supplementary materials


hb7134 scheme

Acta Cryst. (2013). E69, m612-m613    [ doi:10.1107/S1600536813028304 ]

Rubidium penta­aqua­(L-serine)cobalt(II) hexa­hydrogenhexa­molybdocobaltate(III) L-serine monosolvate deca­hydrate

J. Iijima, H. Naruke and H. Takiyama

Abstract top

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.

Comment top

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.

Related literature top

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 top

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.

Refinement top

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 refinement 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 refinement 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.

Computing details top

Data collection: RAPID-AUTO (Rigaku/MSC, 2002); cell refinement: 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).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound with displacement ellipsoids drawn at the 50% probability level. White, red, blue, green, moss green and yellowish brown ellipsoids denote Mo, O, Co, Rb, C, and N atoms, respectively. The H atoms protonated to the CoMo6 polyanion are omitted for clarity.
[Figure 2] Fig. 2. Packing diagram viewed along the a axis. The rectangle traced with standard line indicates the unit cell. Color codes; white octahedron: MoO6, blue octahedron CoO6, and Co(II) complex, green sphere: Rb, red sphere O. The hydrogen bondings are denoted by sky blue dashed lines. The L-Ser molecule and waters of crystallization O atoms unrelated to hydrogen bonding are omitted for clarity.
[Figure 3] Fig. 3. The alternate polyanion stacking of A-type and B-type viewed along the c axis. The square shows the unit cell. The MoO6 octahedron is denoted in open faced manner, and the O atoms in the CoMo6 polyanion are denoted by red spheres. The definition of the least square plane consisting of Co, Mo1, Mo2, Mo3, Mo4, Mo5, and Mo6 in the CoMo6 polyanion is also represented.
Rubidium pentaaqua(L-serine)cobalt(II) hexahydrogenhexamolybdocobaltate(III) L-serine monosolvate decahydrate top
Crystal data top
Rb[Co(C3H7NO3)(H2O)5][H6CoMo6O24]·C3H7NO3·10H2OF(000) = 3212.00
Mr = 1649.42Dx = 2.504 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71075 Å
Hall symbol: P 2ac 2abCell parameters from 59700 reflections
a = 10.8411 (5) Åθ = 3.0–27.5°
b = 11.5923 (4) ŵ = 3.63 mm1
c = 34.8078 (12) ÅT = 183 K
V = 4374.4 (3) Å3Platelet, green
Z = 40.41 × 0.36 × 0.19 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
9728 reflections with F2 > 2σ(F2)
Detector resolution: 10.000 pixels mm-1Rint = 0.062
ω scansθmax = 27.5°
Absorption correction: numerical
(NUMABS; Rigaku, 1999)
h = 1414
Tmin = 0.123, Tmax = 0.500k = 1514
70065 measured reflectionsl = 4545
10010 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-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 reflectionsΔρmax = 3.61 e Å3
559 parametersΔρmin = 1.10 e Å3
0 restraintsAbsolute structure: Flack (1983), 4426 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.025 (7)
Secondary atom site location: difference Fourier map
Crystal data top
Rb[Co(C3H7NO3)(H2O)5][H6CoMo6O24]·C3H7NO3·10H2OV = 4374.4 (3) Å3
Mr = 1649.42Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 10.8411 (5) ŵ = 3.63 mm1
b = 11.5923 (4) ÅT = 183 K
c = 34.8078 (12) Å0.41 × 0.36 × 0.19 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
10010 independent reflections
Absorption correction: numerical
(NUMABS; Rigaku, 1999)
9728 reflections with F2 > 2σ(F2)
Tmin = 0.123, Tmax = 0.500Rint = 0.062
70065 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.099Δρmax = 3.61 e Å3
S = 1.04Δρmin = 1.10 e Å3
10010 reflectionsAbsolute structure: Flack (1983), 4426 Friedel pairs
559 parametersAbsolute structure parameter: 0.025 (7)
0 restraints
Special details top

