4)0.040 (3)0.001 (2)0.000 (2)0.003 (3)
C10.019 (3)0.014 (3)0.018 (3)0.003 (4)0.002 (5)0.004 (2)
C20.037 (4)0.036 (4)0.045 (5)0.006 (7)0.005 (8)0.024 (4)
C30.026 (3)0.017 (3)0.019 (3)0.003 (5)0.002 (6)0.001 (2)
C40.047 (5)0.038 (4)0.026 (4)0.007 (6)0.000 (7)0.017 (3)
Geometric parameters (Å, º) top
Ru1—N1i2.021 (8)N2—Ru1i2.053 (7)
Ru1—N2i2.053 (7)N2—H20.8600
Ru1—O12.043 (6)O2—C31.305 (14)
Ru1—O22.048 (7)C1—C21.505 (9)
Ru1—O32.239 (5)C2—H30.9600
Ru1—Ru1i2.2954 (9)C2—H40.9600
W1—O31.780 (5)C2—H50.9600
N1—C11.282 (14)C3—C41.483 (9)
N1—Ru1i2.021 (8)C4—H60.9600
N1—H10.8600C4—H70.9600
O1—C11.305 (13)C4—H80.9600
N2—C31.291 (14)
N1i—Ru1—O191.7 (2)C1—O1—Ru1117.3 (5)
N1i—Ru1—O2177.9 (3)C3—N2—Ru1i122.1 (6)
O1—Ru1—O290.0 (3)C3—N2—H2119.0
N1i—Ru1—N2i91.1 (3)Ru1i—N2—H2119.0
O1—Ru1—N2i176.7 (3)C3—O2—Ru1117.1 (6)
O2—Ru1—N2i87.1 (2)W1—O3—Ru1149.6 (3)
N1i—Ru1—O387.6 (3)N1—C1—O1120.6 (6)
O1—Ru1—O383.5 (3)N1—C1—C2125.3 (11)
O2—Ru1—O393.8 (3)O1—C1—C2114.1 (10)
N2i—Ru1—O398.3 (3)C1—C2—H3109.5
N1i—Ru1—Ru1i87.1 (2)C1—C2—H4109.5
O1—Ru1—Ru1i91.3 (2)H3—C2—H4109.5
O2—Ru1—Ru1i91.7 (2)C1—C2—H5109.5
N2i—Ru1—Ru1i87.2 (2)H3—C2—H5109.5
O3—Ru1—Ru1i172.48 (15)H4—C2—H5109.5
O3—W1—O3ii107.3 (4)N2—C3—O2121.2 (6)
O3iii—W1—O3iv107.3 (4)N2—C3—C4120.2 (11)
O3iii—W1—O3110.56 (18)O2—C3—C4118.6 (11)
O3iv—W1—O3110.56 (18)C3—C4—H6109.5
O3iii—W1—O3ii110.56 (18)C3—C4—H7109.5
O3iv—W1—O3ii110.56 (18)H6—C4—H7109.5
C1—N1—Ru1i123.3 (7)C3—C4—H8109.5
C1—N1—H1118.4H6—C4—H8109.5
Ru1i—N1—H1118.4H7—C4—H8109.5
N1i—Ru1—O1—C192.1 (6)O1—Ru1—O3—W161.2 (8)
O2—Ru1—O1—C186.7 (6)O2—Ru1—O3—W1150.8 (8)
O3—Ru1—O1—C1179.5 (6)N2i—Ru1—O3—W1121.6 (8)
Ru1i—Ru1—O1—C15.0 (6)Ru1i—N1—C1—O13.1 (9)
O1—Ru1—O2—C3100.5 (6)Ru1i—N1—C1—C2176.4 (6)
N2i—Ru1—O2—C377.9 (6)Ru1—O1—C1—N12.1 (8)
O3—Ru1—O2—C3176.0 (5)Ru1—O1—C1—C2178.4 (5)
Ru1i—Ru1—O2—C39.2 (5)Ru1i—N2—C3—O22.2 (10)
O3iii—W1—O3—Ru138.0 (9)Ru1i—N2—C3—C4178.3 (5)
O3iv—W1—O3—Ru180.7 (10)Ru1—O2—C3—N28.5 (9)
O3ii—W1—O3—Ru1158.7 (10)Ru1—O2—C3—C4172.1 (5)
N1i—Ru1—O3—W130.8 (8)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4; (iv) y+1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1v0.862.403.122 (7)141
N2—H2···O2vi0.862.323.147 (7)163
Symmetry codes: (v) y+5/4, x+1/4, z+1/4; (vi) x+1/2, y, z+1/2.
(VII) top
Crystal data top
C24H48CrN8O12Rh4·1.08(H2O)Z = 2
Mr = 1123.76F(000) = 1116
Triclinic, P1Dx = 1.758 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 12.978 (2) ÅCell parameters from 4246 reflections
b = 13.576 (3) Åθ = 3.1–27.5°
c = 14.498 (3) ŵ = 1.83 mm1
α = 112.405 (5)°T = 296 K
β = 101.362 (4)°Prism, brown
γ = 106.816 (5)°0.30 × 0.10 × 0.10 mm
V = 2120.1 (8) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
9650 independent reflections
Graphite monochromator6828 reflections with I > 2σ(I)
Detector resolution: 14.62 pixels mm-1Rint = 0.065
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: integration
(Higashi, 1999)
h = 1616
Tmin = 0.843, Tmax = 0.945k = 1617
17505 measured reflectionsl = 1813
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.089Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H-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 parametersΔρmax = 0.88 e Å3
394 restraintsΔρmin = 0.93 e Å3
Crystal data top
C24H48CrN8O12Rh4·1.08(H2O)γ = 106.816 (5)°
Mr = 1123.76V = 2120.1 (8) Å3
Triclinic, P1Z = 2
a = 12.978 (2) ÅMo Kα radiation
b = 13.576 (3) ŵ = 1.83 mm1
c = 14.498 (3) ÅT = 296 K
α = 112.405 (5)°0.30 × 0.10 × 0.10 mm
β = 101.362 (4)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
9650 independent reflections
Absorption correction: integration
(Higashi, 1999)
6828 reflections with I > 2σ(I)
Tmin = 0.843, Tmax = 0.945Rint = 0.065
17505 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.089394 restraints
wR(F2) = 0.133H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.P)2 + 19.3981P]
where P = (Fo2 + 2Fc2)/3
9650 reflectionsΔρmax = 0.88 e Å3
588 parametersΔρmin = 0.93 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Rh10.90911 (6)0.43100 (6)0.48748 (6)0.01574 (17)
Rh20.53889 (6)0.44323 (6)0.44196 (6)0.01450 (17)
Rh30.50903 (6)0.05012 (6)0.44729 (6)0.01919 (18)
Rh40.56458 (6)0.05915 (7)0.09075 (6)0.0230 (2)
N10.9308 (6)0.3172 (7)0.3670 (7)0.032 (2)
H10.88080.24640.33370.039*
O11.1015 (5)0.4457 (6)0.3861 (5)0.0312 (18)
N20.8427 (6)0.4852 (7)0.3932 (7)0.029 (2)
H20.76910.45650.36620.035*
O21.0107 (5)0.6132 (7)0.4103 (6)0.042 (2)
N30.6313 (6)0.4490 (6)0.5726 (6)0.0205 (18)
H30.67720.41410.56670.025*
O30.5550 (5)0.5493 (5)0.6828 (5)0.0210 (15)
N40.4072 (6)0.3062 (6)0.4161 (6)0.0216 (18)
H40.40270.23860.37480.026*
O40.3329 (5)0.4074 (5)0.5260 (5)0.0210 (15)
N50.4804 (6)0.1701 (6)0.5566 (6)0.0226 (18)
H50.47980.22970.54890.027*
O50.4655 (5)0.0813 (6)0.6600 (5)0.0251 (16)
N60.6741 (6)0.1250 (6)0.5316 (6)0.0183 (17)
H60.71820.17210.51580.022*
O60.6629 (5)0.0369 (6)0.6365 (5)0.0258 (16)
N70.4821 (7)0.1631 (7)0.1004 (6)0.032 (2)
H70.50470.22510.15970.038*
O70.3547 (6)0.0515 (6)0.0683 (5)0.0345 (19)
N80.4510 (7)0.0406 (7)0.1252 (7)0.037 (2)
H80.46660.02820.19010.045*
O80.3234 (6)0.1515 (6)0.0456 (5)0.036 (2)
Cr10.63841 (11)0.23545 (12)0.35111 (11)0.0143 (3)
O90.7442 (5)0.3007 (5)0.4669 (5)0.0165 (14)
O100.6020 (5)0.3353 (5)0.3297 (4)0.0155 (13)
O110.5248 (5)0.1421 (5)0.3528 (5)0.0186 (14)
O120.6823 (5)0.1681 (5)0.2567 (5)0.0207 (15)
O130.7441 (12)0.0304 (13)0.2723 (13)0.056 (7)0.55 (2)
O140.9443 (17)0.1153 (18)0.4449 (18)0.094 (11)0.53 (3)
C11.0184 (8)0.3451 (9)0.3358 (8)0.035 (3)
C2A1.024 (2)0.273 (2)0.2267 (17)0.027 (7)0.51 (6)
H9A1.01280.31050.18300.032*0.51 (6)
H10A1.10040.27350.23740.032*0.51 (6)
C3A0.939 (2)0.150 (2)0.167 (2)0.032 (6)0.51 (6)
H11A0.94050.11420.21290.047*0.51 (6)
H12A0.95910.10810.10760.047*0.51 (6)
H13A0.86400.14690.14140.047*0.51 (6)
C2B1.031 (2)0.247 (2)0.247 (2)0.026 (7)0.49 (6)
H9B1.02570.26240.18720.031*0.49 (6)
H101.10860.25170.27300.031*0.49 (6)
C3B0.951 (3)0.124 (2)0.207 (3)0.052 (10)0.49 (6)
H11B0.97070.09740.25790.079*0.49 (6)
H12B0.95590.07520.14080.079*0.49 (6)
H13B0.87370.11890.19530.079*0.49 (6)
C40.8988 (9)0.5597 (11)0.3677 (10)0.048 (3)
C5A0.8450 (15)0.579 (2)0.2769 (16)0.069 (7)0.820 (19)
H14A0.86100.66080.30420.083*0.820 (19)
H15A0.88240.55900.22490.083*0.820 (19)
C6A0.7181 (11)0.5109 (16)0.2210 (14)0.070 (6)0.820 (19)
H16A0.70090.42920.19110.105*0.820 (19)
H17A0.69260.52930.16530.105*0.820 (19)
H18A0.67940.53090.27090.105*0.820 (19)
C5B0.838 (8)0.619 (7)0.322 (5)0.042 (11)0.180 (19)
H14B0.76030.60070.32380.051*0.180 (19)
H15B0.88020.70310.35750.051*0.180 (19)
C6B0.840 (6)0.562 (6)0.212 (5)0.048 (13)0.180 (19)
H16B0.83940.61190.17960.072*0.180 (19)
H17B0.77390.48950.16970.072*0.180 (19)
H18B0.90840.54700.21480.072*0.180 (19)
C70.6260 (8)0.5024 (8)0.6660 (7)0.020 (2)
C80.7040 (8)0.5119 (9)0.7649 (7)0.026 (2)
H190.65860.49790.80790.032*
H200.76180.59100.80620.032*
C90.7651 (9)0.4285 (10)0.7446 (8)0.033 (3)
H210.70900.34960.70500.050*
H220.81140.44010.81140.050*
H230.81320.44350.70480.050*
C100.3270 (7)0.3103 (8)0.4566 (8)0.022 (2)
C110.2268 (8)0.2021 (9)0.4277 (9)0.045 (3)
H24A0.25350.14080.42070.054*0.513 (18)
H25A0.17280.17820.35870.054*0.513 (18)
H24B0.16420.22310.44230.054*0.487 (18)
H25B0.24820.16890.47310.054*0.487 (18)
C12A0.1629 (16)0.2140 (17)0.5080 (16)0.037 (6)0.513 (18)
H26A0.21770.25740.57910.055*0.513 (18)
H27A0.11650.13800.49630.055*0.513 (18)
H28A0.11470.25390.49860.055*0.513 (18)
C12B0.1832 (16)0.1083 (16)0.3108 (16)0.037 (6)0.487 (18)
H26B0.18220.14440.26540.056*0.487 (18)
H27B0.10700.05380.29290.056*0.487 (18)
H28B0.23330.06810.30130.056*0.487 (18)
C130.4623 (8)0.1632 (8)0.6399 (8)0.023 (2)
C140.4364 (10)0.2569 (10)0.7208 (9)0.040 (3)
H29A0.44850.32090.70380.048*0.611 (19)
H30A0.35590.22410.71190.048*0.611 (19)
H29B0.49780.29930.78940.048*0.389 (19)
H30B0.42600.31140.69580.048*0.389 (19)
C15A0.508 (2)0.306 (2)0.8378 (15)0.070 (8)0.611 (19)
H31A0.49340.37090.88060.105*0.611 (19)
H32A0.58760.33040.84660.105*0.611 (19)
H33A0.48620.24650.85950.105*0.611 (19)
C15B0.324 (2)0.186 (2)0.728 (3)0.047 (8)0.389 (19)
H31B0.26130.16150.66530.070*0.389 (19)
H32B0.31220.23400.78960.070*0.389 (19)
H33B0.33000.11940.73280.070*0.389 (19)
C160.7218 (7)0.1087 (8)0.6096 (7)0.019 (2)
C170.8469 (8)0.1746 (10)0.6714 (8)0.033 (3)
H34A0.86540.16830.73650.040*0.57 (2)
H35A0.86930.25620.68980.040*0.57 (2)
H34B0.85550.23640.73840.040*0.43 (2)
H35B0.88070.21160.63280.040*0.43 (2)
C18A0.9106 (16)0.1202 (19)0.599 (2)0.060 (8)0.57 (2)
H36A0.98830.14340.64200.091*0.57 (2)
H37A0.91060.14670.54660.091*0.57 (2)
H38A0.87220.03690.56450.091*0.57 (2)
C18B0.9183 (19)0.111 (2)0.697 (2)0.050 (10)0.43 (2)
H36B0.88600.07230.73400.076*0.43 (2)
H37B0.99560.16640.74090.076*0.43 (2)
H38B0.91860.05520.63200.076*0.43 (2)
C190.3968 (9)0.1434 (9)0.0235 (9)0.038 (3)
C20A0.350 (3)0.234 (3)0.033 (5)0.055 (11)0.52 (6)
H39A0.37760.29180.10670.066*0.52 (6)
H40A0.37840.27290.00670.066*0.52 (6)
C21A0.221 (3)0.186 (4)0.008 (5)0.10 (2)0.52 (6)
H41A0.19070.10410.03110.149*0.52 (6)
H42A0.19550.19980.06740.149*0.52 (6)
H43A0.19490.22400.04710.149*0.52 (6)
C20B0.326 (3)0.214 (3)0.044 (5)0.042 (8)0.48 (6)
H39B0.37340.28970.10570.051*0.48 (6)
H40B0.30350.22760.01650.051*0.48 (6)
C21B0.222 (4)0.157 (3)0.063 (6)0.099 (19)0.48 (6)
H41B0.17310.08450.00140.149*0.48 (6)
H42B0.18100.20690.07810.149*0.48 (6)
H43B0.24400.14350.12300.149*0.48 (6)
C220.3524 (9)0.1252 (9)0.0542 (8)0.036 (3)
C23A0.257 (3)0.174 (3)0.092 (3)0.047 (10)0.40 (2)
H44A0.20390.13590.09120.056*0.40 (2)
H45A0.28850.16250.16320.056*0.40 (2)
C23B0.286 (3)0.211 (5)0.087 (5)0.046 (9)0.37 (3)
H44B0.30520.17480.16360.056*0.37 (3)
H45B0.30550.27850.06560.056*0.37 (3)
C23C0.265 (6)0.197 (10)0.085 (11)0.042 (10)0.23 (3)
H44C0.29830.18160.15750.050*0.23 (3)
H45C0.23890.27920.03800.050*0.23 (3)
C24A0.195 (3)0.308 (2)0.008 (2)0.044 (7)0.40 (2)
H46A0.24880.34390.01070.065*0.40 (2)
H47A0.16620.31720.06180.065*0.40 (2)
H48A0.13230.34520.02610.065*0.40 (2)
C24B0.153 (3)0.249 (4)0.029 (3)0.066 (11)0.37 (3)
H46B0.14210.18470.02150.098*0.37 (3)
H47B0.11030.27030.06960.098*0.37 (3)
H48B0.12770.31380.04080.098*0.37 (3)
C24C0.160 (4)0.158 (6)0.074 (5)0.058 (13)0.23 (3)
H46C0.18840.07480.11600.087*0.23 (3)
H47C0.10550.19550.09830.087*0.23 (3)
H48C0.12420.17900.00060.087*0.23 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0116 (3)0.0149 (4)0.0192 (4)0.0032 (3)0.0050 (3)0.0083 (3)
Rh20.0154 (3)0.0142 (4)0.0152 (4)0.0070 (3)0.0069 (3)0.0066 (3)
Rh30.0164 (4)0.0183 (4)0.0217 (4)0.0025 (3)0.0032 (3)0.0131 (3)
Rh40.0212 (4)0.0181 (4)0.0162 (4)0.0019 (3)0.0070 (3)0.0007 (3)
N10.013 (4)0.011 (4)0.051 (6)0.004 (3)0.010 (4)0.000 (4)
O10.013 (3)0.035 (4)0.023 (4)0.002 (3)0.006 (3)0.003 (3)
N20.010 (4)0.040 (5)0.040 (5)0.002 (4)0.008 (4)0.027 (5)
O20.017 (4)0.056 (5)0.060 (5)0.000 (3)0.004 (4)0.049 (5)
N30.024 (4)0.026 (4)0.018 (4)0.020 (4)0.009 (3)0.008 (4)
O30.027 (3)0.027 (4)0.013 (3)0.015 (3)0.007 (3)0.010 (3)
N40.019 (4)0.014 (4)0.026 (4)0.008 (3)0.012 (3)0.001 (3)
O40.019 (3)0.023 (4)0.028 (4)0.011 (3)0.015 (3)0.013 (3)
N50.027 (4)0.018 (4)0.034 (5)0.015 (4)0.013 (4)0.018 (4)
O50.032 (4)0.023 (4)0.024 (4)0.007 (3)0.012 (3)0.016 (3)
N60.010 (3)0.020 (4)0.021 (4)0.001 (3)0.003 (3)0.013 (3)
O60.023 (3)0.028 (4)0.028 (4)0.008 (3)0.004 (3)0.019 (3)
N70.026 (4)0.029 (5)0.018 (4)0.007 (4)0.005 (4)0.003 (4)
O70.030 (4)0.033 (4)0.018 (4)0.008 (3)0.004 (3)0.004 (3)
N80.037 (5)0.031 (5)0.018 (5)0.004 (4)0.003 (4)0.003 (4)
O80.029 (4)0.031 (4)0.018 (4)0.009 (3)0.007 (3)0.003 (3)
Cr10.0130 (7)0.0121 (7)0.0153 (7)0.0037 (6)0.0052 (6)0.0048 (6)
O90.011 (3)0.019 (3)0.020 (3)0.004 (3)0.007 (3)0.010 (3)
O100.015 (3)0.014 (3)0.014 (3)0.005 (2)0.004 (2)0.003 (3)
O110.016 (3)0.017 (3)0.020 (3)0.005 (3)0.005 (3)0.009 (3)
O120.018 (3)0.015 (3)0.020 (3)0.009 (3)0.007 (3)0.002 (3)
O130.042 (10)0.057 (11)0.079 (14)0.020 (8)0.028 (9)0.038 (10)
O140.093 (17)0.086 (17)0.11 (2)0.037 (13)0.018 (14)0.059 (15)
C10.015 (5)0.029 (5)0.028 (6)0.000 (4)0.003 (4)0.009 (4)
C2A0.021 (10)0.029 (10)0.031 (11)0.015 (8)0.010 (9)0.010 (8)
C3A0.030 (7)0.031 (6)0.031 (7)0.017 (5)0.016 (5)0.007 (4)
C2B0.025 (11)0.022 (10)0.009 (10)0.004 (9)0.006 (8)0.003 (8)
C3B0.056 (17)0.023 (9)0.05 (2)0.005 (11)0.010 (15)0.000 (12)
C40.025 (6)0.064 (8)0.065 (8)0.010 (5)0.002 (5)0.051 (7)
C5A0.028 (7)0.099 (14)0.089 (15)0.003 (9)0.002 (10)0.085 (13)
C6A0.028 (7)0.112 (15)0.087 (13)0.011 (8)0.003 (7)0.086 (12)
C5B0.031 (18)0.048 (18)0.063 (18)0.012 (14)0.009 (15)0.047 (15)
C6B0.03 (2)0.06 (2)0.058 (16)0.003 (18)0.002 (17)0.047 (18)
C70.023 (5)0.020 (5)0.014 (5)0.006 (4)0.004 (4)0.007 (4)
C80.033 (5)0.042 (6)0.020 (5)0.025 (5)0.011 (4)0.022 (5)
C90.039 (6)0.048 (7)0.022 (5)0.025 (5)0.011 (5)0.020 (5)
C100.015 (4)0.021 (5)0.031 (6)0.009 (4)0.011 (4)0.012 (4)
C110.022 (5)0.016 (5)0.071 (8)0.005 (4)0.017 (5)0.004 (5)
C12A0.024 (10)0.029 (12)0.049 (13)0.003 (8)0.006 (9)0.025 (10)
C12B0.019 (10)0.018 (9)0.066 (12)0.007 (8)0.002 (10)0.017 (8)
C130.022 (5)0.017 (5)0.035 (5)0.011 (4)0.012 (4)0.015 (4)
C140.057 (7)0.042 (7)0.045 (6)0.034 (6)0.034 (6)0.026 (5)
C15A0.11 (2)0.065 (16)0.038 (8)0.043 (15)0.035 (11)0.022 (10)
C15B0.066 (15)0.037 (15)0.068 (19)0.043 (11)0.049 (14)0.025 (13)
C160.016 (4)0.018 (5)0.017 (5)0.003 (4)0.002 (4)0.007 (4)
C170.022 (5)0.044 (7)0.028 (6)0.001 (4)0.001 (4)0.025 (5)
C18A0.026 (9)0.060 (15)0.10 (2)0.020 (10)0.026 (11)0.041 (14)
