The very stable title crystals, K
3[H
6CoMo
6O
24]·7H
2O, that include the well known
B-type Anderson-Evans heteropolyoxometalate, were obtained by recrystallization of powder K
3[H
6CoMo
6O
24]·
nH
2O at pH 3.5. The unit cell consists of two different crystallographically discrete [H
6CoMo
6O
24]
3- polyanions. The two anions have the Co atoms at inversion centers and have close to
m symmetry, with Co-O bond lengths in the range 1.898 (3)-1.912 (3) Å, Mo-O bond lengths in the ranges 1.700 (4)-1.726 (4), 1.895 (3)-1.960 (3) and 2.259 (3)-2.313 (3) Å.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (Co-O) = 0.003 Å
- H-atom completeness 1%
- R factor = 0.031
- wR factor = 0.082
- Data-to-parameter ratio = 17.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level A:
DIFF_012 Alert A _diffrn_reflns_av_R_equivalents is missing
R factor for symmetry-equivalent intensities.
The following tests will not be performed
RINTA
Alert Level B:
CHEMS_01 Alert B The sum formula contains elements in the wrong order.
H precedes Co
Sequence must be C, H, then alphabetical.
General Notes
FORMU_01 There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: H20 Co1 K3 Mo6 O31
Atom count from _chemical_formula_moiety:
FORMU_01 There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:H20 Co1 K3 Mo6 O31
Atom count from the _atom_site data: Co1 K3 Mo6 O31
CELLZ_01
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum H20 Co K3 Mo6 O31
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
H 80.00 0.00 80.00
Co 4.00 4.00 0.00
K 12.00 12.00 0.00
Mo 24.00 24.00 0.00
O 124.00 124.00 0.00
Difference between formula and atom_site contents detected.
WARNING: H atoms missing from atom site list. Is this intentional?
CHEMW_03
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 1268.03
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
K 39.10 3.00 117.29
Co 58.93 1.00 58.93
Mo 95.94 6.00 575.64
O 16.00 31.00 495.97
H 1.01 0.00 0.00
Calculated formula weight 1247.84
The ratio of given/expected molecular weight as calculated
from the _atom_site* data lies outside
the range 0.99 <> 1.01
1 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check
Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997).
Crystal data top
K3[H6CoMo6O24]·7H2O | F(000) = 2416 |
Mr = 1268.03 | Dx = 2.923 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71069 Å |
a = 22.461 (4) Å | Cell parameters from 30 reflections |
b = 11.295 (2) Å | θ = 9.6–10.4° |
c = 11.394 (2) Å | µ = 3.63 mm−1 |
β = 94.557 (9)° | T = 298 K |
V = 2881.5 (9) Å3 | Monoclinic, blue |
Z = 4 | 0.25 × 0.20 × 0.20 mm |
Data collection top
Stoe Stadi-4 diffractometer | 5649 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | θmax = 27.5°, θmin = 1.8° |