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).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.98964 (4)0.94684 (3)0.207793 (11)0.01204 (9)
Mo20.74633 (3)0.84989 (3)0.159456 (12)0.01213 (9)
Mo30.49911 (3)0.75710 (3)0.205914 (11)0.01245 (9)
Mo40.50288 (4)0.74903 (3)0.301413 (11)0.01297 (9)
Mo50.74159 (3)0.84414 (3)0.349594 (12)0.01364 (9)
Mo60.98220 (4)0.94607 (3)0.303320 (11)0.01208 (9)
Rb10.73248 (5)0.52247 (4)0.145507 (15)0.02399 (11)
Co10.74451 (5)0.84817 (4)0.254347 (19)0.00969 (12)
Co20.67086 (6)0.46834 (6)0.043914 (18)0.01672 (14)
O11.0518 (4)1.0822 (4)0.20918 (11)0.0217 (8)
O21.0846 (4)0.8663 (4)0.17903 (10)0.0212 (8)
O30.8426 (4)0.7691 (3)0.13123 (10)0.0196 (7)
O40.6534 (4)0.9266 (4)0.12866 (10)0.0203 (8)
O50.4363 (4)0.6206 (3)0.20593 (11)0.0205 (8)
O60.4087 (4)0.8391 (4)0.17621 (10)0.0205 (8)
O70.4401 (4)0.6137 (3)0.29822 (11)0.0211 (8)
O80.4089 (4)0.8259 (3)0.33182 (10)0.0181 (8)
O90.6422 (4)0.9134 (4)0.37969 (11)0.0233 (8)
O100.8398 (4)0.7659 (4)0.37805 (10)0.0229 (8)
O111.0744 (3)0.8673 (3)0.33354 (10)0.0174 (7)
O121.0443 (4)1.0825 (3)0.30257 (11)0.0200 (8)
O130.8528 (3)0.9780 (3)0.17385 (9)0.0140 (7)
O140.6360 (3)0.7246 (3)0.17290 (10)0.0146 (7)
O150.4347 (3)0.8152 (3)0.25403 (10)0.0156 (7)
O160.6406 (4)0.7154 (3)0.33395 (10)0.0172 (7)
O170.8416 (3)0.9759 (3)0.33605 (10)0.0166 (7)
O181.0544 (3)0.8863 (3)0.25617 (10)0.0143 (7)
O190.8487 (3)0.7967 (3)0.29521 (9)0.0122 (7)
O200.8484 (3)0.9818 (3)0.25489 (9)0.0120 (6)
O210.8514 (3)0.7968 (3)0.21394 (9)0.0109 (7)
O220.6412 (3)0.9013 (3)0.21348 (9)0.0117 (7)
O230.6387 (3)0.7160 (3)0.25320 (10)0.0130 (6)
O240.6384 (3)0.8976 (3)0.29495 (9)0.0124 (7)
O251.0441 (4)0.5935 (4)0.04817 (12)0.0314 (10)
O261.2444 (4)0.5865 (4)0.06457 (11)0.0256 (8)
O271.1876 (4)0.8681 (4)0.06784 (11)0.0254 (8)
O280.7536 (3)0.3482 (3)0.08204 (10)0.0184 (7)
O290.9125 (4)0.2885 (4)0.04575 (11)0.0243 (8)
O300.7725 (4)0.0466 (4)0.05742 (11)0.0334 (10)
O310.7102 (3)0.5053 (3)0.23535 (11)0.0208 (8)
O320.5473 (4)0.5398 (4)0.08612 (11)0.0229 (8)
O330.5412 (4)0.3362 (4)0.03548 (11)0.0247 (8)
O340.7917 (4)0.4190 (4)0.00155 (10)0.0216 (8)
O350.7958 (4)0.5901 (4)0.06412 (11)0.0243 (8)
O360.5870 (4)0.5650 (4)0.00168 (11)0.0316 (10)
O370.6585 (4)0.2721 (4)0.04481 (11)0.0275 (9)
O380.2036 (4)0.6949 (4)0.2567 (2)0.0565 (18)
O390.9618 (4)0.2655 (4)0.09497 (11)0.0265 (9)
O400.8044 (4)0.0929 (4)0.01818 (11)0.0250 (9)
O411.3218 (5)1.0091 (4)0.12069 (12)0.0361 (10)
O420.2127 (4)0.6982 (4)0.04824 (14)0.0353 (10)
O430.5376 (5)0.1397 (4)0.08536 (14)0.0382 (11)
O440.3835 (4)0.6982 (4)0.01085 (12)0.0326 (10)
O450.4649 (5)0.9210 (4)0.02937 (13)0.0389 (11)
N11.2151 (5)0.6988 (4)0.13015 (12)0.0201 (9)
N20.7690 (4)0.1719 (4)0.13211 (14)0.0199 (9)
C11.1344 (5)0.6185 (5)0.06875 (15)0.0201 (10)
C21.1089 (5)0.7005 (5)0.10294 (14)0.0178 (10)
C31.0849 (6)0.8225 (5)0.08854 (16)0.0240 (11)
C40.8428 (5)0.2819 (5)0.07428 (13)0.0170 (10)
C50.8689 (5)0.1813 (5)0.10152 (15)0.0193 (10)
C60.8809 (6)0.0683 (5)0.07916 (16)0.0253 (12)
H11.03370.67270.11680.0214*
H21.01150.82210.07160.0288*
H130.69410.16420.12060.0238*
H120.76930.23670.14690.0238*
H140.78390.10920.14720.0238*
H31.06680.87320.11070.0288*
H41.24970.87000.08230.0305*
H51.19810.74490.15060.0241*
H61.28390.72510.11800.0241*
H71.22820.62540.13840.0241*
H80.94920.19660.11470.0231*
H90.95280.07280.06170.0304*
H100.89500.00390.09730.0304*
H110.78050.01570.04530.0401*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.00991 (17)0.01256 (18)0.01365 (17)0.00216 (14)0.00079 (14)0.00013 (14)
Mo20.01080 (18)0.01307 (19)0.01252 (18)0.00066 (15)0.00029 (13)0.00023 (13)
Mo30.00977 (18)0.01192 (18)0.01566 (18)0.00179 (15)0.00060 (14)0.00069 (14)
Mo40.01106 (18)0.01205 (18)0.01579 (18)0.00148 (15)0.00241 (15)0.00050 (14)
Mo50.01245 (19)0.01610 (19)0.01237 (18)0.00063 (16)0.00120 (13)0.00002 (14)
Mo60.00996 (17)0.01245 (18)0.01384 (18)0.00125 (14)0.00103 (14)0.00076 (14)
Rb10.0239 (3)0.0221 (3)0.0259 (3)0.0034 (2)0.00233 (19)0.0013 (2)
Co10.0077 (3)0.0092 (3)0.0121 (3)0.0002 (2)0.0003 (2)0.0001 (2)
Co20.0147 (3)0.0177 (3)0.0177 (3)0.0013 (3)0.0006 (3)0.0017 (3)
O10.0194 (18)0.0199 (18)0.0257 (19)0.0014 (15)0.0031 (15)0.0068 (16)
O20.0160 (17)0.029 (2)0.0191 (18)0.0003 (15)0.0028 (14)0.0047 (16)
O30.0191 (18)0.0188 (17)0.0210 (17)0.0008 (15)0.0011 (14)0.0049 (15)
O40.0196 (18)0.0209 (17)0.0204 (17)0.0006 (15)0.0066 (14)0.0056 (15)
O50.0197 (18)0.0162 (16)0.0257 (19)0.0058 (14)0.0034 (15)0.0026 (15)
O60.0161 (17)0.027 (2)0.0188 (17)0.0060 (16)0.0053 (14)0.0008 (16)
O70.0223 (19)0.0164 (17)0.0246 (19)0.0067 (15)0.0016 (16)0.0025 (15)
O80.0188 (18)0.0186 (18)0.0170 (17)0.0014 (14)0.0040 (14)0.0021 (15)
O90.0195 (18)0.030 (2)0.0208 (18)0.0012 (15)0.0054 (15)0.0027 (16)