C18B0.029 (11)0.028 (13)0.06 (2)0.009 (10)0.027 (13)0.024 (14)
C190.039 (6)0.025 (6)0.033 (6)0.012 (5)0.007 (5)0.001 (5)
C20A0.062 (14)0.035 (13)0.032 (18)0.028 (12)0.009 (15)0.011 (12)
C21A0.065 (14)0.07 (2)0.11 (3)0.044 (15)0.00 (2)0.01 (2)
C20B0.046 (13)0.044 (14)0.019 (13)0.027 (10)0.010 (10)0.008 (11)
C21B0.069 (19)0.06 (2)0.15 (4)0.032 (16)0.07 (2)0.02 (2)
C220.035 (6)0.033 (6)0.025 (6)0.000 (5)0.014 (5)0.006 (5)
C23A0.029 (13)0.046 (12)0.043 (14)0.004 (13)0.016 (11)0.013 (11)
C23B0.049 (13)0.039 (16)0.025 (13)0.005 (14)0.028 (13)0.001 (12)
C23C0.038 (16)0.036 (18)0.033 (17)0.001 (13)0.022 (15)0.005 (15)
C24A0.045 (8)0.043 (7)0.042 (8)0.008 (4)0.018 (5)0.024 (5)
C24B0.050 (11)0.060 (18)0.057 (16)0.001 (10)0.031 (12)0.009 (13)
C24C0.043 (13)0.06 (2)0.06 (2)0.012 (14)0.031 (15)0.026 (15)
Geometric parameters (Å, º) top
Rh1—N11.976 (8)C8—C91.534 (13)
Rh1—N21.956 (8)C8—H190.9700
Rh1—O1i2.019 (7)C8—H200.9700
Rh1—O2i2.017 (7)C9—H210.9600
Rh1—O92.226 (5)C9—H220.9600
Rh1—Rh1i2.4071 (14)C9—H230.9600
Rh2—N31.992 (7)C10—C111.495 (12)
Rh2—N41.975 (7)C11—C12B1.541 (18)
Rh2—O3ii2.027 (6)C11—C12A1.545 (18)
Rh2—O4ii2.030 (6)C11—H24A0.9700
Rh2—O102.207 (6)C11—H25A0.9700
Rh2—Rh2ii2.4122 (15)C11—H24B0.9700
Rh3—N51.980 (8)C11—H25B0.9700
Rh3—N61.969 (6)C12A—H26A0.9600
Rh3—O5iii2.034 (7)C12A—H27A0.9600
Rh3—O6iii2.040 (6)C12A—H28A0.9600
Rh3—O112.179 (6)C12B—H26B0.9600
Rh3—Rh3iii2.4053 (15)C12B—H27B0.9600
Rh4—N71.985 (9)C12B—H28B0.9600
Rh4—N81.977 (9)C13—C141.540 (14)
Rh4—O7iv2.033 (7)C14—C15A1.530 (19)
Rh4—O8iv2.016 (7)C14—C15B1.54 (2)
Rh4—O122.201 (6)C14—H29A0.9700
Rh4—Rh4iv2.4076 (15)C14—H30A0.9700
N1—C11.313 (12)C14—H29B0.9700
N1—H10.8600C14—H30B0.9700
O1—C11.280 (11)C15A—H31A0.9600
N2—C41.286 (13)C15A—H32A0.9600
N2—H20.8600C15A—H33A0.9600
O2—C41.309 (12)C15B—H31B0.9600
N3—C71.296 (11)C15B—H32B0.9600
N3—H30.8600C15B—H33B0.9600
O3—C71.275 (11)C16—C171.488 (12)
N4—C101.297 (11)C17—C18B1.52 (2)
N4—H40.8600C17—C18A1.56 (2)
O4—C101.286 (11)C17—H34A0.9700
N5—C131.306 (12)C17—H35A0.9700
N5—H50.8600C17—H34B0.9700
O5—C131.262 (11)C17—H35B0.9700
N6—C161.306 (11)C18A—H36A0.9600
N6—H60.8600C18A—H37A0.9600
O6—C161.290 (11)C18A—H38A0.9600
N7—C191.286 (13)C18B—H36B0.9600
N7—H70.8600C18B—H37B0.9600
O7—C191.296 (11)C18B—H38B0.9600
N8—C221.322 (12)C19—C20B1.50 (2)
N8—H80.8600C19—C20A1.50 (2)
O8—C221.294 (12)C20A—C21A1.50 (3)
Cr1—O121.639 (6)C20A—H39A0.9700
Cr1—O111.654 (6)C20A—H40A0.9700
Cr1—O91.656 (6)C21A—H41A0.9600
Cr1—O101.670 (6)C21A—H42A0.9600
C1—C2B1.540 (18)C21A—H43A0.9600
C1—C2A1.541 (18)C20B—C21B1.49 (3)
C2A—C3A1.485 (19)C20B—H39B0.9700
C2A—H9A0.9700C20B—H40B0.9700
C2A—H10A0.9700C21B—H41B0.9600
C3A—H11A0.9600C21B—H42B0.9600
C3A—H12A0.9600C21B—H43B0.9600
C3A—H13A0.9600C22—C23C1.53 (2)
C2B—C3B1.49 (2)C22—C23B1.53 (2)
C2B—H9B0.9700C22—C23A1.526 (19)
C2B—H100.9700C23A—C24A1.59 (4)
C3B—H11B0.9600C23A—H44A0.9700
C3B—H12B0.9600C23A—H45A0.9700
C3B—H13B0.9600C23B—C24B1.59 (4)
C4—C5A1.511 (16)C23B—H44B0.9700
C4—C5B1.51 (2)C23B—H45B0.9700
C5A—C6A1.50 (2)C23C—C24C1.59 (4)
C5A—H14A0.9700C23C—H44C0.9700
C5A—H15A0.9700C23C—H45C0.9700
C6A—H16A0.9600C24A—H46A0.9600
C6A—H17A0.9600C24A—H47A0.9600
C6A—H18A0.9600C24A—H48A0.9600
C5B—C6B1.51 (3)C24B—H46B0.9600
C5B—H14B0.9700C24B—H47B0.9600
C5B—H15B0.9700C24B—H48B0.9600
C6B—H16B0.9600C24C—H46C0.9600
C6B—H17B0.9600C24C—H47C0.9600
C6B—H18B0.9600C24C—H48C0.9600
C7—C81.521 (12)
N2—Rh1—N189.6 (4)C9—C8—H19108.4
N2—Rh1—O2i175.4 (3)C7—C8—H20108.4
N1—Rh1—O2i91.5 (4)C9—C8—H20108.4
N2—Rh1—O1i91.1 (3)H19—C8—H20107.5
N1—Rh1—O1i176.1 (3)C8—C9—H21109.5
O2i—Rh1—O1i87.5 (3)C8—C9—H22109.5
N2—Rh1—O996.6 (3)H21—C9—H22109.5
N1—Rh1—O993.0 (3)C8—C9—H23109.5
O2i—Rh1—O987.8 (2)H21—C9—H23109.5
O1i—Rh1—O990.8 (2)H22—C9—H23109.5
N2—Rh1—Rh1i85.3 (2)O4—C10—N4121.1 (8)
N1—Rh1—Rh1i86.5 (2)O4—C10—C11117.6 (8)
O2i—Rh1—Rh1i90.29 (18)N4—C10—C11121.2 (9)
O1i—Rh1—Rh1i89.67 (18)C10—C11—C12B114.8 (11)
O9—Rh1—Rh1i178.04 (17)C10—C11—C12A114.8 (10)
N4—Rh2—N392.0 (3)C12B—C11—C12A128.0 (12)
N4—Rh2—O3ii90.0 (3)C10—C11—H24A108.6
N3—Rh2—O3ii175.1 (3)C12A—C11—H24A108.6
N4—Rh2—O4ii175.1 (3)C10—C11—H25A108.6
N3—Rh2—O4ii88.8 (3)C12A—C11—H25A108.6
O3ii—Rh2—O4ii88.8 (3)H24A—C11—H25A107.5
N4—Rh2—O1092.6 (3)C10—C11—H24B108.6
N3—Rh2—O1097.0 (3)C12B—C11—H24B108.6
O3ii—Rh2—O1087.3 (2)C10—C11—H25B108.6
O4ii—Rh2—O1092.1 (2)C12B—C11—H25B108.6
N4—Rh2—Rh2ii85.8 (2)H24B—C11—H25B107.6
N3—Rh2—Rh2ii85.2 (2)C11—C12A—H26A109.5
O3ii—Rh2—Rh2ii90.50 (18)C11—C12A—H27A109.5
O4ii—Rh2—Rh2ii89.47 (18)H26A—C12A—H27A109.5
O10—Rh2—Rh2ii177.28 (15)C11—C12A—H28A109.5
N6—Rh3—N590.8 (3)H26A—C12A—H28A109.5
N6—Rh3—O5iii89.8 (3)H27A—C12A—H28A109.5
N5—Rh3—O5iii175.6 (3)C11—C12B—H26B109.5
N6—Rh3—O6iii175.7 (3)C11—C12B—H27B109.5
N5—Rh3—O6iii90.3 (3)H26B—C12B—H27B109.5
O5iii—Rh3—O6iii88.7 (3)C11—C12B—H28B109.5
N6—Rh3—O1194.3 (3)H26B—C12B—H28B109.5
N5—Rh3—O1193.3 (3)H27B—C12B—H28B109.5
O5iii—Rh3—O1191.0 (2)O5—C13—N5123.0 (9)
O6iii—Rh3—O1189.8 (2)O5—C13—C14115.8 (9)
N6—Rh3—Rh3iii85.8 (2)N5—C13—C14121.2 (9)
N5—Rh3—Rh3iii86.2 (2)C15A—C14—C13115.9 (12)
O5iii—Rh3—Rh3iii89.51 (19)C15B—C14—C13103.5 (13)
O6iii—Rh3—Rh3iii90.12 (19)C15A—C14—H29A108.3
O11—Rh3—Rh3iii179.44 (18)C13—C14—H29A108.3
N8—Rh4—N791.9 (4)C15A—C14—H30A108.3
N8—Rh4—O8iv176.1 (3)C13—C14—H30A108.3
N7—Rh4—O8iv89.7 (3)H29A—C14—H30A107.4
N8—Rh4—O7iv89.8 (4)C15B—C14—H29B111.1
N7—Rh4—O7iv175.5 (3)C13—C14—H29B111.1
O8iv—Rh4—O7iv88.4 (3)C15B—C14—H30B111.1
N8—Rh4—O1294.1 (3)C13—C14—H30B111.1
N7—Rh4—O1293.7 (3)H30A—C14—H30B92.3
O8iv—Rh4—O1289.4 (2)H29B—C14—H30B109.0
O7iv—Rh4—O1290.4 (2)C14—C15A—H31A109.5
N8—Rh4—Rh4iv85.9 (2)C14—C15A—H32A109.5
N7—Rh4—Rh4iv85.9 (2)H31A—C15A—H32A109.5
O8iv—Rh4—Rh4iv90.58 (19)C14—C15A—H33A109.5
O7iv—Rh4—Rh4iv89.97 (18)H31A—C15A—H33A109.5
O12—Rh4—Rh4iv179.67 (18)H32A—C15A—H33A109.5
C1—N1—Rh1122.7 (6)C14—C15B—H31B109.5
C1—N1—H1118.6C14—C15B—H32B109.5
Rh1—N1—H1118.6H31B—C15B—H32B109.5
C1—O1—Rh1i118.1 (6)C14—C15B—H33B109.5
C4—N2—Rh1126.2 (7)H31B—C15B—H33B109.5
C4—N2—H2116.9H32B—C15B—H33B109.5
Rh1—N2—H2116.9O6—C16—N6121.7 (8)
C4—O2—Rh1i117.2 (7)O6—C16—C17117.9 (8)
C7—N3—Rh2123.6 (6)N6—C16—C17120.4 (8)
C7—N3—H3118.2C16—C17—C18B119.7 (12)
Rh2—N3—H3118.2C16—C17—C18A106.9 (11)
C7—O3—Rh2ii116.6 (6)C16—C17—H34A110.3
C10—N4—Rh2124.9 (6)C18A—C17—H34A110.3
C10—N4—H4117.5C16—C17—H35A110.3
Rh2—N4—H4117.5C18A—C17—H35A110.3
C10—O4—Rh2ii118.4 (6)H34A—C17—H35A108.6
C13—N5—Rh3123.2 (7)C16—C17—H34B107.4
C13—N5—H5118.4C18B—C17—H34B107.4
Rh3—N5—H5118.4C16—C17—H35B107.4
C13—O5—Rh3iii118.0 (6)C18B—C17—H35B107.4
C16—N6—Rh3125.0 (6)H34B—C17—H35B106.9
C16—N6—H6117.5C17—C18A—H36A109.5
Rh3—N6—H6117.5C17—C18A—H37A109.5
C16—O6—Rh3iii117.3 (6)H36A—C18A—H37A109.5
C19—N7—Rh4124.0 (7)C17—C18A—H38A109.5
C19—N7—H7118.0H36A—C18A—H38A109.5
Rh4—N7—H7118.0H37A—C18A—H38A109.5
C19—O7—Rh4iv117.1 (7)C17—C18B—H36B109.5
C22—N8—Rh4123.7 (8)C17—C18B—H37B109.5
C22—N8—H8118.1H36B—C18B—H37B109.5
Rh4—N8—H8118.1C17—C18B—H38B109.5
C22—O8—Rh4iv117.6 (6)H36B—C18B—H38B109.5
O9—Cr1—O10109.2 (3)H37B—C18B—H38B109.5
O11—Cr1—O9110.1 (3)N7—C19—O7122.8 (10)
O12—Cr1—O9108.9 (3)N7—C19—C20B120 (2)
O11—Cr1—O10108.4 (3)O7—C19—C20B116 (2)
O12—Cr1—O10109.8 (3)N7—C19—C20A121 (2)
O12—Cr1—O11110.4 (3)O7—C19—C20A116 (2)
Cr1—O9—Rh1118.1 (3)C21A—C20A—C19114 (2)
Cr1—O10—Rh2119.7 (3)C21A—C20A—H39A108.8
Cr1—O11—Rh3131.4 (3)C19—C20A—H39A108.8
Cr1—O12—Rh4121.1 (3)C21A—C20A—H40A108.8
O1—C1—N1122.8 (9)C19—C20A—H40A108.8
O1—C1—C2B118.5 (13)H39A—C20A—H40A107.7
N1—C1—C2B117.8 (14)C20A—C21A—H41A109.5
O1—C1—C2A111.4 (13)C20A—C21A—H42A109.5
N1—C1—C2A124.9 (12)H41A—C21A—H42A109.5
C3A—C2A—C1115.9 (18)C20A—C21A—H43A109.5
C3A—C2A—H9A108.3H41A—C21A—H43A109.5
C1—C2A—H9A108.3H42A—C21A—H43A109.5
C3A—C2A—H10A108.3C21B—C20B—C19113 (3)
C1—C2A—H10A108.3C21B—C20B—H39B109.1
H9A—C2A—H10A107.4C19—C20B—H39B109.1
C2A—C3A—H11A109.5C21B—C20B—H40B109.1
C2A—C3A—H12A109.5C19—C20B—H40B109.1
H11A—C3A—H12A109.5H39B—C20B—H40B107.8
C2A—C3A—H13A109.5C20B—C21B—H41B109.5
H11A—C3A—H13A109.5C20B—C21B—H42B109.5
H12A—C3A—H13A109.5H41B—C21B—H42B109.5
C3B—C2B—C1119 (2)C20B—C21B—H43B109.5
C3B—C2B—H9B107.5H41B—C21B—H43B109.5
C1—C2B—H9B107.5H42B—C21B—H43B109.5
C3B—C2B—H10107.5O8—C22—N8122.1 (10)
C1—C2B—H10107.5O8—C22—C23C116 (5)
H9B—C2B—H10107.0N8—C22—C23C122 (5)
C2B—C3B—H11B109.5O8—C22—C23B119 (3)
C2B—C3B—H12B109.5N8—C22—C23B117 (2)
H11B—C3B—H12B109.5O8—C22—C23A117 (2)
C2B—C3B—H13B109.5N8—C22—C23A119.4 (19)
H11B—C3B—H13B109.5C22—C23A—C24A104 (2)
H12B—C3B—H13B109.5C22—C23A—H44A110.9
N2—C4—O2121.0 (10)C24A—C23A—H44A110.9
N2—C4—C5A123.4 (11)C22—C23A—H45A110.9
O2—C4—C5A115.0 (12)C24A—C23A—H45A110.9
N2—C4—C5B119 (4)H44A—C23A—H45A108.9
O2—C4—C5B116 (4)C22—C23B—C24B107 (3)
C6A—C5A—C4116.1 (14)C22—C23B—H44B110.4
C6A—C5A—H14A108.3C24B—C23B—H44B110.4
C4—C5A—H14A108.3C22—C23B—H45B110.4
C6A—C5A—H15A108.3C24B—C23B—H45B110.4
C4—C5A—H15A108.3H44B—C23B—H45B108.6
H14A—C5A—H15A107.4C22—C23C—C24C106 (4)
C5A—C6A—H16A109.5C22—C23C—H44C110.5
C5A—C6A—H17A109.5C24C—C23C—H44C110.5
H16A—C6A—H17A109.5C22—C23C—H45C110.5
C5A—C6A—H18A109.5C24C—C23C—H45C110.5
H16A—C6A—H18A109.5H44C—C23C—H45C108.7
H17A—C6A—H18A109.5C23A—C24A—H46A109.5
C6B—C5B—C497 (4)C23A—C24A—H47A109.5
C6B—C5B—H14B112.4H46A—C24A—H47A109.5
C4—C5B—H14B112.4C23A—C24A—H48A109.5
C6B—C5B—H15B112.4H46A—C24A—H48A109.5
C4—C5B—H15B112.4H47A—C24A—H48A109.5
H14B—C5B—H15B110.0C23B—C24B—H46B109.5
C5B—C6B—H16B109.5C23B—C24B—H47B109.5
C5B—C6B—H17B109.5H46B—C24B—H47B109.5
H16B—C6B—H17B109.5C23B—C24B—H48B109.5
C5B—C6B—H18B109.5H46B—C24B—H48B109.5
H16B—C6B—H18B109.5H47B—C24B—H48B109.5
H17B—C6B—H18B109.5C23C—C24C—H46C109.5
O3—C7—N3123.6 (8)C23C—C24C—H47C109.5
O3—C7—C8114.4 (8)H46C—C24C—H47C109.5
N3—C7—C8122.0 (9)C23C—C24C—H48C109.5
C7—C8—C9115.5 (8)H46C—C24C—H48C109.5
C7—C8—H19108.4H47C—C24C—H48C109.5
N2—Rh1—N1—C181.6 (9)N1—C1—C2B—C3B5 (3)
O2i—Rh1—N1—C193.9 (9)C2A—C1—C2B—C3B120 (6)
O9—Rh1—N1—C1178.2 (9)Rh1—N2—C4—O24.3 (19)
Rh1i—Rh1—N1—C13.7 (9)Rh1—N2—C4—C5A166.1 (14)
N1—Rh1—N2—C483.1 (11)Rh1—N2—C4—C5B162 (3)
O1i—Rh1—N2—C493.0 (11)Rh1i—O2—C4—N22.3 (17)
O9—Rh1—N2—C4176.1 (11)Rh1i—O2—C4—C5A168.9 (13)
Rh1i—Rh1—N2—C43.4 (11)Rh1i—O2—C4—C5B160 (3)
N4—Rh2—N3—C786.1 (8)N2—C4—C5A—C6A4 (3)
O4ii—Rh2—N3—C789.1 (8)O2—C4—C5A—C6A175.3 (16)
O10—Rh2—N3—C7178.9 (7)C5B—C4—C5A—C6A86 (9)
Rh2ii—Rh2—N3—C70.5 (7)N2—C4—C5B—C6B111 (5)
N3—Rh2—N4—C1086.8 (8)O2—C4—C5B—C6B90 (5)
O3ii—Rh2—N4—C1088.7 (8)C5A—C4—C5B—C6B5 (5)
O10—Rh2—N4—C10176.0 (8)Rh2ii—O3—C7—N38.0 (12)
Rh2ii—Rh2—N4—C101.8 (8)Rh2ii—O3—C7—C8173.1 (6)
N6—Rh3—N5—C1386.1 (7)Rh2—N3—C7—O35.5 (13)
O6iii—Rh3—N5—C1389.8 (7)Rh2—N3—C7—C8175.6 (7)
O11—Rh3—N5—C13179.6 (7)O3—C7—C8—C9163.2 (9)
Rh3iii—Rh3—N5—C130.3 (7)N3—C7—C8—C915.7 (14)
N5—Rh3—N6—C1683.8 (8)Rh2ii—O4—C10—N47.1 (12)
O5iii—Rh3—N6—C1691.9 (8)Rh2ii—O4—C10—C11175.2 (7)
O11—Rh3—N6—C16177.1 (8)Rh2—N4—C10—O46.0 (14)
Rh3iii—Rh3—N6—C162.4 (8)Rh2—N4—C10—C11176.5 (8)
N8—Rh4—N7—C1984.6 (10)O4—C10—C11—C12B145.9 (12)
O8iv—Rh4—N7—C1991.8 (9)N4—C10—C11—C12B36.5 (16)
O12—Rh4—N7—C19178.9 (9)O4—C10—C11—C12A18.1 (16)
Rh4iv—Rh4—N7—C191.2 (9)N4—C10—C11—C12A159.6 (12)
N7—Rh4—N8—C2283.4 (10)Rh3iii—O5—C13—N53.6 (12)
O7iv—Rh4—N8—C2292.4 (10)Rh3iii—O5—C13—C14176.9 (6)
O12—Rh4—N8—C22177.2 (9)Rh3—N5—C13—O52.6 (13)
Rh4iv—Rh4—N8—C222.4 (9)Rh3—N5—C13—C14177.9 (7)
O12—Cr1—O9—Rh158.5 (4)O5—C13—C14—C15A48.9 (16)
O11—Cr1—O9—Rh1179.7 (3)N5—C13—C14—C15A130.7 (14)
O10—Cr1—O9—Rh161.3 (4)O5—C13—C14—C15B53.7 (17)
N2—Rh1—O9—Cr131.2 (4)N5—C13—C14—C15B126.8 (16)
N1—Rh1—O9—Cr158.8 (4)Rh3iii—O6—C16—N60.4 (12)
O2i—Rh1—O9—Cr1150.2 (4)Rh3iii—O6—C16—C17178.8 (7)
O1i—Rh1—O9—Cr1122.4 (4)Rh3—N6—C16—O62.2 (13)
O12—Cr1—O10—Rh2179.9 (3)Rh3—N6—C16—C17176.9 (7)
O11—Cr1—O10—Rh259.3 (4)O6—C16—C17—C18B46 (2)
O9—Cr1—O10—Rh260.6 (4)N6—C16—C17—C18B134.9 (18)
N4—Rh2—O10—Cr160.2 (4)O6—C16—C17—C18A106.3 (14)
N3—Rh2—O10—Cr132.2 (4)N6—C16—C17—C18A74.5 (15)
O3ii—Rh2—O10—Cr1150.1 (3)Rh4—N7—C19—O71.2 (17)
O4ii—Rh2—O10—Cr1121.2 (3)Rh4—N7—C19—C20B169 (2)
O12—Cr1—O11—Rh395.8 (5)Rh4—N7—C19—C20A172 (3)
O9—Cr1—O11—Rh324.4 (5)Rh4iv—O7—C19—N73.4 (15)
O10—Cr1—O11—Rh3143.8 (4)Rh4iv—O7—C19—C20B171 (2)
N6—Rh3—O11—Cr12.9 (5)Rh4iv—O7—C19—C20A170 (2)
N5—Rh3—O11—Cr194.0 (5)N7—C19—C20A—C21A137 (4)
O5iii—Rh3—O11—Cr187.0 (5)O7—C19—C20A—C21A49 (5)
O6iii—Rh3—O11—Cr1175.7 (5)C20B—C19—C20A—C21A44 (11)
O11—Cr1—O12—Rh454.6 (5)N7—C19—C20B—C21B95 (5)
O9—Cr1—O12—Rh4175.6 (3)O7—C19—C20B—C21B73 (5)
O10—Cr1—O12—Rh465.0 (4)C20A—C19—C20B—C21B168 (18)
N8—Rh4—O12—Cr155.7 (5)Rh4iv—O8—C22—N80.5 (15)
N7—Rh4—O12—Cr136.4 (5)Rh4iv—O8—C22—C23C180 (4)
O8iv—Rh4—O12—Cr1126.1 (4)Rh4iv—O8—C22—C23B164 (2)
O7iv—Rh4—O12—Cr1145.5 (4)Rh4iv—O8—C22—C23A165 (2)
Rh1i—O1—C1—N14.5 (15)Rh4—N8—C22—O81.7 (17)
Rh1i—O1—C1—C2B173.2 (18)Rh4—N8—C22—C23C177 (4)
Rh1i—O1—C1—C2A165.0 (16)Rh4—N8—C22—C23B167 (2)
Rh1—N1—C1—O16.0 (16)Rh4—N8—C22—C23A163 (2)
Rh1—N1—C1—C2B174.7 (17)O8—C22—C23A—C24A49 (4)
Rh1—N1—C1—C2A162.1 (19)N8—C22—C23A—C24A145 (2)
O1—C1—C2A—C3A173.2 (18)O8—C22—C23B—C24B48 (5)
N1—C1—C2A—C3A18 (3)N8—C22—C23B—C24B146 (3)
C2B—C1—C2A—C3A59 (4)O8—C22—C23C—C24C71 (9)
O1—C1—C2B—C3B165 (2)N8—C22—C23C—C24C109 (6)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O120.862.322.963 (9)132
N2—H2···O100.862.122.917 (9)153
N3—H3···O90.862.192.965 (9)150
N4—H4···O110.862.333.015 (10)137
N5—H5···N40.862.663.404 (11)146
N6—H6···O90.862.092.860 (9)149
N7—H7···O100.862.192.978 (9)153
N8—H8···O110.862.373.016 (10)132
N8—H8···O5iii0.862.613.392 (11)151
Symmetry code: (iii) x+1, y, z+1.