Graphite monochromator | h = −29→29 |
ω/2–θ scans | k = 0→14 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996) | l = 0→14 |
Tmin = 0.502, Tmax = 0.669 | 3 standard reflections every 60 min |
6611 measured reflections | intensity decay: 3.0% |
6611 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.031 | w = 1/[σ2(Fo2) + (0.0321P)2 + 11.8333P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.082 | (Δ/σ)max = 0.001 |
S = 1.11 | Δρmax = 0.98 e Å−3 |
6611 reflections | Δρmin = −0.69 e Å−3 |
374 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00144 (6) |
Primary atom site location: structure-invariant direct methods | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | −0.5000 | 0.5000 | 0.01235 (16) | |
Mo1 | 0.426417 (19) | −0.40348 (4) | 0.72168 (4) | 0.01845 (10) | |
Mo2 | 0.351662 (18) | −0.49988 (4) | 0.47835 (4) | 0.01910 (10) | |
Mo3 | 0.425424 (18) | −0.59309 (4) | 0.25543 (3) | 0.01767 (10) | |
Oc1 | 0.43780 (14) | −0.5532 (3) | 0.5906 (3) | 0.0160 (6) | |
Oc2 | 0.43637 (14) | −0.4450 (3) | 0.3922 (3) | 0.0150 (6) | |
Oc3 | 0.49917 (14) | −0.6341 (3) | 0.3979 (3) | 0.0144 (6) | |
Ob4 | 0.50015 (15) | −0.4698 (3) | 0.7958 (3) | 0.0204 (7) | |
Ob5 | 0.37508 (15) | −0.3693 (3) | 0.5829 (3) | 0.0222 (7) | |
Ob6 | 0.37492 (15) | −0.6283 (3) | 0.3763 (3) | 0.0216 (7) | |
Ot7 | 0.43138 (18) | −0.2641 (3) | 0.7814 (4) | 0.0339 (9) | |
Ot8 | 0.37882 (17) | −0.4806 (4) | 0.8027 (3) | 0.0324 (9) | |
Ot9 | 0.31165 (17) | −0.5847 (4) | 0.5670 (3) | 0.0332 (9) | |
Ot10 | 0.30139 (18) | −0.4266 (4) | 0.3847 (3) | 0.0340 (9) | |
Ot11 | 0.37926 (17) | −0.5121 (3) | 0.1596 (3) | 0.0286 (8) | |
Ot12 | 0.42780 (17) | −0.7311 (3) | 0.1932 (3) | 0.0289 (8) | |
Co2 | 0.0000 | −0.5000 | 0.5000 | 0.01222 (16) | |
Mo4 | 0.147416 (18) | −0.51008 (4) | 0.53218 (4) | 0.01812 (10) | |
Mo5 | 0.080823 (18) | −0.26527 (4) | 0.43018 (4) | 0.01786 (10) | |
Mo6 | −0.067656 (18) | −0.25942 (4) | 0.39516 (3) | 0.01728 (10) | |
Oc13 | 0.06176 (14) | −0.6020 (3) | 0.4570 (3) | 0.0157 (6) | |
Oc14 | 0.06339 (14) | −0.4054 (3) | 0.5715 (3) | 0.0157 (6) | |
Oc15 | 0.00459 (14) | −0.3942 (3) | 0.3705 (3) | 0.0152 (6) | |
Ob16 | 0.11984 (15) | −0.6136 (3) | 0.6533 (3) | 0.0216 (7) | |
Ob17 | 0.12996 (15) | −0.4005 (3) | 0.4040 (3) | 0.0215 (7) | |
Ob18 | 0.00664 (15) | −0.1996 (3) | 0.4757 (3) | 0.0200 (7) | |
Ot19 | 0.19104 (16) | −0.6064 (3) | 0.4606 (3) | 0.0279 (8) | |
Ot20 | 0.19376 (17) | −0.4267 (4) | 0.6250 (3) | 0.0305 (8) | |
Ot21 | 0.12725 (17) | −0.1838 (3) | 0.5238 (3) | 0.0307 (8) | |
Ot22 | 0.08389 (17) | −0.1990 (4) | 0.2948 (3) | 0.0300 (8) | |
Ot23 | −0.06261 (18) | −0.1934 (4) | 0.2609 (3) | 0.0318 (9) | |
Ot24 | −0.11327 (17) | −0.1707 (3) | 0.4698 (4) | 0.0318 (9) | |