O100.0213 (18)0.030 (2)0.0174 (18)0.0017 (16)0.0018 (15)0.0075 (16)
O110.0159 (16)0.0191 (18)0.0174 (17)0.0009 (14)0.0011 (13)0.0013 (15)
O120.0177 (18)0.0194 (17)0.0228 (18)0.0024 (14)0.0017 (15)0.0010 (15)
O130.0140 (15)0.0110 (15)0.0169 (16)0.0037 (13)0.0031 (13)0.0025 (13)
O140.0139 (16)0.0130 (15)0.0168 (16)0.0049 (13)0.0029 (13)0.0019 (14)
O150.0102 (14)0.0157 (15)0.0209 (17)0.0005 (11)0.0018 (14)0.0014 (14)
O160.0189 (18)0.0165 (17)0.0164 (17)0.0017 (14)0.0010 (13)0.0024 (14)
O170.0148 (16)0.0171 (17)0.0179 (16)0.0012 (14)0.0000 (13)0.0055 (14)
O180.0099 (14)0.0153 (15)0.0178 (16)0.0010 (11)0.0008 (13)0.0011 (14)
O190.0120 (15)0.0107 (15)0.0139 (16)0.0004 (12)0.0012 (12)0.0006 (13)
O200.0105 (14)0.0095 (13)0.0161 (15)0.0002 (11)0.0004 (12)0.0011 (13)
O210.0072 (14)0.0104 (14)0.0152 (16)0.0005 (11)0.0016 (12)0.0014 (13)
O220.0095 (15)0.0098 (15)0.0159 (16)0.0007 (12)0.0020 (12)0.0007 (13)
O230.0108 (14)0.0098 (13)0.0184 (16)0.0018 (11)0.0014 (13)0.0002 (14)
O240.0108 (15)0.0109 (15)0.0154 (16)0.0013 (12)0.0018 (13)0.0016 (13)
O250.022 (2)0.041 (3)0.031 (3)0.0027 (17)0.0023 (17)0.0115 (19)
O260.0184 (18)0.0302 (19)0.028 (2)0.0011 (16)0.0004 (16)0.0045 (17)
O270.0224 (19)0.029 (2)0.0243 (19)0.0013 (16)0.0044 (16)0.0040 (17)
O280.0178 (17)0.0171 (17)0.0203 (17)0.0046 (15)0.0001 (13)0.0011 (13)
O290.0192 (18)0.030 (2)0.0237 (19)0.0063 (15)0.0047 (15)0.0074 (17)
O300.044 (3)0.028 (2)0.028 (2)0.014 (2)0.0039 (18)0.0053 (18)
O310.0145 (16)0.0127 (16)0.035 (2)0.0019 (13)0.0039 (14)0.0001 (15)
O320.0158 (16)0.0253 (19)0.0276 (19)0.0024 (15)0.0028 (14)0.0021 (16)
O330.0200 (18)0.0232 (18)0.031 (2)0.0027 (15)0.0017 (15)0.0007 (17)
O340.0203 (18)0.0229 (17)0.0217 (18)0.0000 (15)0.0020 (14)0.0005 (15)
O350.0225 (19)0.0197 (18)0.031 (2)0.0033 (14)0.0032 (16)0.0035 (16)
O360.026 (2)0.042 (3)0.028 (2)0.0136 (19)0.0042 (16)0.0127 (19)
O370.0190 (18)0.040 (3)0.0231 (19)0.0027 (17)0.0008 (15)0.0048 (18)
O380.0155 (19)0.0092 (17)0.145 (6)0.0025 (14)0.003 (3)0.008 (3)
O390.0219 (19)0.029 (2)0.0283 (19)0.0050 (17)0.0029 (15)0.0050 (17)
O400.023 (2)0.027 (2)0.025 (2)0.0047 (15)0.0025 (15)0.0065 (16)
O410.050 (3)0.027 (2)0.031 (3)0.010 (2)0.007 (2)0.0032 (19)
O420.034 (3)0.027 (2)0.045 (3)0.0032 (18)0.005 (2)0.0022 (19)
O430.034 (3)0.033 (3)0.047 (3)0.0042 (19)0.000 (2)0.010 (2)
O440.028 (3)0.037 (3)0.032 (3)0.0086 (18)0.0041 (18)0.0043 (19)
O450.034 (3)0.044 (3)0.039 (3)0.015 (2)0.003 (2)0.006 (2)
N10.028 (3)0.017 (2)0.016 (2)0.0029 (17)0.0006 (17)0.0017 (17)
N20.0127 (19)0.0080 (16)0.039 (3)0.0054 (15)0.0093 (18)0.0129 (18)
C10.019 (3)0.021 (3)0.020 (3)0.003 (2)0.0010 (19)0.003 (2)
C20.016 (3)0.019 (3)0.018 (3)0.0013 (18)0.0034 (19)0.001 (2)
C30.026 (3)0.022 (3)0.024 (3)0.010 (2)0.003 (2)0.007 (3)
C40.017 (3)0.019 (3)0.015 (2)0.0000 (19)0.0012 (18)0.0021 (19)
C50.015 (3)0.020 (3)0.023 (3)0.0019 (19)0.0035 (19)0.006 (2)
C60.028 (3)0.020 (3)0.028 (3)0.009 (3)0.008 (3)0.001 (3)
Geometric parameters (Å, º) top
Mo1—O11.709 (4)Rb1—O283.002 (4)
Mo1—O21.713 (4)Rb1—O313.143 (4)
Mo1—O131.931 (4)Rb1—O322.889 (4)
Mo1—O181.955 (4)Rb1—O353.018 (4)
Mo1—O202.280 (3)Co1—O191.912 (4)
Mo1—O212.306 (3)Co1—O201.915 (3)
Mo2—O31.712 (4)Co1—O211.917 (4)
Mo2—O41.719 (4)Co1—O221.913 (4)
Mo2—O131.946 (4)Co1—O231.915 (3)
Mo2—O141.939 (4)Co1—O241.910 (4)
Mo2—O212.296 (4)Co2—O282.123 (4)
Mo2—O222.278 (4)Co2—O322.154 (4)
Mo3—O51.722 (4)Co2—O332.099 (4)
Mo3—O61.713 (4)Co2—O342.132 (4)
Mo3—O141.914 (4)Co2—O352.078 (4)
Mo3—O151.936 (4)Co2—O362.060 (5)
Mo3—O222.288 (3)O25—C11.248 (7)
Mo3—O232.286 (4)O26—C11.257 (7)
Mo4—Mo53.2749 (6)O27—C31.428 (7)
Mo4—O71.713 (4)O28—C41.264 (6)
Mo4—O81.718 (4)O29—C41.250 (6)
Mo4—O151.964 (4)O30—C61.420 (7)
Mo4—O161.914 (4)N1—C21.491 (7)
Mo4—O232.265 (4)N2—C51.523 (7)
Mo4—O242.275 (4)C1—C21.548 (8)
Mo5—O91.704 (4)C2—C31.523 (8)
Mo5—O101.713 (4)C4—C51.529 (7)
Mo5—O161.929 (4)C5—C61.530 (8)
Mo5—O171.931 (4)O27—H40.840
Mo5—O192.288 (4)O30—H110.840
Mo5—O242.292 (4)N1—H50.910
Mo6—O111.714 (4)N1—H60.910
Mo6—O121.719 (4)N1—H70.910
Mo6—O171.934 (4)N2—H130.910
Mo6—O181.946 (4)N2—H120.910
Mo6—O192.274 (4)N2—H140.910
Mo6—O202.262 (3)C2—H11.000
Rb1—O33.138 (4)C3—H20.990
Rb1—O8i2.858 (4)C3—H30.990
Rb1—O11ii2.855 (4)C5—H81.000
Rb1—O12ii3.099 (4)C6—H90.990
Rb1—O142.737 (4)C6—H100.990
Co1···O133.390 (4)O7···H12v3.2919
Co1···O143.387 (4)O7···H14v3.0848
Co1···O153.380 (3)O8···H13v2.7395
Co1···O163.364 (4)O8···H12v2.3132
Co1···O173.374 (4)O8···H14v3.3485
Co1···O183.389 (3)O10···H8iii2.4384
Co2···O293.349 (4)O11···H12iii2.3729
O1···O123.252 (6)O11···H14iii3.4299
O1···O19iii2.714 (5)O11···H8iii2.6886
O1···O31iii3.344 (6)O13···H13vi3.3249
O2···O33.305 (5)O13···H12vi3.2702
O2···O6iv3.528 (5)O13···H14vi1.9329
O4···O63.287 (5)O13···H8vi3.4279