(VIII) top
Crystal data top
C24H48MoN8O12Rh4·2.44(OH2)Z = 2
Mr = 1191.52F(000) = 1180
Triclinic, P1Dx = 1.815 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 12.952 (4) ÅCell parameters from 6964 reflections
b = 13.849 (5) Åθ = 3.1–27.5°
c = 14.679 (5) ŵ = 1.83 mm1
α = 112.460 (2)°T = 223 K
β = 99.574 (2)°Block, brown
γ = 108.472 (3)°0.50 × 0.30 × 0.20 mm
V = 2180.4 (13) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
9884 independent reflections
Graphite monochromator8783 reflections with I > 2σ(I)
Detector resolution: 14.62 pixels mm-1Rint = 0.030
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: integration
(Higashi, 1999)
h = 1016
Tmin = 0.581, Tmax = 0.859k = 1717
17845 measured reflectionsl = 1917
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.078H-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 parametersΔρmax = 0.72 e Å3
178 restraintsΔρmin = 0.84 e Å3
Crystal data top
C24H48MoN8O12Rh4·2.44(OH2)γ = 108.472 (3)°
Mr = 1191.52V = 2180.4 (13) Å3
Triclinic, P1Z = 2
a = 12.952 (4) ÅMo Kα radiation
b = 13.849 (5) ŵ = 1.83 mm1
c = 14.679 (5) ÅT = 223 K
α = 112.460 (2)°0.50 × 0.30 × 0.20 mm
β = 99.574 (2)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
9884 independent reflections
Absorption correction: integration
(Higashi, 1999)
8783 reflections with I > 2σ(I)
Tmin = 0.581, Tmax = 0.859Rint = 0.030
17845 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036178 restraints
wR(F2) = 0.078H-atom parameters constrained
S = 1.09Δρmax = 0.72 e Å3
9884 reflectionsΔρmin = 0.84 e Å3
543 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Rh10.96536 (2)0.03178 (3)0.44022 (2)0.02026 (7)
Rh20.93213 (2)0.40664 (2)0.48075 (2)0.02081 (7)
Rh30.57970 (2)0.04872 (3)0.07975 (2)0.02054 (7)
Rh40.55655 (2)0.00010 (2)0.44237 (2)0.01812 (7)
N10.8188 (3)0.1028 (3)0.3925 (3)0.0260 (7)
H10.76110.11260.34480.031*
O10.8775 (2)0.1655 (2)0.5049 (2)0.0284 (6)
N20.9303 (3)0.1340 (3)0.5567 (2)0.0248 (7)
H20.89950.17760.54570.030*
O20.9859 (2)0.0700 (3)0.6692 (2)0.0292 (6)
N30.8766 (3)0.3867 (3)0.3379 (3)0.0276 (7)
H30.81720.32350.29280.033*
O31.0050 (2)0.5602 (2)0.3692 (2)0.0290 (6)
N41.0517 (3)0.3537 (3)0.4450 (3)0.0277 (7)
H41.03820.28260.42920.033*
O41.1814 (2)0.5266 (2)0.4753 (2)0.0305 (6)
N50.5087 (3)0.1573 (3)0.1341 (3)0.0303 (8)
H50.54290.21330.19740.036*
O50.3553 (3)0.0656 (3)0.0139 (2)0.0368 (7)
N60.4856 (3)0.0595 (3)0.1213 (2)0.0278 (7)
H60.51400.05240.18270.033*
O60.3326 (2)0.1535 (3)0.0264 (2)0.0324 (7)
N70.6541 (3)0.0370 (3)0.5314 (3)0.0240 (7)
H70.71450.04370.51640.029*
O70.5501 (2)0.0394 (2)0.6407 (2)0.0274 (6)
N80.6433 (3)0.1648 (3)0.5391 (2)0.0228 (6)
H80.69870.20400.52390.027*
O80.5434 (2)0.1708 (2)0.6529 (2)0.0264 (6)
Mo10.76942 (2)0.11035 (3)0.33011 (2)0.01589 (7)
O90.8928 (2)0.0823 (2)0.3257 (2)0.0268 (6)
O100.8080 (2)0.2355 (2)0.4486 (2)0.0226 (5)
O110.7270 (2)0.1361 (2)0.2252 (2)0.0239 (6)
O120.6568 (2)0.0043 (2)0.3284 (2)0.0215 (5)
O130.5799 (3)0.2864 (4)0.3722 (3)0.0672 (11)
O140.8897 (8)0.0055 (14)0.1111 (6)0.221 (11)0.74 (2)
O151.0649 (16)0.153 (2)0.0531 (18)0.249 (17)0.50 (3)
O160.897 (2)0.149 (3)0.092 (3)0.13 (2)0.196 (17)
C10.8021 (3)0.1784 (4)0.4275 (3)0.0267 (8)
C20.6908 (4)0.2856 (4)0.3772 (4)0.0424 (11)
H90.66120.29630.43150.051*
H100.63350.27650.33240.051*
C30.7077 (6)0.3900 (6)0.3133 (6)0.084 (2)
H110.76750.39690.35660.126*
H120.73050.38260.25570.126*
H130.63620.45800.28620.126*
C40.9512 (3)0.1391 (3)0.6491 (3)0.0256 (8)
C50.9325 (4)0.2274 (4)0.7360 (4)0.0405 (11)
H140.85480.19230.73810.049*
H150.93670.29110.72050.049*
C61.0187 (6)0.2749 (5)0.8422 (4)0.0650 (17)
H161.09610.30850.84060.097*
H171.01140.21330.86050.097*
H181.00410.33340.89370.097*
C70.9226 (3)0.4611 (3)0.3067 (3)0.0271 (8)
C80.8835 (4)0.4327 (4)0.1936 (3)0.0436 (12)
H190.81350.36080.15610.052*
H200.86440.49370.18800.052*
C90.9726 (6)0.4202 (7)0.1435 (5)0.092 (3)
H210.98440.35340.14040.138*
H221.04440.48840.18400.138*
H230.94710.41060.07340.138*
C101.1490 (3)0.4171 (4)0.4432 (3)0.0299 (9)
C111.2278 (4)0.3663 (4)0.4005 (5)0.0478 (12)
H24A1.20900.29300.40250.057*0.610 (11)
H25A1.21060.34920.32700.057*0.610 (11)
H24B1.30410.42770.42150.057*0.390 (11)
H25B1.23650.31450.42870.057*0.390 (11)
C12A1.3546 (7)0.4375 (7)0.4541 (8)0.056 (3)0.610 (11)
H26A1.37420.51290.45800.084*0.610 (11)
H27A1.39630.40010.41510.084*0.610 (11)
H28A1.37550.44550.52410.084*0.610 (11)
C12B1.1805 (17)0.3039 (18)0.2887 (12)0.097 (7)0.390 (11)
H26B1.16690.35410.26150.145*0.390 (11)
H27B1.10830.23890.26830.145*0.390 (11)
H28B1.23420.27640.26090.145*0.390 (11)
C130.4130 (4)0.1480 (4)0.0786 (3)0.0366 (10)
C14A0.3707 (11)0.2417 (11)0.1198 (8)0.063 (3)0.84 (2)
H29A0.29010.20630.11520.075*0.84 (2)
H30A0.41600.29360.19350.075*0.84 (2)
C15A0.3792 (19)0.3085 (12)0.0627 (11)0.144 (7)0.84 (2)
H31A0.34830.25680.01170.216*0.84 (2)
H32A0.45940.35880.08110.216*0.84 (2)
H33A0.33560.35430.08080.216*0.84 (2)
C14B0.357 (4)0.225 (4)0.131 (3)0.040 (8)0.16 (2)
H29B0.31980.19480.17330.048*0.16 (2)
H30B0.41840.30140.17920.048*0.16 (2)
C15B0.272 (7)0.238 (6)0.064 (5)0.13 (2)0.16 (2)
H31B0.22890.27160.10360.189*0.16 (2)
H32B0.22040.16360.00610.189*0.16 (2)
H33B0.31150.28830.03730.189*0.16 (2)
C160.3832 (4)0.1410 (4)0.0623 (3)0.0321 (9)
C170.3223 (4)0.2285 (5)0.0946 (4)0.0539 (15)
H340.34620.19320.17090.065*
H350.23900.25260.06820.065*
C180.3484 (7)0.3315 (6)0.0540 (6)0.084 (2)
H360.42910.30970.08750.126*
H370.33210.36210.02080.126*
H380.30100.38970.06890.126*
C190.6352 (3)0.0519 (3)0.6104 (3)0.0265 (8)
C20A0.7079 (5)0.0899 (8)0.6683 (7)0.0379 (15)0.943 (10)
H39A0.66350.17090.64870.045*0.943 (10)
H40A0.77590.08460.64600.045*0.943 (10)
C21A0.7474 (5)0.0209 (6)0.7854 (4)0.0575 (19)0.943 (10)
H41A0.68080.02700.80860.086*0.943 (10)
H42A0.79360.05910.80600.086*0.943 (10)
H43A0.79320.05040.81710.086*0.943 (10)
C20B0.732 (6)0.067 (16)0.668 (13)0.040 (13)0.057 (10)
H39B0.76280.11200.62010.048*0.057 (10)
H40B0.79470.00740.71940.048*0.057 (10)
C21B0.672 (8)0.131 (9)0.721 (8)0.045 (14)0.057 (10)
H41B0.60640.20100.66820.068*0.057 (10)
H42B0.64510.08310.76960.068*0.057 (10)
H43B0.72490.15030.75750.068*0.057 (10)
C220.6242 (3)0.2204 (3)0.6245 (3)0.0246 (8)
C230.6999 (4)0.3472 (3)0.6949 (3)0.0340 (9)
H44A0.75070.35630.75790.041*0.91 (3)
H45A0.74860.37670.65880.041*0.91 (3)
H44B0.72050.36260.76800.041*0.09 (3)
H45B0.77110.36940.67810.041*0.09 (3)
C24A0.6327 (6)0.4177 (5)0.7263 (11)0.051 (3)0.91 (3)
H46A0.58820.39250.76640.076*0.91 (3)
H47A0.58100.40800.66440.076*0.91 (3)
H48A0.68530.49810.76860.076*0.91 (3)
C24B0.635 (7)0.416 (6)0.679 (9)0.055 (15)0.09 (3)
H46B0.68950.49160.69500.083*0.09 (3)
H47B0.58910.42350.72520.083*0.09 (3)
H48B0.58500.37670.60730.083*0.09 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.01803 (14)0.02761 (16)0.02194 (15)0.01231 (12)0.00773 (11)0.01530 (13)
Rh20.01839 (14)0.01624 (14)0.02128 (15)0.00054 (11)0.00243 (11)0.00951 (12)
Rh30.01777 (14)0.02307 (15)0.01422 (14)0.00418 (12)0.00010 (11)0.00807 (12)
Rh40.01614 (13)0.01826 (14)0.01854 (14)0.00455 (11)0.00782 (11)0.00843 (12)
N10.0195 (15)0.0321 (18)0.0287 (18)0.0115 (14)0.0059 (13)0.0166 (16)
O10.0220 (13)0.0330 (16)0.0354 (16)0.0114 (12)0.0081 (12)0.0216 (14)
N20.0244 (16)0.0343 (19)0.0255 (17)0.0183 (15)0.0096 (14)0.0179 (15)
O20.0354 (15)0.0385 (17)0.0274 (15)0.0230 (14)0.0163 (13)0.0198 (14)
N30.0231 (16)0.0190 (16)0.0258 (18)0.0029 (13)0.0020 (14)0.0098 (14)
O30.0305 (15)0.0205 (14)0.0218 (14)0.0026 (12)0.0002 (12)0.0106 (12)
N40.0241 (16)0.0191 (16)0.038 (2)0.0045 (14)0.0084 (15)0.0163 (16)
O40.0246 (14)0.0264 (15)0.0401 (17)0.0078 (12)0.0129 (13)0.0167 (14)
N50.0321 (18)0.0299 (19)0.0199 (17)0.0128 (16)0.0034 (14)0.0051 (15)
O50.0337 (16)0.0414 (18)0.0312 (17)0.0185 (15)0.0048 (13)0.0131 (15)
N60.0274 (17)0.0303 (18)0.0173 (16)0.0030 (15)0.0000 (13)0.0132 (15)
O60.0250 (14)0.0372 (17)0.0208 (14)0.0009 (13)0.0030 (11)0.0153 (13)
N70.0205 (15)0.0303 (18)0.0276 (17)0.0126 (14)0.0124 (13)0.0161 (15)
O70.0247 (14)0.0382 (16)0.0260 (15)0.0142 (13)0.0116 (12)0.0190 (13)
N80.0224 (15)0.0210 (16)0.0224 (16)0.0042 (13)0.0104 (13)0.0103 (14)
O80.0264 (14)0.0224 (14)0.0235 (14)0.0041 (11)0.0123 (11)0.0073 (12)
Mo10.01268 (13)0.01782 (15)0.01501 (15)0.00316 (12)0.00231 (11)0.00905 (12)
O90.0208 (13)0.0411 (17)0.0304 (15)0.0157 (13)0.0117 (12)0.0245 (14)
O100.0191 (12)0.0193 (13)0.0201 (13)0.0010 (10)0.0030 (10)0.0090 (11)
O110.0183 (12)0.0244 (14)0.0212 (13)0.0019 (11)0.0012 (10)0.0120 (12)
O120.0201 (12)0.0190 (13)0.0210 (13)0.0039 (11)0.0062 (10)0.0086 (11)
O130.054 (2)0.081 (3)0.055 (3)0.028 (2)0.010 (2)0.024 (2)
O140.112 (8)0.45 (3)0.060 (6)0.165 (12)0.032 (5)0.040 (9)
O150.147 (18)0.39 (4)0.24 (3)0.08 (2)0.115 (17)0.17 (3)
O160.058 (18)0.12 (3)0.25 (5)0.038 (18)0.09 (2)0.10 (3)
C10.0207 (18)0.032 (2)0.032 (2)0.0141 (17)0.0099 (16)0.0162 (19)
C20.031 (2)0.038 (3)0.052 (3)0.008 (2)0.006 (2)0.025 (2)
C30.074 (5)0.051 (4)0.087 (5)0.010 (4)0.007 (4)0.015 (4)
C40.0206 (18)0.031 (2)0.032 (2)0.0132 (17)0.0112 (16)0.0171 (18)
C50.051 (3)0.047 (3)0.034 (3)0.029 (2)0.020 (2)0.018 (2)
C60.096 (5)0.059 (4)0.029 (3)0.039 (4)0.013 (3)0.009 (3)
C70.027 (2)0.025 (2)0.024 (2)0.0043 (17)0.0031 (16)0.0133 (17)