K1 | 0.20759 (6) | −0.30373 (13) | 0.23275 (12) | 0.0394 (3) | |
K2 | 0.16341 (7) | −0.53286 (14) | −0.13338 (12) | 0.0448 (4) | |
K3 | 0.35375 (6) | −0.65458 (11) | −0.04259 (12) | 0.0342 (3) | |
Ow1 | 0.48401 (19) | −0.6430 (3) | −0.0362 (3) | 0.0325 (9) | |
Ow2 | 0.1958 (3) | −0.5533 (6) | 0.2205 (5) | 0.085 (2) | |
Ow3 | 0.2471 (2) | −0.6611 (5) | 0.0392 (6) | 0.0654 (16) | |
Ow4 | 0.30158 (18) | −0.3235 (4) | 0.0960 (4) | 0.0374 (10) | |
Ow5 | 0.0164 (3) | −0.5373 (4) | −0.1499 (4) | 0.0472 (12) | |
Ow6 | 0.2578 (2) | −0.3792 (4) | −0.1302 (4) | 0.0476 (11) | |
Ow7 | 0.2620 (2) | −0.6699 (5) | −0.2265 (5) | 0.0606 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0152 (4) | 0.0094 (4) | 0.0123 (4) | 0.0002 (3) | 0.0002 (3) | 0.0000 (3) |
Mo1 | 0.0211 (2) | 0.0177 (2) | 0.01682 (19) | 0.00208 (16) | 0.00272 (15) | −0.00319 (15) |
Mo2 | 0.01541 (19) | 0.0212 (2) | 0.0204 (2) | 0.00147 (16) | −0.00061 (15) | −0.00010 (16) |
Mo3 | 0.0205 (2) | 0.01611 (19) | 0.01582 (19) | 0.00001 (15) | −0.00194 (15) | −0.00307 (15) |
Oc1 | 0.0169 (15) | 0.0146 (15) | 0.0165 (15) | −0.0017 (12) | 0.0021 (12) | 0.0001 (12) |
Oc2 | 0.0173 (15) | 0.0122 (15) | 0.0152 (15) | −0.0001 (12) | −0.0011 (12) | −0.0004 (12) |
Oc3 | 0.0168 (15) | 0.0122 (14) | 0.0142 (15) | −0.0010 (12) | 0.0007 (12) | −0.0032 (12) |
Ob4 | 0.0250 (18) | 0.0227 (17) | 0.0135 (15) | −0.0003 (14) | 0.0023 (13) | 0.0035 (13) |
Ob5 | 0.0221 (17) | 0.0212 (17) | 0.0228 (17) | 0.0077 (14) | −0.0013 (13) | −0.0035 (14) |
Ob6 | 0.0234 (18) | 0.0195 (17) | 0.0218 (17) | −0.0046 (14) | 0.0011 (14) | −0.0038 (14) |
Ot7 | 0.038 (2) | 0.027 (2) | 0.036 (2) | 0.0058 (17) | 0.0008 (17) | −0.0135 (17) |
Ot8 | 0.027 (2) | 0.043 (2) | 0.029 (2) | 0.0000 (17) | 0.0112 (16) | 0.0021 (17) |
Ot9 | 0.0237 (19) | 0.047 (2) | 0.029 (2) | −0.0064 (18) | 0.0052 (15) | 0.0017 (18) |
Ot10 | 0.029 (2) | 0.039 (2) | 0.033 (2) | 0.0102 (18) | −0.0065 (16) | 0.0022 (18) |
Ot11 | 0.0263 (19) | 0.034 (2) | 0.0242 (18) | 0.0058 (16) | −0.0060 (15) | −0.0008 (16) |
Ot12 | 0.032 (2) | 0.0227 (19) | 0.032 (2) | −0.0023 (16) | 0.0023 (16) | −0.0089 (16) |
Co2 | 0.0133 (4) | 0.0126 (4) | 0.0106 (4) | 0.0006 (3) | 0.0002 (3) | −0.0001 (3) |
Mo4 | 0.01426 (19) | 0.0192 (2) | 0.0206 (2) | 0.00052 (15) | −0.00048 (15) | 0.00042 (16) |
Mo5 | 0.0179 (2) | 0.0170 (2) | 0.01882 (19) | −0.00162 (15) | 0.00190 (15) | 0.00324 (15) |
Mo6 | 0.0183 (2) | 0.01575 (19) | 0.01764 (19) | 0.00248 (15) | 0.00027 (15) | 0.00263 (15) |
Oc13 | 0.0158 (15) | 0.0161 (15) | 0.0150 (15) | 0.0028 (12) | 0.0009 (12) | 0.0003 (12) |
Oc14 | 0.0147 (15) | 0.0154 (15) | 0.0169 (15) | −0.0011 (12) | 0.0013 (12) | −0.0011 (12) |