O4···O7v3.494 (6)O13···H10vi2.7195
O4···O30vi3.122 (6)O25···H12.5619
O4···N2vi3.110 (6)O25···H22.7950
O4···C6vi3.427 (7)O26···H13.0852
O5···O73.214 (6)O26···H43.3433
O5···O24i2.710 (5)O26···H53.5492
O5···O313.414 (5)O26···H62.4944
O7···O22i2.647 (5)O26···H72.6156
O7···N2v3.387 (6)O27···H13.2887
O8···O93.194 (6)O27···H53.2180
O8···N2v2.912 (6)O27···H62.6237
O9···O32v2.789 (6)O28···H132.6015
O10···O113.202 (5)O28···H122.6064
O10···C5iii3.383 (7)O28···H143.5942
O11···N2iii3.073 (6)O28···H82.9795
O11···C4iii3.476 (6)O29···H82.6561
O11···C5iii3.184 (7)O29···H92.5982
O12···O21iii2.790 (5)O30···H132.7231
O13···N2vi2.827 (6)O30···H143.2090
O13···C5vi3.453 (6)O30···H83.2665
O13···C6vi3.472 (7)O36···H9ix3.0878
O15···O31v2.731 (5)N1···H23.3264
O18···O31iii2.915 (5)N1···H32.6702
O23···O312.637 (5)N1···H42.6186
O25···C33.036 (7)N2···H93.3613
O26···O273.323 (6)N2···H102.6694
O26···N12.647 (6)C1···H22.7114
O26···C33.342 (7)C1···H33.3743
O27···N12.940 (6)C1···H43.2060
O27···C12.950 (7)C1···H53.2783
O28···N22.691 (6)C1···H62.6629
O28···C63.528 (7)C1···H72.6307
O29···O303.215 (6)C2···H42.5901
O29···O33vii3.469 (6)C3···H52.6429
O29···O342.592 (6)C3···H62.6418
O29···C62.826 (7)C3···H73.2631
O30···N22.978 (6)C4···H132.6571
O30···C42.893 (7)C4···H122.7012
O33···C43.593 (6)C4···H143.2938
O34···C43.130 (6)C4···H92.7369
O1···O38v3.283 (6)C4···H103.3691
O2···O38iv3.594 (7)C5···H113.1558
O2···N12.944 (6)C6···H132.7233
O2···C23.283 (6)C6···H123.2912
O2···C33.190 (7)C6···H142.6329
O3···O42viii3.236 (6)H1···H22.3511
O3···C23.152 (7)H1···H32.3608
O3···C33.081 (7)H1···H43.4866
O4···O39ix3.030 (6)H1···H52.2942
O4···O42viii3.216 (6)H1···H62.7796
O4···O43vi3.154 (6)H1···H72.3045
O5···O383.198 (7)H2···H42.6673
O6···O39ix3.009 (6)H2···H53.5292
O6···O41x2.916 (6)H2···H63.5481
O6···N1x3.101 (6)H13···H82.7983
O7···O383.091 (7)H13···H102.9751
O9···O26iii3.050 (6)H13···H113.4765
O10···O37xi2.721 (6)H12···H82.2966
O10···O41ii3.455 (6)H12···H103.4808
O13···O38v3.541 (7)H14···H82.3477
O14···O39ix3.339 (6)H14···H93.5184
O15···O382.869 (5)H14···H102.4393
O16···O41ii2.894 (6)H3···H42.2173
O16···O43v3.520 (6)H3···H52.4834
O17···N1iii2.905 (6)H3···H62.9242
O17···C2iii3.403 (6)H3···H73.4992
O18···O38iv2.746 (5)H4···H52.8423
O20···O38v2.566 (5)H4···H62.1224
O25···O352.749 (6)H4···H73.4521
O25···O45viii2.837 (7)H8···H92.3377
O26···O9ii3.050 (6)H8···H102.3876
O26···O32iv3.411 (6)H9···H112.2061
O26···O39vii3.313 (6)H10···H112.2058
O26···O40vii2.713 (6)Mo1···H33.5841
O26···O44iv2.729 (6)Mo5···H7iii3.3029
O27···O34viii3.562 (6)O2···H13.1673
O27···O36viii2.766 (6)O2···H32.3869
O27···O39vii3.337 (6)O2···H52.1144
O27···O412.859 (6)O2···H63.4440
O27···O44iv3.511 (6)O2···H73.4959
O27···O45iv3.347 (6)O3···H12.4073
O28···O433.367 (6)O3···H22.8346
O29···O37vii2.758 (6)O3···H32.8059
O29···O403.386 (6)O5···H5x3.5281
O30···O402.708 (6)O5···H7x3.2581
O30···O42vii2.928 (6)O6···H5x2.6821
O30···O432.931 (7)O6···H6x2.7716
O32···O26x3.411 (6)O6···H7x3.4202
O32···O39ix2.793 (6)O9···H7iii2.9001
O33···O373.159 (6)O12···H1iii3.1126
O33···O40ix2.762 (6)O13···H33.4190
O33···O432.864 (6)O17···H1iii3.1189
O34···O27xii3.562 (6)O17···H5iii3.1826
O34···O372.693 (6)O17···H6iii3.5719
O34···O45viii2.812 (6)O17···H7iii2.0891
O35···O252.749 (6)O27···H9vi3.4869
O35···O42viii2.672 (6)O35···H13.3071
O36···O27xii2.766 (6)O35···H23.5739
O36···O42viii3.467 (6)O36···H2xii2.9821
O36···O442.711 (6)O36···H4xii3.4952
O36···C3xii3.401 (7)O37···H8ix3.3473
O37···O10xiii2.721 (6)O37···H9ix2.9248
O37···O29ix2.758 (6)O38···H12v3.4037
O37···O333.159 (6)O38···H14v3.4937
O37···O342.693 (6)O39···H4ix2.6354
O37···O402.770 (6)O39···H5ix3.4609
O38···O1i3.283 (6)O39···H6ix2.1396
O38···O2x3.594 (7)O39···H7ix3.3673
O38···O53.198 (7)O40···H93.2207
O38···O73.091 (7)O40···H112.5578
O38···O13i3.541 (7)O41···H33.2008
O38···O152.869 (5)O41···H42.2367
O38···O18x2.746 (5)O41···H53.5017
O38···O20i2.566 (5)O41···H63.3191
O39···O4vii3.030 (6)O42···H2xii3.3487
O39···O6vii3.009 (6)O42···H10ix3.5090
O39···O14vii3.339 (6)O42···H11ix2.2422
O39···O26ix3.313 (6)O43···H132.1120
O39···O27ix3.337 (6)O43···H123.4863
O39···O32vii2.793 (6)O43···H143.4463
O39···O41ix3.328 (6)O43···H113.4813
O39···O42xiv3.197 (6)O44···H2xii3.1971
O39···O44vii3.147 (6)O44···H4x3.4995
O39···O45vii2.909 (6)O44···H11ix3.0896
O39···N1ix3.041 (6)O45···H4x3.0294
O40···O26ix2.713 (6)O45···H11vi3.5431
O40···O293.386 (6)C3···H9vi3.3681
O40···O302.708 (6)C3···H10vi2.9592
O40···O33vii2.762 (6)C6···H2xvii3.1970
O40···O372.770 (6)C6···H3xvii3.2224
O40···O44vii3.491 (6)H1···O23.1673
O40···C1ix3.536 (7)H1···O32.4073
O40···C63.500 (7)H1···O12ii3.1126
O41···O6iv2.916 (6)H1···O17ii3.1189
O41···O10iii3.455 (6)H1···O353.3071
O41···O16iii2.894 (6)H2···O32.8346
O41···O272.859 (6)H2···O353.5739
