![](/logos/buttonlogos/cross.png)
![](/logos/buttonlogos/cross.png)
metal-organic compounds
Rubidium pentaaqua(L-serine)cobalt(II) hexahydrogenhexamolybdocobaltate(III) L-serine monosolvate decahydrate
aDepartment of Chemical Engineering, School of Engineering, Tokyo University of Agriculture and Technology, 2-24-16, Naka-cho, Koganei-city, Tokyo, Japan, bChemical Resouces Laboratory, Tokyo Institute of Technology, 4259, Nagatsuta, Midori-ku, Yokohama-city, Kanagawa, Japan, and cDivision of Applied Chemistry, Institute of Engineering, Tokyo University of Agriculture and Technology, 2-24-16, Naka-cho, Koganei-city, Tokyo, Japan
*Correspondence e-mail: j_iijima@cc.tuat.ac.jp
The Co2+ ion in the title compound, Rb[Co(C3H7NO3)(H2O)5][H6CoMo6O24]·C3H7NO3·10H2O, is coordinated by five water molecules and one O-monodentate L-serine ligand in a slightly distorted octahedral geometry. The Rb+ ion is irregularly coordinated by nine O atoms. In the crystal, the [H6CoIIIMo6O24]3− polyanions are stacked along the b-axis direction, mediated by bridging Rb—O bonds. N—H⋯O and O—H⋯O hydrogen bonds are observed involving the L-serine molecules.
CCDC reference: 966483
Related literature
For background to polyoxidometallates (POMs), see: Hasenknopf et al. (2008); Du et al. (2013
); Fang et al. (2005
); Kortz et al. (2002
); Sadakane et al. (2001
); Tan et al. (2007
); Inoue & Yamase (1995
). For C—O bond lengths in carboxylates, see: Lide (2007
). For bond-valence sums, see: Brown (1980
). For protonation of POMs, see: Perloff (1970
); Honda et al. (2007
); Yang et al. (2013
). For chiral POMs constructed from an Anderson-type POM as a building block, see: An et al. (2008
).
Experimental
Crystal data
|
|
Data collection: RAPID-AUTO (Rigaku/MSC, 2002); cell RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008
); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008
); molecular graphics: CrystalStructure (Rigaku, 2010
); software used to prepare material for publication: CrystalStructure.
Supporting information
CCDC reference: 966483
10.1107/S1600536813028304/hb7134sup1.cif
contains datablocks General, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536813028304/hb7134Isup2.hkl
An aqueous solution containing the Na salt of CoMo6, L-Ser, and CoCl2·6H2O with a molar ratio of 1:4:2 was acidified to pH = 3.2 by conc HCl and then boiled for 1 h. After cooling to room temperature, 5 eq. of RbClO4 to CoMo6 was added into the solution. Viridian thin platelets of the title compound were obtained at 4 °C being stood for several days.
Fragile thin platelet crystals of the title compound gave a medium absorption corrections (transmission factor ranging from 12.3 to 50.0%), resulting in a somewhat high residual electron densities around Mo1, Mo2, Mo4, and Mo6. Generally, a complete convergence of structure
with residual density less than 1 e Å-3 in difference Fourier synthesis indicates the success of structural analysis. However, for the compounds containing many heavy atoms, since the anisotropy of electron cloud around the heavy atoms makes difficult to conduct the ellipse approximation, the relative large residual densities cannot help being remaining. In the structural analysis of polyoxometalate consisting of a variety of heavy atoms such as Mo, V, and W, the relatively high residual densities have been frequently observed for the crystals with poor absorption corrections and crystallinity. In fact, after some elements were allocated to the pointed out densities, the refinements resulted in the divergence. Therefore, the pointed out high residual densities for Mo1, Mo2, Mo4, and Mo6 are not responsible for the incompleteness of structural analysis but the intrinsic crystal qualities such as morphology and crystallinity. All the atoms except for H atoms were refined anisotropically, and the H atoms were isotropically. The H atoms in L-Ser molecules were located in the calculated position, and the remaining H atoms were not included in the refinements. The residual density around O31 may be H atom. Due to the undesirable absorption correction, it is conceivable that high residual density corresponding to H atom is remained. In the polyoxometalate bearing many heavy atoms, the electron density for H atom is hard to be found. In order to escape from the divergence and lowering the accuracy of caused by intentional assignment of H atom to remarkable low electron density, for polyoxometalate compounds, the H atoms in water crystallization are not included in refinements. Therefore, the water of crystallization O atoms (O37 to O45) are refined without H atoms.Data collection: RAPID-AUTO (Rigaku/MSC, 2002); cell
RAPID-AUTO (Rigaku/MSC, 2002); data reduction: RAPID-AUTO (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2010); software used to prepare material for publication: CrystalStructure (Rigaku, 2010).Rb[Co(C3H7NO3)(H2O)5][H6CoMo6O24]·C3H7NO3·10H2O | F(000) = 3212.00 |
Mr = 1649.42 | Dx = 2.504 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 59700 reflections |
a = 10.8411 (5) Å | θ = 3.0–27.5° |
b = 11.5923 (4) Å | µ = 3.63 mm−1 |
c = 34.8078 (12) Å | T = 183 K |
V = 4374.4 (3) Å3 | Platelet, green |
Z = 4 | 0.41 × 0.36 × 0.19 mm |
Rigaku R-AXIS RAPID diffractometer | 9728 reflections with F2 > 2σ(F2) |
Detector resolution: 10.000 pixels mm-1 | Rint = 0.062 |
ω scans | θmax = 27.5° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −14→14 |
Tmin = 0.123, Tmax = 0.500 | k = −15→14 |
70065 measured reflections | l = −45→45 |
10010 independent reflections |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.099 | w = 1/[σ2(Fo2) + (0.0641P)2 + 9.0772P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
10010 reflections | Δρmax = 3.61 e Å−3 |
559 parameters | Δρmin = −1.10 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 4426 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.025 (7) |
Secondary atom site location: difference Fourier map |
Rb[Co(C3H7NO3)(H2O)5][H6CoMo6O24]·C3H7NO3·10H2O | V = 4374.4 (3) Å3 |
Mr = 1649.42 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 10.8411 (5) Å | µ = 3.63 mm−1 |
b = 11.5923 (4) Å | T = 183 K |
c = 34.8078 (12) Å | 0.41 × 0.36 × 0.19 mm |
Rigaku R-AXIS RAPID diffractometer | 10010 independent reflections |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | 9728 reflections with F2 > 2σ(F2) |
Tmin = 0.123, Tmax = 0.500 | Rint = 0.062 |
70065 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.099 | Δρmax = 3.61 e Å−3 |
S = 1.04 | Δρmin = −1.10 e Å−3 |
10010 reflections | Absolute structure: Flack (1983), 4426 Friedel pairs |
559 parameters | Absolute structure parameter: 0.025 (7) |
0 restraints |
Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY |
Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.98964 (4) | 0.94684 (3) | 0.207793 (11) | 0.01204 (9) | |