Oc15 | 0.0170 (15) | 0.0165 (15) | 0.0121 (14) | −0.0004 (12) | 0.0006 (12) | 0.0035 (12) |
Ob16 | 0.0217 (17) | 0.0230 (17) | 0.0194 (16) | −0.0007 (14) | −0.0032 (13) | 0.0029 (14) |
Ob17 | 0.0187 (16) | 0.0242 (18) | 0.0222 (17) | 0.0023 (14) | 0.0064 (13) | 0.0020 (14) |
Ob18 | 0.0202 (17) | 0.0176 (16) | 0.0223 (17) | 0.0002 (13) | 0.0022 (13) | −0.0022 (13) |
Ot19 | 0.0157 (16) | 0.032 (2) | 0.036 (2) | 0.0064 (15) | 0.0045 (15) | −0.0018 (17) |
Ot20 | 0.0244 (19) | 0.030 (2) | 0.035 (2) | −0.0051 (16) | −0.0044 (16) | −0.0016 (17) |
Ot21 | 0.0258 (19) | 0.027 (2) | 0.038 (2) | −0.0036 (16) | −0.0010 (16) | −0.0035 (17) |
Ot22 | 0.034 (2) | 0.032 (2) | 0.0249 (19) | 0.0016 (17) | 0.0066 (16) | 0.0107 (16) |
Ot23 | 0.037 (2) | 0.033 (2) | 0.0246 (19) | −0.0035 (18) | −0.0027 (16) | 0.0128 (17) |
Ot24 | 0.028 (2) | 0.028 (2) | 0.039 (2) | 0.0085 (16) | 0.0033 (16) | −0.0072 (17) |
K1 | 0.0406 (7) | 0.0402 (7) | 0.0377 (7) | 0.0038 (6) | 0.0044 (6) | 0.0021 (6) |
K2 | 0.0540 (9) | 0.0514 (9) | 0.0282 (7) | −0.0170 (7) | −0.0007 (6) | 0.0035 (6) |
K3 | 0.0353 (7) | 0.0311 (6) | 0.0360 (7) | 0.0015 (5) | 0.0007 (5) | −0.0057 (5) |
Ow1 | 0.047 (2) | 0.0224 (19) | 0.028 (2) | −0.0020 (17) | 0.0025 (17) | −0.0005 (16) |
Ow2 | 0.129 (6) | 0.076 (4) | 0.053 (3) | −0.032 (4) | 0.033 (4) | −0.021 (3) |
Ow3 | 0.046 (3) | 0.066 (4) | 0.086 (4) | −0.007 (3) | 0.021 (3) | −0.007 (3) |
Ow4 | 0.031 (2) | 0.032 (2) | 0.048 (2) | −0.0045 (18) | −0.0050 (18) | 0.0089 (19) |
Ow5 | 0.091 (4) | 0.026 (2) | 0.025 (2) | 0.000 (2) | 0.008 (2) | −0.0004 (17) |
Ow6 | 0.046 (3) | 0.049 (3) | 0.047 (3) | −0.003 (2) | 0.001 (2) | −0.003 (2) |
Ow7 | 0.055 (3) | 0.076 (4) | 0.049 (3) | −0.003 (3) | −0.003 (2) | −0.002 (3) |
Geometric parameters (Å, º) top
Co1—Oc1i | 1.899 (3) | Mo5—K2v | 3.9393 (19) |
Co1—Oc1 | 1.899 (3) | Mo6—Ot24 | 1.707 (4) |
Co1—Oc3 | 1.909 (3) | Mo6—Ot23 | 1.713 (4) |
Co1—Oc3i | 1.909 (3) | Mo6—Ob16iv | 1.906 (3) |
Co1—Oc2 | 1.912 (3) | Mo6—Ob18 | 1.960 (3) |
Co1—Oc2i | 1.912 (3) | Mo6—Oc15 | 2.259 (3) |
Co1—Mo3 | 3.3068 (6) | Mo6—Oc13iv | 2.295 (3) |
Co1—Mo1 | 3.3111 (6) | Oc13—Mo6iv | 2.295 (3) |
Co1—Mo2 | 3.3213 (7) | Oc1—Ot12ii | 2.720 (5) |
Mo1—Ot8 | 1.706 (4) | Oc2—Ot7vi | 2.676 (5) |
Mo1—Ot7 | 1.715 (4) | Oc13—Ot23vii | 2.691 (5) |
Mo1—Ob5 | 1.921 (3) | Oc14—Ot22v | 2.809 (5) |
Mo1—Ob4 | 1.948 (3) | Ob16—Mo6iv | 1.906 (3) |
Mo1—Oc3i | 2.278 (3) | Ob16—K2iii | 2.705 (4) |
Mo1—Oc1 | 2.283 (3) | Ot20—K1v | 2.884 (4) |
Mo1—Mo2 | 3.3094 (7) | Ot20—K2iii | 3.128 (4) |
Mo2—Ot9 | 1.700 (4) | Ot21—K1v | 2.874 (4) |
Mo2—Ot10 | 1.705 (4) | Ot21—K2v | 3.177 (4) |
Mo2—Ob5 | 1.943 (3) | K1—Ot22 | 3.151 (4) |
Mo2—Ob6 | 1.956 (3) | K1—Ow4 | 2.731 (5) |
Mo2—Oc2 | 2.294 (3) | K1—Ow6v | 2.775 (5) |