O41···O39vii3.328 (6)H2···O36viii2.9821
O41···O43xv3.046 (7)H2···O42viii3.3487
O41···C33.539 (8)H2···O44viii3.1971
O42···O3xii3.236 (6)H2···C6vi3.1970
O42···O4xii3.216 (6)H2···H9vi2.9953
O42···O30ix2.928 (6)H2···H10vi2.6152
O42···O35xii2.672 (6)H2···H11vi3.2630
O42···O36xii3.467 (6)H13···O432.1120
O42···O39xvi3.197 (6)H12···O38i3.4037
O42···O442.768 (7)H12···O433.4863
O42···O45xii3.092 (7)H14···O38i3.4937
O43···O4xvii3.154 (6)H14···O433.4463
O43···O16i3.520 (6)H3···Mo13.5841
O43···O283.367 (6)H3···O22.3869
O43···O302.931 (7)H3···O32.8059
O43···O332.864 (6)H3···O133.4190
O43···O41xviii3.046 (7)H3···O413.2008
O43···O45xvii3.294 (7)H3···C6vi3.2224
O43···N23.013 (7)H3···H9vi3.1293
O44···O26x2.729 (6)H3···H10vi2.4462
O44···O27x3.511 (6)H4···O36viii3.4952
O44···O362.711 (6)H4···O39vii2.6354
O44···O39ix3.147 (6)H4···O412.2367
O44···O40ix3.491 (6)H4···O44iv3.4995
O44···O422.768 (7)H4···O45iv3.0294
O44···O452.805 (7)H5···O22.1144
O44···C1x3.494 (7)H5···O5iv3.5281
O45···O25xii2.837 (7)H5···O6iv2.6821
O45···O27x3.347 (6)H5···O17ii3.1826
O45···O34xii2.812 (6)H5···O39vii3.4609
O45···O39ix2.909 (6)H5···O413.5017
O45···O42viii3.092 (7)H6···O23.4440
O45···O43vi3.294 (7)H6···O6iv2.7716
O45···O442.805 (7)H6···O17ii3.5719
N1···O22.944 (6)H6···O39vii2.1396
N1···O6iv3.101 (6)H6···O413.3191
N1···O17ii2.905 (6)H7···Mo5ii3.3029
N1···O39vii3.041 (6)H7···O23.4959
N2···O433.013 (7)H7···O5iv3.2581
C1···O40vii3.536 (7)H7···O6iv3.4202
C1···O44iv3.494 (7)H7···O9ii2.9001
C2···O23.283 (6)H7···O17ii2.0891
C2···O33.152 (7)H7···O39vii3.3673
C2···O17ii3.403 (6)H8···O37vii3.3473
C3···O23.190 (7)H9···O27xvii3.4869
C3···O33.081 (7)H9···O37vii2.9248
C3···O36viii3.401 (7)H9···O403.2207
C3···O413.539 (8)H9···C3xvii3.3681
C6···O403.500 (7)H9···H2xvii2.9953
Mo2···H14vi3.0638H9···H3xvii3.1293
Mo2···H10vi3.2343H10···O42vii3.5090
Mo4···H13v3.5913H10···C3xvii2.9592
Mo4···H12v3.4589H10···H2xvii2.6152
Rb1···H123.3372H10···H3xvii2.4462
O3···H10vi3.0200H11···O402.5578
O4···H13vi2.8030H11···O42vii2.2422
O4···H14vi2.6260H11···O433.4813
O4···H10vi2.9750H11···O44vii3.0896
O4···H11vi3.2797H11···O45xvii3.5431
O7···H13v3.2320H11···H2xvii3.2630
O1—Mo1—O2106.26 (19)O12ii—Rb1—O28121.37 (10)
O1—Mo1—O1398.55 (16)O12ii—Rb1—O3159.59 (10)
O1—Mo1—O1899.41 (16)O12ii—Rb1—O32160.80 (11)
O1—Mo1—O2094.66 (15)O12ii—Rb1—O35108.16 (10)
O1—Mo1—O21161.17 (15)O14—Rb1—O28149.48 (10)
O2—Mo1—O13101.91 (16)O14—Rb1—O3171.23 (10)
O2—Mo1—O1895.28 (16)O14—Rb1—O3285.65 (11)
O2—Mo1—O20157.08 (15)O14—Rb1—O35101.05 (11)
O2—Mo1—O2191.95 (15)O28—Rb1—O31134.06 (9)
O13—Mo1—O18150.50 (14)O28—Rb1—O3264.74 (10)
O13—Mo1—O2083.71 (13)O28—Rb1—O3557.77 (10)
O13—Mo1—O2172.44 (13)O31—Rb1—O32131.53 (10)
O18—Mo1—O2071.68 (12)O31—Rb1—O35165.42 (10)
O18—Mo1—O2183.28 (12)O32—Rb1—O3557.89 (11)
O20—Mo1—O2168.32 (11)O19—Co1—O2084.13 (14)
O3—Mo2—O4106.40 (17)O19—Co1—O2195.27 (14)
O3—Mo2—O13101.74 (16)O19—Co1—O22179.37 (14)
O3—Mo2—O1496.02 (16)O19—Co1—O2396.87 (14)
O3—Mo2—O2191.44 (14)O19—Co1—O2484.19 (14)
O3—Mo2—O22157.18 (15)O20—Co1—O2184.43 (13)
O4—Mo2—O1396.50 (16)O20—Co1—O2295.24 (13)
O4—Mo2—O14100.17 (16)O20—Co1—O23178.98 (14)
O4—Mo2—O21160.79 (15)O20—Co1—O2495.97 (14)
O4—Mo2—O2294.94 (15)O21—Co1—O2284.74 (14)
O13—Mo2—O14151.07 (14)O21—Co1—O2395.64 (14)
O13—Mo2—O2172.40 (12)O21—Co1—O24179.29 (14)
O13—Mo2—O2283.38 (13)O22—Co1—O2383.75 (14)
O14—Mo2—O2184.61 (13)O22—Co1—O2495.80 (14)
O14—Mo2—O2271.82 (13)O23—Co1—O2483.96 (14)
O21—Mo2—O2268.69 (11)O28—Co2—O3295.09 (14)
O5—Mo3—O6106.47 (18)O28—Co2—O3383.78 (14)
O5—Mo3—O1497.22 (16)O28—Co2—O3491.63 (14)
O5—Mo3—O15100.19 (16)O28—Co2—O3587.62 (14)
O5—Mo3—O22159.57 (15)O28—Co2—O36171.73 (16)
O5—Mo3—O2394.01 (15)O32—Co2—O3387.67 (15)
O6—Mo3—O14100.99 (16)O32—Co2—O34172.49 (15)
O6—Mo3—O1597.04 (16)O32—Co2—O3585.04 (15)
O6—Mo3—O2292.83 (15)O32—Co2—O3690.17 (16)
O6—Mo3—O23158.31 (15)O33—Co2—O3496.41 (15)
O14—Mo3—O15150.19 (14)O33—Co2—O35168.19 (16)
O14—Mo3—O2272.02 (13)O33—Co2—O3690.08 (16)
O14—Mo3—O2382.99 (13)O34—Co2—O3591.89 (15)
O15—Mo3—O2283.62 (12)O34—Co2—O3683.53 (15)
O15—Mo3—O2371.85 (13)O35—Co2—O3699.20 (17)
O22—Mo3—O2367.91 (11)Mo2—O3—Rb1100.10 (15)
Mo5—Mo4—O7130.93 (13)Mo4—O8—Rb1v154.38 (19)
Mo5—Mo4—O888.76 (12)Mo6—O11—Rb1iii104.41 (16)
Mo5—Mo4—O15126.59 (10)Mo6—O12—Rb1iii95.20 (15)
Mo5—Mo4—O1631.70 (11)Mo1—O13—Mo2118.07 (17)
Mo5—Mo4—O2385.56 (8)Mo2—O14—Mo3118.38 (18)
Mo5—Mo4—O2444.39 (8)Mo2—O14—Rb1108.75 (14)
O7—Mo4—O8106.22 (18)Mo3—O14—Rb1132.38 (16)
O7—Mo4—O1598.85 (16)Mo3—O15—Mo4117.05 (16)
O7—Mo4—O1699.30 (17)Mo4—O16—Mo5116.88 (18)
O7—Mo4—O2393.16 (15)Mo5—O17—Mo6116.42 (18)
O7—Mo4—O24160.57 (16)Mo1—O18—Mo6117.03 (16)
O8—Mo4—O1595.26 (16)Mo5—O19—Mo692.14 (12)
O8—Mo4—O16101.74 (16)Mo5—O19—Co1103.93 (15)
O8—Mo4—O23158.36 (15)Mo6—O19—Co1103.34 (14)
O8—Mo4—O2492.94 (15)Mo1—O20—Mo694.15 (11)