Mo2 | 0.74633 (3) | 0.84989 (3) | 0.159456 (12) | 0.01213 (9) | |
Mo3 | 0.49911 (3) | 0.75710 (3) | 0.205914 (11) | 0.01245 (9) | |
Mo4 | 0.50288 (4) | 0.74903 (3) | 0.301413 (11) | 0.01297 (9) | |
Mo5 | 0.74159 (3) | 0.84414 (3) | 0.349594 (12) | 0.01364 (9) | |
Mo6 | 0.98220 (4) | 0.94607 (3) | 0.303320 (11) | 0.01208 (9) | |
Rb1 | 0.73248 (5) | 0.52247 (4) | 0.145507 (15) | 0.02399 (11) | |
Co1 | 0.74451 (5) | 0.84817 (4) | 0.254347 (19) | 0.00969 (12) | |
Co2 | 0.67086 (6) | 0.46834 (6) | 0.043914 (18) | 0.01672 (14) | |
O1 | 1.0518 (4) | 1.0822 (4) | 0.20918 (11) | 0.0217 (8) | |
O2 | 1.0846 (4) | 0.8663 (4) | 0.17903 (10) | 0.0212 (8) | |
O3 | 0.8426 (4) | 0.7691 (3) | 0.13123 (10) | 0.0196 (7) | |
O4 | 0.6534 (4) | 0.9266 (4) | 0.12866 (10) | 0.0203 (8) | |
O5 | 0.4363 (4) | 0.6206 (3) | 0.20593 (11) | 0.0205 (8) | |
O6 | 0.4087 (4) | 0.8391 (4) | 0.17621 (10) | 0.0205 (8) | |
O7 | 0.4401 (4) | 0.6137 (3) | 0.29822 (11) | 0.0211 (8) | |
O8 | 0.4089 (4) | 0.8259 (3) | 0.33182 (10) | 0.0181 (8) | |
O9 | 0.6422 (4) | 0.9134 (4) | 0.37969 (11) | 0.0233 (8) | |
O10 | 0.8398 (4) | 0.7659 (4) | 0.37805 (10) | 0.0229 (8) | |
O11 | 1.0744 (3) | 0.8673 (3) | 0.33354 (10) | 0.0174 (7) | |
O12 | 1.0443 (4) | 1.0825 (3) | 0.30257 (11) | 0.0200 (8) | |
O13 | 0.8528 (3) | 0.9780 (3) | 0.17385 (9) | 0.0140 (7) | |
O14 | 0.6360 (3) | 0.7246 (3) | 0.17290 (10) | 0.0146 (7) | |
O15 | 0.4347 (3) | 0.8152 (3) | 0.25403 (10) | 0.0156 (7) | |
O16 | 0.6406 (4) | 0.7154 (3) | 0.33395 (10) | 0.0172 (7) | |
O17 | 0.8416 (3) | 0.9759 (3) | 0.33605 (10) | 0.0166 (7) | |
O18 | 1.0544 (3) | 0.8863 (3) | 0.25617 (10) | 0.0143 (7) | |
O19 | 0.8487 (3) | 0.7967 (3) | 0.29521 (9) | 0.0122 (7) | |
O20 | 0.8484 (3) | 0.9818 (3) | 0.25489 (9) | 0.0120 (6) | |
O21 | 0.8514 (3) | 0.7968 (3) | 0.21394 (9) | 0.0109 (7) | |
O22 | 0.6412 (3) | 0.9013 (3) | 0.21348 (9) | 0.0117 (7) | |
O23 | 0.6387 (3) | 0.7160 (3) | 0.25320 (10) | 0.0130 (6) | |
O24 | 0.6384 (3) | 0.8976 (3) | 0.29495 (9) | 0.0124 (7) | |
O25 | 1.0441 (4) | 0.5935 (4) | 0.04817 (12) | 0.0314 (10) | |
O26 | 1.2444 (4) | 0.5865 (4) | 0.06457 (11) | 0.0256 (8) | |
O27 | 1.1876 (4) | 0.8681 (4) | 0.06784 (11) | 0.0254 (8) | |
O28 | 0.7536 (3) | 0.3482 (3) | 0.08204 (10) | 0.0184 (7) | |
O29 | 0.9125 (4) | 0.2885 (4) | 0.04575 (11) | 0.0243 (8) | |
O30 | 0.7725 (4) | 0.0466 (4) | 0.05742 (11) | 0.0334 (10) | |
O31 | 0.7102 (3) | 0.5053 (3) | 0.23535 (11) | 0.0208 (8) | |
O32 | 0.5473 (4) | 0.5398 (4) | 0.08612 (11) | 0.0229 (8) | |
O33 | 0.5412 (4) | 0.3362 (4) | 0.03548 (11) | 0.0247 (8) | |
O34 | 0.7917 (4) | 0.4190 (4) | −0.00155 (10) | 0.0216 (8) | |
O35 | 0.7958 (4) | 0.5901 (4) | 0.06412 (11) | 0.0243 (8) | |
O36 | 0.5870 (4) | 0.5650 (4) | 0.00168 (11) | 0.0316 (10) | |
O37 | 0.6585 (4) | 0.2721 (4) | −0.04481 (11) | 0.0275 (9) | |
O38 | 0.2036 (4) | 0.6949 (4) | 0.2567 (2) | 0.0565 (18) | |
O39 | 0.9618 (4) | −0.2655 (4) | −0.09497 (11) | 0.0265 (9) | |
O40 | 0.8044 (4) | 0.0929 (4) | −0.01818 (11) | 0.0250 (9) | |
O41 | 1.3218 (5) | 1.0091 (4) | 0.12069 (12) | 0.0361 (10) | |
O42 | 0.2127 (4) | 0.6982 (4) | −0.04824 (14) | 0.0353 (10) | |
O43 | 0.5376 (5) | 0.1397 (4) | 0.08536 (14) | 0.0382 (11) | |
O44 | 0.3835 (4) | 0.6982 (4) | 0.01085 (12) | 0.0326 (10) | |
O45 | 0.4649 (5) | 0.9210 (4) | 0.02937 (13) | 0.0389 (11) | |
N1 | 1.2151 (5) | 0.6988 (4) | 0.13015 (12) | 0.0201 (9) | |
N2 | 0.7690 (4) | 0.1719 (4) | 0.13211 (14) | 0.0199 (9) | |
C1 | 1.1344 (5) | 0.6185 (5) | 0.06875 (15) | 0.0201 (10) | |
C2 | 1.1089 (5) | 0.7005 (5) | 0.10294 (14) | 0.0178 (10) | |
C3 | 1.0849 (6) | 0.8225 (5) | 0.08854 (16) | 0.0240 (11) | |
C4 | 0.8428 (5) | 0.2819 (5) | 0.07428 (13) | 0.0170 (10) | |
C5 | 0.8689 (5) | 0.1813 (5) | 0.10152 (15) | 0.0193 (10) | |
C6 | 0.8809 (6) | 0.0683 (5) | 0.07916 (16) | 0.0253 (12) | |
H1 | 1.0337 | 0.6727 | 0.1168 | 0.0214* | |
H2 | 1.0115 | 0.8221 | 0.0716 | 0.0288* | |
H13 | 0.6941 | 0.1642 | 0.1206 | 0.0238* | |
H12 | 0.7693 | 0.2367 | 0.1469 | 0.0238* | |
H14 | 0.7839 | 0.1092 | 0.1472 | 0.0238* | |
H3 | 1.0668 | 0.8732 | 0.1107 | 0.0288* | |
H4 | 1.2497 | 0.8700 | 0.0823 | 0.0305* | |
H5 | 1.1981 | 0.7449 | 0.1506 | 0.0241* | |
H6 | 1.2839 | 0.7251 | 0.1180 | 0.0241* | |
H7 | 1.2282 | 0.6254 | 0.1384 | 0.0241* | |
H8 | 0.9492 | 0.1966 | 0.1147 | 0.0231* | |
H9 | 0.9528 | 0.0728 | 0.0617 | 0.0304* | |
H10 | 0.8950 | 0.0039 | 0.0973 | 0.0304* | |
H11 | 0.7805 | −0.0157 | 0.0453 | 0.0401* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.00991 (17) | 0.01256 (18) | 0.01365 (17) | −0.00216 (14) | 0.00079 (14) | 0.00013 (14) |
Mo2 | 0.01080 (18) | 0.01307 (19) | 0.01252 (18) | −0.00066 (15) | −0.00029 (13) | 0.00023 (13) |
Mo3 | 0.00977 (18) | 0.01192 (18) | 0.01566 (18) | −0.00179 (15) | −0.00060 (14) | −0.00069 (14) |
Mo4 | 0.01106 (18) | 0.01205 (18) | 0.01579 (18) | −0.00148 (15) | 0.00241 (15) | 0.00050 (14) |
Mo5 | 0.01245 (19) | 0.01610 (19) | 0.01237 (18) | 0.00063 (16) | 0.00120 (13) | −0.00002 (14) |
Mo6 | 0.00996 (17) | 0.01245 (18) | 0.01384 (18) | −0.00125 (14) | −0.00103 (14) | −0.00076 (14) |
Rb1 | 0.0239 (3) | 0.0221 (3) | 0.0259 (3) | 0.0034 (2) | −0.00233 (19) | −0.0013 (2) |
Co1 | 0.0077 (3) | 0.0092 (3) | 0.0121 (3) | 0.0002 (2) | 0.0003 (2) | −0.0001 (2) |
Co2 | 0.0147 (3) | 0.0177 (3) | 0.0177 (3) | 0.0013 (3) | 0.0006 (3) | 0.0017 (3) |
O1 | 0.0194 (18) | 0.0199 (18) | 0.0257 (19) | −0.0014 (15) | 0.0031 (15) | 0.0068 (16) |
O2 | 0.0160 (17) | 0.029 (2) | 0.0191 (18) | 0.0003 (15) | 0.0028 (14) | −0.0047 (16) |
O3 | 0.0191 (18) | 0.0188 (17) | 0.0210 (17) | 0.0008 (15) | −0.0011 (14) | −0.0049 (15) |
O4 | 0.0196 (18) | 0.0209 (17) | 0.0204 (17) | −0.0006 (15) | −0.0066 (14) | 0.0056 (15) |
O5 | 0.0197 (18) | 0.0162 (16) | 0.0257 (19) | −0.0058 (14) | 0.0034 (15) | −0.0026 (15) |
O6 | 0.0161 (17) | 0.027 (2) | 0.0188 (17) | 0.0060 (16) | −0.0053 (14) | 0.0008 (16) |
O7 | 0.0223 (19) | 0.0164 (17) | 0.0246 (19) | −0.0067 (15) | −0.0016 (16) | 0.0025 (15) |
O8 | 0.0188 (18) | 0.0186 (18) | 0.0170 (17) | 0.0014 (14) | 0.0040 (14) | 0.0021 (15) |
O9 | 0.0195 (18) | 0.030 (2) | 0.0208 (18) | −0.0012 (15) | 0.0054 (15) | −0.0027 (16) |
O10 | 0.0213 (18) | 0.030 (2) | 0.0174 (18) | 0.0017 (16) | −0.0018 (15) | 0.0075 (16) |
O11 | 0.0159 (16) | 0.0191 (18) | 0.0174 (17) | 0.0009 (14) | −0.0011 (13) | 0.0013 (15) |
O12 | 0.0177 (18) | 0.0194 (17) | 0.0228 (18) | 0.0024 (14) | 0.0017 (15) | 0.0010 (15) |
O13 | 0.0140 (15) | 0.0110 (15) | 0.0169 (16) | −0.0037 (13) | −0.0031 (13) | 0.0025 (13) |
O14 | 0.0139 (16) | 0.0130 (15) | 0.0168 (16) | −0.0049 (13) | 0.0029 (13) | −0.0019 (14) |
O15 | 0.0102 (14) | 0.0157 (15) | 0.0209 (17) | 0.0005 (11) | 0.0018 (14) | 0.0014 (14) |
O16 | 0.0189 (18) | 0.0165 (17) | 0.0164 (17) | 0.0017 (14) | 0.0010 (13) | 0.0024 (14) |