Mo2—Oc1 | 2.313 (3) | K1—Ow2 | 2.834 (7) |
Mo2—Mo3 | 3.3125 (7) | K1—Ot10 | 2.964 (4) |
Mo2—K3ii | 3.9106 (15) | K1—Ob17 | 2.930 (4) |
Mo3—Ot11 | 1.710 (4) | K1—Ot21vi | 2.874 (4) |
Mo3—Ot12 | 1.715 (4) | K1—Ot20vi | 2.884 (4) |
Mo3—Ob6 | 1.895 (3) | K1—K2v | 4.243 (2) |
Mo3—Ob4i | 1.948 (3) | K1—K2 | 4.942 (2) |
Mo3—Oc3 | 2.273 (3) | K2—Ob16viii | 2.705 (4) |
Mo3—Oc2 | 2.286 (3) | K2—Ow6 | 2.739 (5) |
Mo3—Mo1i | 3.3175 (8) | K2—Ot24vii | 2.739 (4) |
Mo3—K3 | 3.7063 (15) | K2—Ow7 | 2.966 (6) |
Mo3—K3ii | 4.0743 (14) | K2—Ow3 | 2.986 (7) |
Oc3—Mo1i | 2.278 (3) | K2—Ot20viii | 3.128 (4) |
Ob4—Mo3i | 1.948 (3) | K2—Ot21vi | 3.177 (4) |
Ob6—K3ii | 2.676 (4) | K2—Ot22vi | 3.239 (4) |
Ot8—K3iii | 2.728 (4) | K2—Ow5 | 3.293 (6) |
Ot9—K3ii | 3.363 (5) | K2—Mo4viii | 3.8077 (16) |
Co2—Oc13iv | 1.898 (3) | K2—Mo5vi | 3.9393 (19) |
Co2—Oc13 | 1.898 (3) | K2—K1vi | 4.243 (2) |
Co2—Oc15 | 1.908 (3) | K3—Ow3 | 2.639 (5) |
Co2—Oc15iv | 1.908 (3) | K3—Ob6ix | 2.676 (4) |
Co2—Oc14iv | 1.910 (3) | K3—Ot8viii | 2.728 (4) |
Co2—Oc14 | 1.910 (3) | K3—Ot11 | 2.832 (4) |
Co2—Mo6 | 3.2912 (6) | K3—Ot12 | 3.165 (4) |
Co2—Mo4 | 3.3042 (7) | K3—Ow7 | 2.826 (5) |
Co2—Mo5 | 3.3447 (6) | K3—Ow1 | 2.924 (4) |
Mo4—Ot20 | 1.707 (4) | K3—Ot9ix | 3.363 (5) |
Mo4—Ot19 | 1.713 (4) | K3—Mo2ix | 3.9106 (15) |
Mo4—Ob17 | 1.930 (3) | K3—Mo3ix | 4.0743 (14) |
Mo4—Ob16 | 1.947 (3) | Ow6—K1vi | 2.775 (5) |
Mo4—Oc13 | 2.292 (3) | Ow1—Oc3ix | 2.657 (5) |
Mo4—Oc14 | 2.301 (3) | Ow1—Ob4viii | 2.781 (5) |
Mo4—Mo6iv | 3.3028 (7) | Ow2—Ow3 | 2.731 (8) |
Mo4—Mo5 | 3.3102 (7) | Ow2—Ot24vii | 3.042 (8) |
Mo4—K2iii | 3.8077 (15) | Ow3—Ot24vii | 3.002 (6) |
Mo5—Ot21 | 1.702 (4) | Ow3—Ot19ix | 3.017 (7) |
Mo5—Ot22 | 1.720 (4) | Ow3—Ow7 | 3.074 (8) |
Mo5—Ob17 | 1.922 (3) | Ow4—Ob5vi | 2.744 (5) |
Mo5—Ob18 | 1.932 (3) | Ow4—Ow6 | 2.757 (6) |
Mo5—Oc15 | 2.309 (3) | Ow5—Oc15x | 2.637 (5) |
Mo5—Oc14 | 2.313 (3) | Ow5—Ob18vii | 2.781 (5) |
Mo5—Mo6 | 3.3278 (8) | Ow6—Ot20viii | 3.083 (6) |
Mo5—K1 | 3.7913 (16) | Ow7—Ot9viii | 2.850 (7) |
| | | |
Oc1i—Co1—Oc1 | 180.00 (12) | Ot24—Mo6—Ob18 | 94.98 (17) |
Oc1i—Co1—Oc3 | 83.77 (13) | Ot23—Mo6—Ob18 | 98.85 (16) |
Oc1—Co1—Oc3 | 96.23 (13) | Ob16iv—Mo6—Ob18 | 151.19 (14) |
Oc1i—Co1—Oc3i | 96.23 (13) | Ot24—Mo6—Oc15 | 157.34 (16) |
Oc1—Co1—Oc3i | 83.77 (13) | Ot23—Mo6—Oc15 | 94.77 (16) |
Oc3—Co1—Oc3i | 180.0 (2) | Ob16iv—Mo6—Oc15 | 83.57 (13) |
Oc1i—Co1—Oc2 | 95.32 (13) | Ob18—Mo6—Oc15 | 72.38 (13) |
Oc1—Co1—Oc2 | 84.68 (13) | Ot24—Mo6—Oc13iv | 92.08 (16) |
Oc3—Co1—Oc2 | 84.01 (13) | Ot23—Mo6—Oc13iv | 161.40 (16) |
Oc3i—Co1—Oc2 | 95.99 (13) | Ob16iv—Mo6—Oc13iv | 72.42 (13) |
Oc1i—Co1—Oc2i | 84.68 (13) | Ob18—Mo6—Oc13iv | 83.91 (13) |
Oc1—Co1—Oc2i | 95.32 (13) | Oc15—Mo6—Oc13iv | 68.38 (11) |