O15—Mo4—O16150.49 (14)Mo1—O20—Co1104.13 (14)
O15—Mo4—O2371.86 (13)Mo6—O20—Co1103.67 (14)
O15—Mo4—O2482.20 (12)Mo1—O21—Mo292.51 (12)
O16—Mo4—O2384.08 (14)Mo1—O21—Co1103.11 (14)
O16—Mo4—O2473.07 (14)Mo2—O21—Co1102.89 (14)
O23—Mo4—O2468.58 (11)Mo2—O22—Mo392.91 (12)
Mo4—Mo5—O988.49 (13)Mo2—O22—Co1103.68 (14)
Mo4—Mo5—O10127.50 (14)Mo3—O22—Co1104.17 (14)
Mo4—Mo5—O1631.42 (11)Mo3—O23—Mo493.89 (11)
Mo4—Mo5—O17125.79 (11)Mo3—O23—Co1104.17 (14)
Mo4—Mo5—O1984.06 (9)Mo4—O23—Co1103.81 (15)
Mo4—Mo5—O2443.98 (8)Mo4—O24—Mo591.63 (12)
O9—Mo5—O10106.67 (18)Mo4—O24—Co1103.59 (14)
O9—Mo5—O16100.31 (17)Mo5—O24—Co1103.84 (15)
O9—Mo5—O1797.62 (17)Rb1—O28—Co289.21 (11)
O9—Mo5—O19160.55 (16)Rb1—O28—C4128.6 (3)
O9—Mo5—O2494.26 (16)Co2—O28—C4126.0 (3)
O10—Mo5—O1696.11 (17)Rb1—O32—Co291.66 (12)
O10—Mo5—O17102.17 (17)Rb1—O35—Co289.61 (13)
O10—Mo5—O1992.05 (15)O25—C1—O26127.5 (5)
O10—Mo5—O24157.81 (15)O25—C1—C2116.4 (5)
O16—Mo5—O17149.46 (15)O26—C1—C2116.1 (5)
O16—Mo5—O1982.45 (14)N1—C2—C1110.0 (4)
O16—Mo5—O2472.42 (13)N1—C2—C3110.7 (4)
O17—Mo5—O1972.73 (13)C1—C2—C3110.3 (5)
O17—Mo5—O2481.81 (13)O27—C3—C2112.1 (5)
O19—Mo5—O2468.03 (12)O28—C4—O29126.5 (5)
O11—Mo6—O12105.70 (18)O28—C4—C5118.2 (4)
O11—Mo6—O17101.14 (16)O29—C4—C5115.3 (5)
O11—Mo6—O1895.36 (15)N2—C5—C4110.9 (4)
O11—Mo6—O1992.39 (15)N2—C5—C6110.8 (4)
O11—Mo6—O20158.22 (15)C4—C5—C6110.7 (5)
O12—Mo6—O1798.83 (16)O30—C6—C5110.6 (5)
O12—Mo6—O1899.02 (16)C3—O27—H4109.473
O12—Mo6—O19161.42 (15)C6—O30—H11109.466
O12—Mo6—O2094.11 (15)C2—N1—H5109.471
O17—Mo6—O18151.34 (14)C2—N1—H6109.455
O17—Mo6—O1973.00 (13)C2—N1—H7109.469
O17—Mo6—O2084.30 (13)H5—N1—H6109.477
O18—Mo6—O1983.13 (13)H5—N1—H7109.484
O18—Mo6—O2072.22 (13)H6—N1—H7109.471
O19—Mo6—O2068.83 (11)C5—N2—H13109.480
O3—Rb1—O8i167.01 (10)C5—N2—H12109.476
O3—Rb1—O11ii109.60 (10)C5—N2—H14109.470
O3—Rb1—O12ii65.85 (10)H13—N2—H12109.468
O3—Rb1—O1454.60 (10)H13—N2—H14109.467
O3—Rb1—O28117.88 (9)H12—N2—H14109.467
O3—Rb1—O31104.15 (9)N1—C2—H1108.575
O3—Rb1—O3295.04 (10)C1—C2—H1108.597
O3—Rb1—O3561.86 (10)C3—C2—H1108.589
O8i—Rb1—O11ii79.66 (10)O27—C3—H2109.176
O8i—Rb1—O12ii115.90 (10)O27—C3—H3109.174
O8i—Rb1—O14112.41 (11)C2—C3—H2109.171
O8i—Rb1—O2872.99 (10)C2—C3—H3109.182
O8i—Rb1—O3168.50 (10)H2—C3—H3107.896
O8i—Rb1—O3283.11 (11)N2—C5—H8108.109
O8i—Rb1—O35126.03 (11)C4—C5—H8108.111
O11ii—Rb1—O12ii54.54 (10)C6—C5—H8108.105
O11ii—Rb1—O14136.93 (11)O30—C6—H9109.516
O11ii—Rb1—O2873.03 (10)O30—C6—H10109.526
O11ii—Rb1—O3176.24 (10)C5—C6—H9109.517
O11ii—Rb1—O32137.42 (11)C5—C6—H10109.524
O11ii—Rb1—O35103.69 (10)H9—C6—H10108.087
O12ii—Rb1—O1484.44 (10)
O1—Mo1—O13—Mo2177.9 (2)O17—Mo5—O19—Co188.44 (16)
O1—Mo1—O18—Mo672.4 (2)O19—Mo5—O17—Mo621.03 (16)
O1—Mo1—O20—Mo683.55 (16)O17—Mo5—O24—Mo4179.52 (14)
O1—Mo1—O20—Co1171.23 (17)O17—Mo5—O24—Co175.09 (16)
O2—Mo1—O13—Mo269.2 (2)O24—Mo5—O17—Mo690.48 (19)
O2—Mo1—O18—Mo6179.83 (19)O19—Mo5—O24—Mo4104.90 (13)
O2—Mo1—O20—Mo672.5 (4)O19—Mo5—O24—Co10.47 (12)
O2—Mo1—O20—Co132.7 (5)O24—Mo5—O19—Mo6103.84 (13)
O2—Mo1—O21—Mo287.70 (15)O24—Mo5—O19—Co10.47 (12)
O2—Mo1—O21—Co1168.45 (17)O11—Mo6—O12—Rb1iii3.34 (17)
O13—Mo1—O18—Mo654.4 (4)O12—Mo6—O11—Rb1iii3.73 (19)
O18—Mo1—O13—Mo255.1 (4)O11—Mo6—O17—Mo568.0 (2)
O13—Mo1—O20—Mo6178.34 (13)O17—Mo6—O11—Rb1iii106.31 (15)
O13—Mo1—O20—Co173.12 (15)O11—Mo6—O18—Mo1178.75 (19)
O20—Mo1—O13—Mo288.30 (18)O18—Mo6—O11—Rb1iii97.23 (14)
O13—Mo1—O21—Mo214.17 (12)O11—Mo6—O19—Mo585.10 (15)
O13—Mo1—O21—Co189.68 (15)O11—Mo6—O19—Co1170.05 (17)
O21—Mo1—O13—Mo219.09 (15)O19—Mo6—O11—Rb1iii179.45 (13)
O18—Mo1—O20—Mo614.84 (12)O11—Mo6—O20—Mo172.3 (4)
O18—Mo1—O20—Co190.39 (15)O11—Mo6—O20—Co133.3 (5)
O20—Mo1—O18—Mo619.47 (15)O20—Mo6—O11—Rb1iii151.0 (3)
O18—Mo1—O21—Mo2177.21 (13)O12—Mo6—O17—Mo5176.0 (2)
O18—Mo1—O21—Co173.36 (15)O17—Mo6—O12—Rb1iii107.63 (13)
O21—Mo1—O18—Mo688.82 (17)O12—Mo6—O18—Mo171.9 (2)
O20—Mo1—O21—Mo2104.29 (13)O18—Mo6—O12—Rb1iii94.88 (13)
O20—Mo1—O21—Co10.44 (12)O12—Mo6—O20—Mo183.31 (15)
O21—Mo1—O20—Mo6104.78 (13)O12—Mo6—O20—Co1171.05 (17)
O21—Mo1—O20—Co10.45 (12)O20—Mo6—O12—Rb1iii167.51 (11)
O4—Mo2—O3—Rb1108.37 (16)O17—Mo6—O18—Mo156.0 (4)
O3—Mo2—O13—Mo168.6 (2)O18—Mo6—O17—Mo556.0 (4)
O13—Mo2—O3—Rb1151.16 (12)O17—Mo6—O19—Mo515.82 (13)
O3—Mo2—O14—Mo3180.0 (2)O17—Mo6—O19—Co189.03 (16)
O3—Mo2—O14—Rb17.03 (17)O19—Mo6—O17—Mo521.13 (16)
O14—Mo2—O3—Rb15.89 (15)O17—Mo6—O20—Mo1178.21 (14)
O3—Mo2—O21—Mo187.80 (15)O17—Mo6—O20—Co172.57 (15)
O3—Mo2—O21—Co1168.14 (17)O20—Mo6—O17—Mo590.70 (18)
O21—Mo2—O3—Rb178.84 (12)O18—Mo6—O19—Mo5179.78 (14)
O3—Mo2—O22—Mo374.7 (4)O18—Mo6—O19—Co174.93 (15)
O3—Mo2—O22—Co130.6 (5)O19—Mo6—O18—Mo189.48 (17)
O22—Mo2—O3—Rb150.2 (4)O18—Mo6—O20—Mo114.86 (12)
O4—Mo2—O13—Mo1176.89 (19)O18—Mo6—O20—Co190.78 (15)
O4—Mo2—O14—Mo372.1 (3)O20—Mo6—O18—Mo119.57 (15)