O17 | 0.0148 (16) | 0.0171 (17) | 0.0179 (16) | 0.0012 (14) | 0.0000 (13) | −0.0055 (14) |
O18 | 0.0099 (14) | 0.0153 (15) | 0.0178 (16) | 0.0010 (11) | −0.0008 (13) | −0.0011 (14) |
O19 | 0.0120 (15) | 0.0107 (15) | 0.0139 (16) | 0.0004 (12) | 0.0012 (12) | 0.0006 (13) |
O20 | 0.0105 (14) | 0.0095 (13) | 0.0161 (15) | 0.0002 (11) | 0.0004 (12) | −0.0011 (13) |
O21 | 0.0072 (14) | 0.0104 (14) | 0.0152 (16) | −0.0005 (11) | 0.0016 (12) | −0.0014 (13) |
O22 | 0.0095 (15) | 0.0098 (15) | 0.0159 (16) | −0.0007 (12) | −0.0020 (12) | 0.0007 (13) |
O23 | 0.0108 (14) | 0.0098 (13) | 0.0184 (16) | −0.0018 (11) | 0.0014 (13) | −0.0002 (14) |
O24 | 0.0108 (15) | 0.0109 (15) | 0.0154 (16) | −0.0013 (12) | 0.0018 (13) | 0.0016 (13) |
O25 | 0.022 (2) | 0.041 (3) | 0.031 (3) | −0.0027 (17) | −0.0023 (17) | −0.0115 (19) |
O26 | 0.0184 (18) | 0.0302 (19) | 0.028 (2) | 0.0011 (16) | 0.0004 (16) | −0.0045 (17) |
O27 | 0.0224 (19) | 0.029 (2) | 0.0243 (19) | −0.0013 (16) | −0.0044 (16) | 0.0040 (17) |
O28 | 0.0178 (17) | 0.0171 (17) | 0.0203 (17) | 0.0046 (15) | −0.0001 (13) | −0.0011 (13) |
O29 | 0.0192 (18) | 0.030 (2) | 0.0237 (19) | 0.0063 (15) | 0.0047 (15) | 0.0074 (17) |
O30 | 0.044 (3) | 0.028 (2) | 0.028 (2) | −0.014 (2) | 0.0039 (18) | −0.0053 (18) |
O31 | 0.0145 (16) | 0.0127 (16) | 0.035 (2) | 0.0019 (13) | −0.0039 (14) | −0.0001 (15) |
O32 | 0.0158 (16) | 0.0253 (19) | 0.0276 (19) | 0.0024 (15) | 0.0028 (14) | −0.0021 (16) |
O33 | 0.0200 (18) | 0.0232 (18) | 0.031 (2) | −0.0027 (15) | −0.0017 (15) | 0.0007 (17) |
O34 | 0.0203 (18) | 0.0229 (17) | 0.0217 (18) | 0.0000 (15) | 0.0020 (14) | −0.0005 (15) |
O35 | 0.0225 (19) | 0.0197 (18) | 0.031 (2) | −0.0033 (14) | 0.0032 (16) | −0.0035 (16) |
O36 | 0.026 (2) | 0.042 (3) | 0.028 (2) | 0.0136 (19) | 0.0042 (16) | 0.0127 (19) |
O37 | 0.0190 (18) | 0.040 (3) | 0.0231 (19) | −0.0027 (17) | −0.0008 (15) | −0.0048 (18) |
O38 | 0.0155 (19) | 0.0092 (17) | 0.145 (6) | 0.0025 (14) | 0.003 (3) | −0.008 (3) |
O39 | 0.0219 (19) | 0.029 (2) | 0.0283 (19) | 0.0050 (17) | 0.0029 (15) | −0.0050 (17) |
O40 | 0.023 (2) | 0.027 (2) | 0.025 (2) | −0.0047 (15) | −0.0025 (15) | −0.0065 (16) |
O41 | 0.050 (3) | 0.027 (2) | 0.031 (3) | 0.010 (2) | −0.007 (2) | −0.0032 (19) |
O42 | 0.034 (3) | 0.027 (2) | 0.045 (3) | −0.0032 (18) | 0.005 (2) | −0.0022 (19) |
O43 | 0.034 (3) | 0.033 (3) | 0.047 (3) | 0.0042 (19) | 0.000 (2) | 0.010 (2) |
O44 | 0.028 (3) | 0.037 (3) | 0.032 (3) | 0.0086 (18) | 0.0041 (18) | 0.0043 (19) |
O45 | 0.034 (3) | 0.044 (3) | 0.039 (3) | 0.015 (2) | 0.003 (2) | 0.006 (2) |
N1 | 0.028 (3) | 0.017 (2) | 0.016 (2) | 0.0029 (17) | −0.0006 (17) | 0.0017 (17) |
N2 | 0.0127 (19) | 0.0080 (16) | 0.039 (3) | 0.0054 (15) | 0.0093 (18) | 0.0129 (18) |
C1 | 0.019 (3) | 0.021 (3) | 0.020 (3) | 0.003 (2) | 0.0010 (19) | −0.003 (2) |
C2 | 0.016 (3) | 0.019 (3) | 0.018 (3) | 0.0013 (18) | 0.0034 (19) | 0.001 (2) |
C3 | 0.026 (3) | 0.022 (3) | 0.024 (3) | 0.010 (2) | 0.003 (2) | 0.007 (3) |
C4 | 0.017 (3) | 0.019 (3) | 0.015 (2) | −0.0000 (19) | −0.0012 (18) | −0.0021 (19) |
C5 | 0.015 (3) | 0.020 (3) | 0.023 (3) | 0.0019 (19) | 0.0035 (19) | 0.006 (2) |
C6 | 0.028 (3) | 0.020 (3) | 0.028 (3) | 0.009 (3) | 0.008 (3) | 0.001 (3) |
Mo1—O1 | 1.709 (4) | Rb1—O28 | 3.002 (4) |
Mo1—O2 | 1.713 (4) | Rb1—O31 | 3.143 (4) |
Mo1—O13 | 1.931 (4) | Rb1—O32 | 2.889 (4) |
Mo1—O18 | 1.955 (4) | Rb1—O35 | 3.018 (4) |
Mo1—O20 | 2.280 (3) | Co1—O19 | 1.912 (4) |
Mo1—O21 | 2.306 (3) | Co1—O20 | 1.915 (3) |
Mo2—O3 | 1.712 (4) | Co1—O21 | 1.917 (4) |
Mo2—O4 | 1.719 (4) | Co1—O22 | 1.913 (4) |
Mo2—O13 | 1.946 (4) | Co1—O23 | 1.915 (3) |
Mo2—O14 | 1.939 (4) | Co1—O24 | 1.910 (4) |
Mo2—O21 | 2.296 (4) | Co2—O28 | 2.123 (4) |
Mo2—O22 | 2.278 (4) | Co2—O32 | 2.154 (4) |
Mo3—O5 | 1.722 (4) | Co2—O33 | 2.099 (4) |
Mo3—O6 | 1.713 (4) | Co2—O34 | 2.132 (4) |
Mo3—O14 | 1.914 (4) | Co2—O35 | 2.078 (4) |
Mo3—O15 | 1.936 (4) | Co2—O36 | 2.060 (5) |
Mo3—O22 | 2.288 (3) | O25—C1 | 1.248 (7) |
Mo3—O23 | 2.286 (4) | O26—C1 | 1.257 (7) |
Mo4—Mo5 | 3.2749 (6) | O27—C3 | 1.428 (7) |
Mo4—O7 | 1.713 (4) | O28—C4 | 1.264 (6) |
Mo4—O8 | 1.718 (4) | O29—C4 | 1.250 (6) |
Mo4—O15 | 1.964 (4) | O30—C6 | 1.420 (7) |
Mo4—O16 | 1.914 (4) | N1—C2 | 1.491 (7) |
Mo4—O23 | 2.265 (4) | N2—C5 | 1.523 (7) |
Mo4—O24 | 2.275 (4) | C1—C2 | 1.548 (8) |
Mo5—O9 | 1.704 (4) | C2—C3 | 1.523 (8) |
Mo5—O10 | 1.713 (4) | C4—C5 | 1.529 (7) |
Mo5—O16 | 1.929 (4) | C5—C6 | 1.530 (8) |
Mo5—O17 | 1.931 (4) | O27—H4 | 0.840 |
Mo5—O19 | 2.288 (4) | O30—H11 | 0.840 |
Mo5—O24 | 2.292 (4) | N1—H5 | 0.910 |
Mo6—O11 | 1.714 (4) | N1—H6 | 0.910 |
Mo6—O12 | 1.719 (4) | N1—H7 | 0.910 |
Mo6—O17 | 1.934 (4) | N2—H13 | 0.910 |
Mo6—O18 | 1.946 (4) | N2—H12 | 0.910 |
Mo6—O19 | 2.274 (4) | N2—H14 | 0.910 |
Mo6—O20 | 2.262 (3) | C2—H1 | 1.000 |
Rb1—O3 | 3.138 (4) | C3—H2 | 0.990 |
Rb1—O8i | 2.858 (4) | C3—H3 | 0.990 |
Rb1—O11ii | 2.855 (4) | C5—H8 | 1.000 |
Rb1—O12ii | 3.099 (4) | C6—H9 | 0.990 |
Rb1—O14 | 2.737 (4) | C6—H10 | 0.990 |
Co1···O13 | 3.390 (4) | O7···H12v | 3.2919 |
Co1···O14 | 3.387 (4) | O7···H14v | 3.0848 |
Co1···O15 | 3.380 (3) | O8···H13v | 2.7395 |
Co1···O16 | 3.364 (4) | O8···H12v | 2.3132 |
Co1···O17 | 3.374 (4) | O8···H14v | 3.3485 |
Co1···O18 | 3.389 (3) | O10···H8iii | 2.4384 |
Co2···O29 | 3.349 (4) | O11···H12iii | 2.3729 |
O1···O12 | 3.252 (6) | O11···H14iii | 3.4299 |
O1···O19iii | 2.714 (5) | O11···H8iii | 2.6886 |
O1···O31iii | 3.344 (6) | O13···H13vi | 3.3249 |
O2···O3 | 3.305 (5) | O13···H12vi | 3.2702 |
O2···O6iv | 3.528 (5) | O13···H14vi | 1.9329 |
O4···O6 | 3.287 (5) | O13···H8vi | 3.4279 |
O4···O7v | 3.494 (6) | O13···H10vi | 2.7195 |
O4···O30vi | 3.122 (6) | O25···H1 | 2.5619 |
O4···N2vi | 3.110 (6) | O25···H2 | 2.7950 |
O4···C6vi | 3.427 (7) | O26···H1 | 3.0852 |
O5···O7 | 3.214 (6) | O26···H4 | 3.3433 |
O5···O24i | 2.710 (5) | O26···H5 | 3.5492 |
O5···O31 | 3.414 (5) | O26···H6 | 2.4944 |
O7···O22i | 2.647 (5) | O26···H7 | 2.6156 |
O7···N2v | 3.387 (6) | O27···H1 | 3.2887 |
O8···O9 | 3.194 (6) | O27···H5 | 3.2180 |
O8···N2v | 2.912 (6) | O27···H6 | 2.6237 |
O9···O32v | 2.789 (6) | O28···H13 | 2.6015 |
O10···O11 | 3.202 (5) | O28···H12 | 2.6064 |
O10···C5iii | 3.383 (7) | O28···H14 | 3.5942 |
O11···N2iii | 3.073 (6) | O28···H8 | 2.9795 |
O11···C4iii | 3.476 (6) | O29···H8 | 2.6561 |
O11···C5iii | 3.184 (7) | O29···H9 | 2.5982 |
O12···O21iii | 2.790 (5) | O30···H13 | 2.7231 |
O13···N2vi | 2.827 (6) | O30···H14 | 3.2090 |
O13···C5vi | 3.453 (6) | O30···H8 | 3.2665 |
O13···C6vi | 3.472 (7) | O36···H9ix | 3.0878 |
O15···O31v | 2.731 (5) | N1···H2 | 3.3264 |
O18···O31iii | 2.915 (5) | N1···H3 | 2.6702 |
O23···O31 | 2.637 (5) | N1···H4 | 2.6186 |
O25···C3 | 3.036 (7) | N2···H9 | 3.3613 |
O26···O27 | 3.323 (6) | N2···H10 | 2.6694 |
O26···N1 | 2.647 (6) | C1···H2 | 2.7114 |
O26···C3 | 3.342 (7) | C1···H3 | 3.3743 |