C80.046 (3)0.037 (3)0.023 (2)0.006 (2)0.002 (2)0.015 (2)
C90.066 (4)0.121 (7)0.032 (3)0.001 (4)0.016 (3)0.011 (4)
C100.028 (2)0.029 (2)0.036 (2)0.0097 (18)0.0114 (18)0.019 (2)
C110.043 (3)0.038 (3)0.075 (4)0.021 (2)0.033 (3)0.030 (3)
C12A0.040 (4)0.047 (5)0.109 (8)0.027 (4)0.041 (5)0.050 (6)
C12B0.099 (15)0.114 (17)0.073 (8)0.062 (14)0.057 (10)0.014 (11)
C130.042 (2)0.037 (2)0.029 (2)0.022 (2)0.008 (2)0.012 (2)
C14A0.080 (7)0.073 (7)0.047 (5)0.059 (7)0.020 (4)0.018 (4)
C15A0.268 (19)0.116 (10)0.157 (11)0.152 (12)0.121 (12)0.089 (8)
C14B0.037 (14)0.023 (13)0.061 (17)0.010 (10)0.029 (11)0.019 (12)
C15B0.14 (3)0.11 (3)0.13 (3)0.10 (2)0.00 (2)0.03 (2)
C160.031 (2)0.037 (2)0.021 (2)0.0038 (19)0.0026 (17)0.0164 (19)
C170.045 (3)0.053 (3)0.035 (3)0.014 (2)0.009 (2)0.029 (3)
C180.106 (6)0.059 (4)0.078 (5)0.015 (4)0.006 (4)0.049 (4)
C190.0238 (19)0.030 (2)0.032 (2)0.0147 (17)0.0123 (17)0.0158 (18)
C20A0.034 (3)0.059 (5)0.051 (3)0.029 (3)0.026 (3)0.042 (3)
C21A0.055 (4)0.096 (5)0.048 (3)0.043 (4)0.020 (3)0.050 (4)
C20B0.04 (2)0.06 (2)0.04 (2)0.023 (18)0.009 (19)0.039 (17)
C21B0.06 (3)0.07 (3)0.06 (3)0.05 (3)0.04 (2)0.05 (2)
C220.0276 (19)0.0234 (19)0.026 (2)0.0104 (16)0.0106 (16)0.0142 (17)
C230.033 (2)0.023 (2)0.032 (2)0.0017 (18)0.0123 (19)0.0064 (19)
C24A0.057 (4)0.021 (3)0.063 (6)0.011 (2)0.027 (3)0.011 (3)
C24B0.06 (2)0.039 (19)0.05 (2)0.018 (15)0.015 (15)0.019 (16)
Geometric parameters (Å, º) top
Rh1—N11.971 (3)C8—C91.488 (8)
Rh1—N21.987 (3)C8—H190.9800
Rh1—O1i2.036 (3)C8—H200.9800
Rh1—O2i2.034 (3)C9—H210.9700
Rh1—O92.233 (2)C9—H220.9700
Rh1—Rh1i2.4117 (8)C9—H230.9700
Rh2—N31.980 (3)C10—C111.504 (6)
Rh2—N41.977 (3)C11—C12B1.435 (14)
Rh2—O3ii2.030 (3)C11—C12A1.497 (9)
Rh2—O4ii2.039 (3)C11—H24A0.9800
Rh2—O102.214 (3)C11—H25A0.9800
Rh2—Rh2ii2.4019 (9)C11—H24B0.9800
Rh3—N51.986 (3)C11—H25B0.9800
Rh3—N61.972 (3)C12A—H26A0.9700
Rh3—O5iii2.025 (3)C12A—H27A0.9700
Rh3—O6iii2.032 (3)C12A—H28A0.9700
Rh3—O112.207 (2)C12B—H26B0.9700
Rh3—Rh3iii2.4037 (8)C12B—H27B0.9700
Rh4—N71.983 (3)C12B—H28B0.9700
Rh4—N81.965 (3)C13—C14B1.516 (18)
Rh4—O7iv2.031 (3)C13—C14A1.520 (7)
Rh4—O8iv2.038 (3)C14A—C15A1.459 (13)
Rh4—O122.277 (3)C14A—H29A0.9800
Rh4—Rh4iv2.4148 (8)C14A—H30A0.9800
N1—C11.309 (5)C15A—H31A0.9700
N1—H10.8700C15A—H32A0.9700
O1—C11.281 (4)C15A—H33A0.9700
N2—C41.308 (5)C14B—C15B1.46 (2)
N2—H20.8700C14B—H29B0.9800
O2—C41.284 (4)C14B—H30B0.9800
N3—C71.301 (5)C15B—H31B0.9700
N3—H30.8700C15B—H32B0.9700
O3—C71.284 (5)C15B—H33B0.9700
N4—C101.298 (5)C16—C171.508 (6)
N4—H40.8700C17—C181.492 (9)
O4—C101.296 (5)C17—H340.9800
N5—C131.304 (5)C17—H350.9800
N5—H50.8700C18—H360.9700
O5—C131.282 (5)C18—H370.9700
N6—C161.306 (5)C18—H380.9700
N6—H60.8700C19—C20A1.508 (6)
O6—C161.276 (4)C19—C20B1.51 (2)
N7—C191.301 (5)C20A—C21A1.508 (10)
N7—H70.8700C20A—H39A0.9800
O7—C191.292 (4)C20A—H40A0.9800
N8—C221.308 (5)C21A—H41A0.9700
N8—H80.8700C21A—H42A0.9700
O8—C221.284 (5)C21A—H43A0.9700
Mo1—O111.750 (2)C20B—C21B1.51 (2)
Mo1—O91.766 (2)C20B—H39B0.9800
Mo1—O121.771 (3)C20B—H40B0.9800
Mo1—O101.772 (3)C21B—H41B0.9700
C1—C21.510 (6)C21B—H42B0.9700
C2—C31.500 (8)C21B—H43B0.9700
C2—H90.9800C22—C231.517 (6)
C2—H100.9800C23—C24A1.501 (7)
C3—H110.9700C23—C24B1.51 (2)
C3—H120.9700C23—H44A0.9800
C3—H130.9700C23—H45A0.9800
C4—C51.510 (6)C23—H44B0.9800
C5—C61.510 (7)C23—H45B0.9800
C5—H140.9800C24A—H46A0.9700
C5—H150.9800C24A—H47A0.9700
C6—H160.9700C24A—H48A0.9700
C6—H170.9700C24B—H46B0.9700
C6—H180.9700C24B—H47B0.9700
C7—C81.504 (6)C24B—H48B0.9700
N1—Rh1—N294.51 (14)C9—C8—H20109.1
N1—Rh1—O2i88.21 (13)C7—C8—H20109.1
N2—Rh1—O2i174.84 (11)H19—C8—H20107.8
N1—Rh1—O1i175.65 (11)C8—C9—H21109.5
N2—Rh1—O1i86.26 (13)C8—C9—H22109.5
O2i—Rh1—O1i90.70 (12)H21—C9—H22109.5
N1—Rh1—O991.66 (11)C8—C9—H23109.5
N2—Rh1—O994.46 (11)H21—C9—H23109.5
O2i—Rh1—O989.84 (10)H22—C9—H23109.5
O1i—Rh1—O992.55 (10)O4—C10—N4121.8 (4)
N1—Rh1—Rh1i85.39 (9)O4—C10—C11116.7 (4)
N2—Rh1—Rh1i86.14 (9)N4—C10—C11121.5 (4)
O2i—Rh1—Rh1i89.71 (8)C12B—C11—C10109.5 (8)
O1i—Rh1—Rh1i90.39 (7)C12A—C11—C10117.0 (5)
O9—Rh1—Rh1i177.03 (7)C12A—C11—H24A108.0
N4—Rh2—N390.09 (14)C10—C11—H24A108.0
N4—Rh2—O3ii90.80 (13)C12A—C11—H25A108.0
N3—Rh2—O3ii175.78 (12)C10—C11—H25A108.0
N4—Rh2—O4ii175.64 (13)H24A—C11—H25A107.3
N3—Rh2—O4ii91.35 (13)C12B—C11—H24B109.8
O3ii—Rh2—O4ii87.47 (12)C10—C11—H24B109.8
N4—Rh2—O1094.50 (12)C12B—C11—H25B109.8
N3—Rh2—O1095.81 (11)C10—C11—H25B109.8
O3ii—Rh2—O1088.23 (10)H24B—C11—H25B108.2
O4ii—Rh2—O1089.44 (11)C11—C12A—H26A109.5
N4—Rh2—Rh2ii85.71 (10)C11—C12A—H27A109.5
N3—Rh2—Rh2ii85.29 (9)H26A—C12A—H27A109.5
O3ii—Rh2—Rh2ii90.66 (8)C11—C12A—H28A109.5
O4ii—Rh2—Rh2ii90.31 (8)H26A—C12A—H28A109.5
O10—Rh2—Rh2ii178.87 (7)H27A—C12A—H28A109.5
N6—Rh3—N592.05 (15)C11—C12B—H26B109.5
N6—Rh3—O5iii88.86 (14)C11—C12B—H27B109.5
N5—Rh3—O5iii175.88 (12)H26B—C12B—H27B109.5
N6—Rh3—O6iii175.75 (12)C11—C12B—H28B109.5
N5—Rh3—O6iii88.12 (14)H26B—C12B—H28B109.5
O5iii—Rh3—O6iii90.68 (13)H27B—C12B—H28B109.5
N6—Rh3—O1193.74 (11)O5—C13—N5122.5 (4)
N5—Rh3—O1194.04 (12)O5—C13—C14B118 (2)
O5iii—Rh3—O1189.91 (11)N5—C13—C14B118.8 (19)
O6iii—Rh3—O1190.49 (10)O5—C13—C14A117.3 (5)
N6—Rh3—Rh3iii86.15 (9)N5—C13—C14A120.0 (6)
N5—Rh3—Rh3iii86.83 (10)C15A—C14A—C13112.9 (7)
O5iii—Rh3—Rh3iii89.22 (9)C15A—C14A—H29A109.0
O6iii—Rh3—Rh3iii89.61 (8)C13—C14A—H29A109.0
O11—Rh3—Rh3iii179.13 (7)C15A—C14A—H30A109.0
N8—Rh4—N790.44 (13)C13—C14A—H30A109.0
N8—Rh4—O7iv88.66 (12)H29A—C14A—H30A107.8
N7—Rh4—O7iv175.56 (12)C14A—C15A—H31A109.5
N8—Rh4—O8iv175.50 (11)C14A—C15A—H32A109.5
N7—Rh4—O8iv90.52 (13)H31A—C15A—H32A109.5
O7iv—Rh4—O8iv90.05 (11)C14A—C15A—H33A109.5
N8—Rh4—O1296.02 (11)H31A—C15A—H33A109.5
N7—Rh4—O1296.51 (11)H32A—C15A—H33A109.5
O7iv—Rh4—O1287.91 (10)C15B—C14B—C13117 (3)
O8iv—Rh4—O1288.23 (10)C15B—C14B—H29B108.0
N8—Rh4—Rh4iv85.49 (9)C13—C14B—H29B108.0
N7—Rh4—Rh4iv85.07 (9)C15B—C14B—H30B108.0
O7iv—Rh4—Rh4iv90.53 (8)C13—C14B—H30B108.0
O8iv—Rh4—Rh4iv90.22 (8)H29B—C14B—H30B107.2
O12—Rh4—Rh4iv177.80 (6)C14B—C15B—H31B109.5
C1—N1—Rh1124.7 (3)C14B—C15B—H32B109.5
C1—N1—H1117.6H31B—C15B—H32B109.5
Rh1—N1—H1117.6C14B—C15B—H33B109.5
C1—O1—Rh1i116.7 (2)H31B—C15B—H33B109.5
C4—N2—Rh1123.4 (3)H32B—C15B—H33B109.5
C4—N2—H2118.3O6—C16—N6122.0 (4)
Rh1—N2—H2118.3O6—C16—C17117.1 (4)
C4—O2—Rh1i117.6 (2)N6—C16—C17120.8 (3)
C7—N3—Rh2124.7 (3)C18—C17—C16111.7 (5)
C7—N3—H3117.7C18—C17—H34109.3
Rh2—N3—H3117.7C16—C17—H34109.3
C7—O3—Rh2ii116.9 (2)C18—C17—H35109.3
C10—N4—Rh2124.9 (3)C16—C17—H35109.3
C10—N4—H4117.6H34—C17—H35108.0
Rh2—N4—H4117.6C17—C18—H36109.5
C10—O4—Rh2ii117.0 (2)C17—C18—H37109.5
C13—N5—Rh3122.7 (3)H36—C18—H37109.5
C13—N5—H5118.7C17—C18—H38109.5
Rh3—N5—H5118.7H36—C18—H38109.5
C13—O5—Rh3iii118.7 (3)H37—C18—H38109.5
C16—N6—Rh3124.0 (3)O7—C19—N7121.6 (3)
C16—N6—H6118.0O7—C19—C20A116.4 (4)
Rh3—N6—H6118.0N7—C19—C20A122.0 (4)
C16—O6—Rh3iii118.1 (3)O7—C19—C20B126 (5)
C19—N7—Rh4125.4 (3)N7—C19—C20B112 (4)
C19—N7—H7117.3C21A—C20A—C19114.2 (6)
Rh4—N7—H7117.3C21A—C20A—H39A108.7
C19—O7—Rh4iv117.4 (2)C19—C20A—H39A108.7
C22—N8—Rh4125.1 (3)C21A—C20A—H40A108.7
C22—N8—H8117.5C19—C20A—H40A108.7
Rh4—N8—H8117.5H39A—C20A—H40A107.6
C22—O8—Rh4iv116.9 (2)C20A—C21A—H41A109.5
O9—Mo1—O10107.90 (13)C20A—C21A—H42A109.5
O11—Mo1—O9108.53 (12)H41A—C21A—H42A109.5
O9—Mo1—O12111.38 (12)C20A—C21A—H43A109.5
O11—Mo1—O10109.17 (12)H41A—C21A—H43A109.5
O12—Mo1—O10108.12 (12)H42A—C21A—H43A109.5
O11—Mo1—O12111.64 (12)C21B—C20B—C19102 (4)
Mo1—O9—Rh1119.29 (13)C21B—C20B—H39B111.5
Mo1—O10—Rh2122.07 (13)C19—C20B—H39B111.5
Mo1—O11—Rh3136.57 (14)C21B—C20B—H40B111.5
Mo1—O12—Rh4129.21 (13)C19—C20B—H40B111.5
O1—C1—N1122.4 (4)H39B—C20B—H40B109.3
O1—C1—C2117.2 (4)C20B—C21B—H41B109.5
N1—C1—C2120.4 (4)C20B—C21B—H42B109.5
C3—C2—C1111.4 (4)H41B—C21B—H42B109.5
C3—C2—H9109.3C20B—C21B—H43B109.5
C1—C2—H9109.3H41B—C21B—H43B109.5
C3—C2—H10109.3H42B—C21B—H43B109.5
C1—C2—H10109.3O8—C22—N8122.3 (4)
H9—C2—H10108.0O8—C22—C23117.6 (3)
C2—C3—H11109.5N8—C22—C23120.1 (3)
C2—C3—H12109.5C24A—C23—C22113.2 (4)
H11—C3—H12109.5C24B—C23—C22109 (3)
C2—C3—H13109.5C24A—C23—H44A108.9
H11—C3—H13109.5C22—C23—H44A108.9
H12—C3—H13109.5C24A—C23—H45A108.9
O2—C4—N2122.4 (4)C22—C23—H45A108.9
O2—C4—C5117.8 (3)H44A—C23—H45A107.7
N2—C4—C5119.8 (3)C24B—C23—H44B109.9
C4—C5—C6113.7 (4)C22—C23—H44B109.9
C4—C5—H14108.8C24A—C23—H45B127.0
C6—C5—H14108.8C24B—C23—H45B109.9
C4—C5—H15108.8C22—C23—H45B109.9
C6—C5—H15108.8H44B—C23—H45B108.3
H14—C5—H15107.7C23—C24A—H46A109.5
C5—C6—H16109.5C23—C24A—H47A109.5
C5—C6—H17109.5H46A—C24A—H47A109.5
H16—C6—H17109.5C23—C24A—H48A109.5
C5—C6—H18109.5H46A—C24A—H48A109.5
H16—C6—H18109.5H47A—C24A—H48A109.5
H17—C6—H18109.5C23—C24B—H46B109.5
O3—C7—N3122.3 (4)C23—C24B—H47B109.5
O3—C7—C8116.8 (3)H46B—C24B—H47B109.5
N3—C7—C8120.9 (4)C23—C24B—H48B109.5
C9—C8—C7112.5 (4)H46B—C24B—H48B109.5
C9—C8—H19109.1H47B—C24B—H48B109.5
C7—C8—H19109.1
Symmetry codes: (i) x+2, y, z+1; (ii) x+2, y+1, z+1; (iii) x+1, y, z; (iv) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O120.872.363.049 (4)136
N2—H2···O100.872.243.048 (4)156
N3—H3···O110.872.192.970 (4)148
N4—H4···O90.872.463.210 (4)144
N4—H4···O1i0.872.593.307 (4)140
N5—H5···O130.872.273.061 (5)152
N6—H6···O120.872.293.107 (4)156
N7—H7···N10.872.493.286 (5)153
N8—H8···O100.871.982.808 (4)159
Symmetry code: (i) x+2, y, z+1.