O4—Mo2—O14—Rb1114.93 (16)O19—Mo6—O20—Mo1104.26 (13)
O4—Mo2—O22—Mo384.66 (15)O19—Mo6—O20—Co11.38 (12)
O4—Mo2—O22—Co1170.00 (17)O20—Mo6—O19—Mo5106.23 (13)
O13—Mo2—O14—Mo352.1 (4)O20—Mo6—O19—Co11.38 (12)
O13—Mo2—O14—Rb1120.8 (3)O3—Rb1—O11ii—Mo6ii40.54 (18)
O14—Mo2—O13—Mo158.1 (4)O11ii—Rb1—O3—Mo2129.20 (14)
O13—Mo2—O21—Mo114.06 (12)O3—Rb1—O12ii—Mo6ii142.79 (18)
O13—Mo2—O21—Co190.00 (15)O12ii—Rb1—O3—Mo295.77 (16)
O21—Mo2—O13—Mo119.17 (15)O3—Rb1—O14—Mo24.67 (12)
O13—Mo2—O22—Mo3179.35 (13)O3—Rb1—O14—Mo3176.3 (3)
O13—Mo2—O22—Co174.01 (15)O14—Rb1—O3—Mo25.09 (13)
O22—Mo2—O13—Mo188.87 (18)O3—Rb1—O28—Co253.19 (14)
O14—Mo2—O21—Mo1176.28 (14)O3—Rb1—O28—C484.8 (3)
O14—Mo2—O21—Co172.22 (15)O28—Rb1—O3—Mo2150.14 (13)
O21—Mo2—O14—Mo389.09 (19)O31—Rb1—O3—Mo249.02 (16)
O21—Mo2—O14—Rb183.85 (14)O3—Rb1—O32—Co290.18 (13)
O14—Mo2—O22—Mo314.44 (12)O32—Rb1—O3—Mo286.11 (15)
O14—Mo2—O22—Co190.90 (16)O3—Rb1—O35—Co2156.67 (16)
O22—Mo2—O14—Mo319.78 (17)O35—Rb1—O3—Mo2135.39 (18)
O22—Mo2—O14—Rb1153.17 (17)O8i—Rb1—O11ii—Mo6ii130.02 (17)
O21—Mo2—O22—Mo3105.70 (13)O11ii—Rb1—O8i—Mo4i105.3 (5)
O21—Mo2—O22—Co10.35 (12)O8i—Rb1—O12ii—Mo6ii51.42 (18)
O22—Mo2—O21—Mo1103.71 (13)O12ii—Rb1—O8i—Mo4i63.4 (5)
O22—Mo2—O21—Co10.35 (12)O8i—Rb1—O14—Mo2175.29 (13)
O5—Mo3—O14—Mo2178.2 (2)O8i—Rb1—O14—Mo33.7 (3)
O5—Mo3—O14—Rb110.9 (3)O14—Rb1—O8i—Mo4i31.4 (5)
O5—Mo3—O15—Mo470.6 (2)O8i—Rb1—O28—Co2119.11 (13)
O5—Mo3—O22—Mo275.1 (5)O8i—Rb1—O28—C4102.9 (3)
O5—Mo3—O22—Co129.8 (5)O28—Rb1—O8i—Mo4i179.4 (5)
O5—Mo3—O23—Mo483.85 (15)O31—Rb1—O8i—Mo4i26.2 (4)
O5—Mo3—O23—Co1170.86 (17)O8i—Rb1—O32—Co2102.75 (13)
O6—Mo3—O14—Mo269.7 (3)O32—Rb1—O8i—Mo4i113.8 (5)
O6—Mo3—O14—Rb1119.3 (3)O8i—Rb1—O35—Co211.12 (18)
O6—Mo3—O15—Mo4178.83 (19)O35—Rb1—O8i—Mo4i155.2 (4)
O6—Mo3—O22—Mo286.02 (15)O11ii—Rb1—O12ii—Mo6ii2.37 (12)
O6—Mo3—O22—Co1169.08 (17)O12ii—Rb1—O11ii—Mo6ii2.44 (13)
O6—Mo3—O23—Mo477.2 (4)O11ii—Rb1—O14—Mo276.3 (2)
O6—Mo3—O23—Co128.1 (5)O11ii—Rb1—O14—Mo395.3 (3)
O14—Mo3—O15—Mo454.2 (4)O14—Rb1—O11ii—Mo6ii18.2 (3)
O15—Mo3—O14—Mo256.4 (4)O11ii—Rb1—O28—Co2156.80 (13)
O15—Mo3—O14—Rb1114.5 (3)O11ii—Rb1—O28—C418.9 (3)
O14—Mo3—O22—Mo214.62 (13)O28—Rb1—O11ii—Mo6ii154.77 (17)
O14—Mo3—O22—Co190.28 (16)O31—Rb1—O11ii—Mo6ii59.83 (15)
O22—Mo3—O14—Mo219.67 (17)O11ii—Rb1—O32—Co236.2 (2)
O22—Mo3—O14—Rb1151.3 (3)O32—Rb1—O11ii—Mo6ii162.24 (13)
O14—Mo3—O23—Mo4179.36 (14)O11ii—Rb1—O35—Co298.18 (13)
O14—Mo3—O23—Co174.06 (16)O35—Rb1—O11ii—Mo6ii105.17 (16)
O23—Mo3—O14—Mo288.66 (19)O12ii—Rb1—O14—Mo259.53 (15)
O23—Mo3—O14—Rb182.3 (2)O12ii—Rb1—O14—Mo3112.1 (3)
O15—Mo3—O22—Mo2177.20 (14)O14—Rb1—O12ii—Mo6ii163.66 (16)
O15—Mo3—O22—Co172.30 (15)O12ii—Rb1—O28—Co2130.50 (11)
O22—Mo3—O15—Mo489.09 (17)O12ii—Rb1—O28—C47.4 (3)
O15—Mo3—O23—Mo415.57 (12)O28—Rb1—O12ii—Mo6ii33.72 (19)
O15—Mo3—O23—Co189.73 (16)O31—Rb1—O12ii—Mo6ii92.19 (16)
O23—Mo3—O15—Mo420.29 (15)O12ii—Rb1—O35—Co2154.91 (11)
O22—Mo3—O23—Mo4105.96 (13)O35—Rb1—O12ii—Mo6ii96.50 (15)
O22—Mo3—O23—Co10.66 (12)O14—Rb1—O28—Co213.7 (3)
O23—Mo3—O22—Mo2104.23 (13)O14—Rb1—O28—C4151.6 (2)
O23—Mo3—O22—Co10.67 (13)O28—Rb1—O14—Mo290.3 (3)
O7—Mo4—Mo5—O9108.32 (17)O28—Rb1—O14—Mo398.1 (3)
O7—Mo4—Mo5—O101.64 (18)O31—Rb1—O14—Mo2119.27 (16)
O7—Mo4—Mo5—O164.43 (17)O31—Rb1—O14—Mo352.3 (2)
O7—Mo4—Mo5—O17153.37 (17)O14—Rb1—O32—Co2144.03 (13)
O7—Mo4—Mo5—O1989.66 (17)O32—Rb1—O14—Mo2104.00 (16)
O7—Mo4—Mo5—O24153.96 (18)O32—Rb1—O14—Mo384.4 (3)
Mo5—Mo4—O8—Rb1v94.4 (5)O14—Rb1—O35—Co2117.37 (12)
O8—Mo4—Mo5—O92.23 (12)O35—Rb1—O14—Mo247.92 (16)
O8—Mo4—Mo5—O10112.20 (12)O35—Rb1—O14—Mo3140.5 (2)
O8—Mo4—Mo5—O16114.98 (12)O31—Rb1—O28—Co2153.09 (10)
O8—Mo4—Mo5—O1796.07 (12)O31—Rb1—O28—C469.0 (3)
O8—Mo4—Mo5—O19159.78 (12)O28—Rb1—O32—Co228.34 (11)
O8—Mo4—Mo5—O2495.48 (12)O32—Rb1—O28—Co228.78 (11)
Mo5—Mo4—O15—Mo390.33 (17)O32—Rb1—O28—C4166.7 (3)
O15—Mo4—Mo5—O997.86 (12)O28—Rb1—O35—Co238.75 (11)
O15—Mo4—Mo5—O10152.17 (12)O35—Rb1—O28—Co237.80 (11)
O15—Mo4—Mo5—O16149.39 (12)O35—Rb1—O28—C4100.1 (3)
O15—Mo4—Mo5—O170.44 (12)O31—Rb1—O32—Co2155.87 (10)
O15—Mo4—Mo5—O1964.15 (12)O32—Rb1—O35—Co239.72 (12)
O15—Mo4—Mo5—O240.15 (12)O35—Rb1—O32—Co238.08 (11)
Mo5—Mo4—O16—Mo50.000 (13)O19—Co1—O20—Mo196.40 (14)
O16—Mo4—Mo5—O9112.8 (2)O19—Co1—O20—Mo61.54 (14)
O16—Mo4—Mo5—O102.8 (2)O20—Co1—O19—Mo597.16 (14)
O16—Mo4—Mo5—O160.0 (2)O20—Co1—O19—Mo61.53 (14)
O16—Mo4—Mo5—O17148.9 (2)O19—Co1—O21—Mo184.05 (14)
O16—Mo4—Mo5—O1985.2 (2)O19—Co1—O21—Mo2179.76 (14)
O16—Mo4—Mo5—O24149.5 (2)O21—Co1—O19—Mo5179.00 (14)
Mo5—Mo4—O23—Mo3146.22 (9)O21—Co1—O19—Mo685.36 (14)
Mo5—Mo4—O23—Co140.60 (12)O19—Co1—O23—Mo3179.18 (14)
O23—Mo4—Mo5—O9161.34 (8)O19—Co1—O23—Mo481.48 (15)
O23—Mo4—Mo5—O1088.70 (9)O23—Co1—O19—Mo582.65 (15)
O23—Mo4—Mo5—O1685.91 (8)O23—Co1—O19—Mo6178.29 (14)
O23—Mo4—Mo5—O1763.03 (8)O19—Co1—O24—Mo495.67 (15)
O23—Mo4—Mo5—O190.68 (8)O19—Co1—O24—Mo50.53 (14)