O27···N1 | 2.940 (6) | C1···H4 | 3.2060 |
O27···C1 | 2.950 (7) | C1···H5 | 3.2783 |
O28···N2 | 2.691 (6) | C1···H6 | 2.6629 |
O28···C6 | 3.528 (7) | C1···H7 | 2.6307 |
O29···O30 | 3.215 (6) | C2···H4 | 2.5901 |
O29···O33vii | 3.469 (6) | C3···H5 | 2.6429 |
O29···O34 | 2.592 (6) | C3···H6 | 2.6418 |
O29···C6 | 2.826 (7) | C3···H7 | 3.2631 |
O30···N2 | 2.978 (6) | C4···H13 | 2.6571 |
O30···C4 | 2.893 (7) | C4···H12 | 2.7012 |
O33···C4 | 3.593 (6) | C4···H14 | 3.2938 |
O34···C4 | 3.130 (6) | C4···H9 | 2.7369 |
O1···O38v | 3.283 (6) | C4···H10 | 3.3691 |
O2···O38iv | 3.594 (7) | C5···H11 | 3.1558 |
O2···N1 | 2.944 (6) | C6···H13 | 2.7233 |
O2···C2 | 3.283 (6) | C6···H12 | 3.2912 |
O2···C3 | 3.190 (7) | C6···H14 | 2.6329 |
O3···O42viii | 3.236 (6) | H1···H2 | 2.3511 |
O3···C2 | 3.152 (7) | H1···H3 | 2.3608 |
O3···C3 | 3.081 (7) | H1···H4 | 3.4866 |
O4···O39ix | 3.030 (6) | H1···H5 | 2.2942 |
O4···O42viii | 3.216 (6) | H1···H6 | 2.7796 |
O4···O43vi | 3.154 (6) | H1···H7 | 2.3045 |
O5···O38 | 3.198 (7) | H2···H4 | 2.6673 |
O6···O39ix | 3.009 (6) | H2···H5 | 3.5292 |
O6···O41x | 2.916 (6) | H2···H6 | 3.5481 |
O6···N1x | 3.101 (6) | H13···H8 | 2.7983 |
O7···O38 | 3.091 (7) | H13···H10 | 2.9751 |
O9···O26iii | 3.050 (6) | H13···H11 | 3.4765 |
O10···O37xi | 2.721 (6) | H12···H8 | 2.2966 |
O10···O41ii | 3.455 (6) | H12···H10 | 3.4808 |
O13···O38v | 3.541 (7) | H14···H8 | 2.3477 |
O14···O39ix | 3.339 (6) | H14···H9 | 3.5184 |
O15···O38 | 2.869 (5) | H14···H10 | 2.4393 |
O16···O41ii | 2.894 (6) | H3···H4 | 2.2173 |
O16···O43v | 3.520 (6) | H3···H5 | 2.4834 |
O17···N1iii | 2.905 (6) | H3···H6 | 2.9242 |
O17···C2iii | 3.403 (6) | H3···H7 | 3.4992 |
O18···O38iv | 2.746 (5) | H4···H5 | 2.8423 |
O20···O38v | 2.566 (5) | H4···H6 | 2.1224 |
O25···O35 | 2.749 (6) | H4···H7 | 3.4521 |
O25···O45viii | 2.837 (7) | H8···H9 | 2.3377 |
O26···O9ii | 3.050 (6) | H8···H10 | 2.3876 |
O26···O32iv | 3.411 (6) | H9···H11 | 2.2061 |
O26···O39vii | 3.313 (6) | H10···H11 | 2.2058 |
O26···O40vii | 2.713 (6) | Mo1···H3 | 3.5841 |
O26···O44iv | 2.729 (6) | Mo5···H7iii | 3.3029 |
O27···O34viii | 3.562 (6) | O2···H1 | 3.1673 |
O27···O36viii | 2.766 (6) | O2···H3 | 2.3869 |
O27···O39vii | 3.337 (6) | O2···H5 | 2.1144 |
O27···O41 | 2.859 (6) | O2···H6 | 3.4440 |
O27···O44iv | 3.511 (6) | O2···H7 | 3.4959 |
O27···O45iv | 3.347 (6) | O3···H1 | 2.4073 |
O28···O43 | 3.367 (6) | O3···H2 | 2.8346 |
O29···O37vii | 2.758 (6) | O3···H3 | 2.8059 |
O29···O40 | 3.386 (6) | O5···H5x | 3.5281 |
O30···O40 | 2.708 (6) | O5···H7x | 3.2581 |
O30···O42vii | 2.928 (6) | O6···H5x | 2.6821 |
O30···O43 | 2.931 (7) | O6···H6x | 2.7716 |
O32···O26x | 3.411 (6) | O6···H7x | 3.4202 |
O32···O39ix | 2.793 (6) | O9···H7iii | 2.9001 |
O33···O37 | 3.159 (6) | O12···H1iii | 3.1126 |
O33···O40ix | 2.762 (6) | O13···H3 | 3.4190 |
O33···O43 | 2.864 (6) | O17···H1iii | 3.1189 |
O34···O27xii | 3.562 (6) | O17···H5iii | 3.1826 |
O34···O37 | 2.693 (6) | O17···H6iii | 3.5719 |
O34···O45viii | 2.812 (6) | O17···H7iii | 2.0891 |
O35···O25 | 2.749 (6) | O27···H9vi | 3.4869 |
O35···O42viii | 2.672 (6) | O35···H1 | 3.3071 |
O36···O27xii | 2.766 (6) | O35···H2 | 3.5739 |
O36···O42viii | 3.467 (6) | O36···H2xii | 2.9821 |
O36···O44 | 2.711 (6) | O36···H4xii | 3.4952 |
O36···C3xii | 3.401 (7) | O37···H8ix | 3.3473 |
O37···O10xiii | 2.721 (6) | O37···H9ix | 2.9248 |
O37···O29ix | 2.758 (6) | O38···H12v | 3.4037 |
O37···O33 | 3.159 (6) | O38···H14v | 3.4937 |
O37···O34 | 2.693 (6) | O39···H4ix | 2.6354 |
O37···O40 | 2.770 (6) | O39···H5ix | 3.4609 |
O38···O1i | 3.283 (6) | O39···H6ix | 2.1396 |
O38···O2x | 3.594 (7) | O39···H7ix | 3.3673 |
O38···O5 | 3.198 (7) | O40···H9 | 3.2207 |
O38···O7 | 3.091 (7) | O40···H11 | 2.5578 |
O38···O13i | 3.541 (7) | O41···H3 | 3.2008 |
O38···O15 | 2.869 (5) | O41···H4 | 2.2367 |
O38···O18x | 2.746 (5) | O41···H5 | 3.5017 |
O38···O20i | 2.566 (5) | O41···H6 | 3.3191 |
O39···O4vii | 3.030 (6) | O42···H2xii | 3.3487 |
O39···O6vii | 3.009 (6) | O42···H10ix | 3.5090 |
O39···O14vii | 3.339 (6) | O42···H11ix | 2.2422 |
O39···O26ix | 3.313 (6) | O43···H13 | 2.1120 |
O39···O27ix | 3.337 (6) | O43···H12 | 3.4863 |
O39···O32vii | 2.793 (6) | O43···H14 | 3.4463 |
O39···O41ix | 3.328 (6) | O43···H11 | 3.4813 |
O39···O42xiv | 3.197 (6) | O44···H2xii | 3.1971 |
O39···O44vii | 3.147 (6) | O44···H4x | 3.4995 |
O39···O45vii | 2.909 (6) | O44···H11ix | 3.0896 |
O39···N1ix | 3.041 (6) | O45···H4x | 3.0294 |
O40···O26ix | 2.713 (6) | O45···H11vi | 3.5431 |
O40···O29 | 3.386 (6) | C3···H9vi | 3.3681 |
O40···O30 | 2.708 (6) | C3···H10vi | 2.9592 |
O40···O33vii | 2.762 (6) | C6···H2xvii | 3.1970 |
O40···O37 | 2.770 (6) | C6···H3xvii | 3.2224 |
O40···O44vii | 3.491 (6) | H1···O2 | 3.1673 |
O40···C1ix | 3.536 (7) | H1···O3 | 2.4073 |
O40···C6 | 3.500 (7) | H1···O12ii | 3.1126 |
O41···O6iv | 2.916 (6) | H1···O17ii | 3.1189 |
O41···O10iii | 3.455 (6) | H1···O35 | 3.3071 |
O41···O16iii | 2.894 (6) | H2···O3 | 2.8346 |
O41···O27 | 2.859 (6) | H2···O35 | 3.5739 |
O41···O39vii | 3.328 (6) | H2···O36viii | 2.9821 |
O41···O43xv | 3.046 (7) | H2···O42viii | 3.3487 |
O41···C3 | 3.539 (8) | H2···O44viii | 3.1971 |
O42···O3xii | 3.236 (6) | H2···C6vi | 3.1970 |
O42···O4xii | 3.216 (6) | H2···H9vi | 2.9953 |
O42···O30ix | 2.928 (6) | H2···H10vi | 2.6152 |
O42···O35xii | 2.672 (6) | H2···H11vi | 3.2630 |
O42···O36xii | 3.467 (6) | H13···O43 | 2.1120 |
O42···O39xvi | 3.197 (6) | H12···O38i | 3.4037 |
O42···O44 | 2.768 (7) | H12···O43 | 3.4863 |
O42···O45xii | 3.092 (7) | H14···O38i | 3.4937 |
O43···O4xvii | 3.154 (6) | H14···O43 | 3.4463 |
O43···O16i | 3.520 (6) | H3···Mo1 | 3.5841 |
O43···O28 | 3.367 (6) | H3···O2 | 2.3869 |
O43···O30 | 2.931 (7) | H3···O3 | 2.8059 |
O43···O33 | 2.864 (6) | H3···O13 | 3.4190 |
O43···O41xviii | 3.046 (7) | H3···O41 | 3.2008 |
O43···O45xvii | 3.294 (7) | H3···C6vi | 3.2224 |
O43···N2 | 3.013 (7) | H3···H9vi | 3.1293 |
O44···O26x | 2.729 (6) | H3···H10vi | 2.4462 |
O44···O27x | 3.511 (6) | H4···O36viii | 3.4952 |
O44···O36 | 2.711 (6) | H4···O39vii | 2.6354 |
O44···O39ix | 3.147 (6) | H4···O41 | 2.2367 |
O44···O40ix | 3.491 (6) | H4···O44iv | 3.4995 |
O44···O42 | 2.768 (7) | H4···O45iv | 3.0294 |
O44···O45 | 2.805 (7) | H5···O2 | 2.1144 |
O44···C1x | 3.494 (7) | H5···O5iv | 3.5281 |
O45···O25xii | 2.837 (7) | H5···O6iv | 2.6821 |
O45···O27x | 3.347 (6) | H5···O17ii | 3.1826 |
O45···O34xii | 2.812 (6) | H5···O39vii | 3.4609 |
O45···O39ix | 2.909 (6) | H5···O41 | 3.5017 |
O45···O42viii | 3.092 (7) | H6···O2 | 3.4440 |
O45···O43vi | 3.294 (7) | H6···O6iv | 2.7716 |
O45···O44 | 2.805 (7) | H6···O17ii | 3.5719 |
N1···O2 | 2.944 (6) | H6···O39vii | 2.1396 |
N1···O6iv | 3.101 (6) | H6···O41 | 3.3191 |
N1···O17ii | 2.905 (6) | H7···Mo5ii | 3.3029 |
N1···O39vii | 3.041 (6) | H7···O2 | 3.4959 |
N2···O43 | 3.013 (7) | H7···O5iv | 3.2581 |
C1···O40vii | 3.536 (7) | H7···O6iv | 3.4202 |