(IX) top
Crystal data top
C32H64MoN8O12Rh4Z = 4
Mr = 1260.49F(000) = 2520
Triclinic, P1Dx = 1.811 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 15.567 (4) ÅCell parameters from 8708 reflections
b = 15.778 (4) Åθ = 3.2–27.5°
c = 19.221 (5) ŵ = 1.72 mm1
α = 87.720 (6)°T = 118 K
β = 89.872 (6)°Block, brown
γ = 78.448 (5)°0.10 × 0.10 × 0.10 mm
V = 4621.6 (19) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
21025 independent reflections
Graphite monochromator13532 reflections with I > 2σ(I)
Detector resolution: 14.62 pixels mm-1Rint = 0.066
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: integration
NUMABS (Higashi, 1999)
h = 2015
Tmin = 0.804, Tmax = 0.902k = 2019
38498 measured reflectionsl = 2424
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H-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 parametersΔρmax = 1.09 e Å3
33 restraintsΔρmin = 0.96 e Å3
Crystal data top
C32H64MoN8O12Rh4γ = 78.448 (5)°
Mr = 1260.49V = 4621.6 (19) Å3
Triclinic, P1Z = 4
a = 15.567 (4) ÅMo Kα radiation
b = 15.778 (4) ŵ = 1.72 mm1
c = 19.221 (5) ÅT = 118 K
α = 87.720 (6)°0.10 × 0.10 × 0.10 mm
β = 89.872 (6)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
21025 independent reflections
Absorption correction: integration
NUMABS (Higashi, 1999)
13532 reflections with I > 2σ(I)
Tmin = 0.804, Tmax = 0.902Rint = 0.066
38498 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06233 restraints
wR(F2) = 0.104H-atom parameters constrained
S = 1.02Δρmax = 1.09 e Å3
21025 reflectionsΔρmin = 0.96 e Å3
1043 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Rh10.15014 (4)0.27528 (3)0.24126 (3)0.01180 (13)
Rh20.30164 (4)0.24005 (3)0.27786 (3)0.01195 (13)
Rh30.22217 (4)0.26759 (3)0.19721 (3)0.01093 (13)
Rh40.31888 (4)0.24687 (3)0.29173 (3)0.01124 (13)
Rh50.01650 (4)0.42438 (3)0.01760 (3)0.01075 (13)
Rh60.00771 (4)0.04862 (3)0.04559 (3)0.01138 (13)
Rh70.47703 (4)0.07599 (3)0.48433 (3)0.01132 (13)
Rh80.48546 (4)0.45860 (3)0.45154 (3)0.01110 (13)
Mo10.01569 (4)0.24969 (4)0.12292 (3)0.00904 (14)
Mo20.48237 (4)0.25815 (4)0.37689 (3)0.00942 (14)
N10.1959 (4)0.2876 (3)0.1462 (3)0.0121 (13)
H10.15840.30890.11260.015*
O10.3393 (3)0.2473 (3)0.1772 (2)0.0188 (12)
N20.1612 (4)0.1497 (3)0.2299 (3)0.0158 (14)
H20.11490.13150.21510.019*
O20.3037 (3)0.1117 (3)0.2648 (2)0.0134 (11)
O30.1127 (3)0.2604 (3)0.3421 (2)0.0159 (12)
N30.2563 (4)0.2244 (3)0.3733 (3)0.0163 (14)
H30.29470.21000.40740.020*
O40.1454 (3)0.4022 (3)0.2573 (2)0.0131 (11)
N40.2893 (4)0.3662 (3)0.2885 (3)0.0137 (13)
H40.33650.38530.30000.016*
N50.1500 (4)0.3063 (3)0.2694 (3)0.0121 (13)
H50.10370.32640.25550.015*
O50.2353 (3)0.2809 (3)0.3616 (2)0.0151 (11)
N60.1628 (4)0.1451 (3)0.2156 (3)0.0123 (13)
H60.11730.12340.19020.015*
O60.2542 (3)0.1210 (3)0.3037 (2)0.0168 (12)
O70.3048 (3)0.2295 (3)0.1284 (2)0.0136 (11)
N70.3963 (4)0.2165 (3)0.2187 (3)0.0152 (14)
H70.44590.20230.23210.018*
O80.2920 (3)0.3904 (3)0.1805 (2)0.0159 (11)
N80.3748 (4)0.3708 (3)0.2749 (3)0.0148 (14)
H80.41450.39510.30440.018*
N90.0137 (4)0.4651 (3)0.1139 (3)0.0145 (14)
H90.02810.42580.14800.017*
O90.0224 (3)0.6090 (3)0.0836 (2)0.0165 (12)
N100.1112 (4)0.4322 (3)0.0197 (3)0.0122 (13)
H100.13060.38450.02970.015*
O100.1459 (3)0.5761 (3)0.0113 (2)0.0147 (11)
N110.0212 (4)0.1332 (3)0.0316 (3)0.0146 (14)
H110.03270.18340.02070.018*
O110.0018 (3)0.0454 (3)0.1186 (2)0.0177 (12)
N120.1215 (4)0.0849 (3)0.0402 (3)0.0157 (14)
H120.14720.12580.06750.019*
O120.1398 (3)0.0055 (3)0.0462 (2)0.0172 (12)
N130.6032 (4)0.0730 (3)0.4719 (3)0.0162 (14)
H130.61830.12240.45990.019*
O130.6505 (3)0.0701 (3)0.4982 (2)0.0166 (12)
N140.4653 (4)0.0390 (4)0.3883 (3)0.0158 (14)
H140.44530.07880.35570.019*
O140.5127 (3)0.1048 (3)0.4145 (2)0.0154 (11)
N150.5999 (4)0.3821 (3)0.4743 (3)0.0148 (13)
H150.61920.33910.44680.018*
O150.6276 (3)0.4547 (3)0.5685 (2)0.0142 (11)
N160.4262 (4)0.3943 (3)0.5200 (3)0.0159 (14)
H160.40080.35370.50430.019*
O160.4523 (3)0.4674 (3)0.6131 (2)0.0158 (11)
O170.0127 (3)0.3003 (3)0.1975 (2)0.0100 (11)
O180.1295 (3)0.2798 (3)0.1083 (2)0.0154 (11)
O190.0410 (3)0.2836 (3)0.0504 (2)0.0126 (11)
O200.0140 (3)0.1358 (3)0.1353 (2)0.0135 (11)
O210.4453 (3)0.2106 (3)0.3036 (2)0.0125 (11)
O220.5981 (3)0.2283 (3)0.3832 (2)0.0107 (11)
O230.4360 (3)0.2196 (3)0.4528 (2)0.0128 (11)
O240.4537 (3)0.3724 (3)0.3676 (2)0.0122 (11)
C10.2783 (5)0.2659 (4)0.1305 (4)0.0131 (16)
C20.3060 (5)0.2549 (4)0.0561 (3)0.0161 (17)
H2A0.36190.27470.04850.019*0.37 (3)
H2B0.26100.29010.02480.019*0.37 (3)
H2C0.35490.28530.04690.019*0.63 (3)
H2D0.25640.28220.02530.019*0.63 (3)
C3A0.336 (3)0.1583 (10)0.0380 (15)0.039 (13)*0.37 (3)
H3A0.30000.11950.06020.047*0.37 (3)
H3B0.39910.13510.04550.047*0.37 (3)
C4A0.310 (4)0.185 (4)0.0404 (19)0.18 (2)*0.37 (3)
H4A0.32360.13330.06850.272*0.37 (3)
H4B0.34370.22740.05760.272*0.37 (3)
H4C0.24740.20970.04370.272*0.37 (3)
C3B0.3177 (19)0.1586 (8)0.0398 (8)0.046 (9)*0.63 (3)
H3C0.26020.14090.04230.056*0.63 (3)
H3D0.35710.12310.07490.056*0.63 (3)
C4B0.3573 (9)0.1421 (8)0.0343 (6)0.024 (5)*0.63 (3)
H4D0.36310.08080.04420.036*0.63 (3)
H4E0.41510.15770.03620.036*0.63 (3)
H4F0.31840.17750.06900.036*0.63 (3)
C50.2322 (5)0.0921 (4)0.2427 (3)0.0149 (16)
C60.2304 (5)0.0017 (4)0.2345 (4)0.0218 (19)
H6A0.28860.03220.21860.026*
H6B0.18670.00680.19840.026*
C70.2075 (6)0.0452 (5)0.3027 (5)0.039 (2)
H7A0.21600.10840.29680.047*
H7B0.24820.03560.33970.047*
C80.1139 (7)0.0111 (6)0.3253 (5)0.065 (4)
H8A0.10680.05020.33580.097*
H8B0.10100.04400.36700.097*
H8C0.07350.01740.28770.097*
C90.1734 (5)0.2340 (4)0.3888 (4)0.0142 (16)
C100.1432 (5)0.2152 (4)0.4611 (3)0.0200 (18)
H10A0.19460.18500.48890.024*
H10B0.10190.17530.45830.024*
C110.0986 (5)0.2948 (5)0.4994 (4)0.0252 (19)
H11A0.05380.33120.46860.030*
H11B0.14260.32960.51110.030*
C120.0548 (6)0.2683 (6)0.5666 (4)0.051 (3)
H12A0.01280.23230.55510.077*
H12B0.02410.32040.58910.077*
H12C0.09980.23550.59830.077*
C130.2157 (5)0.4239 (4)0.2795 (3)0.0123 (16)
C140.2089 (5)0.5174 (4)0.2971 (4)0.0182 (17)
H14A0.19390.55480.25450.022*
H14B0.26640.52570.31450.022*
C150.1398 (5)0.5440 (5)0.3519 (4)0.0253 (19)
H15A0.13710.60550.36200.030*
H15B0.08200.53890.33310.030*
C160.1574 (5)0.4898 (5)0.4189 (4)0.031 (2)
H16A0.15010.43070.41090.046*
H16B0.11600.51510.45450.046*
H16C0.21750.48860.43470.046*
C170.1660 (5)0.3042 (4)0.3368 (4)0.0124 (16)
C180.1044 (5)0.3297 (4)0.3862 (4)0.0151 (16)
H18A0.04520.29390.37930.018*
H18B0.12280.31760.43430.018*
C190.0991 (5)0.4258 (4)0.3778 (4)0.0242 (19)
H19A0.05850.43930.41330.029*
H19B0.07490.43670.33140.029*
C200.1883 (6)0.4857 (5)0.3851 (4)0.035 (2)
H20A0.22820.47400.34900.052*
H20B0.18150.54610.38000.052*
H20C0.21240.47550.43120.052*
C210.1890 (5)0.0954 (4)0.2642 (4)0.0151 (16)
C220.1449 (4)0.0016 (4)0.2717 (4)0.0163 (17)
H22A0.11880.01030.31890.020*
H22B0.09680.01050.23750.020*
C230.2082 (5)0.0582 (5)0.2605 (4)0.0238 (19)
H23A0.17710.11900.26850.029*
H23B0.25610.04640.29490.029*
C240.2471 (5)0.0469 (5)0.1878 (4)0.030 (2)
H24A0.27620.01360.17910.045*
H24B0.29000.08420.18360.045*
H24C0.20030.06290.15370.045*
C250.3789 (5)0.2161 (4)0.1524 (4)0.0151 (17)
C260.4452 (5)0.2036 (5)0.0992 (4)0.0197 (17)
H26A0.50300.20770.12190.024*
H26B0.42790.14500.08080.024*
C270.4536 (5)0.2703 (4)0.0391 (4)0.0231 (19)
H27A0.39610.26540.01580.028*
H27B0.49600.25780.00460.028*
C280.4836 (5)0.3619 (5)0.0625 (4)0.036 (2)
H28A0.53460.36460.09280.055*
H28B0.49960.40110.02160.055*
H28C0.43600.37930.08800.055*
C290.3550 (4)0.4178 (4)0.2218 (4)0.0125 (16)
C300.4052 (5)0.5086 (4)0.2064 (4)0.0181 (17)
H30A0.39440.52460.15730.022*
H30B0.38080.54820.23590.022*
C310.5042 (5)0.5246 (5)0.2176 (4)0.030 (2)
H31A0.52990.48490.18900.036*
H31B0.51640.51210.26710.036*
C320.5465 (6)0.6178 (5)0.1975 (5)0.047 (3)
H32A0.52390.65690.22780.071*
H32B0.61020.62590.20280.071*
H32C0.53270.63070.14890.071*
C330.0079 (5)0.5462 (4)0.1305 (4)0.0158 (17)
C340.0208 (5)0.5706 (4)0.2046 (3)0.0186 (17)
H34A0.02090.60770.21640.022*
H34B0.00750.51750.23510.022*
C350.1120 (6)0.6177 (5)0.2187 (5)0.043 (3)
H35A0.11730.62960.26890.051*
H35B0.12270.67410.19240.051*
C360.1791 (6)0.5702 (6)0.1998 (4)0.048 (3)
H36A0.18430.57060.14900.072*
H36B0.23550.59770.21960.072*
H36C0.16280.51020.21820.072*
C370.1693 (4)0.5035 (4)0.0074 (3)0.0118 (16)
C380.2654 (4)0.5023 (4)0.0133 (4)0.0167 (17)
H38A0.27580.47130.05730.020*
H38B0.29900.56250.01500.020*
C390.2982 (5)0.4590 (5)0.0467 (4)0.029 (2)
H39A0.36200.46230.04130.035*
H39B0.26930.39700.04490.035*
C400.2818 (5)0.4983 (5)0.1173 (4)0.039 (2)
H40A0.31710.55710.12240.058*
H40B0.29800.46280.15390.058*
H40C0.21950.50060.12150.058*
C410.0141 (5)0.1185 (4)0.0968 (4)0.0179 (17)
C420.0173 (5)0.1888 (4)0.1528 (4)0.0243 (19)
H42A0.05990.16550.18910.029*
H42B0.03730.23790.13190.029*
C430.0739 (7)0.2208 (5)0.1862 (5)0.045 (3)
H43A0.09840.17030.19930.054*
H43B0.06800.25570.22930.054*
C440.1379 (6)0.2762 (6)0.1363 (5)0.061 (3)
H44A0.14430.24170.09380.091*
H44B0.19510.29490.15900.091*
H44C0.11460.32710.12430.091*
C450.1710 (5)0.0517 (4)0.0014 (4)0.0170 (17)
C460.2690 (5)0.0767 (5)0.0048 (4)0.027 (2)
H46A0.28350.13390.02600.033*
H46B0.28870.03440.03750.033*
C470.3215 (5)0.0814 (5)0.0620 (4)0.029 (2)
H47A0.38470.08920.05100.035*
H47B0.30400.02650.08630.035*
C480.3060 (6)0.1571 (5)0.1098 (4)0.038 (2)
H48A0.31920.21090.08460.057*
H48B0.34430.16240.15080.057*
H48C0.24470.14650.12470.057*
C490.6670 (5)0.0051 (5)0.4795 (4)0.0193 (18)
C500.7610 (5)0.0086 (4)0.4671 (4)0.027 (2)
H50A0.77560.00740.41860.032*
H50B0.79770.03560.49820.032*
C510.7858 (5)0.0951 (5)0.4784 (4)0.032 (2)
H51A0.77050.11240.52650.039*
H51B0.75120.13940.44610.039*
C520.8827 (5)0.0931 (5)0.4669 (4)0.037 (2)
H52A0.91740.04760.49730.055*
H52B0.89600.14920.47780.055*
H52C0.89730.08100.41820.055*
C530.4860 (5)0.0428 (5)0.3705 (4)0.0185 (18)
C540.4773 (5)0.0641 (4)0.2961 (3)0.0175 (17)
H54A0.41430.05910.28520.021*
H54B0.50660.12510.29030.021*
C550.5158 (5)0.0071 (5)0.2437 (4)0.027 (2)
H55A0.57870.01120.25470.032*
H55B0.48570.05390.24830.032*
C560.5069 (6)0.0327 (5)0.1685 (4)0.035 (2)
H56A0.54390.08980.16190.052*
H56B0.52560.01020.13670.052*
H56C0.44560.03480.15890.052*
C570.6482 (5)0.3915 (4)0.5274 (4)0.0144 (16)
C580.7278 (5)0.3247 (4)0.5464 (4)0.0212 (18)
H58A0.77980.35210.54590.025*
H58B0.73690.27960.51130.025*
C590.7196 (5)0.2826 (4)0.6181 (4)0.0234 (19)
H59A0.71600.32700.65350.028*
H59B0.77310.23800.62800.028*
C600.6395 (5)0.2407 (5)0.6247 (4)0.037 (2)
H60A0.58610.28480.61640.055*
H60B0.63790.21430.67150.055*
H60C0.64300.19600.59020.055*
C610.4215 (4)0.4070 (4)0.5865 (4)0.0128 (16)
C620.3811 (5)0.3497 (4)0.6357 (4)0.0176 (17)
H62A0.42800.31640.66640.021*
H62B0.33890.38700.66560.021*
C630.3344 (5)0.2868 (4)0.6026 (4)0.0219 (18)
H63A0.37660.24720.57420.026*
H63B0.28810.31920.57100.026*
C640.2926 (5)0.2329 (5)0.6566 (4)0.034 (2)
H64A0.33820.19990.68760.050*
H64B0.26320.19290.63250.050*
H64C0.24950.27160.68400.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0091 (3)0.0128 (3)0.0133 (3)0.0019 (2)0.0012 (2)0.0005 (2)
Rh20.0089 (3)0.0133 (3)0.0134 (3)0.0018 (2)0.0008 (2)0.0006 (2)
Rh30.0098 (3)0.0125 (3)0.0110 (3)0.0032 (2)0.0015 (2)0.0010 (2)
Rh40.0105 (3)0.0129 (3)0.0108 (3)0.0036 (2)0.0017 (2)0.0008 (2)
Rh50.0114 (3)0.0098 (3)0.0111 (3)0.0024 (2)0.0002 (2)0.0004 (2)
Rh60.0128 (3)0.0104 (3)0.0115 (3)0.0031 (2)0.0000 (2)0.0034 (2)
Rh70.0123 (3)0.0088 (3)0.0124 (3)0.0012 (2)0.0002 (2)0.0006 (2)
Rh80.0120 (3)0.0110 (3)0.0107 (3)0.0031 (2)0.0003 (2)0.0017 (2)
Mo10.0091 (3)0.0092 (3)0.0094 (3)0.0030 (2)0.0004 (3)0.0012 (3)
Mo20.0088 (3)0.0095 (3)0.0102 (3)0.0025 (2)0.0001 (3)0.0003 (3)
N10.009 (3)0.008 (3)0.019 (3)0.003 (2)0.007 (3)0.002 (3)
O10.011 (3)0.033 (3)0.013 (3)0.008 (2)0.002 (2)0.007 (2)
N20.010 (3)0.016 (3)0.021 (3)0.001 (3)0.000 (3)0.005 (3)
O20.014 (3)0.012 (2)0.014 (3)0.004 (2)0.001 (2)0.002 (2)
O30.013 (3)0.020 (3)0.014 (3)0.003 (2)0.003 (2)0.003 (2)
N30.010 (3)0.023 (3)0.015 (3)0.000 (3)0.004 (3)0.001 (3)
O40.011 (3)0.011 (2)0.017 (3)0.001 (2)0.002 (2)0.002 (2)
N40.013 (3)0.015 (3)0.014 (3)0.004 (3)0.000 (3)0.005 (3)
N50.013 (3)0.016 (3)0.011 (3)0.012 (3)0.002 (3)0.006 (3)
O50.016 (3)0.021 (3)0.010 (3)0.005 (2)0.003 (2)0.003 (2)
N60.014 (3)0.010 (3)0.014 (3)0.004 (2)0.006 (3)0.005 (3)
O60.015 (3)0.015 (3)0.017 (3)0.003 (2)0.004 (2)0.001 (2)
O70.010 (3)0.016 (3)0.016 (3)0.007 (2)0.003 (2)0.000 (2)
N70.009 (3)0.023 (3)0.015 (3)0.004 (3)0.004 (3)0.005 (3)
O80.017 (3)0.014 (3)0.016 (3)0.000 (2)0.001 (2)0.003 (2)
N80.010 (3)0.016 (3)0.016 (3)0.003 (2)0.007 (2)0.004 (2)
N90.019 (4)0.010 (3)0.014 (3)0.003 (3)0.000 (3)0.003 (3)
O90.026 (3)0.008 (2)0.015 (3)0.002 (2)0.001 (2)0.002 (2)
N100.012 (3)0.009 (3)0.014 (3)0.001 (2)0.001 (3)0.005 (3)
O100.012 (3)0.015 (3)0.017 (3)0.002 (2)0.001 (2)0.004 (2)
N110.019 (4)0.010 (3)0.016 (3)0.004 (3)0.006 (3)0.003 (3)
O110.023 (3)0.014 (3)0.016 (3)0.005 (2)0.000 (2)0.000 (2)
N120.015 (4)0.014 (3)0.019 (3)0.002 (3)0.000 (3)0.008 (3)
O120.015 (3)0.011 (2)0.026 (3)0.002 (2)0.002 (2)0.008 (2)
N130.012 (3)0.012 (3)0.025 (4)0.002 (3)0.003 (3)0.001 (3)
O130.014 (3)0.018 (3)0.017 (3)0.002 (2)0.000 (2)0.003 (2)