Oc3—Co1—Oc2i | 95.99 (13) | Co2—Oc13—Mo4 | 103.73 (14) |
Oc3i—Co1—Oc2i | 84.01 (13) | Co2—Oc13—Mo6iv | 103.02 (13) |
Oc2—Co1—Oc2i | 180.00 (13) | Mo4—Oc13—Mo6iv | 92.11 (11) |
Ot8—Mo1—Ot7 | 106.1 (2) | Co2—Oc14—Mo4 | 102.98 (13) |
Ot8—Mo1—Ob5 | 100.79 (17) | Co2—Oc14—Mo5 | 104.35 (14) |
Ot7—Mo1—Ob5 | 99.08 (17) | Mo4—Oc14—Mo5 | 91.69 (11) |
Ot8—Mo1—Ob4 | 96.71 (17) | Co2—Oc15—Mo6 | 104.04 (13) |
Ot7—Mo1—Ob4 | 98.90 (17) | Co2—Oc15—Mo5 | 104.58 (13) |
Ob5—Mo1—Ob4 | 150.26 (14) | Mo6—Oc15—Mo5 | 93.52 (12) |
Ot8—Mo1—Oc3i | 159.99 (16) | Mo6iv—Ob16—Mo4 | 118.00 (17) |
Ot7—Mo1—Oc3i | 92.21 (16) | Mo6iv—Ob16—K2iii | 133.17 (16) |
Ob5—Mo1—Oc3i | 83.76 (13) | Mo4—Ob16—K2iii | 108.77 (15) |
Ob4—Mo1—Oc3i | 72.06 (12) | Mo5—Ob17—Mo4 | 118.47 (17) |
Ot8—Mo1—Oc1 | 94.78 (16) | Mo5—Ob17—K1 | 100.72 (14) |
Ot7—Mo1—Oc1 | 158.74 (17) | Mo4—Ob17—K1 | 130.33 (15) |
Ob5—Mo1—Oc1 | 72.65 (13) | Mo5—Ob18—Mo6 | 117.54 (17) |
Ob4—Mo1—Oc1 | 82.13 (13) | Mo4—Ot20—K1v | 143.3 (2) |
Oc3i—Mo1—Oc1 | 67.76 (11) | Mo4—Ot20—K2iii | 99.73 (16) |
Ot9—Mo2—Ot10 | 106.9 (2) | K1v—Ot20—K2iii | 89.70 (11) |
Ot9—Mo2—Ob5 | 101.19 (18) | Mo5—Ot21—K1v | 143.7 (2) |
Ot10—Mo2—Ob5 | 98.56 (18) | Mo5—Ot21—K2v | 103.55 (17) |
Ot9—Mo2—Ob6 | 96.52 (18) | K1v—Ot21—K2v | 109.44 (12) |
Ot10—Mo2—Ob6 | 100.55 (17) | Mo5—Ot22—K1 | 97.86 (16) |
Ob5—Mo2—Ob6 | 148.85 (14) | Mo5—Ot22—K2v | 100.71 (17) |
Ot9—Mo2—Oc2 | 154.40 (16) | K1—Ot22—K2v | 83.21 (10) |
Ot10—Mo2—Oc2 | 97.58 (16) | Mo6—Ot24—K2xi | 165.5 (2) |
Ob5—Mo2—Oc2 | 82.18 (13) | Ow4—K1—Ow6v | 94.81 (14) |
Ob6—Mo2—Oc2 | 71.12 (13) | Ow4—K1—Ow2 | 87.93 (16) |
Ot9—Mo2—Oc1 | 89.05 (16) | Ow6v—K1—Ow2 | 143.21 (18) |
Ot10—Mo2—Oc1 | 162.91 (17) | Ow4—K1—Ot21vi | 89.22 (13) |
Ob5—Mo2—Oc1 | 71.61 (13) | Ow6v—K1—Ot21vi | 134.66 (14) |
Ob6—Mo2—Oc1 | 83.37 (13) | Ow2—K1—Ot21vi | 81.97 (17) |
Oc2—Mo2—Oc1 | 67.73 (11) | Ow4—K1—Ot20vi | 83.85 (12) |
Ot11—Mo3—Ot12 | 105.05 (18) | Ow6v—K1—Ot20vi | 65.98 (13) |
Ot11—Mo3—Ob6 | 102.05 (17) | Ow2—K1—Ot20vi | 150.47 (17) |
Ot12—Mo3—Ob6 | 98.61 (17) | Ot21vi—K1—Ot20vi | 69.64 (11) |
Ot11—Mo3—Ob4i | 96.03 (17) | Ow4—K1—Ob17 | 151.33 (12) |
Ot12—Mo3—Ob4i | 98.74 (16) | Ow6v—K1—Ob17 | 98.05 (13) |
Ob6—Mo3—Ob4i | 150.67 (14) | Ow2—K1—Ob17 | 66.62 (14) |
Ot11—Mo3—Oc3 | 159.31 (15) | Ot21vi—K1—Ob17 | 99.53 (11) |
Ot12—Mo3—Oc3 | 93.73 (15) | Ot20vi—K1—Ob17 | 124.80 (11) |
Ob6—Mo3—Oc3 | 83.25 (13) | Ow4—K1—Ot10 | 75.47 (12) |
Ob4i—Mo3—Oc3 | 72.18 (12) | Ow6v—K1—Ot10 | 77.38 (13) |
Ot11—Mo3—Oc2 | 94.05 (15) | Ow2—K1—Ot10 | 67.82 (18) |
Ot12—Mo3—Oc2 | 160.33 (15) | Ot21vi—K1—Ot10 | 146.24 (13) |
Ob6—Mo3—Oc2 | 72.32 (13) | Ot20vi—K1—Ot10 | 135.97 (12) |
Ob4i—Mo3—Oc2 | 83.63 (13) | Ob17—K1—Ot10 | 82.48 (11) |
Oc3—Mo3—Oc2 | 68.25 (11) | Ow4—K1—Ot22 | 153.40 (12) |