C1···O44iv | 3.494 (7) | H7···O9ii | 2.9001 |
C2···O2 | 3.283 (6) | H7···O17ii | 2.0891 |
C2···O3 | 3.152 (7) | H7···O39vii | 3.3673 |
C2···O17ii | 3.403 (6) | H8···O37vii | 3.3473 |
C3···O2 | 3.190 (7) | H9···O27xvii | 3.4869 |
C3···O3 | 3.081 (7) | H9···O37vii | 2.9248 |
C3···O36viii | 3.401 (7) | H9···O40 | 3.2207 |
C3···O41 | 3.539 (8) | H9···C3xvii | 3.3681 |
C6···O40 | 3.500 (7) | H9···H2xvii | 2.9953 |
Mo2···H14vi | 3.0638 | H9···H3xvii | 3.1293 |
Mo2···H10vi | 3.2343 | H10···O42vii | 3.5090 |
Mo4···H13v | 3.5913 | H10···C3xvii | 2.9592 |
Mo4···H12v | 3.4589 | H10···H2xvii | 2.6152 |
Rb1···H12 | 3.3372 | H10···H3xvii | 2.4462 |
O3···H10vi | 3.0200 | H11···O40 | 2.5578 |
O4···H13vi | 2.8030 | H11···O42vii | 2.2422 |
O4···H14vi | 2.6260 | H11···O43 | 3.4813 |
O4···H10vi | 2.9750 | H11···O44vii | 3.0896 |
O4···H11vi | 3.2797 | H11···O45xvii | 3.5431 |
O7···H13v | 3.2320 | H11···H2xvii | 3.2630 |
O1—Mo1—O2 | 106.26 (19) | O12ii—Rb1—O28 | 121.37 (10) |
O1—Mo1—O13 | 98.55 (16) | O12ii—Rb1—O31 | 59.59 (10) |
O1—Mo1—O18 | 99.41 (16) | O12ii—Rb1—O32 | 160.80 (11) |
O1—Mo1—O20 | 94.66 (15) | O12ii—Rb1—O35 | 108.16 (10) |
O1—Mo1—O21 | 161.17 (15) | O14—Rb1—O28 | 149.48 (10) |
O2—Mo1—O13 | 101.91 (16) | O14—Rb1—O31 | 71.23 (10) |
O2—Mo1—O18 | 95.28 (16) | O14—Rb1—O32 | 85.65 (11) |
O2—Mo1—O20 | 157.08 (15) | O14—Rb1—O35 | 101.05 (11) |
O2—Mo1—O21 | 91.95 (15) | O28—Rb1—O31 | 134.06 (9) |
O13—Mo1—O18 | 150.50 (14) | O28—Rb1—O32 | 64.74 (10) |
O13—Mo1—O20 | 83.71 (13) | O28—Rb1—O35 | 57.77 (10) |
O13—Mo1—O21 | 72.44 (13) | O31—Rb1—O32 | 131.53 (10) |
O18—Mo1—O20 | 71.68 (12) | O31—Rb1—O35 | 165.42 (10) |
O18—Mo1—O21 | 83.28 (12) | O32—Rb1—O35 | 57.89 (11) |
O20—Mo1—O21 | 68.32 (11) | O19—Co1—O20 | 84.13 (14) |
O3—Mo2—O4 | 106.40 (17) | O19—Co1—O21 | 95.27 (14) |
O3—Mo2—O13 | 101.74 (16) | O19—Co1—O22 | 179.37 (14) |
O3—Mo2—O14 | 96.02 (16) | O19—Co1—O23 | 96.87 (14) |
O3—Mo2—O21 | 91.44 (14) | O19—Co1—O24 | 84.19 (14) |
O3—Mo2—O22 | 157.18 (15) | O20—Co1—O21 | 84.43 (13) |
O4—Mo2—O13 | 96.50 (16) | O20—Co1—O22 | 95.24 (13) |
O4—Mo2—O14 | 100.17 (16) | O20—Co1—O23 | 178.98 (14) |
O4—Mo2—O21 | 160.79 (15) | O20—Co1—O24 | 95.97 (14) |
O4—Mo2—O22 | 94.94 (15) | O21—Co1—O22 | 84.74 (14) |
O13—Mo2—O14 | 151.07 (14) | O21—Co1—O23 | 95.64 (14) |
O13—Mo2—O21 | 72.40 (12) | O21—Co1—O24 | 179.29 (14) |
O13—Mo2—O22 | 83.38 (13) | O22—Co1—O23 | 83.75 (14) |
O14—Mo2—O21 | 84.61 (13) | O22—Co1—O24 | 95.80 (14) |
O14—Mo2—O22 | 71.82 (13) | O23—Co1—O24 | 83.96 (14) |
O21—Mo2—O22 | 68.69 (11) | O28—Co2—O32 | 95.09 (14) |
O5—Mo3—O6 | 106.47 (18) | O28—Co2—O33 | 83.78 (14) |
O5—Mo3—O14 | 97.22 (16) | O28—Co2—O34 | 91.63 (14) |
O5—Mo3—O15 | 100.19 (16) | O28—Co2—O35 | 87.62 (14) |
O5—Mo3—O22 | 159.57 (15) | O28—Co2—O36 | 171.73 (16) |
O5—Mo3—O23 | 94.01 (15) | O32—Co2—O33 | 87.67 (15) |
O6—Mo3—O14 | 100.99 (16) | O32—Co2—O34 | 172.49 (15) |
O6—Mo3—O15 | 97.04 (16) | O32—Co2—O35 | 85.04 (15) |
O6—Mo3—O22 | 92.83 (15) | O32—Co2—O36 | 90.17 (16) |
O6—Mo3—O23 | 158.31 (15) | O33—Co2—O34 | 96.41 (15) |
O14—Mo3—O15 | 150.19 (14) | O33—Co2—O35 | 168.19 (16) |
O14—Mo3—O22 | 72.02 (13) | O33—Co2—O36 | 90.08 (16) |
O14—Mo3—O23 | 82.99 (13) | O34—Co2—O35 | 91.89 (15) |
O15—Mo3—O22 | 83.62 (12) | O34—Co2—O36 | 83.53 (15) |
O15—Mo3—O23 | 71.85 (13) | O35—Co2—O36 | 99.20 (17) |
O22—Mo3—O23 | 67.91 (11) | Mo2—O3—Rb1 | 100.10 (15) |
Mo5—Mo4—O7 | 130.93 (13) | Mo4—O8—Rb1v | 154.38 (19) |
Mo5—Mo4—O8 | 88.76 (12) | Mo6—O11—Rb1iii | 104.41 (16) |
Mo5—Mo4—O15 | 126.59 (10) | Mo6—O12—Rb1iii | 95.20 (15) |
Mo5—Mo4—O16 | 31.70 (11) | Mo1—O13—Mo2 | 118.07 (17) |
Mo5—Mo4—O23 | 85.56 (8) | Mo2—O14—Mo3 | 118.38 (18) |
Mo5—Mo4—O24 | 44.39 (8) | Mo2—O14—Rb1 | 108.75 (14) |
O7—Mo4—O8 | 106.22 (18) | Mo3—O14—Rb1 | 132.38 (16) |
O7—Mo4—O15 | 98.85 (16) | Mo3—O15—Mo4 | 117.05 (16) |
O7—Mo4—O16 | 99.30 (17) | Mo4—O16—Mo5 | 116.88 (18) |
O7—Mo4—O23 | 93.16 (15) | Mo5—O17—Mo6 | 116.42 (18) |
O7—Mo4—O24 | 160.57 (16) | Mo1—O18—Mo6 | 117.03 (16) |
O8—Mo4—O15 | 95.26 (16) | Mo5—O19—Mo6 | 92.14 (12) |
O8—Mo4—O16 | 101.74 (16) | Mo5—O19—Co1 | 103.93 (15) |
O8—Mo4—O23 | 158.36 (15) | Mo6—O19—Co1 | 103.34 (14) |
O8—Mo4—O24 | 92.94 (15) | Mo1—O20—Mo6 | 94.15 (11) |
O15—Mo4—O16 | 150.49 (14) | Mo1—O20—Co1 | 104.13 (14) |
O15—Mo4—O23 | 71.86 (13) | Mo6—O20—Co1 | 103.67 (14) |
O15—Mo4—O24 | 82.20 (12) | Mo1—O21—Mo2 | 92.51 (12) |
O16—Mo4—O23 | 84.08 (14) | Mo1—O21—Co1 | 103.11 (14) |
O16—Mo4—O24 | 73.07 (14) | Mo2—O21—Co1 | 102.89 (14) |
O23—Mo4—O24 | 68.58 (11) | Mo2—O22—Mo3 | 92.91 (12) |
Mo4—Mo5—O9 | 88.49 (13) | Mo2—O22—Co1 | 103.68 (14) |
Mo4—Mo5—O10 | 127.50 (14) | Mo3—O22—Co1 | 104.17 (14) |
Mo4—Mo5—O16 | 31.42 (11) | Mo3—O23—Mo4 | 93.89 (11) |
Mo4—Mo5—O17 | 125.79 (11) | Mo3—O23—Co1 | 104.17 (14) |
Mo4—Mo5—O19 | 84.06 (9) | Mo4—O23—Co1 | 103.81 (15) |
Mo4—Mo5—O24 | 43.98 (8) | Mo4—O24—Mo5 | 91.63 (12) |
O9—Mo5—O10 | 106.67 (18) | Mo4—O24—Co1 | 103.59 (14) |
O9—Mo5—O16 | 100.31 (17) | Mo5—O24—Co1 | 103.84 (15) |
O9—Mo5—O17 | 97.62 (17) | Rb1—O28—Co2 | 89.21 (11) |
O9—Mo5—O19 | 160.55 (16) | Rb1—O28—C4 | 128.6 (3) |
O9—Mo5—O24 | 94.26 (16) | Co2—O28—C4 | 126.0 (3) |
O10—Mo5—O16 | 96.11 (17) | Rb1—O32—Co2 | 91.66 (12) |
O10—Mo5—O17 | 102.17 (17) | Rb1—O35—Co2 | 89.61 (13) |
O10—Mo5—O19 | 92.05 (15) | O25—C1—O26 | 127.5 (5) |
O10—Mo5—O24 | 157.81 (15) | O25—C1—C2 | 116.4 (5) |
O16—Mo5—O17 | 149.46 (15) | O26—C1—C2 | 116.1 (5) |
O16—Mo5—O19 | 82.45 (14) | N1—C2—C1 | 110.0 (4) |
O16—Mo5—O24 | 72.42 (13) | N1—C2—C3 | 110.7 (4) |
O17—Mo5—O19 | 72.73 (13) | C1—C2—C3 | 110.3 (5) |
O17—Mo5—O24 | 81.81 (13) | O27—C3—C2 | 112.1 (5) |
O19—Mo5—O24 | 68.03 (12) | O28—C4—O29 | 126.5 (5) |
O11—Mo6—O12 | 105.70 (18) | O28—C4—C5 | 118.2 (4) |
O11—Mo6—O17 | 101.14 (16) | O29—C4—C5 | 115.3 (5) |
O11—Mo6—O18 | 95.36 (15) | N2—C5—C4 | 110.9 (4) |
O11—Mo6—O19 | 92.39 (15) | N2—C5—C6 | 110.8 (4) |
O11—Mo6—O20 | 158.22 (15) | C4—C5—C6 | 110.7 (5) |
O12—Mo6—O17 | 98.83 (16) | O30—C6—C5 | 110.6 (5) |
O12—Mo6—O18 | 99.02 (16) | C3—O27—H4 | 109.473 |
O12—Mo6—O19 | 161.42 (15) | C6—O30—H11 | 109.466 |
O12—Mo6—O20 | 94.11 (15) | C2—N1—H5 | 109.471 |
O17—Mo6—O18 | 151.34 (14) | C2—N1—H6 | 109.455 |
O17—Mo6—O19 | 73.00 (13) | C2—N1—H7 | 109.469 |
O17—Mo6—O20 | 84.30 (13) | H5—N1—H6 | 109.477 |
O18—Mo6—O19 | 83.13 (13) | H5—N1—H7 | 109.484 |
O18—Mo6—O20 | 72.22 (13) | H6—N1—H7 | 109.471 |
O19—Mo6—O20 | 68.83 (11) | C5—N2—H13 | 109.480 |
O3—Rb1—O8i | 167.01 (10) | C5—N2—H12 | 109.476 |
O3—Rb1—O11ii | 109.60 (10) | C5—N2—H14 | 109.470 |
O3—Rb1—O12ii | 65.85 (10) | H13—N2—H12 | 109.468 |
O3—Rb1—O14 | 54.60 (10) | H13—N2—H14 | 109.467 |
O3—Rb1—O28 | 117.88 (9) | H12—N2—H14 | 109.467 |
O3—Rb1—O31 | 104.15 (9) | N1—C2—H1 | 108.575 |
O3—Rb1—O32 | 95.04 (10) | C1—C2—H1 | 108.597 |
O3—Rb1—O35 | 61.86 (10) | C3—C2—H1 | 108.589 |
O8i—Rb1—O11ii | 79.66 (10) | O27—C3—H2 | 109.176 |