O23—Mo4—Mo5—O2463.62 (8)O24—Co1—O19—Mo50.53 (14)
Mo5—Mo4—O24—Mo50.0O24—Co1—O19—Mo695.11 (15)
Mo5—Mo4—O24—Co1104.66 (16)O20—Co1—O21—Mo10.49 (13)
O24—Mo4—Mo5—O997.71 (12)O20—Co1—O21—Mo296.20 (14)
O24—Mo4—Mo5—O10152.32 (12)O21—Co1—O20—Mo10.50 (14)
O24—Mo4—Mo5—O16149.54 (12)O21—Co1—O20—Mo697.44 (14)
O24—Mo4—Mo5—O170.59 (12)O20—Co1—O22—Mo284.29 (14)
O24—Mo4—Mo5—O1964.30 (12)O20—Co1—O22—Mo3179.08 (14)
O24—Mo4—Mo5—O240.00 (12)O22—Co1—O20—Mo183.68 (14)
O7—Mo4—O8—Rb1v133.0 (5)O22—Co1—O20—Mo6178.39 (14)
O7—Mo4—O15—Mo370.0 (2)O20—Co1—O24—Mo4179.13 (14)
O7—Mo4—O16—Mo5176.6 (2)O20—Co1—O24—Mo583.98 (14)
O7—Mo4—O23—Mo382.94 (16)O24—Co1—O20—Mo1179.91 (14)
O7—Mo4—O23—Co1171.43 (17)O24—Co1—O20—Mo681.97 (14)
O8—Mo4—O15—Mo3177.30 (19)O21—Co1—O22—Mo20.39 (13)
O15—Mo4—O8—Rb1v32.2 (5)O21—Co1—O22—Mo397.02 (14)
O8—Mo4—O16—Mo567.8 (3)O22—Co1—O21—Mo195.31 (14)
O16—Mo4—O8—Rb1v123.6 (5)O22—Co1—O21—Mo20.39 (13)
O8—Mo4—O23—Mo371.0 (4)O21—Co1—O23—Mo384.80 (15)
O8—Mo4—O23—Co134.7 (5)O21—Co1—O23—Mo4177.50 (14)
O23—Mo4—O8—Rb1v19.8 (8)O23—Co1—O21—Mo1178.48 (14)
O8—Mo4—O24—Mo585.21 (15)O23—Co1—O21—Mo282.78 (14)
O8—Mo4—O24—Co1170.13 (17)O22—Co1—O23—Mo30.74 (14)
O24—Mo4—O8—Rb1v50.2 (5)O22—Co1—O23—Mo498.44 (15)
O15—Mo4—O16—Mo556.1 (4)O23—Co1—O22—Mo295.89 (15)
O16—Mo4—O15—Mo357.4 (4)O23—Co1—O22—Mo30.74 (14)
O15—Mo4—O23—Mo315.34 (12)O22—Co1—O24—Mo484.96 (15)
O15—Mo4—O23—Co190.28 (16)O22—Co1—O24—Mo5179.89 (14)
O23—Mo4—O15—Mo320.49 (15)O24—Co1—O22—Mo2179.14 (14)
O15—Mo4—O24—Mo5179.88 (14)O24—Co1—O22—Mo382.51 (15)
O15—Mo4—O24—Co175.22 (15)O23—Co1—O24—Mo41.89 (14)
O24—Mo4—O15—Mo390.43 (17)O23—Co1—O24—Mo597.04 (15)
O16—Mo4—O23—Mo3178.02 (14)O24—Co1—O23—Mo395.80 (15)
O16—Mo4—O23—Co172.40 (16)O24—Co1—O23—Mo41.90 (14)
O23—Mo4—O16—Mo591.14 (19)O28—Co2—O32—Rb137.56 (13)
O16—Mo4—O24—Mo516.17 (13)O32—Co2—O28—Rb135.90 (12)
O16—Mo4—O24—Co188.49 (17)O32—Co2—O28—C4175.6 (3)
O24—Mo4—O16—Mo521.76 (17)O33—Co2—O28—Rb1122.99 (13)
O23—Mo4—O24—Mo5106.37 (13)O33—Co2—O28—C497.3 (3)
O23—Mo4—O24—Co11.71 (13)O34—Co2—O28—Rb1140.73 (12)
O24—Mo4—O23—Mo3103.91 (13)O34—Co2—O28—C41.0 (3)
O24—Mo4—O23—Co11.71 (13)O28—Co2—O35—Rb148.56 (12)
Mo4—Mo5—O16—Mo40.000 (14)O35—Co2—O28—Rb148.91 (13)
Mo4—Mo5—O17—Mo690.06 (18)O35—Co2—O28—C490.8 (3)
Mo4—Mo5—O19—Mo6146.27 (9)O33—Co2—O32—Rb1121.10 (14)
Mo4—Mo5—O19—Co141.96 (12)O32—Co2—O35—Rb146.77 (13)
Mo4—Mo5—O24—Mo40.0O35—Co2—O32—Rb149.60 (13)
Mo4—Mo5—O24—Co1104.43 (16)O36—Co2—O32—Rb1148.82 (15)
O9—Mo5—O16—Mo469.6 (3)O34—Co2—O35—Rb1140.10 (12)
O9—Mo5—O17—Mo6176.3 (2)O36—Co2—O35—Rb1136.14 (13)
O9—Mo5—O24—Mo483.39 (16)Rb1—O28—C4—O29110.3 (5)
O9—Mo5—O24—Co1172.19 (18)Rb1—O28—C4—C571.0 (5)
O10—Mo5—O16—Mo4177.8 (2)Co2—O28—C4—O2913.8 (7)
O10—Mo5—O17—Mo667.3 (3)Co2—O28—C4—C5164.9 (3)
O10—Mo5—O19—Mo686.24 (16)O25—C1—C2—N1165.7 (4)
O10—Mo5—O19—Co1169.46 (18)O25—C1—C2—C371.9 (6)
O10—Mo5—O24—Mo477.3 (5)O26—C1—C2—N115.5 (6)
O10—Mo5—O24—Co127.1 (5)O26—C1—C2—C3106.9 (5)
O16—Mo5—O17—Mo658.1 (4)N1—C2—C3—O2761.8 (6)
O17—Mo5—O16—Mo455.4 (4)C1—C2—C3—O2760.2 (6)
O16—Mo5—O19—Mo6177.87 (14)O28—C4—C5—N26.4 (6)
O16—Mo5—O19—Co173.57 (16)O28—C4—C5—C6129.8 (4)
O19—Mo5—O16—Mo490.95 (19)O29—C4—C5—N2172.4 (4)
O16—Mo5—O24—Mo416.10 (13)O29—C4—C5—C649.0 (6)
O16—Mo5—O24—Co188.33 (17)N2—C5—C6—O3066.2 (5)
O24—Mo5—O16—Mo421.67 (17)C4—C5—C6—O3057.3 (6)
O17—Mo5—O19—Mo615.87 (12)
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+2, y1/2, 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) x1/2, y+1/2, z; (x) x1, y, z; (xi) x+3/2, y+1, z+1/2; (xii) x1/2, y+3/2, z; (xiii) x+3/2, y+1, z1/2; (xiv) x+1, y1, z; (xv) x+1, y+1, z; (xvi) x1, y+1, z; (xvii) x, y1, z; (xviii) x1, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O27—H4···O410.842.242.859 (6)131
O27—H4···N10.842.622.940 (6)104
O30—H11···O400.842.562.708 (6)91
O30—H11···O42vii0.842.242.928 (6)139
N1—H5···O20.912.112.944 (6)151
N1—H6···O260.912.492.647 (6)89
N1—H6···O39vii0.912.143.041 (6)170
N1—H7···O17ii0.912.092.905 (6)149
N2—H13···O280.912.602.691 (6)86
N2—H13···O430.912.113.013 (7)170
N2—H12···O8i0.912.312.912 (6)123
N2—H12···O280.912.612.691 (6)85
N2—H14···O13xvii0.911.932.827 (6)167
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+2, y1/2, z+1/2; (vii) x+1/2, y+1/2, z; (xvii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O27—H4···O410.842.242.859 (6)131
O27—H4···N10.842.622.940 (6)104
O30—H11···O42i0.842.242.928 (6)139
N1—H5···O20.912.112.944 (6)151
N1—H6···O39i0.912.143.041 (6)170
N1—H7···O17ii0.912.092.905 (6)149
N2—H13···O430.912.113.013 (7)170
N2—H12···O8iii0.912.312.912 (6)123
N2—H14···O13iv0.911.932.827 (6)167
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+2, y1/2, z+1/2; (iii) x+1, y1/2, z+1/2; (iv) x, y1, z.
references
References top

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