N140.022 (4)0.015 (3)0.010 (3)0.005 (3)0.000 (3)0.003 (3)
O140.019 (3)0.012 (2)0.012 (3)0.002 (2)0.004 (2)0.003 (2)
N150.018 (4)0.014 (3)0.014 (3)0.008 (3)0.001 (3)0.006 (3)
O150.013 (3)0.014 (2)0.016 (3)0.001 (2)0.002 (2)0.004 (2)
N160.021 (4)0.015 (3)0.013 (3)0.007 (3)0.001 (3)0.001 (3)
O160.018 (3)0.015 (3)0.016 (3)0.006 (2)0.002 (2)0.001 (2)
O170.009 (3)0.013 (2)0.009 (2)0.004 (2)0.001 (2)0.001 (2)
O180.009 (3)0.020 (3)0.017 (3)0.004 (2)0.000 (2)0.001 (2)
O190.011 (3)0.013 (2)0.015 (3)0.005 (2)0.003 (2)0.001 (2)
O200.013 (3)0.014 (2)0.013 (3)0.001 (2)0.000 (2)0.002 (2)
O210.007 (3)0.012 (2)0.018 (3)0.001 (2)0.001 (2)0.001 (2)
O220.010 (3)0.012 (2)0.010 (2)0.001 (2)0.003 (2)0.000 (2)
O230.015 (3)0.012 (2)0.012 (3)0.004 (2)0.004 (2)0.002 (2)
O240.014 (3)0.007 (2)0.015 (3)0.001 (2)0.000 (2)0.001 (2)
C10.011 (4)0.009 (3)0.019 (4)0.002 (3)0.002 (3)0.001 (3)
C20.014 (4)0.024 (4)0.014 (4)0.012 (3)0.002 (3)0.001 (3)
C50.019 (4)0.015 (4)0.010 (4)0.002 (3)0.001 (3)0.004 (3)
C60.022 (5)0.008 (4)0.034 (5)0.001 (3)0.012 (4)0.003 (3)
C70.040 (6)0.024 (5)0.054 (6)0.011 (4)0.002 (5)0.013 (5)
C80.061 (8)0.062 (7)0.073 (8)0.020 (6)0.026 (6)0.029 (6)
C90.015 (4)0.014 (4)0.013 (4)0.001 (3)0.000 (3)0.005 (3)
C100.026 (5)0.020 (4)0.011 (4)0.003 (3)0.006 (3)0.001 (3)
C110.020 (5)0.033 (5)0.019 (4)0.003 (4)0.002 (4)0.002 (4)
C120.043 (7)0.080 (7)0.024 (5)0.001 (6)0.015 (5)0.006 (5)
C130.020 (4)0.007 (3)0.010 (4)0.003 (3)0.003 (3)0.001 (3)
C140.023 (5)0.013 (4)0.018 (4)0.003 (3)0.005 (3)0.002 (3)
C150.018 (5)0.034 (5)0.025 (5)0.006 (4)0.005 (4)0.014 (4)
C160.041 (6)0.027 (5)0.029 (5)0.016 (4)0.010 (4)0.010 (4)
C170.012 (4)0.006 (3)0.020 (4)0.003 (3)0.008 (3)0.005 (3)
C180.018 (4)0.013 (4)0.015 (4)0.002 (3)0.002 (3)0.006 (3)
C190.021 (5)0.030 (4)0.026 (5)0.013 (4)0.007 (4)0.004 (4)
C200.052 (6)0.016 (4)0.032 (5)0.003 (4)0.004 (5)0.002 (4)
C210.013 (4)0.017 (4)0.015 (4)0.003 (3)0.006 (3)0.001 (3)
C220.012 (4)0.020 (4)0.014 (4)0.004 (3)0.005 (3)0.001 (3)
C230.022 (5)0.024 (4)0.027 (5)0.011 (4)0.009 (4)0.001 (4)
C240.024 (5)0.037 (5)0.032 (5)0.010 (4)0.007 (4)0.016 (4)
C250.013 (4)0.018 (4)0.011 (4)0.003 (3)0.003 (3)0.004 (3)
C260.012 (4)0.031 (4)0.019 (4)0.011 (3)0.001 (3)0.009 (4)
C270.018 (5)0.027 (4)0.024 (4)0.003 (3)0.002 (4)0.001 (4)
C280.029 (5)0.033 (5)0.048 (6)0.012 (4)0.011 (5)0.009 (5)
C290.009 (4)0.012 (4)0.016 (4)0.001 (3)0.004 (3)0.001 (3)
C300.018 (4)0.018 (4)0.017 (4)0.002 (3)0.007 (3)0.001 (3)
C310.022 (5)0.029 (5)0.033 (5)0.008 (4)0.005 (4)0.000 (4)
C320.043 (6)0.021 (5)0.071 (7)0.013 (4)0.012 (6)0.013 (5)
C330.013 (4)0.013 (4)0.021 (4)0.002 (3)0.003 (3)0.002 (3)
C340.028 (4)0.021 (4)0.010 (4)0.010 (3)0.002 (3)0.009 (3)
C350.050 (7)0.040 (6)0.040 (6)0.014 (5)0.010 (5)0.005 (5)
C360.056 (7)0.065 (7)0.029 (5)0.028 (6)0.023 (5)0.011 (5)
C370.009 (4)0.021 (4)0.006 (3)0.004 (3)0.000 (3)0.003 (3)
C380.007 (4)0.016 (4)0.026 (4)0.002 (3)0.000 (3)0.007 (3)
C390.017 (5)0.036 (5)0.037 (5)0.010 (4)0.002 (4)0.000 (4)
C400.019 (5)0.055 (6)0.044 (6)0.011 (4)0.004 (4)0.010 (5)
C410.015 (4)0.014 (4)0.025 (4)0.003 (3)0.007 (3)0.005 (3)
C420.035 (5)0.015 (4)0.023 (5)0.007 (4)0.010 (4)0.001 (3)
C430.079 (8)0.022 (5)0.041 (6)0.029 (5)0.020 (6)0.009 (4)
C440.036 (7)0.042 (6)0.099 (9)0.005 (5)0.004 (6)0.011 (6)
C450.021 (5)0.016 (4)0.014 (4)0.002 (3)0.001 (3)0.003 (3)
C460.027 (5)0.029 (5)0.025 (5)0.000 (4)0.011 (4)0.014 (4)
C470.028 (5)0.026 (4)0.031 (5)0.001 (4)0.007 (4)0.009 (4)
C480.036 (6)0.030 (5)0.046 (6)0.002 (4)0.008 (5)0.009 (4)
C490.019 (5)0.020 (4)0.019 (4)0.004 (3)0.003 (3)0.002 (3)
C500.017 (5)0.008 (4)0.053 (6)0.000 (3)0.012 (4)0.006 (4)
C510.024 (5)0.037 (5)0.037 (5)0.009 (4)0.002 (4)0.005 (4)
C520.034 (6)0.040 (5)0.042 (6)0.022 (4)0.003 (5)0.011 (4)
C530.015 (4)0.022 (4)0.020 (4)0.007 (3)0.000 (3)0.002 (4)
C540.017 (4)0.018 (4)0.018 (4)0.004 (3)0.001 (3)0.004 (3)
C550.034 (5)0.030 (5)0.021 (4)0.013 (4)0.006 (4)0.007 (4)
C560.041 (6)0.039 (5)0.024 (5)0.008 (4)0.011 (4)0.007 (4)
C570.012 (4)0.011 (3)0.023 (4)0.009 (3)0.002 (3)0.002 (3)
C580.022 (5)0.012 (4)0.028 (5)0.001 (3)0.003 (4)0.001 (3)
C590.023 (5)0.014 (4)0.030 (5)0.005 (3)0.001 (4)0.001 (3)
C600.027 (5)0.041 (5)0.041 (6)0.007 (4)0.007 (4)0.014 (5)
C610.005 (4)0.015 (4)0.018 (4)0.000 (3)0.001 (3)0.011 (3)
C620.019 (4)0.018 (4)0.016 (4)0.004 (3)0.007 (3)0.001 (3)
C630.023 (5)0.018 (4)0.025 (4)0.005 (3)0.011 (4)0.004 (3)
C640.035 (6)0.029 (5)0.043 (6)0.021 (4)0.009 (4)0.003 (4)
Geometric parameters (Å, º) top
Rh1—N21.975 (5)C9—C101.503 (9)
Rh1—N11.977 (6)C10—C111.524 (10)
Rh1—O42.024 (4)C10—H10A0.9900
Rh1—O32.041 (4)C10—H10B0.9900
Rh1—O172.254 (4)C11—C121.541 (9)
Rh1—Rh22.4119 (9)C11—H11A0.9900
Rh2—N41.980 (5)C11—H11B0.9900
Rh2—N31.988 (6)C12—H12A0.9800
Rh2—O12.025 (5)C12—H12B0.9800
Rh2—O22.044 (4)C12—H12C0.9800
Rh2—O212.243 (4)C13—C141.510 (9)
Rh3—N51.978 (5)C14—C151.513 (9)
Rh3—N61.986 (5)C14—H14A0.9900
Rh3—O82.036 (4)C14—H14B0.9900
Rh3—O72.036 (5)C15—C161.511 (9)
Rh3—O182.261 (4)C15—H15A0.9900
Rh3—Rh42.4108 (9)C15—H15B0.9900
Rh4—N71.987 (6)C16—H16A0.9800
Rh4—N81.988 (5)C16—H16B0.9800
Rh4—O52.031 (5)C16—H16C0.9800
Rh4—O62.043 (4)C17—C181.473 (9)
Rh4—O22i2.225 (4)C18—C191.536 (9)
Rh5—N101.968 (5)C18—H18A0.9900
Rh5—N91.981 (6)C18—H18B0.9900
Rh5—O10ii2.017 (5)C19—C201.524 (10)
Rh5—O9ii2.032 (5)C19—H19A0.9900
Rh5—O192.242 (4)C19—H19B0.9900
Rh5—Rh5ii2.4080 (11)C20—H20A0.9800
Rh6—N121.980 (6)C20—H20B0.9800
Rh6—N111.995 (5)C20—H20C0.9800
Rh6—O11iii2.027 (4)C21—C221.503 (9)
Rh6—O12iii2.032 (5)C22—C231.516 (9)
Rh6—O202.262 (5)C22—H22A0.9900
Rh6—Rh6iii2.4179 (12)C22—H22B0.9900
Rh7—N131.969 (6)C23—C241.513 (10)
Rh7—N141.978 (6)C23—H23A0.9900
Rh7—O14iv2.028 (5)C23—H23B0.9900
Rh7—O13iv2.033 (5)C24—H24A0.9800
Rh7—O232.285 (4)C24—H24B0.9800
Rh7—Rh7iv2.4134 (11)C24—H24C0.9800
Rh8—N161.968 (5)C25—C261.501 (9)
Rh8—N151.981 (5)C26—C271.519 (8)
Rh8—O15v2.028 (4)C26—H26A0.9900
Rh8—O16v2.044 (4)C26—H26B0.9900
Rh8—O242.269 (5)C27—C281.512 (10)
Rh8—Rh8v2.4118 (12)C27—H27A0.9900
Mo1—O181.760 (4)C27—H27B0.9900
Mo1—O171.768 (5)C28—H28A0.9800
Mo1—O191.770 (4)C28—H28B0.9800
Mo1—O201.770 (4)C28—H28C0.9800
Mo2—O231.766 (4)C29—C301.507 (8)
Mo2—O241.769 (4)C30—C311.527 (10)
Mo2—O211.772 (5)C30—H30A0.9900
Mo2—O221.772 (4)C30—H30B0.9900
N1—C11.298 (8)C31—C321.521 (9)
N1—H10.8800C31—H31A0.9900
O1—C11.291 (8)C31—H31B0.9900
N2—C51.300 (8)C32—H32A0.9800
N2—H20.8800C32—H32B0.9800
O2—C51.291 (8)C32—H32C0.9800
O3—C91.300 (7)C33—C341.492 (9)
N3—C91.304 (8)C34—C351.495 (10)
N3—H30.8800C34—H34A0.9900
O4—C131.290 (8)C34—H34B0.9900
N4—C131.319 (8)C35—C361.457 (11)
N4—H40.8800C35—H35A0.9900
N5—C171.320 (8)C35—H35B0.9900
N5—H50.8800C36—H36A0.9800
O5—C171.293 (7)C36—H36B0.9800
N6—C211.312 (7)C36—H36C0.9800
N6—H60.8800C37—C381.505 (9)
O6—C211.275 (8)C38—C391.503 (10)
O7—C251.294 (8)C38—H38A0.9900
N7—C251.302 (8)C38—H38B0.9900
N7—H70.8800C39—C401.513 (9)
O8—C291.279 (8)C39—H39A0.9900
N8—C291.309 (7)C39—H39B0.9900
N8—H80.8800C40—H40A0.9800
N9—C331.309 (8)C40—H40B0.9800
N9—H90.8800C40—H40C0.9800
O9—C331.299 (7)C41—C421.523 (8)
O9—Rh5ii2.032 (5)C42—C431.542 (11)
N10—C371.308 (8)C42—H42A0.9900
N10—H100.8800C42—H42B0.9900
O10—C371.306 (7)C43—C441.546 (12)
O10—Rh5ii2.017 (5)C43—H43A0.9900
N11—C411.291 (9)C43—H43B0.9900
N11—H110.8800C44—H44A0.9800
O11—C411.292 (8)C44—H44B0.9800
O11—Rh6iii2.027 (4)C44—H44C0.9800
N12—C451.305 (9)C45—C461.504 (10)
N12—H120.8800C46—C471.515 (10)
O12—C451.294 (8)C46—H46A0.9900
O12—Rh6iii2.032 (5)C46—H46B0.9900
N13—C491.311 (8)C47—C481.535 (9)
N13—H130.8800C47—H47A0.9900
O13—C491.299 (7)C47—H47B0.9900
O13—Rh7iv2.033 (5)C48—H48A0.9800
N14—C531.325 (9)C48—H48B0.9800
N14—H140.8800C48—H48C0.9800
O14—C531.271 (7)C49—C501.494 (10)
O14—Rh7iv2.028 (5)C50—C511.515 (10)
N15—C571.300 (8)C50—H50A0.9900
N15—H150.8800C50—H50B0.9900
O15—C571.286 (8)C51—C521.518 (10)
O15—Rh8v2.028 (4)C51—H51A0.9900
N16—C611.302 (8)C51—H51B0.9900
N16—H160.8800C52—H52A0.9800
O16—C611.273 (8)C52—H52B0.9800
O16—Rh8v2.044 (4)C52—H52C0.9800
O22—Rh4vi2.225 (4)C53—C541.495 (10)
C1—C21.500 (9)C54—C551.524 (8)
C2—C3B1.539 (12)C54—H54A0.9900
C2—C3A1.555 (16)C54—H54B0.9900
C2—H2A0.9900C55—C561.530 (10)
C2—H2B0.9900C55—H55A0.9900
C2—H2C0.9900C55—H55B0.9900
C2—H2D0.9900C56—H56A0.9800
C3A—C4A1.577 (17)C56—H56B0.9800
C3A—H3A0.9900C56—H56C0.9800
C3A—H3B0.9900C57—C581.493 (9)
C4A—H4A0.9800C58—C591.522 (9)
C4A—H4B0.9800C58—H58A0.9900
C4A—H4C0.9800C58—H58B0.9900
C3B—C4B1.561 (14)C59—C601.528 (10)
C3B—H3C0.9900C59—H59A0.9900
C3B—H3D0.9900C59—H59B0.9900
C4B—H4D0.9800C60—H60A0.9800
C4B—H4E0.9800C60—H60B0.9800
C4B—H4F0.9800C60—H60C0.9800
C5—C61.501 (9)C61—C621.505 (8)
C6—C71.529 (9)C62—C631.502 (9)
C6—H6A0.9900C62—H62A0.9900
C6—H6B0.9900C62—H62B0.9900
C7—C81.518 (11)C63—C641.541 (8)
C7—H7A0.9900C63—H63A0.9900
C7—H7B0.9900C63—H63B0.9900
C8—H8A0.9800C64—H64A0.9800
C8—H8B0.9800C64—H64B0.9800
C8—H8C0.9800C64—H64C0.9800
N2—Rh1—N189.9 (2)C12—C11—H11A109.5
N2—Rh1—O4176.3 (2)C10—C11—H11B109.5
N1—Rh1—O491.24 (19)C12—C11—H11B109.5
N2—Rh1—O389.8 (2)H11A—C11—H11B108.1
N1—Rh1—O3175.6 (2)C11—C12—H12A109.5
O4—Rh1—O388.74 (18)C11—C12—H12B109.5
N2—Rh1—O1790.5 (2)H12A—C12—H12B109.5
N1—Rh1—O1789.55 (19)C11—C12—H12C109.5
O4—Rh1—O1792.95 (17)H12A—C12—H12C109.5
O3—Rh1—O1794.84 (17)H12B—C12—H12C109.5
N2—Rh1—Rh285.82 (17)O4—C13—N4121.3 (6)
N1—Rh1—Rh285.98 (16)O4—C13—C14116.9 (6)
O4—Rh1—Rh290.78 (13)N4—C13—C14121.8 (6)
O3—Rh1—Rh289.63 (13)C13—C14—C15111.2 (6)
O17—Rh1—Rh2174.23 (12)C13—C14—H14A109.4
N4—Rh2—N391.6 (2)C15—C14—H14A109.4
N4—Rh2—O192.9 (2)C13—C14—H14B109.4
N3—Rh2—O1173.7 (2)C15—C14—H14B109.4
N4—Rh2—O2175.3 (2)H14A—C14—H14B108.0
N3—Rh2—O287.8 (2)C16—C15—C14113.0 (6)
O1—Rh2—O287.36 (19)C16—C15—H15A109.0
N4—Rh2—O2194.0 (2)C14—C15—H15A109.0
N3—Rh2—O2198.1 (2)C16—C15—H15B109.0
O1—Rh2—O2185.88 (17)C14—C15—H15B109.0
O2—Rh2—O2190.72 (17)H15A—C15—H15B107.8
N4—Rh2—Rh185.14 (17)C15—C16—H16A109.5
N3—Rh2—Rh186.23 (16)C15—C16—H16B109.5
O1—Rh2—Rh189.82 (13)H16A—C16—H16B109.5
O2—Rh2—Rh190.14 (13)C15—C16—H16C109.5
O21—Rh2—Rh1175.57 (11)H16A—C16—H16C109.5
N5—Rh3—N691.0 (2)H16B—C16—H16C109.5
N5—Rh3—O891.2 (2)O5—C17—N5121.9 (7)
N6—Rh3—O8175.5 (2)O5—C17—C18118.2 (6)
N5—Rh3—O7175.3 (2)N5—C17—C18120.0 (6)
N6—Rh3—O790.2 (2)C17—C18—C19113.0 (5)
O8—Rh3—O787.23 (18)C17—C18—H18A109.0
N5—Rh3—O1895.7 (2)C19—C18—H18A109.0
N6—Rh3—O1890.46 (19)C17—C18—H18B109.0
O8—Rh3—O1893.22 (17)C19—C18—H18B109.0
O7—Rh3—O1888.82 (17)H18A—C18—H18B107.8
N5—Rh3—Rh485.23 (16)C20—C19—C18112.5 (6)
N6—Rh3—Rh486.84 (16)C20—C19—H19A109.1
O8—Rh3—Rh489.44 (13)C18—C19—H19A109.1
O7—Rh3—Rh490.35 (13)C20—C19—H19B109.1
O18—Rh3—Rh4177.17 (12)C18—C19—H19B109.1
N7—Rh4—N888.9 (2)H19A—C19—H19B107.8
N7—Rh4—O5176.4 (2)C19—C20—H20A109.5
N8—Rh4—O590.1 (2)C19—C20—H20B109.5
N7—Rh4—O691.4 (2)H20A—C20—H20B109.5
N8—Rh4—O6175.6 (2)C19—C20—H20C109.5
O5—Rh4—O689.36 (18)H20A—C20—H20C109.5
N7—Rh4—O22i97.7 (2)H20B—C20—H20C109.5
N8—Rh4—O22i94.35 (19)O6—C21—N6123.4 (6)
O5—Rh4—O22i85.80 (17)O6—C21—C22117.0 (6)
O6—Rh4—O22i89.99 (16)N6—C21—C22119.5 (7)
N7—Rh4—Rh385.56 (16)C21—C22—C23112.1 (6)
N8—Rh4—Rh386.33 (16)C21—C22—H22A109.2
O5—Rh4—Rh390.94 (13)C23—C22—H22A109.2
O6—Rh4—Rh389.29 (13)C21—C22—H22B109.2
O22i—Rh4—Rh3176.67 (12)C23—C22—H22B109.2
N10—Rh5—N990.2 (2)H22A—C22—H22B107.9
N10—Rh5—O10ii176.06 (17)C24—C23—C22112.1 (6)
N9—Rh5—O10ii90.8 (2)C24—C23—H23A109.2
N10—Rh5—O9ii91.7 (2)C22—C23—H23A109.2
N9—Rh5—O9ii175.65 (19)C24—C23—H23B109.2
O10ii—Rh5—O9ii87.09 (19)C22—C23—H23B109.2
N10—Rh5—O1991.50 (18)H23A—C23—H23B107.9
N9—Rh5—O1994.56 (19)C23—C24—H24A109.5
O10ii—Rh5—O1992.23 (16)C23—C24—H24B109.5
O9ii—Rh5—O1989.31 (16)H24A—C24—H24B109.5
N10—Rh5—Rh5ii86.02 (14)C23—C24—H24C109.5
N9—Rh5—Rh5ii85.53 (15)H24A—C24—H24C109.5
O10ii—Rh5—Rh5ii90.25 (12)H24B—C24—H24C109.5
O9ii—Rh5—Rh5ii90.69 (12)O7—C25—N7122.1 (7)
O19—Rh5—Rh5ii177.52 (12)O7—C25—C26116.2 (6)
N12—Rh6—N1190.8 (2)N7—C25—C26121.7 (6)
N12—Rh6—O11iii91.2 (2)C25—C26—C27112.3 (6)
N11—Rh6—O11iii175.2 (2)C25—C26—H26A109.1
N12—Rh6—O12iii176.1 (2)C27—C26—H26A109.1
N11—Rh6—O12iii89.1 (2)C25—C26—H26B109.1
O11iii—Rh6—O12iii88.61 (18)C27—C26—H26B109.1
N12—Rh6—O2091.3 (2)H26A—C26—H26B107.9
N11—Rh6—O2097.7 (2)C28—C27—C26112.5 (6)
O11iii—Rh6—O2086.63 (17)C28—C27—H27A109.1
O12iii—Rh6—O2092.51 (18)C26—C27—H27A109.1
N12—Rh6—Rh6iii85.80 (18)C28—C27—H27B109.1
N11—Rh6—Rh6iii85.57 (18)C26—C27—H27B109.1
O11iii—Rh6—Rh6iii90.17 (15)H27A—C27—H27B107.8
O12iii—Rh6—Rh6iii90.34 (14)C27—C28—H28A109.5
O20—Rh6—Rh6iii175.65 (12)C27—C28—H28B109.5
N13—Rh7—N1491.7 (2)H28A—C28—H28B109.5
N13—Rh7—O14iv89.9 (2)C27—C28—H28C109.5
N14—Rh7—O14iv175.50 (19)H28A—C28—H28C109.5
N13—Rh7—O13iv175.40 (18)H28B—C28—H28C109.5
N14—Rh7—O13iv89.4 (2)O8—C29—N8122.6 (6)
O14iv—Rh7—O13iv88.61 (19)O8—C29—C30115.9 (5)
N13—Rh7—O2394.36 (19)N8—C29—C30121.5 (6)
N14—Rh7—O2393.09 (19)C29—C30—C31116.6 (6)
O14iv—Rh7—O2390.96 (16)C29—C30—H30A108.2
O13iv—Rh7—O2390.03 (17)C31—C30—H30A108.2
N13—Rh7—Rh7iv84.59 (15)C29—C30—H30B108.2
N14—Rh7—Rh7iv86.16 (15)C31—C30—H30B108.2
O14iv—Rh7—Rh7iv89.84 (12)H30A—C30—H30B107.3
O13iv—Rh7—Rh7iv91.04 (12)C32—C31—C30110.8 (6)
O23—Rh7—Rh7iv178.68 (12)C32—C31—H31A109.5
N16—Rh8—N1590.9 (2)C30—C31—H31A109.5
N16—Rh8—O15v91.2 (2)C32—C31—H31B109.5
N15—Rh8—O15v175.1 (2)C30—C31—H31B109.5