Ot11—Mo3—Co1 | 127.49 (13) | Ow6v—K1—Ot22 | 85.45 (13) |
Ot12—Mo3—Co1 | 127.39 (13) | Ow2—K1—Ot22 | 107.67 (17) |
Ob6—Mo3—Co1 | 75.32 (10) | Ot21vi—K1—Ot22 | 72.39 (11) |
Ob4i—Mo3—Co1 | 75.35 (10) | Ot20vi—K1—Ot22 | 71.93 (11) |
Oc3—Mo3—Co1 | 34.05 (8) | Ob17—K1—Ot22 | 53.75 (10) |
Oc2—Mo3—Co1 | 34.20 (8) | Ot10—K1—Ot22 | 130.03 (11) |
Co1—Oc1—Mo1 | 104.29 (14) | Ob16viii—K2—Ow6 | 116.74 (13) |
Co1—Oc1—Mo2 | 103.66 (13) | Ob16viii—K2—Ot24vii | 106.31 (12) |
Mo1—Oc1—Mo2 | 92.11 (12) | Ow6—K2—Ot24vii | 135.34 (14) |
Co1—Oc2—Mo3 | 103.58 (13) | Ob16viii—K2—Ow7 | 74.31 (13) |
Co1—Oc2—Mo2 | 103.92 (13) | Ow6—K2—Ow7 | 74.70 (16) |
Mo3—Oc2—Mo2 | 92.65 (11) | Ot24vii—K2—Ow7 | 107.80 (15) |
Co1—Oc3—Mo3 | 104.16 (13) | Ob16viii—K2—Ow3 | 126.31 (15) |
Co1—Oc3—Mo1i | 104.14 (13) | Ow6—K2—Ow3 | 81.51 (15) |
Mo3—Oc3—Mo1i | 93.59 (11) | Ot24vii—K2—Ow3 | 63.08 (13) |
Mo1—Ob4—Mo3i | 116.77 (16) | Ow7—K2—Ow3 | 62.20 (15) |
Mo1—Ob5—Mo2 | 117.88 (17) | Ob16viii—K2—Ot20viii | 55.03 (10) |
Mo3—Ob6—Mo2 | 118.66 (17) | Ow6—K2—Ot20viii | 62.99 (12) |
Mo3—Ob6—K3ii | 125.20 (16) | Ot24vii—K2—Ot20viii | 161.31 (12) |
Mo2—Ob6—K3ii | 114.30 (15) | Ow7—K2—Ot20viii | 70.36 (14) |
Mo1—Ot8—K3iii | 152.6 (2) | Ow3—K2—Ot20viii | 126.58 (14) |
Mo2—Ot9—K3ii | 95.48 (16) | Ob16viii—K2—Ot21vi | 132.52 (12) |
Mo2—Ot10—K1 | 176.1 (2) | Ow6—K2—Ot21vi | 74.73 (13) |
Mo3—Ot11—K3 | 106.76 (17) | Ot24vii—K2—Ot21vi | 85.24 (12) |
Mo3—Ot12—K3 | 94.09 (16) | Ow7—K2—Ot21vi | 146.67 (14) |
Oc13iv—Co2—Oc13 | 180.0 | Ow3—K2—Ot21vi | 100.27 (14) |
Oc13iv—Co2—Oc15 | 84.54 (13) | Ot20viii—K2—Ot21vi | 106.53 (11) |
Oc13—Co2—Oc15 | 95.46 (13) | Ob16viii—K2—Ot22vi | 83.84 (11) |
Oc13iv—Co2—Oc15iv | 95.46 (13) | Ow6—K2—Ot22vi | 84.36 (13) |
Oc13—Co2—Oc15iv | 84.54 (13) | Ot24vii—K2—Ot22vi | 112.55 (12) |
Oc15—Co2—Oc15iv | 180.00 (19) | Ow7—K2—Ot22vi | 138.08 (14) |
Oc13iv—Co2—Oc14iv | 85.09 (13) | Ow3—K2—Ot22vi | 149.85 (14) |
Oc13—Co2—Oc14iv | 94.91 (13) | Ot20viii—K2—Ot22vi | 67.79 (10) |
Oc15—Co2—Oc14iv | 96.02 (13) | Ot21vi—K2—Ot22vi | 50.11 (10) |
Oc15iv—Co2—Oc14iv | 83.98 (13) | Ob16viii—K2—Ow5 | 69.76 (11) |
Oc13iv—Co2—Oc14 | 94.91 (13) | Ow6—K2—Ow5 | 141.47 (14) |
Oc13—Co2—Oc14 | 85.09 (13) | Ot24vii—K2—Ow5 | 64.25 (11) |
Oc15—Co2—Oc14 | 83.98 (13) | Ow7—K2—Ow5 | 138.19 (14) |
Oc15iv—Co2—Oc14 | 96.02 (13) | Ow3—K2—Ow5 | 127.33 (13) |
Oc14iv—Co2—Oc14 | 180.0 (2) | Ot20viii—K2—Ow5 | 104.08 (11) |
Ot20—Mo4—Ot19 | 107.54 (18) | Ot21vi—K2—Ow5 | 75.15 (11) |
Ot20—Mo4—Ob17 | 101.09 (17) | Ot22vi—K2—Ow5 | 57.81 (11) |
Ot19—Mo4—Ob17 | 97.82 (16) | Ow3—K3—Ob6ix | 106.70 (15) |
Ot20—Mo4—Ob16 | 96.02 (17) | Ow3—K3—Ot8viii | 119.22 (17) |
Ot19—Mo4—Ob16 | 100.51 (17) | Ob6ix—K3—Ot8viii | 112.68 (12) |