O8i—Rb1—O12ii | 115.90 (10) | O27—C3—H3 | 109.174 |
O8i—Rb1—O14 | 112.41 (11) | C2—C3—H2 | 109.171 |
O8i—Rb1—O28 | 72.99 (10) | C2—C3—H3 | 109.182 |
O8i—Rb1—O31 | 68.50 (10) | H2—C3—H3 | 107.896 |
O8i—Rb1—O32 | 83.11 (11) | N2—C5—H8 | 108.109 |
O8i—Rb1—O35 | 126.03 (11) | C4—C5—H8 | 108.111 |
O11ii—Rb1—O12ii | 54.54 (10) | C6—C5—H8 | 108.105 |
O11ii—Rb1—O14 | 136.93 (11) | O30—C6—H9 | 109.516 |
O11ii—Rb1—O28 | 73.03 (10) | O30—C6—H10 | 109.526 |
O11ii—Rb1—O31 | 76.24 (10) | C5—C6—H9 | 109.517 |
O11ii—Rb1—O32 | 137.42 (11) | C5—C6—H10 | 109.524 |
O11ii—Rb1—O35 | 103.69 (10) | H9—C6—H10 | 108.087 |
O12ii—Rb1—O14 | 84.44 (10) | ||
O1—Mo1—O13—Mo2 | 177.9 (2) | O17—Mo5—O19—Co1 | −88.44 (16) |
O1—Mo1—O18—Mo6 | 72.4 (2) | O19—Mo5—O17—Mo6 | −21.03 (16) |
O1—Mo1—O20—Mo6 | −83.55 (16) | O17—Mo5—O24—Mo4 | 179.52 (14) |
O1—Mo1—O20—Co1 | 171.23 (17) | O17—Mo5—O24—Co1 | 75.09 (16) |
O2—Mo1—O13—Mo2 | 69.2 (2) | O24—Mo5—O17—Mo6 | −90.48 (19) |
O2—Mo1—O18—Mo6 | 179.83 (19) | O19—Mo5—O24—Mo4 | 104.90 (13) |
O2—Mo1—O20—Mo6 | 72.5 (4) | O19—Mo5—O24—Co1 | 0.47 (12) |
O2—Mo1—O20—Co1 | −32.7 (5) | O24—Mo5—O19—Mo6 | 103.84 (13) |
O2—Mo1—O21—Mo2 | −87.70 (15) | O24—Mo5—O19—Co1 | −0.47 (12) |
O2—Mo1—O21—Co1 | 168.45 (17) | O11—Mo6—O12—Rb1iii | 3.34 (17) |
O13—Mo1—O18—Mo6 | −54.4 (4) | O12—Mo6—O11—Rb1iii | −3.73 (19) |
O18—Mo1—O13—Mo2 | −55.1 (4) | O11—Mo6—O17—Mo5 | −68.0 (2) |
O13—Mo1—O20—Mo6 | 178.34 (13) | O17—Mo6—O11—Rb1iii | −106.31 (15) |
O13—Mo1—O20—Co1 | 73.12 (15) | O11—Mo6—O18—Mo1 | −178.75 (19) |
O20—Mo1—O13—Mo2 | −88.30 (18) | O18—Mo6—O11—Rb1iii | 97.23 (14) |
O13—Mo1—O21—Mo2 | 14.17 (12) | O11—Mo6—O19—Mo5 | 85.10 (15) |
O13—Mo1—O21—Co1 | −89.68 (15) | O11—Mo6—O19—Co1 | −170.05 (17) |
O21—Mo1—O13—Mo2 | −19.09 (15) | O19—Mo6—O11—Rb1iii | −179.45 (13) |
O18—Mo1—O20—Mo6 | 14.84 (12) | O11—Mo6—O20—Mo1 | −72.3 (4) |
O18—Mo1—O20—Co1 | −90.39 (15) | O11—Mo6—O20—Co1 | 33.3 (5) |
O20—Mo1—O18—Mo6 | −19.47 (15) | O20—Mo6—O11—Rb1iii | 151.0 (3) |
O18—Mo1—O21—Mo2 | 177.21 (13) | O12—Mo6—O17—Mo5 | −176.0 (2) |
O18—Mo1—O21—Co1 | 73.36 (15) | O17—Mo6—O12—Rb1iii | 107.63 (13) |
O21—Mo1—O18—Mo6 | −88.82 (17) | O12—Mo6—O18—Mo1 | −71.9 (2) |
O20—Mo1—O21—Mo2 | 104.29 (13) | O18—Mo6—O12—Rb1iii | −94.88 (13) |
O20—Mo1—O21—Co1 | 0.44 (12) | O12—Mo6—O20—Mo1 | 83.31 (15) |
O21—Mo1—O20—Mo6 | 104.78 (13) | O12—Mo6—O20—Co1 | −171.05 (17) |
O21—Mo1—O20—Co1 | −0.45 (12) | O20—Mo6—O12—Rb1iii | −167.51 (11) |
O4—Mo2—O3—Rb1 | −108.37 (16) | O17—Mo6—O18—Mo1 | 56.0 (4) |
O3—Mo2—O13—Mo1 | −68.6 (2) | O18—Mo6—O17—Mo5 | 56.0 (4) |
O13—Mo2—O3—Rb1 | 151.16 (12) | O17—Mo6—O19—Mo5 | −15.82 (13) |
O3—Mo2—O14—Mo3 | 180.0 (2) | O17—Mo6—O19—Co1 | 89.03 (16) |
O3—Mo2—O14—Rb1 | 7.03 (17) | O19—Mo6—O17—Mo5 | 21.13 (16) |
O14—Mo2—O3—Rb1 | −5.89 (15) | O17—Mo6—O20—Mo1 | −178.21 (14) |
O3—Mo2—O21—Mo1 | 87.80 (15) | O17—Mo6—O20—Co1 | −72.57 (15) |
O3—Mo2—O21—Co1 | −168.14 (17) | O20—Mo6—O17—Mo5 | 90.70 (18) |
O21—Mo2—O3—Rb1 | 78.84 (12) | O18—Mo6—O19—Mo5 | −179.78 (14) |
O3—Mo2—O22—Mo3 | −74.7 (4) | O18—Mo6—O19—Co1 | −74.93 (15) |
O3—Mo2—O22—Co1 | 30.6 (5) | O19—Mo6—O18—Mo1 | 89.48 (17) |
O22—Mo2—O3—Rb1 | 50.2 (4) | O18—Mo6—O20—Mo1 | −14.86 (12) |
O4—Mo2—O13—Mo1 | −176.89 (19) | O18—Mo6—O20—Co1 | 90.78 (15) |
O4—Mo2—O14—Mo3 | −72.1 (3) | O20—Mo6—O18—Mo1 | 19.57 (15) |
O4—Mo2—O14—Rb1 | 114.93 (16) | O19—Mo6—O20—Mo1 | −104.26 (13) |
O4—Mo2—O22—Mo3 | 84.66 (15) | O19—Mo6—O20—Co1 | 1.38 (12) |
O4—Mo2—O22—Co1 | −170.00 (17) | O20—Mo6—O19—Mo5 | −106.23 (13) |
O13—Mo2—O14—Mo3 | 52.1 (4) | O20—Mo6—O19—Co1 | −1.38 (12) |
O13—Mo2—O14—Rb1 | −120.8 (3) | O3—Rb1—O11ii—Mo6ii | 40.54 (18) |
O14—Mo2—O13—Mo1 | 58.1 (4) | O11ii—Rb1—O3—Mo2 | −129.20 (14) |
O13—Mo2—O21—Mo1 | −14.06 (12) | O3—Rb1—O12ii—Mo6ii | −142.79 (18) |
O13—Mo2—O21—Co1 | 90.00 (15) | O12ii—Rb1—O3—Mo2 | −95.77 (16) |
O21—Mo2—O13—Mo1 | 19.17 (15) | O3—Rb1—O14—Mo2 | −4.67 (12) |
O13—Mo2—O22—Mo3 | −179.35 (13) | O3—Rb1—O14—Mo3 | −176.3 (3) |
O13—Mo2—O22—Co1 | −74.01 (15) | O14—Rb1—O3—Mo2 | 5.09 (13) |
O22—Mo2—O13—Mo1 | 88.87 (18) | O3—Rb1—O28—Co2 | −53.19 (14) |
O14—Mo2—O21—Mo1 | −176.28 (14) | O3—Rb1—O28—C4 | 84.8 (3) |
O14—Mo2—O21—Co1 | −72.22 (15) | O28—Rb1—O3—Mo2 | 150.14 (13) |
O21—Mo2—O14—Mo3 | 89.09 (19) | O31—Rb1—O3—Mo2 | −49.02 (16) |
O21—Mo2—O14—Rb1 | −83.85 (14) | O3—Rb1—O32—Co2 | 90.18 (13) |
O14—Mo2—O22—Mo3 | −14.44 (12) | O32—Rb1—O3—Mo2 | 86.11 (15) |
O14—Mo2—O22—Co1 | 90.90 (16) | O3—Rb1—O35—Co2 | −156.67 (16) |
O22—Mo2—O14—Mo3 | 19.78 (17) | O35—Rb1—O3—Mo2 | 135.39 (18) |
O22—Mo2—O14—Rb1 | −153.17 (17) | O8i—Rb1—O11ii—Mo6ii | −130.02 (17) |
O21—Mo2—O22—Mo3 | −105.70 (13) | O11ii—Rb1—O8i—Mo4i | 105.3 (5) |
O21—Mo2—O22—Co1 | −0.35 (12) | O8i—Rb1—O12ii—Mo6ii | 51.42 (18) |
O22—Mo2—O21—Mo1 | −103.71 (13) | O12ii—Rb1—O8i—Mo4i | 63.4 (5) |
O22—Mo2—O21—Co1 | 0.35 (12) | O8i—Rb1—O14—Mo2 | 175.29 (13) |
O5—Mo3—O14—Mo2 | 178.2 (2) | O8i—Rb1—O14—Mo3 | 3.7 (3) |
O5—Mo3—O14—Rb1 | −10.9 (3) | O14—Rb1—O8i—Mo4i | −31.4 (5) |
O5—Mo3—O15—Mo4 | 70.6 (2) | O8i—Rb1—O28—Co2 | 119.11 (13) |
O5—Mo3—O22—Mo2 | 75.1 (5) | O8i—Rb1—O28—C4 | −102.9 (3) |
O5—Mo3—O22—Co1 | −29.8 (5) | O28—Rb1—O8i—Mo4i | −179.4 (5) |
O5—Mo3—O23—Mo4 | −83.85 (15) | O31—Rb1—O8i—Mo4i | 26.2 (4) |
O5—Mo3—O23—Co1 | 170.86 (17) | O8i—Rb1—O32—Co2 | −102.75 (13) |
O6—Mo3—O14—Mo2 | 69.7 (3) | O32—Rb1—O8i—Mo4i | −113.8 (5) |
O6—Mo3—O14—Rb1 | −119.3 (3) | O8i—Rb1—O35—Co2 | 11.12 (18) |
O6—Mo3—O15—Mo4 | 178.83 (19) | O35—Rb1—O8i—Mo4i | −155.2 (4) |
O6—Mo3—O22—Mo2 | −86.02 (15) | O11ii—Rb1—O12ii—Mo6ii | −2.37 (12) |
O6—Mo3—O22—Co1 | 169.08 (17) | O12ii—Rb1—O11ii—Mo6ii | 2.44 (13) |
O6—Mo3—O23—Mo4 | 77.2 (4) | O11ii—Rb1—O14—Mo2 | 76.3 (2) |
O6—Mo3—O23—Co1 | −28.1 (5) | O11ii—Rb1—O14—Mo3 | −95.3 (3) |
O14—Mo3—O15—Mo4 | −54.2 (4) | O14—Rb1—O11ii—Mo6ii | −18.2 (3) |
O15—Mo3—O14—Mo2 | −56.4 (4) | O11ii—Rb1—O28—Co2 | −156.80 (13) |
O15—Mo3—O14—Rb1 | 114.5 (3) | O11ii—Rb1—O28—C4 | −18.9 (3) |
O14—Mo3—O22—Mo2 | 14.62 (13) | O28—Rb1—O11ii—Mo6ii | 154.77 (17) |
O14—Mo3—O22—Co1 | −90.28 (16) | O31—Rb1—O11ii—Mo6ii | −59.83 (15) |
O22—Mo3—O14—Mo2 | −19.67 (17) | O11ii—Rb1—O32—Co2 | −36.2 (2) |
O22—Mo3—O14—Rb1 | 151.3 (3) | O32—Rb1—O11ii—Mo6ii | 162.24 (13) |
O14—Mo3—O23—Mo4 | 179.36 (14) | O11ii—Rb1—O35—Co2 | 98.18 (13) |
O14—Mo3—O23—Co1 | 74.06 (16) | O35—Rb1—O11ii—Mo6ii | 105.17 (16) |
O23—Mo3—O14—Mo2 | −88.66 (19) | O12ii—Rb1—O14—Mo2 | 59.53 (15) |
O23—Mo3—O14—Rb1 | 82.3 (2) | O12ii—Rb1—O14—Mo3 | −112.1 (3) |
O15—Mo3—O22—Mo2 | 177.20 (14) | O14—Rb1—O12ii—Mo6ii | 163.66 (16) |
O15—Mo3—O22—Co1 | 72.30 (15) | O12ii—Rb1—O28—Co2 | −130.50 (11) |
O22—Mo3—O15—Mo4 | −89.09 (17) | O12ii—Rb1—O28—C4 | 7.4 (3) |
O15—Mo3—O23—Mo4 | 15.57 (12) | O28—Rb1—O12ii—Mo6ii | −33.72 (19) |
O15—Mo3—O23—Co1 | −89.73 (16) | O31—Rb1—O12ii—Mo6ii | 92.19 (16) |
O23—Mo3—O15—Mo4 | −20.29 (15) | O12ii—Rb1—O35—Co2 | 154.91 (11) |
O22—Mo3—O23—Mo4 | 105.96 (13) | O35—Rb1—O12ii—Mo6ii | −96.50 (15) |