N16—Rh8—O16v175.1 (2)H31A—C31—H31B108.1
N15—Rh8—O16v89.54 (19)C31—C32—H32A109.5
O15v—Rh8—O16v88.03 (18)C31—C32—H32B109.5
N16—Rh8—O2489.2 (2)H32A—C32—H32B109.5
N15—Rh8—O2493.3 (2)C31—C32—H32C109.5
O15v—Rh8—O2491.09 (17)H32A—C32—H32C109.5
O16v—Rh8—O2495.60 (17)H32B—C32—H32C109.5
N16—Rh8—Rh8v85.60 (18)O9—C33—N9121.9 (7)
N15—Rh8—Rh8v85.89 (17)O9—C33—C34116.8 (6)
O15v—Rh8—Rh8v89.87 (14)N9—C33—C34121.2 (6)
O16v—Rh8—Rh8v89.59 (14)C33—C34—C35112.6 (6)
O24—Rh8—Rh8v174.75 (10)C33—C34—H34A109.1
O18—Mo1—O17109.4 (2)C35—C34—H34A109.1
O18—Mo1—O19109.70 (19)C33—C34—H34B109.1
O17—Mo1—O19108.7 (2)C35—C34—H34B109.1
O18—Mo1—O20109.4 (2)H34A—C34—H34B107.8
O17—Mo1—O20109.97 (19)C36—C35—C34113.4 (8)
O19—Mo1—O20109.6 (2)C36—C35—H35A108.9
O23—Mo2—O24111.3 (2)C34—C35—H35A108.9
O23—Mo2—O21108.8 (2)C36—C35—H35B108.9
O24—Mo2—O21110.12 (19)C34—C35—H35B108.9
O23—Mo2—O22108.86 (19)H35A—C35—H35B107.7
O24—Mo2—O22108.0 (2)C35—C36—H36A109.5
O21—Mo2—O22109.7 (2)C35—C36—H36B109.5
C1—N1—Rh1123.4 (5)H36A—C36—H36B109.5
C1—N1—H1118.3C35—C36—H36C109.5
Rh1—N1—H1118.3H36A—C36—H36C109.5
C1—O1—Rh2117.4 (4)H36B—C36—H36C109.5
C5—N2—Rh1124.5 (5)O10—C37—N10121.5 (6)
C5—N2—H2117.7O10—C37—C38118.7 (6)
Rh1—N2—H2117.7N10—C37—C38119.8 (6)
C5—O2—Rh2116.7 (4)C39—C38—C37112.1 (6)
C9—O3—Rh1118.2 (4)C39—C38—H38A109.2
C9—N3—Rh2124.4 (5)C37—C38—H38A109.2
C9—N3—H3117.8C39—C38—H38B109.2
Rh2—N3—H3117.8C37—C38—H38B109.2
C13—O4—Rh1117.6 (4)H38A—C38—H38B107.9
C13—N4—Rh2125.0 (5)C38—C39—C40113.9 (6)
C13—N4—H4117.5C38—C39—H39A108.8
Rh2—N4—H4117.5C40—C39—H39A108.8
C17—N5—Rh3124.9 (5)C38—C39—H39B108.8
C17—N5—H5117.6C40—C39—H39B108.8
Rh3—N5—H5117.6H39A—C39—H39B107.7
C17—O5—Rh4116.9 (4)C39—C40—H40A109.5
C21—N6—Rh3122.5 (5)C39—C40—H40B109.5
C21—N6—H6118.7H40A—C40—H40B109.5
Rh3—N6—H6118.7C39—C40—H40C109.5
C21—O6—Rh4117.9 (4)H40A—C40—H40C109.5
C25—O7—Rh3117.0 (4)H40B—C40—H40C109.5
C25—N7—Rh4124.5 (5)N11—C41—O11123.1 (6)
C25—N7—H7117.7N11—C41—C42121.0 (7)
Rh4—N7—H7117.7O11—C41—C42115.9 (7)
C29—O8—Rh3118.2 (4)C41—C42—C43110.5 (6)
C29—N8—Rh4123.0 (5)C41—C42—H42A109.5
C29—N8—H8118.5C43—C42—H42A109.5
Rh4—N8—H8118.5C41—C42—H42B109.5
C33—N9—Rh5124.6 (5)C43—C42—H42B109.5
C33—N9—H9117.7H42A—C42—H42B108.1
Rh5—N9—H9117.7C42—C43—C44111.7 (8)
C33—O9—Rh5ii117.0 (4)C42—C43—H43A109.3
C37—N10—Rh5124.5 (5)C44—C43—H43A109.3
C37—N10—H10117.8C42—C43—H43B109.3
Rh5—N10—H10117.8C44—C43—H43B109.3
C37—O10—Rh5ii117.6 (4)H43A—C43—H43B107.9
C41—N11—Rh6123.8 (5)C43—C44—H44A109.5
C41—N11—H11118.1C43—C44—H44B109.5
Rh6—N11—H11118.1H44A—C44—H44B109.5
C41—O11—Rh6iii117.3 (4)C43—C44—H44C109.5
C45—N12—Rh6123.9 (5)H44A—C44—H44C109.5
C45—N12—H12118.0H44B—C44—H44C109.5
Rh6—N12—H12118.0O12—C45—N12123.1 (7)
C45—O12—Rh6iii116.8 (5)O12—C45—C46117.5 (7)
C49—N13—Rh7126.8 (5)N12—C45—C46119.3 (7)
C49—N13—H13116.6C45—C46—C47116.6 (6)
Rh7—N13—H13116.6C45—C46—H46A108.1
C49—O13—Rh7iv117.0 (4)C47—C46—H46A108.1
C53—N14—Rh7123.2 (5)C45—C46—H46B108.1
C53—N14—H14118.4C47—C46—H46B108.1
Rh7—N14—H14118.4H46A—C46—H46B107.3
C53—O14—Rh7iv118.1 (5)C46—C47—C48110.6 (7)
C57—N15—Rh8123.9 (5)C46—C47—H47A109.5
C57—N15—H15118.0C48—C47—H47A109.5
Rh8—N15—H15118.0C46—C47—H47B109.5
C57—O15—Rh8v117.7 (4)C48—C47—H47B109.5
C61—N16—Rh8125.3 (5)H47A—C47—H47B108.1
C61—N16—H16117.4C47—C48—H48A109.5
Rh8—N16—H16117.4C47—C48—H48B109.5
C61—O16—Rh8v117.9 (4)H48A—C48—H48B109.5
Mo1—O17—Rh1122.7 (2)C47—C48—H48C109.5
Mo1—O18—Rh3119.2 (2)H48A—C48—H48C109.5
Mo1—O19—Rh5119.4 (2)H48B—C48—H48C109.5
Mo1—O20—Rh6120.5 (2)O13—C49—N13120.5 (7)
Mo2—O21—Rh2118.9 (2)O13—C49—C50116.5 (6)
Mo2—O22—Rh4vi120.3 (2)N13—C49—C50123.0 (6)
Mo2—O23—Rh7118.2 (2)C49—C50—C51115.7 (6)
Mo2—O24—Rh8121.6 (2)C49—C50—H50A108.3
O1—C1—N1122.6 (6)C51—C50—H50A108.3
O1—C1—C2116.8 (6)C49—C50—H50B108.3
N1—C1—C2120.4 (6)C51—C50—H50B108.3
C1—C2—C3B108.7 (7)H50A—C50—H50B107.4
C1—C2—C3A112.8 (13)C50—C51—C52112.7 (7)
C3B—C2—C3A10 (2)C50—C51—H51A109.0
C1—C2—H2A109.9C52—C51—H51A109.0
C3B—C2—H2A109.9C50—C51—H51B109.0
C3A—C2—H2A99.5C52—C51—H51B109.0
C1—C2—H2B109.9H51A—C51—H51B107.8
C3B—C2—H2B109.9C51—C52—H52A109.5
C3A—C2—H2B115.7C51—C52—H52B109.5
H2A—C2—H2B108.3H52A—C52—H52B109.5
C1—C2—H2C109.0C51—C52—H52C109.5
C3B—C2—H2C119.3H52A—C52—H52C109.5
C3A—C2—H2C109.0H52B—C52—H52C109.5
H2A—C2—H2C10.6O14—C53—N14122.6 (7)
H2B—C2—H2C99.4O14—C53—C54118.2 (6)
C1—C2—H2D109.0N14—C53—C54119.3 (6)
C3B—C2—H2D102.4C53—C54—C55114.8 (6)
C3A—C2—H2D109.0C53—C54—H54A108.6
H2A—C2—H2D116.3C55—C54—H54A108.6
H2B—C2—H2D9.0C53—C54—H54B108.6
H2C—C2—H2D107.8C55—C54—H54B108.6
C2—C3A—C4A89 (3)H54A—C54—H54B107.6
C2—C3A—H3A113.8C54—C55—C56112.7 (6)
C4A—C3A—H3A113.8C54—C55—H55A109.1
C2—C3A—H3B113.8C56—C55—H55A109.1
C4A—C3A—H3B113.8C54—C55—H55B109.1
H3A—C3A—H3B111.1C56—C55—H55B109.1
C3A—C4A—H4A109.5H55A—C55—H55B107.8
C3A—C4A—H4B109.5C55—C56—H56A109.5
H4A—C4A—H4B109.5C55—C56—H56B109.5
C3A—C4A—H4C109.5H56A—C56—H56B109.5
H4A—C4A—H4C109.5C55—C56—H56C109.5
H4B—C4A—H4C109.5H56A—C56—H56C109.5
C2—C3B—C4B110.6 (11)H56B—C56—H56C109.5
C2—C3B—H3C109.5O15—C57—N15122.5 (6)
C4B—C3B—H3C109.5O15—C57—C58116.7 (7)
C2—C3B—H3D109.5N15—C57—C58120.6 (7)
C4B—C3B—H3D109.5C57—C58—C59111.8 (6)
H3C—C3B—H3D108.1C57—C58—H58A109.3
C3B—C4B—H4D109.5C59—C58—H58A109.3
C3B—C4B—H4E109.5C57—C58—H58B109.3
H4D—C4B—H4E109.5C59—C58—H58B109.3
C3B—C4B—H4F109.5H58A—C58—H58B107.9
H4D—C4B—H4F109.5C58—C59—C60113.1 (6)
H4E—C4B—H4F109.5C58—C59—H59A109.0
O2—C5—N2122.8 (6)C60—C59—H59A109.0
O2—C5—C6118.2 (6)C58—C59—H59B109.0
N2—C5—C6118.9 (7)C60—C59—H59B109.0
C5—C6—C7111.9 (6)H59A—C59—H59B107.8
C5—C6—H6A109.2C59—C60—H60A109.5
C7—C6—H6A109.2C59—C60—H60B109.5
C5—C6—H6B109.2H60A—C60—H60B109.5
C7—C6—H6B109.2C59—C60—H60C109.5
H6A—C6—H6B107.9H60A—C60—H60C109.5
C8—C7—C6112.6 (6)H60B—C60—H60C109.5
C8—C7—H7A109.1O16—C61—N16121.6 (6)
C6—C7—H7A109.1O16—C61—C62117.0 (6)
C8—C7—H7B109.1N16—C61—C62121.4 (6)
C6—C7—H7B109.1C63—C62—C61116.1 (6)
H7A—C7—H7B107.8C63—C62—H62A108.3
C7—C8—H8A109.5C61—C62—H62A108.3
C7—C8—H8B109.5C63—C62—H62B108.3
H8A—C8—H8B109.5C61—C62—H62B108.3
C7—C8—H8C109.5H62A—C62—H62B107.4
H8A—C8—H8C109.5C62—C63—C64112.6 (6)
H8B—C8—H8C109.5C62—C63—H63A109.1
O3—C9—N3121.3 (6)C64—C63—H63A109.1
O3—C9—C10116.8 (6)C62—C63—H63B109.1
N3—C9—C10121.9 (6)C64—C63—H63B109.1
C9—C10—C11114.7 (5)H63A—C63—H63B107.8
C9—C10—H10A108.6C63—C64—H64A109.5
C11—C10—H10A108.6C63—C64—H64B109.5
C9—C10—H10B108.6H64A—C64—H64B109.5
C11—C10—H10B108.6C63—C64—H64C109.5
H10A—C10—H10B107.6H64A—C64—H64C109.5
C10—C11—C12110.8 (6)H64B—C64—H64C109.5
C10—C11—H11A109.5
N2—Rh1—Rh2—N4179.7 (2)N2—Rh1—O17—Mo144.2 (3)
N1—Rh1—Rh2—N489.5 (2)N1—Rh1—O17—Mo145.7 (3)
O4—Rh1—Rh2—N41.7 (2)O4—Rh1—O17—Mo1137.0 (2)
O3—Rh1—Rh2—N490.4 (2)O3—Rh1—O17—Mo1134.1 (2)
O17—Rh1—Rh2—N4128.7 (10)Rh2—Rh1—O17—Mo16.7 (12)
N2—Rh1—Rh2—N388.3 (2)O17—Mo1—O18—Rh350.3 (3)
N1—Rh1—Rh2—N3178.5 (2)O19—Mo1—O18—Rh3169.6 (2)
O4—Rh1—Rh2—N390.3 (2)O20—Mo1—O18—Rh370.2 (3)
O3—Rh1—Rh2—N31.5 (2)N5—Rh3—O18—Mo138.8 (3)
O17—Rh1—Rh2—N3139.4 (10)N6—Rh3—O18—Mo152.2 (3)
N2—Rh1—Rh2—O186.8 (2)O8—Rh3—O18—Mo1130.4 (3)
N1—Rh1—Rh2—O13.4 (2)O7—Rh3—O18—Mo1142.5 (3)
O4—Rh1—Rh2—O194.58 (19)Rh4—Rh3—O18—Mo170 (3)
O3—Rh1—Rh2—O1176.69 (19)O18—Mo1—O19—Rh558.3 (3)
O17—Rh1—Rh2—O135.8 (10)O17—Mo1—O19—Rh561.4 (3)
N2—Rh1—Rh2—O20.5 (2)O20—Mo1—O19—Rh5178.4 (2)
N1—Rh1—Rh2—O290.75 (19)N10—Rh5—O19—Mo149.2 (3)
O4—Rh1—Rh2—O2178.07 (17)N9—Rh5—O19—Mo141.1 (3)
O3—Rh1—Rh2—O289.33 (18)O10ii—Rh5—O19—Mo1132.0 (3)
O17—Rh1—Rh2—O251.6 (10)O9ii—Rh5—O19—Mo1140.9 (3)
N2—Rh1—Rh2—O21100.8 (16)Rh5ii—Rh5—O19—Mo151 (3)
N1—Rh1—Rh2—O2110.5 (16)O18—Mo1—O20—Rh669.3 (3)
O4—Rh1—Rh2—O2180.7 (16)O17—Mo1—O20—Rh6170.5 (2)
O3—Rh1—Rh2—O21169.4 (16)O19—Mo1—O20—Rh651.0 (3)
O17—Rh1—Rh2—O2149.7 (18)N12—Rh6—O20—Mo165.9 (3)
N5—Rh3—Rh4—N7175.9 (2)N11—Rh6—O20—Mo125.1 (3)
N6—Rh3—Rh4—N792.8 (2)O11iii—Rh6—O20—Mo1157.0 (3)
O8—Rh3—Rh4—N784.7 (2)O12iii—Rh6—O20—Mo1114.6 (3)
O7—Rh3—Rh4—N72.56 (19)Rh6iii—Rh6—O20—Mo1114.4 (13)
O18—Rh3—Rh4—N775 (2)O23—Mo2—O21—Rh263.5 (3)
N5—Rh3—Rh4—N886.8 (2)O24—Mo2—O21—Rh258.7 (3)
N6—Rh3—Rh4—N8178.1 (2)O22—Mo2—O21—Rh2177.47 (19)
O8—Rh3—Rh4—N84.5 (2)N4—Rh2—O21—Mo246.6 (3)
O7—Rh3—Rh4—N891.7 (2)N3—Rh2—O21—Mo245.6 (3)
O18—Rh3—Rh4—N8165 (2)O1—Rh2—O21—Mo2139.2 (2)
N5—Rh3—Rh4—O53.25 (19)O2—Rh2—O21—Mo2133.5 (2)
N6—Rh3—Rh4—O588.0 (2)Rh1—Rh2—O21—Mo2125.2 (15)
O8—Rh3—Rh4—O594.52 (19)O23—Mo2—O22—Rh4vi170.7 (2)
O7—Rh3—Rh4—O5178.25 (17)O24—Mo2—O22—Rh4vi68.3 (3)
O18—Rh3—Rh4—O5105 (2)O21—Mo2—O22—Rh4vi51.7 (3)
N5—Rh3—Rh4—O692.6 (2)O24—Mo2—O23—Rh7172.4 (2)
N6—Rh3—Rh4—O61.3 (2)O21—Mo2—O23—Rh766.1 (3)
O8—Rh3—Rh4—O6176.13 (19)O22—Mo2—O23—Rh753.4 (3)
O7—Rh3—Rh4—O688.90 (18)N13—Rh7—O23—Mo247.0 (3)
O18—Rh3—Rh4—O616 (2)N14—Rh7—O23—Mo245.0 (3)
N5—Rh3—Rh4—O22i15.1 (19)O14iv—Rh7—O23—Mo2137.0 (3)
N6—Rh3—Rh4—O22i76.2 (19)O13iv—Rh7—O23—Mo2134.4 (3)
O8—Rh3—Rh4—O22i106.4 (19)Rh7iv—Rh7—O23—Mo210 (6)
O7—Rh3—Rh4—O22i166.4 (19)O23—Mo2—O24—Rh857.4 (3)
O18—Rh3—Rh4—O22i94 (3)O21—Mo2—O24—Rh8178.2 (2)
N2—Rh1—N1—C177.4 (5)O22—Mo2—O24—Rh862.1 (3)
O4—Rh1—N1—C199.1 (5)N16—Rh8—O24—Mo253.4 (3)
O3—Rh1—N1—C19 (3)N15—Rh8—O24—Mo237.4 (3)
O17—Rh1—N1—C1167.9 (5)O15v—Rh8—O24—Mo2144.6 (3)
Rh2—Rh1—N1—C18.4 (5)O16v—Rh8—O24—Mo2127.3 (3)
N4—Rh2—O1—C185.3 (5)Rh8v—Rh8—O24—Mo244.0 (14)
N3—Rh2—O1—C151 (2)Rh2—O1—C1—N16.5 (8)
O2—Rh2—O1—C190.0 (5)Rh2—O1—C1—C2168.9 (4)
O21—Rh2—O1—C1179.1 (5)Rh1—N1—C1—O111.3 (9)
Rh1—Rh2—O1—C10.2 (5)Rh1—N1—C1—C2164.0 (4)
N1—Rh1—N2—C586.3 (6)O1—C1—C2—C3B80.6 (13)
O4—Rh1—N2—C522 (4)N1—C1—C2—C3B94.9 (13)
O3—Rh1—N2—C589.3 (6)O1—C1—C2—C3A70 (2)
O17—Rh1—N2—C5175.9 (6)N1—C1—C2—C3A105 (2)
Rh2—Rh1—N2—C50.4 (5)C1—C2—C3A—C4A154 (3)
N4—Rh2—O2—C54 (3)C3B—C2—C3A—C4A85 (9)
N3—Rh2—O2—C587.1 (5)C1—C2—C3B—C4B173.2 (14)
O1—Rh2—O2—C589.0 (5)C3A—C2—C3B—C4B59 (8)
O21—Rh2—O2—C5174.8 (5)Rh2—O2—C5—N20.8 (9)
Rh1—Rh2—O2—C50.8 (5)Rh2—O2—C5—C6178.2 (5)
N2—Rh1—O3—C981.6 (5)Rh1—N2—C5—O20.2 (10)
N1—Rh1—O3—C95 (3)Rh1—N2—C5—C6177.5 (5)
O4—Rh1—O3—C995.0 (5)O2—C5—C6—C785.5 (8)
O17—Rh1—O3—C9172.1 (5)N2—C5—C6—C792.0 (8)
Rh2—Rh1—O3—C94.3 (5)C5—C6—C7—C867.3 (9)
N4—Rh2—N3—C985.8 (6)Rh1—O3—C9—N35.9 (9)
O1—Rh2—N3—C950 (2)Rh1—O3—C9—C10174.0 (4)
O2—Rh2—N3—C989.5 (6)Rh2—N3—C9—O34.3 (10)
O21—Rh2—N3—C9180.0 (6)Rh2—N3—C9—C10175.6 (5)
Rh1—Rh2—N3—C90.7 (5)O3—C9—C10—C1169.5 (9)
N2—Rh1—O4—C1322 (3)N3—C9—C10—C11110.6 (8)
N1—Rh1—O4—C1386.1 (5)C9—C10—C11—C12169.3 (7)
O3—Rh1—O4—C1389.5 (5)Rh1—O4—C13—N43.1 (8)
O17—Rh1—O4—C13175.7 (5)Rh1—O4—C13—C14174.9 (4)
Rh2—Rh1—O4—C130.1 (5)Rh2—N4—C13—O45.5 (9)
N3—Rh2—N4—C1381.9 (6)Rh2—N4—C13—C14172.3 (4)
O1—Rh2—N4—C1393.8 (5)O4—C13—C14—C1557.9 (8)
O2—Rh2—N4—C131 (3)N4—C13—C14—C15120.1 (7)
O21—Rh2—N4—C13179.9 (5)C13—C14—C15—C1658.8 (8)
Rh1—Rh2—N4—C134.2 (5)Rh4—O5—C17—N50.2 (8)
N6—Rh3—N5—C1781.7 (5)Rh4—O5—C17—C18179.7 (4)
O8—Rh3—N5—C1794.4 (5)Rh3—N5—C17—O54.4 (9)
O7—Rh3—N5—C1724 (3)Rh3—N5—C17—C18176.1 (4)
O18—Rh3—N5—C17172.3 (5)O5—C17—C18—C19114.1 (7)
Rh4—Rh3—N5—C175.0 (5)N5—C17—C18—C1965.4 (8)
N7—Rh4—O5—C1710 (4)C17—C18—C19—C2056.7 (8)
N8—Rh4—O5—C1783.6 (5)Rh4—O6—C21—N61.5 (9)
O6—Rh4—O5—C1792.0 (5)Rh4—O6—C21—C22177.4 (5)
O22i—Rh4—O5—C17178.0 (5)Rh3—N6—C21—O60.1 (10)
Rh3—Rh4—O5—C172.7 (4)Rh3—N6—C21—C22175.7 (5)
N5—Rh3—N6—C2186.4 (6)O6—C21—C22—C2357.2 (8)
O8—Rh3—N6—C2133 (3)N6—C21—C22—C23118.8 (7)
O7—Rh3—N6—C2189.1 (6)C21—C22—C23—C2461.9 (8)
O18—Rh3—N6—C21177.9 (6)Rh3—O7—C25—N78.1 (8)
Rh4—Rh3—N6—C211.3 (5)Rh3—O7—C25—C26169.5 (4)
N7—Rh4—O6—C2187.4 (5)Rh4—N7—C25—O75.4 (9)
N8—Rh4—O6—C216 (3)Rh4—N7—C25—C26172.0 (5)
O5—Rh4—O6—C2189.1 (5)O7—C25—C26—C2745.7 (9)
O22i—Rh4—O6—C21174.9 (5)N7—C25—C26—C27131.8 (7)
Rh3—Rh4—O6—C211.9 (5)C25—C26—C27—C2861.2 (9)
N5—Rh3—O7—C2512 (2)Rh3—O8—C29—N81.5 (9)
N6—Rh3—O7—C2593.0 (5)Rh3—O8—C29—C30179.2 (5)
O8—Rh3—O7—C2583.3 (5)Rh4—N8—C29—O87.3 (10)
O18—Rh3—O7—C25176.6 (5)Rh4—N8—C29—C30173.5 (5)
Rh4—Rh3—O7—C256.1 (4)O8—C29—C30—C31141.9 (7)
N8—Rh4—N7—C2586.1 (6)N8—C29—C30—C3138.8 (10)
O5—Rh4—N7—C2513 (4)C29—C30—C31—C32177.9 (7)
O6—Rh4—N7—C2589.5 (5)Rh5ii—O9—C33—N93.3 (9)
O22i—Rh4—N7—C25179.7 (5)Rh5ii—O9—C33—C34174.3 (5)
Rh3—Rh4—N7—C250.3 (5)Rh5—N9—C33—O96.3 (10)
N5—Rh3—O8—C2982.1 (5)Rh5—N9—C33—C34171.1 (5)
N6—Rh3—O8—C2938 (3)O9—C33—C34—C3559.1 (9)
O7—Rh3—O8—C2993.5 (5)N9—C33—C34—C35118.4 (8)
O18—Rh3—O8—C29177.8 (5)C33—C34—C35—C3655.9 (9)
Rh4—Rh3—O8—C293.2 (5)Rh5ii—O10—C37—N101.8 (9)
N7—Rh4—N8—C2978.1 (6)Rh5ii—O10—C37—C38179.3 (5)
O5—Rh4—N8—C2998.4 (6)Rh5—N10—C37—O103.5 (9)
O6—Rh4—N8—C2915 (3)Rh5—N10—C37—C38177.6 (5)
O22i—Rh4—N8—C29175.8 (6)O10—C37—C38—C39104.9 (8)
Rh3—Rh4—N8—C297.5 (5)N10—C37—C38—C3974.0 (8)
N10—Rh5—N9—C3381.0 (6)C37—C38—C39—C4056.1 (8)
O10ii—Rh5—N9—C3395.2 (6)Rh6—N11—C41—O113.6 (10)
O9ii—Rh5—N9—C3335 (3)Rh6—N11—C41—C42174.6 (5)
O19—Rh5—N9—C33172.5 (6)Rh6iii—O11—C41—N110.6 (9)
Rh5ii—Rh5—N9—C335.0 (6)Rh6iii—O11—C41—C42177.7 (5)
N9—Rh5—N10—C3782.6 (6)N11—C41—C42—C43109.2 (8)
O10ii—Rh5—N10—C3722 (4)O11—C41—C42—C4369.2 (9)
O9ii—Rh5—N10—C3793.4 (6)C41—C42—C43—C4472.2 (8)
O19—Rh5—N10—C37177.2 (6)Rh6iii—O12—C45—N123.6 (8)
Rh5ii—Rh5—N10—C372.9 (5)Rh6iii—O12—C45—C46172.9 (4)
N12—Rh6—N11—C4182.0 (6)Rh6—N12—C45—O123.7 (9)
O11iii—Rh6—N11—C4132 (3)Rh6—N12—C45—C46172.8 (4)
O12iii—Rh6—N11—C4194.2 (6)O12—C45—C46—C4736.8 (9)
O20—Rh6—N11—C41173.4 (6)N12—C45—C46—C47146.5 (7)
Rh6iii—Rh6—N11—C413.8 (6)C45—C46—C47—C4868.0 (9)
N11—Rh6—N12—C4587.1 (5)Rh7iv—O13—C49—N130.7 (9)