Ob17—Mo4—Ob16 | 149.79 (14) | Ow3—K3—Ow7 | 68.36 (18) |
Ot20—Mo4—Oc13 | 159.10 (16) | Ob6ix—K3—Ow7 | 80.05 (15) |
Ot19—Mo4—Oc13 | 91.67 (15) | Ot8viii—K3—Ow7 | 74.98 (15) |
Ob17—Mo4—Oc13 | 83.90 (13) | Ow3—K3—Ot11 | 81.91 (16) |
Ob16—Mo4—Oc13 | 71.81 (12) | Ob6ix—K3—Ot11 | 140.51 (11) |
Ot20—Mo4—Oc14 | 93.74 (16) | Ot8viii—K3—Ot11 | 94.44 (12) |
Ot19—Mo4—Oc14 | 158.09 (15) | Ow7—K3—Ot11 | 136.61 (15) |
Ob17—Mo4—Oc14 | 72.39 (13) | Ow3—K3—Ow1 | 157.95 (17) |
Ob16—Mo4—Oc14 | 81.88 (13) | Ob6ix—K3—Ow1 | 81.06 (11) |
Oc13—Mo4—Oc14 | 68.19 (11) | Ot8viii—K3—Ow1 | 74.11 (12) |
Ot21—Mo5—Ot22 | 105.13 (19) | Ow7—K3—Ow1 | 133.69 (14) |
Ot21—Mo5—Ob17 | 101.31 (17) | Ot11—K3—Ow1 | 79.46 (11) |
Ot22—Mo5—Ob17 | 98.18 (17) | Ow3—K3—Ot12 | 97.06 (16) |
Ot21—Mo5—Ob18 | 97.05 (17) | Ob6ix—K3—Ot12 | 86.96 (10) |
Ot22—Mo5—Ob18 | 99.82 (16) | Ot8viii—K3—Ot12 | 128.56 (12) |
Ob17—Mo5—Ob18 | 149.87 (14) | Ow7—K3—Ot12 | 156.33 (15) |
Ot21—Mo5—Oc15 | 158.26 (16) | Ot11—K3—Ot12 | 53.56 (10) |
Ot22—Mo5—Oc15 | 95.28 (15) | Ow1—K3—Ot12 | 62.22 (11) |
Ob17—Mo5—Oc15 | 82.78 (13) | Ow3—K3—Ot9ix | 63.54 (15) |
Ob18—Mo5—Oc15 | 71.70 (13) | Ob6ix—K3—Ot9ix | 52.32 (10) |
Ot21—Mo5—Oc14 | 93.58 (16) | Ot8viii—K3—Ot9ix | 161.62 (12) |
Ot22—Mo5—Oc14 | 160.48 (16) | Ow7—K3—Ot9ix | 90.67 (14) |
Ob17—Mo5—Oc14 | 72.25 (13) | Ot11—K3—Ot9ix | 103.91 (11) |
Ob18—Mo5—Oc14 | 83.01 (13) | Ow1—K3—Ot9ix | 109.89 (10) |
Oc15—Mo5—Oc14 | 67.09 (11) | Ot12—K3—Ot9ix | 65.81 (10) |
Ot24—Mo6—Ot23 | 105.9 (2) | K3—Ow3—K2 | 107.2 (2) |
Ot24—Mo6—Ob16iv | 101.90 (17) | K2—Ow6—K1vi | 100.64 (16) |
Ot23—Mo6—Ob16iv | 98.72 (17) | K3—Ow7—K2 | 102.94 (17) |
Symmetry codes: (i) −x+1, −y−1, −z+1; (ii) x, −y−3/2, z+1/2; (iii) x, y, z+1; (iv) −x, −y−1, −z+1; (v) x, −y−1/2, z+1/2; (vi) x, −y−1/2, z−1/2; (vii) −x, y−1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y−3/2, z−1/2; (x) −x, −y−1, −z; (xi) −x, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å) top
D—H···A | D···A |
Oc1···Ot12ii | 2.720 (5) |
Oc2···Ot7vi | 2.676 (5) |
Oc13···Ot23vii | 2.691 (5) |
Oc14···Ot22v | 2.809 (5) |
Ow1···Oc3ix | 2.657 (5) |
Ow1···Ob4viii | 2.781 (5) |
Ow1···Ob4i | 3.016 (5) |
Ow2···Ow3 | 2.731 (8) |
Ow2···Ot19 | 2.811 (7) |
Ow2···Ot24vii | 3.042 (8) |
Ow3···Ot24vii | 3.002 (6) |
Ow3···Ot19ix | 3.017 (7) |
Ow3···Ow7 | 3.074 (8) |
Ow4···Ob5vi | 2.744 (5) |
Ow4···Ot11 | 2.810 (5) |
Ow4···Ow6 | 2.757 (6) |
Ow5···Oc15x | 2.636 (5) |
Ow5···Ob18vii | 2.779 (5) |
Ow5···Ob18vi | 3.047 (5) |
Ow6···Ot20viii | 3.082 (6) |
Ow6···Ot8viii | 3.100 (6) |
Ow7···Ot9viii | 2.849 (7) |
Symmetry codes: (i) −x+1, −y−1, −z+1; (ii) x, −y−3/2, z+1/2; (v) x, −y−1/2, z+1/2; (vi) x, −y−1/2, z−1/2; (vii) −x, y−1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y−3/2, z−1/2; (x) −x, −y−1, −z. |