O22—Mo3—O23—Co1 | 0.66 (12) | O14—Rb1—O28—Co2 | 13.7 (3) |
O23—Mo3—O22—Mo2 | 104.23 (13) | O14—Rb1—O28—C4 | 151.6 (2) |
O23—Mo3—O22—Co1 | −0.67 (13) | O28—Rb1—O14—Mo2 | −90.3 (3) |
O7—Mo4—Mo5—O9 | −108.32 (17) | O28—Rb1—O14—Mo3 | 98.1 (3) |
O7—Mo4—Mo5—O10 | 1.64 (18) | O31—Rb1—O14—Mo2 | 119.27 (16) |
O7—Mo4—Mo5—O16 | 4.43 (17) | O31—Rb1—O14—Mo3 | −52.3 (2) |
O7—Mo4—Mo5—O17 | 153.37 (17) | O14—Rb1—O32—Co2 | 144.03 (13) |
O7—Mo4—Mo5—O19 | 89.66 (17) | O32—Rb1—O14—Mo2 | −104.00 (16) |
O7—Mo4—Mo5—O24 | 153.96 (18) | O32—Rb1—O14—Mo3 | 84.4 (3) |
Mo5—Mo4—O8—Rb1v | 94.4 (5) | O14—Rb1—O35—Co2 | −117.37 (12) |
O8—Mo4—Mo5—O9 | 2.23 (12) | O35—Rb1—O14—Mo2 | −47.92 (16) |
O8—Mo4—Mo5—O10 | 112.20 (12) | O35—Rb1—O14—Mo3 | 140.5 (2) |
O8—Mo4—Mo5—O16 | 114.98 (12) | O31—Rb1—O28—Co2 | 153.09 (10) |
O8—Mo4—Mo5—O17 | −96.07 (12) | O31—Rb1—O28—C4 | −69.0 (3) |
O8—Mo4—Mo5—O19 | −159.78 (12) | O28—Rb1—O32—Co2 | −28.34 (11) |
O8—Mo4—Mo5—O24 | −95.48 (12) | O32—Rb1—O28—Co2 | 28.78 (11) |
Mo5—Mo4—O15—Mo3 | 90.33 (17) | O32—Rb1—O28—C4 | 166.7 (3) |
O15—Mo4—Mo5—O9 | 97.86 (12) | O28—Rb1—O35—Co2 | 38.75 (11) |
O15—Mo4—Mo5—O10 | −152.17 (12) | O35—Rb1—O28—Co2 | −37.80 (11) |
O15—Mo4—Mo5—O16 | −149.39 (12) | O35—Rb1—O28—C4 | 100.1 (3) |
O15—Mo4—Mo5—O17 | −0.44 (12) | O31—Rb1—O32—Co2 | −155.87 (10) |
O15—Mo4—Mo5—O19 | −64.15 (12) | O32—Rb1—O35—Co2 | −39.72 (12) |
O15—Mo4—Mo5—O24 | 0.15 (12) | O35—Rb1—O32—Co2 | 38.08 (11) |
Mo5—Mo4—O16—Mo5 | 0.000 (13) | O19—Co1—O20—Mo1 | 96.40 (14) |
O16—Mo4—Mo5—O9 | −112.8 (2) | O19—Co1—O20—Mo6 | −1.54 (14) |
O16—Mo4—Mo5—O10 | −2.8 (2) | O20—Co1—O19—Mo5 | 97.16 (14) |
O16—Mo4—Mo5—O16 | 0.0 (2) | O20—Co1—O19—Mo6 | 1.53 (14) |
O16—Mo4—Mo5—O17 | 148.9 (2) | O19—Co1—O21—Mo1 | −84.05 (14) |
O16—Mo4—Mo5—O19 | 85.2 (2) | O19—Co1—O21—Mo2 | −179.76 (14) |
O16—Mo4—Mo5—O24 | 149.5 (2) | O21—Co1—O19—Mo5 | −179.00 (14) |
Mo5—Mo4—O23—Mo3 | −146.22 (9) | O21—Co1—O19—Mo6 | 85.36 (14) |
Mo5—Mo4—O23—Co1 | −40.60 (12) | O19—Co1—O23—Mo3 | 179.18 (14) |
O23—Mo4—Mo5—O9 | 161.34 (8) | O19—Co1—O23—Mo4 | 81.48 (15) |
O23—Mo4—Mo5—O10 | −88.70 (9) | O23—Co1—O19—Mo5 | −82.65 (15) |
O23—Mo4—Mo5—O16 | −85.91 (8) | O23—Co1—O19—Mo6 | −178.29 (14) |
O23—Mo4—Mo5—O17 | 63.03 (8) | O19—Co1—O24—Mo4 | −95.67 (15) |
O23—Mo4—Mo5—O19 | −0.68 (8) | O19—Co1—O24—Mo5 | −0.53 (14) |
O23—Mo4—Mo5—O24 | 63.62 (8) | O24—Co1—O19—Mo5 | 0.53 (14) |
Mo5—Mo4—O24—Mo5 | 0.0 | O24—Co1—O19—Mo6 | −95.11 (15) |
Mo5—Mo4—O24—Co1 | 104.66 (16) | O20—Co1—O21—Mo1 | −0.49 (13) |
O24—Mo4—Mo5—O9 | 97.71 (12) | O20—Co1—O21—Mo2 | −96.20 (14) |
O24—Mo4—Mo5—O10 | −152.32 (12) | O21—Co1—O20—Mo1 | 0.50 (14) |
O24—Mo4—Mo5—O16 | −149.54 (12) | O21—Co1—O20—Mo6 | −97.44 (14) |
O24—Mo4—Mo5—O17 | −0.59 (12) | O20—Co1—O22—Mo2 | 84.29 (14) |
O24—Mo4—Mo5—O19 | −64.30 (12) | O20—Co1—O22—Mo3 | −179.08 (14) |
O24—Mo4—Mo5—O24 | 0.00 (12) | O22—Co1—O20—Mo1 | −83.68 (14) |
O7—Mo4—O8—Rb1v | −133.0 (5) | O22—Co1—O20—Mo6 | 178.39 (14) |
O7—Mo4—O15—Mo3 | −70.0 (2) | O20—Co1—O24—Mo4 | −179.13 (14) |
O7—Mo4—O16—Mo5 | −176.6 (2) | O20—Co1—O24—Mo5 | −83.98 (14) |
O7—Mo4—O23—Mo3 | 82.94 (16) | O24—Co1—O20—Mo1 | 179.91 (14) |
O7—Mo4—O23—Co1 | −171.43 (17) | O24—Co1—O20—Mo6 | 81.97 (14) |
O8—Mo4—O15—Mo3 | −177.30 (19) | O21—Co1—O22—Mo2 | 0.39 (13) |
O15—Mo4—O8—Rb1v | −32.2 (5) | O21—Co1—O22—Mo3 | 97.02 (14) |
O8—Mo4—O16—Mo5 | −67.8 (3) | O22—Co1—O21—Mo1 | 95.31 (14) |
O16—Mo4—O8—Rb1v | 123.6 (5) | O22—Co1—O21—Mo2 | −0.39 (13) |
O8—Mo4—O23—Mo3 | −71.0 (4) | O21—Co1—O23—Mo3 | −84.80 (15) |
O8—Mo4—O23—Co1 | 34.7 (5) | O21—Co1—O23—Mo4 | 177.50 (14) |
O23—Mo4—O8—Rb1v | 19.8 (8) | O23—Co1—O21—Mo1 | 178.48 (14) |
O8—Mo4—O24—Mo5 | 85.21 (15) | O23—Co1—O21—Mo2 | 82.78 (14) |
O8—Mo4—O24—Co1 | −170.13 (17) | O22—Co1—O23—Mo3 | −0.74 (14) |
O24—Mo4—O8—Rb1v | 50.2 (5) | O22—Co1—O23—Mo4 | −98.44 (15) |
O15—Mo4—O16—Mo5 | 56.1 (4) | O23—Co1—O22—Mo2 | −95.89 (15) |
O16—Mo4—O15—Mo3 | 57.4 (4) | O23—Co1—O22—Mo3 | 0.74 (14) |
O15—Mo4—O23—Mo3 | −15.34 (12) | O22—Co1—O24—Mo4 | 84.96 (15) |
O15—Mo4—O23—Co1 | 90.28 (16) | O22—Co1—O24—Mo5 | −179.89 (14) |
O23—Mo4—O15—Mo3 | 20.49 (15) | O24—Co1—O22—Mo2 | −179.14 (14) |
O15—Mo4—O24—Mo5 | −179.88 (14) | O24—Co1—O22—Mo3 | −82.51 (15) |
O15—Mo4—O24—Co1 | −75.22 (15) | O23—Co1—O24—Mo4 | 1.89 (14) |
O24—Mo4—O15—Mo3 | 90.43 (17) | O23—Co1—O24—Mo5 | 97.04 (15) |
O16—Mo4—O23—Mo3 | −178.02 (14) | O24—Co1—O23—Mo3 | 95.80 (15) |
O16—Mo4—O23—Co1 | −72.40 (16) | O24—Co1—O23—Mo4 | −1.90 (14) |
O23—Mo4—O16—Mo5 | 91.14 (19) | O28—Co2—O32—Rb1 | 37.56 (13) |
O16—Mo4—O24—Mo5 | −16.17 (13) | O32—Co2—O28—Rb1 | −35.90 (12) |
O16—Mo4—O24—Co1 | 88.49 (17) | O32—Co2—O28—C4 | −175.6 (3) |
O24—Mo4—O16—Mo5 | 21.76 (17) | O33—Co2—O28—Rb1 | −122.99 (13) |
O23—Mo4—O24—Mo5 | −106.37 (13) | O33—Co2—O28—C4 | 97.3 (3) |
O23—Mo4—O24—Co1 | −1.71 (13) | O34—Co2—O28—Rb1 | 140.73 (12) |
O24—Mo4—O23—Mo3 | −103.91 (13) | O34—Co2—O28—C4 | 1.0 (3) |
O24—Mo4—O23—Co1 | 1.71 (13) | O28—Co2—O35—Rb1 | −48.56 (12) |
Mo4—Mo5—O16—Mo4 | 0.000 (14) | O35—Co2—O28—Rb1 | 48.91 (13) |
Mo4—Mo5—O17—Mo6 | −90.06 (18) | O35—Co2—O28—C4 | −90.8 (3) |
Mo4—Mo5—O19—Mo6 | 146.27 (9) | O33—Co2—O32—Rb1 | 121.10 (14) |
Mo4—Mo5—O19—Co1 | 41.96 (12) | O32—Co2—O35—Rb1 | 46.77 (13) |
Mo4—Mo5—O24—Mo4 | 0.0 | O35—Co2—O32—Rb1 | −49.60 (13) |
Mo4—Mo5—O24—Co1 | −104.43 (16) | O36—Co2—O32—Rb1 | −148.82 (15) |
O9—Mo5—O16—Mo4 | 69.6 (3) | O34—Co2—O35—Rb1 | −140.10 (12) |
O9—Mo5—O17—Mo6 | 176.3 (2) | O36—Co2—O35—Rb1 | 136.14 (13) |
O9—Mo5—O24—Mo4 | −83.39 (16) | Rb1—O28—C4—O29 | −110.3 (5) |
O9—Mo5—O24—Co1 | 172.19 (18) | Rb1—O28—C4—C5 | 71.0 (5) |
O10—Mo5—O16—Mo4 | 177.8 (2) | Co2—O28—C4—O29 | 13.8 (7) |
O10—Mo5—O17—Mo6 | 67.3 (3) | Co2—O28—C4—C5 | −164.9 (3) |
O10—Mo5—O19—Mo6 | −86.24 (16) | O25—C1—C2—N1 | 165.7 (4) |
O10—Mo5—O19—Co1 | 169.46 (18) | O25—C1—C2—C3 | −71.9 (6) |
O10—Mo5—O24—Mo4 | 77.3 (5) | O26—C1—C2—N1 | −15.5 (6) |
O10—Mo5—O24—Co1 | −27.1 (5) | O26—C1—C2—C3 | 106.9 (5) |
O16—Mo5—O17—Mo6 | −58.1 (4) | N1—C2—C3—O27 | 61.8 (6) |
O17—Mo5—O16—Mo4 | −55.4 (4) | C1—C2—C3—O27 | −60.2 (6) |
O16—Mo5—O19—Mo6 | 177.87 (14) | O28—C4—C5—N2 | 6.4 (6) |
O16—Mo5—O19—Co1 | 73.57 (16) | O28—C4—C5—C6 | 129.8 (4) |
O19—Mo5—O16—Mo4 | −90.95 (19) | O29—C4—C5—N2 | −172.4 (4) |
O16—Mo5—O24—Mo4 | 16.10 (13) | O29—C4—C5—C6 | −49.0 (6) |
O16—Mo5—O24—Co1 | −88.33 (17) | N2—C5—C6—O30 | 66.2 (5) |
O24—Mo5—O16—Mo4 | −21.67 (17) | C4—C5—C6—O30 | −57.3 (6) |
O17—Mo5—O19—Mo6 | 15.87 (12) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+2, y−1/2, −z+1/2; (iii) −x+2, y+1/2, −z+1/2; (iv) x+1, y, z; (v) −x+1, y+1/2, −z+1/2; (vi) x, y+1, z; (vii) x+1/2, −y+1/2, −z; (viii) x+1/2, −y+3/2, −z; (ix) x−1/2, −y+1/2, −z; (x) x−1, y, z; (xi) −x+3/2, −y+1, z+1/2; (xii) x−1/2, −y+3/2, −z; (xiii) −x+3/2, −y+1, z−1/2; (xiv) x+1, y−1, z; (xv) x+1, y+1, z; (xvi) x−1, y+1, z; (xvii) x, y−1, z; (xviii) x−1, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O27—H4···O41 | 0.84 | 2.24 | 2.859 (6) | 131 |