O11iii—Rh6—N12—C4588.5 (5)Rh7iv—O13—C49—C50179.8 (5)
O12iii—Rh6—N12—C451 (3)Rh7—N13—C49—O131.2 (10)
O20—Rh6—N12—C45175.2 (5)Rh7—N13—C49—C50178.3 (6)
Rh6iii—Rh6—N12—C451.6 (5)O13—C49—C50—C51152.7 (7)
N14—Rh7—N13—C4984.1 (6)N13—C49—C50—C5127.7 (11)
O14iv—Rh7—N13—C4991.7 (6)C49—C50—C51—C52178.3 (7)
O13iv—Rh7—N13—C4920 (3)Rh7iv—O14—C53—N140.3 (9)
O23—Rh7—N13—C49177.3 (6)Rh7iv—O14—C53—C54179.2 (5)
Rh7iv—Rh7—N13—C491.9 (6)Rh7—N14—C53—O142.3 (10)
N13—Rh7—N14—C5381.5 (6)Rh7—N14—C53—C54178.2 (5)
O14iv—Rh7—N14—C5330 (3)O14—C53—C54—C55133.7 (7)
O13iv—Rh7—N14—C5394.0 (6)N14—C53—C54—C5546.8 (9)
O23—Rh7—N14—C53176.0 (6)C53—C54—C55—C56178.8 (6)
Rh7iv—Rh7—N14—C532.9 (6)Rh8v—O15—C57—N150.4 (8)
N16—Rh8—N15—C5781.7 (5)Rh8v—O15—C57—C58175.3 (4)
O15v—Rh8—N15—C5733 (3)Rh8—N15—C57—O153.4 (9)
O16v—Rh8—N15—C5793.4 (5)Rh8—N15—C57—C58172.0 (5)
O24—Rh8—N15—C57171.0 (5)O15—C57—C58—C5958.8 (8)
Rh8v—Rh8—N15—C573.8 (5)N15—C57—C58—C59117.0 (7)
N15—Rh8—N16—C6183.3 (6)C57—C58—C59—C6057.3 (9)
O15v—Rh8—N16—C6192.3 (6)Rh8v—O16—C61—N162.6 (8)
O16v—Rh8—N16—C6112 (3)Rh8v—O16—C61—C62176.1 (4)
O24—Rh8—N16—C61176.6 (6)Rh8—N16—C61—O163.8 (9)
Rh8v—Rh8—N16—C612.5 (5)Rh8—N16—C61—C62174.9 (5)
O18—Mo1—O17—Rh1176.1 (2)O16—C61—C62—C63172.0 (6)
O19—Mo1—O17—Rh164.0 (3)N16—C61—C62—C639.3 (10)
O20—Mo1—O17—Rh156.0 (3)C61—C62—C63—C64178.1 (6)
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z; (iii) x, y, z; (iv) x+1, y, z+1; (v) x+1, y+1, z+1; (vi) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O190.882.303.049 (7)144
N1—H1···O10ii0.882.593.294 (6)138
N2—H2···O200.882.192.976 (7)149
N3—H3···O230.882.403.177 (7)147
N4—H4···O240.882.213.001 (7)149
N5—H5···O170.882.102.868 (7)145
N6—H6···O200.882.343.133 (7)151
N7—H7···O21i0.882.172.969 (7)151
N8—H8···O24i0.882.463.203 (7)142
N9—H9···O170.882.223.004 (6)148
N10—H10···O180.882.192.950 (6)144
N11—H11···O190.882.152.967 (7)154
N12—H12···O180.882.653.370 (8)140
N13—H13···O220.882.162.916 (6)144
N14—H14···O210.882.273.064 (6)150
N15—H15···O220.882.253.053 (7)152
N16—H16···O230.882.343.067 (7)140
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formulaC16H32CrN8O12Rh4C16H32MoN8O12Rh4C16H32N8O12Rh4WC16H32CrN8O12Ru4
Mr992.141036.081123.99984.78
Crystal system, space groupTetragonal, I41/aTetragonal, I41/aTetragonal, I41/aTetragonal, I41/a
Temperature (K)296296296296
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, 9090, 90, 9090, 90, 9090, 90, 90
V3)2650.2 (4)2714.8 (4)2724.8 (4)2678.9 (3)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)2.912.906.652.67
Crystal size (mm)0.10 × 0.10 × 0.100.10 × 0.10 × 0.060.05 × 0.03 × 0.030.08 × 0.08 × 0.06
Data collection
DiffractometerRigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Absorption correctionIntegration
(Higashi, 1999)
Integration
(Higashi, 1999)
Integration
(Higashi, 1999)
Integration
(Higashi, 1999)
Tmin, Tmax0.759, 0.8060.731, 0.8560.672, 0.8010.833, 0.871
No. of measured, independent and
observed [I > 2σ(I)] reflections
10792, 1528, 1383 11116, 1557, 1393 11140, 1566, 1265 10957, 1539, 1475
Rint0.0600.0670.0800.042
(sin θ/λ)max1)0.6490.6490.6490.649
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 reflections1528155715661539
No. of parameters95959595
No. of restraints0000
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-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 Å3)0.49, 0.680.71, 0.710.86, 0.630.58, 0.49


(V)(VI)(VII)(VIII)
Crystal data
Chemical formulaC16H32MoN8O12Ru4C16H32N8O12Ru4WC24H48CrN8O12Rh4·1.08(H2O)C24H48MoN8O12Rh4·2.44(OH2)
Mr1028.721116.631123.761191.52
Crystal system, space groupTetragonal, I41/aTetragonal, I41/aTriclinic, P1Triclinic, P1
Temperature (K)296296296223
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, 9090, 90, 90112.405 (5), 101.362 (4), 106.816 (5)112.460 (2), 99.574 (2), 108.472 (3)
V3)2730.2 (3)2743.9 (4)2120.1 (8)2180.4 (13)
Z4422
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)2.686.401.831.83
Crystal size (mm)0.30 × 0.10 × 0.100.06 × 0.06 × 0.040.30 × 0.10 × 0.100.50 × 0.30 × 0.20
Data collection
DiffractometerRigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Absorption correctionIntegration
(Higashi, 1999)
Integration
(Higashi, 1999)
Integration
(Higashi, 1999)
Integration
(Higashi, 1999)
Tmin, Tmax0.844, 0.9310.621, 0.8310.843, 0.9450.581, 0.859
No. of measured, independent and
observed [I > 2σ(I)] reflections
10984, 1568, 1156 10895, 1580, 1543 17505, 9650, 6828 17845, 9884, 8783
Rint0.1120.0500.0650.030
(sin θ/λ)max1)0.6490.6490.6490.649
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 reflections1568158096509884
No. of parameters9696588543
No. of restraints00394178
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-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 Å3)0.99, 0.840.64, 0.800.88, 0.930.72, 0.84


(IX)
Crystal data
Chemical formulaC32H64MoN8O12Rh4
Mr1260.49
Crystal system, space groupTriclinic, 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)
V3)4621.6 (19)
Z4
Radiation typeMo Kα
µ (mm1)1.72
Crystal size (mm)0.10 × 0.10 × 0.10
Data collection
DiffractometerRigaku/MSC Mercury CCD
diffractometer
Absorption correctionIntegration
NUMABS (Higashi, 1999)
Tmin, Tmax0.804, 0.902
No. of measured, independent and
observed [I > 2σ(I)] reflections
38498, 21025, 13532
Rint0.066
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.062, 0.104, 1.02
No. of reflections21025
No. of parameters1043
No. of restraints33
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0273P)2]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)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).

Selected geometric parameters (Å, º) for (I) top
Rh1—N1i1.959 (4)Rh1—O32.235 (4)
Rh1—N2i1.998 (4)Rh1—Rh1i2.4225 (8)
Rh1—O12.014 (4)Cr1—O31.653 (4)
Rh1—O22.041 (4)
O3—Rh1—Rh1i171.99 (11)O3iii—Cr1—O3110.79 (14)
O3—Cr1—O3ii106.9 (3)Cr1—O3—Rh1147.9 (2)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.383.076 (5)137.8
N2—H2···O2v0.862.323.150 (5)162.0
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (II) top
Rh1—N1i1.975 (6)Rh1—O32.219 (5)
Rh1—N2i1.986 (6)Rh1—Rh1i2.4170 (11)
Rh1—O12.026 (5)Mo1—O31.758 (5)
Rh1—O22.034 (5)
O3—Rh1—Rh1i173.02 (14)O3iii—Mo1—O3111.12 (18)
O3—Mo1—O3ii106.2 (3)Mo1—O3—Rh1147.0 (3)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.443.152 (8)140.2
N2—H2···O2v0.862.333.170 (7)164.4
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (III) top
Rh1—N1i1.965 (7)Rh1—O32.221 (5)
Rh1—N2i2.000 (6)Rh1—Rh1i2.4161 (11)
Rh1—O22.033 (5)W1—O31.770 (6)
Rh1—O12.034 (5)
O3—Rh1—Rh1i173.05 (16)O3iii—W1—O3111.1 (2)
O3—W1—O3ii106.3 (4)W1—O3—Rh1146.8 (3)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.473.174 (8)139.7
N2—H2···O2v0.862.333.168 (8)165.3
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (IV) top
Ru1—N1i2.006 (3)Ru1—O32.261 (3)
Ru1—N2i2.033 (3)Ru1—Ru1i2.3068 (6)
Ru1—O12.041 (3)Cr1—O31.657 (3)
Ru1—O22.059 (3)
O3—Ru1—Ru1i171.26 (8)O3iii—Cr1—O3110.32 (11)
O3ii—Cr1—O3107.8 (2)Cr1—O3—Ru1151.18 (18)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.353.046 (4)137.7
N2—H2···O2v0.862.333.146 (4)159.4
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (V) top
Ru1—N1i2.015 (9)Ru1—O32.244 (5)
Ru1—N2i2.020 (9)Ru1—Ru1i2.2958 (12)
Ru1—O22.045 (7)Mo1—O31.769 (6)
Ru1—O12.063 (7)
O3—Ru1—Ru1i172.86 (18)O3—Mo1—O3iii111.1 (2)
O3ii—Mo1—O3106.2 (4)Mo1—O3—Ru1149.0 (4)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (V) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.423.122 (8)139.6
N2—H2···O2v0.862.323.154 (8)162.4
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (VI) top
Ru1—N1i2.021 (8)Ru1—O32.239 (5)
Ru1—N2i2.053 (7)Ru1—Ru1i2.2954 (9)
Ru1—O12.043 (6)W1—O31.780 (5)
Ru1—O22.048 (7)
O3—Ru1—Ru1i172.48 (15)O3iii—W1—O3110.56 (18)
O3—W1—O3ii107.3 (4)W1—O3—Ru1149.6 (3)
Symmetry codes: (i) x+1, y+1/2, z; (ii) x, y+1/2, z; (iii) y1/4, x+1/4, z+1/4.
Hydrogen-bond geometry (Å, º) for (VI) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O1iv0.862.403.122 (7)141.3
N2—H2···O2v0.862.323.147 (7)162.6
Symmetry codes: (iv) y+5/4, x+1/4, z+1/4; (v) x+1/2, y, z+1/2.
Selected geometric parameters (Å, º) for (VII) top
Rh1—N11.976 (8)Rh3—N51.980 (8)
Rh1—N21.956 (8)Rh3—N61.969 (6)
Rh1—O1i2.019 (7)Rh3—O5iii2.034 (7)
Rh1—O2i2.017 (7)Rh3—O6iii2.040 (6)
Rh1—O92.226 (5)Rh3—O112.179 (6)
Rh1—Rh1i2.4071 (14)Rh3—Rh3iii2.4053 (15)
Rh2—N31.992 (7)Rh4—N71.985 (9)
Rh2—N41.975 (7)Rh4—N81.977 (9)
Rh2—O3ii2.027 (6)Rh4—O7iv2.033 (7)
Rh2—O4ii2.030 (6)Rh4—O8iv2.016 (7)
Rh2—O102.207 (6)Rh4—O122.201 (6)
Rh2—Rh2ii2.4122 (15)Rh4—Rh4iv2.4076 (15)
O9—Rh1—Rh1i178.04 (17)O11—Cr1—O10108.4 (3)
O10—Rh2—Rh2ii177.28 (15)O12—Cr1—O10109.8 (3)
O11—Rh3—Rh3iii179.44 (18)O12—Cr1—O11110.4 (3)
O12—Rh4—Rh4iv179.67 (18)Cr1—O9—Rh1118.1 (3)
O9—Cr1—O10109.2 (3)Cr1—O10—Rh2119.7 (3)
O11—Cr1—O9110.1 (3)Cr1—O11—Rh3131.4 (3)
O12—Cr1—O9108.9 (3)Cr1—O12—Rh4121.1 (3)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x+1, y, z.
Hydrogen-bond geometry (Å, º) for (VII) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O120.862.322.963 (9)131.5
N2—H2···O100.862.122.917 (9)153.2
N3—H3···O90.862.192.965 (9)149.9
N4—H4···O110.862.333.015 (10)137.3
N5—H5···N40.862.663.404 (11)146.3
N6—H6···O90.862.092.860 (9)149.0
N7—H7···O100.862.192.978 (9)153.1
N8—H8···O110.862.373.016 (10)132.4
N8—H8···O5iii0.862.613.392 (11)151.3
Symmetry code: (iii) x+1, y, z+1.
Selected geometric parameters (Å, º) for (VIII) top
Rh1—N11.971 (3)Rh3—N51.986 (3)
Rh1—N21.987 (3)Rh3—N61.972 (3)
Rh1—O1i2.036 (3)Rh3—O5iii2.025 (3)
Rh1—O2i2.034 (3)Rh3—O6iii2.032 (3)
Rh1—O92.233 (2)Rh3—O112.207 (2)
Rh1—Rh1i2.4117 (8)Rh3—Rh3iii2.4037 (8)
Rh2—N31.980 (3)Rh4—N71.983 (3)
Rh2—N41.977 (3)Rh4—N81.965 (3)
Rh2—O3ii2.030 (3)Rh4—O7iv2.031 (3)
Rh2—O4ii2.039 (3)Rh4—O8iv2.038 (3)
Rh2—O102.214 (3)Rh4—O122.277 (3)
Rh2—Rh2ii2.4019 (9)Rh4—Rh4iv2.4148 (8)
O9—Rh1—Rh1i177.03 (7)O11—Mo1—O10109.17 (12)
O10—Rh2—Rh2ii178.87 (7)O12—Mo1—O10108.12 (12)
O11—Rh3—Rh3iii179.13 (7)O11—Mo1—O12111.64 (12)
O12—Rh4—Rh4iv177.80 (6)Mo1—O9—Rh1119.29 (13)
O9—Mo1—O10107.90 (13)Mo1—O10—Rh2122.07 (13)
O11—Mo1—O9108.53 (12)Mo1—O11—Rh3136.57 (14)
O9—Mo1—O12111.38 (12)Mo1—O12—Rh4129.21 (13)
Symmetry codes: (i) x+2, y, z+1; (ii) x+2, y+1, z+1; (iii) x+1, y, z; (iv) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) for (VIII) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O120.872.363.049 (4)135.8
N2—H2···O100.872.243.048 (4)155.5
N3—H3···O110.872.192.970 (4)148.4
N4—H4···O90.872.463.210 (4)144.2
N4—H4···O1i0.872.593.307 (4)139.8
N5—H5···O130.872.273.061 (5)152.0
N6—H6···O120.872.293.107 (4)156.0
N7—H7···N10.872.493.286 (5)153.1
N8—H8···O100.871.982.808 (4)158.9
Symmetry code: (i) x+2, y, z+1.
Selected geometric parameters (Å, º) for (IX) top
Rh1—N21.975 (5)Rh5—Rh5ii2.4080 (11)
Rh1—N11.977 (6)Rh6—N121.980 (6)
Rh1—O42.024 (4)Rh6—N111.995 (5)
Rh1—O32.041 (4)Rh6—O11iii2.027 (4)
Rh1—O172.254 (4)Rh6—O12iii2.032 (5)
Rh1—Rh22.4119 (9)Rh6—O202.262 (5)
Rh2—N41.980 (5)Rh6—Rh6iii2.4179 (12)
Rh2—N31.988 (6)Rh7—N131.969 (6)
Rh2—O12.025 (5)Rh7—N141.978 (6)
Rh2—O22.044 (4)Rh7—O14iv2.028 (5)
Rh2—O212.243 (4)Rh7—O13iv2.033 (5)
Rh3—N51.978 (5)Rh7—O232.285 (4)
Rh3—N61.986 (5)Rh7—Rh7iv2.4134 (11)
Rh3—O82.036 (4)Rh8—N161.968 (5)
Rh3—O72.036 (5)Rh8—N151.981 (5)
Rh3—O182.261 (4)Rh8—O15v2.028 (4)
Rh3—Rh42.4108 (9)Rh8—O16v2.044 (4)
Rh4—N71.987 (6)Rh8—O242.269 (5)
Rh4—N81.988 (5)Rh8—Rh8v2.4118 (12)
Rh4—O52.031 (5)Mo1—O181.760 (4)
Rh4—O62.043 (4)Mo1—O171.768 (5)
Rh4—O22i2.225 (4)Mo1—O191.770 (4)
Rh5—N101.968 (5)Mo1—O201.770 (4)
Rh5—N91.981 (6)Mo2—O231.766 (4)
Rh5—O10ii2.017 (5)Mo2—O241.769 (4)
Rh5—O9ii2.032 (5)Mo2—O211.772 (5)
Rh5—O192.242 (4)Mo2—O221.772 (4)
O17—Rh1—Rh2174.23 (12)O23—Mo2—O24111.3 (2)
O21—Rh2—Rh1175.57 (11)O23—Mo2—O21108.8 (2)
O18—Rh3—Rh4177.17 (12)O24—Mo2—O21110.12 (19)
O22i—Rh4—Rh3176.67 (12)O23—Mo2—O22108.86 (19)
O19—Rh5—Rh5ii177.52 (12)O24—Mo2—O22108.0 (2)
O20—Rh6—Rh6iii175.65 (12)O21—Mo2—O22109.7 (2)
O23—Rh7—Rh7iv178.68 (12)Mo1—O17—Rh1122.7 (2)
O24—Rh8—Rh8v174.75 (10)Mo1—O18—Rh3119.2 (2)
O18—Mo1—O17109.4 (2)Mo1—O19—Rh5119.4 (2)
O18—Mo1—O19109.70 (19)Mo1—O20—Rh6120.5 (2)
O17—Mo1—O19108.7 (2)Mo2—O21—Rh2118.9 (2)
O18—Mo1—O20109.4 (2)Mo2—O22—Rh4vi120.3 (2)
O17—Mo1—O20109.97 (19)Mo2—O23—Rh7118.2 (2)
O19—Mo1—O20109.6 (2)Mo2—O24—Rh8121.6 (2)
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z; (iii) x, y, z; (iv) x+1, y, z+1; (v) x+1, y+1, z+1; (vi) x+1, y, z.
Hydrogen-bond geometry (Å, º) for (IX) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O190.882.303.049 (7)143.6
N1—H1···O10ii0.882.593.294 (6)137.6
N2—H2···O200.882.192.976 (7)149.0
N3—H3···O230.882.403.177 (7)146.9
N4—H4···O240.882.213.001 (7)148.8
N5—H5···O170.882.102.868 (7)144.9
N6—H6···O200.882.343.133 (7)150.6
N7—H7···O21i0.882.172.969 (7)151.3
N8—H8···O24i0.882.463.203 (7)142.3
N9—H9···O170.882.223.004 (6)148.3
N10—H10···O180.882.192.950 (6)144.3
N11—H11···O190.882.152.967 (7)153.6
N12—H12···O180.882.653.370 (8)139.9
N13—H13···O220.882.162.916 (6)143.9
N14—H14···O210.882.273.064 (6)149.8
N15—H15···O220.882.253.053 (7)151.5
N16—H16···O230.882.343.067 (7)140.4
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z.
 

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