O27—H4···N1 | 0.84 | 2.62 | 2.940 (6) | 104 |
O30—H11···O40 | 0.84 | 2.56 | 2.708 (6) | 91 |
O30—H11···O42vii | 0.84 | 2.24 | 2.928 (6) | 139 |
N1—H5···O2 | 0.91 | 2.11 | 2.944 (6) | 151 |
N1—H6···O26 | 0.91 | 2.49 | 2.647 (6) | 89 |
N1—H6···O39vii | 0.91 | 2.14 | 3.041 (6) | 170 |
N1—H7···O17ii | 0.91 | 2.09 | 2.905 (6) | 149 |
N2—H13···O28 | 0.91 | 2.60 | 2.691 (6) | 86 |
N2—H13···O43 | 0.91 | 2.11 | 3.013 (7) | 170 |
N2—H12···O8i | 0.91 | 2.31 | 2.912 (6) | 123 |
N2—H12···O28 | 0.91 | 2.61 | 2.691 (6) | 85 |
N2—H14···O13xvii | 0.91 | 1.93 | 2.827 (6) | 167 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+2, y−1/2, −z+1/2; (vii) x+1/2, −y+1/2, −z; (xvii) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O27—H4···O41 | 0.84 | 2.24 | 2.859 (6) | 131 |
O27—H4···N1 | 0.84 | 2.62 | 2.940 (6) | 104 |
O30—H11···O42i | 0.84 | 2.24 | 2.928 (6) | 139 |
N1—H5···O2 | 0.91 | 2.11 | 2.944 (6) | 151 |
N1—H6···O39i | 0.91 | 2.14 | 3.041 (6) | 170 |
N1—H7···O17ii | 0.91 | 2.09 | 2.905 (6) | 149 |
N2—H13···O43 | 0.91 | 2.11 | 3.013 (7) | 170 |
N2—H12···O8iii | 0.91 | 2.31 | 2.912 (6) | 123 |
N2—H14···O13iv | 0.91 | 1.93 | 2.827 (6) | 167 |
Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) −x+2, y−1/2, −z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) x, y−1, z. |
References
An, H., Han, Z., Xu, T., Meng, C. & Wang, E. (2008). Inorg. Chem. Commun. 11, 914–917. Web of Science CSD CrossRef CAS Google Scholar
Brown, I. D. (1980). Structure and Bonding in Crystals, Vol. II, pp. 1–30. New York: Academic Press. Google Scholar
Du, D. Y., Yan, L. K., Su, Z. M., Li, S. L., Lan, Y. Q. & Wang, E. B. (2013). Coord. Chem. Rev. 257, 702–717. Web of Science CrossRef CAS Google Scholar
Fang, X. K., Anderson, T. M. & Hill, C. L. (2005). Angew. Chem. Int. Ed. 44, 3540–3544. Web of Science CSD CrossRef CAS Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Hasenknopf, B., Micoine, K., Lacóte, E., Thorimbert, S., Malacria, M. & Thoubenot, R. (2008). Eur. J. Inorg. Chem. pp. 5001–5013. Web of Science CrossRef Google Scholar
Honda, D., Ikegami, S., Inoue, T., Ozeki, T. & Yagasaki, A. (2007). Inorg. Chem. 46, 1464–1470. Web of Science CSD CrossRef PubMed CAS Google Scholar
Inoue, M. & Yamase, T. (1995). Bull. Chem. Soc. Jpn, 38, 3055–3063. CrossRef Web of Science Google Scholar
Kortz, U., Savelieff, M. G., Ghalim, F. Y. A., Khali, L. M., Maalouf, S. A. & Sinno, D. I. (2002). Angew. Chem. Int. Ed. 41, 4070–4073. CrossRef CAS Google Scholar
Lide, D. E. (2007). Handbook of Chemistry and Physics, 88th ed., pp. 7–8. Boca Raton: CRC Press. Google Scholar
Perloff, A. (1970). Inorg. Chem. 9, 2228–2239. CrossRef CAS Web of Science Google Scholar
Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku (2010). CrystalStructure. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku/MSC (2002). RAPID-AUTO. Rigaku/MSC, The Woodlands, Texas, USA. Google Scholar
Sadakane, M., Dickman, M. H. & Pope, M. T. (2001). Inorg. Chem. 40, 2715–2719. Web of Science CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tan, H., Li, Y., Zhang, Z., Qin, C., Wang, X., Wang, E. & Su, Z. (2007). J. Am. Chem. Soc. 129, 10066–10067. Web of Science CrossRef PubMed CAS Google Scholar
Yang, Y., Xu, L., Li, F. & Qu, X. (2013). Inorg. Chem. Commun. 33, 142–146. Web of Science CSD CrossRef CAS Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Continuous interests in chiral polyoxometalates (POMs) are endowed owing to their prominent molecular applications such as nonlinear optics, magneto optical effect, and circular polarized luminescence (Hasenknopf et al., 2008; Du et al., 2013). Two synthetic procedures for chiral POMs have been delivered to date. One is the way based on the connection of chiral organic ligands and achiral inorganic POMs possible to propagate the local chirality to POM framework, which have been extensively studied by the groups of Hill, Kortz, Pope, Wang, and Yamase for a long time (Fang et al., 2005; Kortz et al., 2002; Sadakane et al., 2001; Tan et al., 2007, Inoue & Yamase, 1995). Although Anderson type POM is one of the typical achiral structures along with Keggin and Wells-Dawson types, there are little chiral POMs constructed from Anderson type POM as building block (An et al., 2008). Herein, the structural characterization of the chiral crystal containing Anderson type [H6CoMo6O24]3- as building block and amino acid L-Serine (L-Ser) as chiral organic ligand is reported. The crystallization of enantiomeric unit (Figure 1) consisting of the CoMo6 polyanion, [Co(H2O)5(L-Ser)]2+ (Co(II) complex), Rb+, one water molecule, and free L-Ser, and the other water molecules with noncentrosymmetric space group P212121 provided the title compound, of which the absolute configuration was supported by Flack parameter 0.025 (7). The pKa (2.2 and 9.2) of L-Ser and the acidic condition (pH 3.2) in the synthetic procedure suggest that all L-Ser molecules are zwitterionic. In fact, the carboxylate group in L-Ser coordinating to Co2+ and that in free L-Ser have similar C—O distances (1.250 (7), 1.264 (7) Å and 1.247 (7), 1.257 (7) Å) due to their resonance state (Lide, 2007). The BVS values calculated from the observed bond lengths are 2.0 and 3.2 for Co in Co(II) complex and the CoMo6 polyanion, 5.9–6.0 for Mo, indicating that the original valences of Co2+, Co3+, and Mo6+ are retained in the title compound. Additionally, the BVS values for six O atoms forming CoO6 octahedra in the CoMo6 polyanion are 1.1–1.2, suggesting that they are protonated (Brown, 1980). Similar protonation in Anderson type POMs have been frequently observed for [H6CrMo6O24]3-, [H2IMo6O24]3-, and [H6NiMo6O24]4- (Perloff, 1970; Honda et al., 2007; Yang et al., 2013). Figure 2 shows the crystal structure viewed along the a axis. The two kinds of polyanion (A-type and B-type) with different orientation in the ac plane are alternately connected along the crystallographic b axis by Rb+-bridging of terminal O atoms in the CoMo6 polyanion, forming the b-axially stacked polyanion unit. The polyanion units are aligned along the c axis with a help of hydrogen bonding (O···O < 3.3 Å) relating with some waters of crystallization and aqua ligands in Co(II) complex, of which the unit distance is the half of c axis value. The both distance of A-type···A-type and B-type···B-type are 11.6 Å; (Co···Co distance), which corresponds to the b axis value. Figure 3 is the representation of the b-axially polyanion stacking mentioned above along the c axis. It is clearly demonstrated that A-type polyanion and B-type polyanion are altenately stacked with a cross angle of 46.1°, which is calculated from the dihedral angle of the least square plane defined by Co, Mo1, Mo2, Mo3, Mo4, Mo5, and Mo6 in the CoMo6 polyanion.