The title compound, tetrapotassium bis(glycine)hexacosaoxooctamolybdenum(VI) hexahydrate, K4[Mo8O26(NH3CH2COO)2]·6H2O, consists of a molecular network of centrosymmetric [Mo8O26(NH3CH2COO)2]4- anions, K+ cations and water molecules, which interact by an extensive hydrogen-bonding network. The [Mo8O26(NH3CH2COO)2]4- anion is constructed from MoO6 and MoO5(OOCCH2NH3) octahedral units, where the latter has O atoms of terminal and bridging oxo groups as well as those of glycine ligands.
Supporting information
CCDC reference: 245115
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.012 Å
- H-atom completeness 46%
- R factor = 0.041
- wR factor = 0.112
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
PLAT031_ALERT_4_C Refined Extinction Parameter within Range ...... 2.75 Sigma
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.73 Ratio
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.69 Ratio
Alert level G
FORMU01_ALERT_1_G 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: C4 H22 K4 Mo8 N2 O36
Atom count from _chemical_formula_moiety:C4 H22 K4 Mo6 N2 O36
FORMU01_ALERT_2_G 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:C4 H22 K4 Mo8 N2 O36
Atom count from the _atom_site data: C4 H10 K4 Mo8 N2 O36
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 1
From the CIF: _chemical_formula_sum C4 H22 K4 Mo8 N2 O36
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 4.00 4.00 0.00
H 22.00 10.00 12.00
K 4.00 4.00 0.00
Mo 8.00 8.00 0.00
N 2.00 2.00 0.00
O 36.00 36.00 0.00
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
Tetrapotassium bis(glycine)hexacosaoxooctamolybdenum(VI) hexahydrate
top
Crystal data top
K4[Mo8O26(C2H5NO2)2]·6H2O | V = 878.66 (5) Å3 |
Mr = 1598.16 | Z = 1 |
Triclinic, P1 | F(000) = 760 |
Hall symbol: -P 1 | Dx = 3.020 Mg m−3 |
a = 8.1065 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.8767 (2) Å | µ = 3.35 mm−1 |
c = 12.4936 (5) Å | T = 293 K |
α = 98.638 (2)° | Block, yellow |
β = 99.295 (2)° | 0.22 × 0.14 × 0.10 mm |
γ = 113.606 (1)° | |
Data collection top
Bruker SMART CCD diffractometer | 3026 independent reflections |
Radiation source: fine-focus sealed tube | 2740 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
ω scans | θmax = 25.0°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.523, Tmax = 0.715 | k = −11→11 |
4462 measured reflections | l = −13→14 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.041 | H-atom parameters constrained |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0581P)2 + 9.0351P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.010 |
3026 reflections | Δρmax = 0.80 e Å−3 |
245 parameters | Δρmin = −1.03 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0011 (4) |
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 | |
K1 | 0.6497 (3) | 0.3573 (2) | 0.01667 (16) | 0.0303 (4) | |
K2 | −0.1223 (3) | 0.3490 (2) | 0.35463 (18) | 0.0361 (5) | |
Mo1 | 0.20526 (8) | 0.35655 (7) | 0.16523 (5) | 0.01592 (19) | |
Mo2 | −0.14873 (8) | −0.11665 (7) | −0.32640 (5) | 0.01577 (19) | |
Mo3 | 0.15764 (8) | 0.00546 (7) | −0.07868 (5) | 0.01348 (19) | |
Mo4 | −0.03268 (9) | 0.23935 (7) | −0.09631 (5) | 0.01641 (19) | |
O1 | −0.3136 (7) | −0.2506 (6) | −0.2553 (4) | 0.0183 (11) | |
O2 | 0.1167 (7) | 0.1517 (6) | 0.0226 (4) | 0.0176 (10) | |
O3 | 0.0327 (7) | −0.1672 (5) | −0.2013 (4) | 0.0168 (10) | |
O4 | 0.0207 (7) | 0.3649 (6) | 0.0507 (4) | 0.0194 (11) | |
O5 | 0.4017 (7) | 0.4528 (6) | 0.1232 (5) | 0.0261 (12) | |
O6 | 0.2024 (8) | 0.4834 (6) | 0.2743 (4) | 0.0243 (12) | |
O7 | −0.0515 (7) | 0.0504 (6) | −0.1757 (4) | 0.0173 (10) | |
O8 | 0.0915 (7) | 0.0462 (6) | −0.3509 (4) | 0.0246 (12) | |
O9 | −0.1512 (7) | −0.2525 (6) | −0.4312 (4) | 0.0243 (12) | |
O10 | −0.2952 (8) | −0.0495 (6) | −0.3878 (4) | 0.0252 (12) | |
O11 | 0.3455 (7) | 0.1198 (6) | −0.1186 (4) | 0.0245 (12) | |
O12 | 0.2486 (7) | −0.0725 (6) | 0.0176 (4) | 0.0195 (11) | |
O13 | 0.1450 (8) | 0.3586 (6) | −0.1427 (5) | 0.0289 (13) | |
O14 | −0.2239 (8) | 0.2513 (6) | −0.1666 (4) | 0.0270 (12) | |
O15 | 0.2714 (8) | −0.0686 (7) | −0.3951 (6) | 0.0357 (14) | |
O16 | 0.5777 (9) | 0.1929 (8) | 0.1751 (5) | 0.0382 (15) | |
O17 | −0.3741 (9) | 0.4132 (8) | 0.4563 (6) | 0.0432 (16) | |
O18 | 0.0106 (11) | 0.6684 (8) | 0.3841 (6) | 0.0479 (18) | |
C1 | 0.2441 (10) | 0.0439 (9) | −0.3676 (6) | 0.0225 (16) | |
C2 | 0.3973 (11) | 0.2020 (9) | −0.3536 (7) | 0.0247 (17) | |
H2A | 0.3507 | 0.2568 | −0.3989 | 0.030* | |
H2B | 0.4335 | 0.2572 | −0.2762 | 0.030* | |
N1 | 0.5636 (10) | 0.1956 (8) | −0.3874 (6) | 0.0312 (16) | |
H1A | 0.6506 | 0.2897 | −0.3784 | 0.047* | |
H1B | 0.5311 | 0.1464 | −0.4587 | 0.047* | |
H1C | 0.6079 | 0.1470 | −0.3451 | 0.047* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0274 (9) | 0.0269 (9) | 0.0304 (10) | 0.0084 (8) | 0.0046 (8) | 0.0021 (8) |
K2 | 0.0374 (11) | 0.0322 (10) | 0.0448 (12) | 0.0193 (9) | 0.0163 (9) | 0.0075 (9) |
Mo1 | 0.0179 (3) | 0.0137 (3) | 0.0131 (3) | 0.0049 (3) | 0.0021 (2) | 0.0020 (2) |
Mo2 | 0.0170 (3) | 0.0167 (3) | 0.0114 (3) | 0.0064 (3) | 0.0010 (2) | 0.0023 (2) |
Mo3 | 0.0132 (3) | 0.0142 (3) | 0.0115 (3) | 0.0053 (2) | 0.0025 (2) | 0.0013 (2) |
Mo4 | 0.0203 (3) | 0.0145 (3) | 0.0132 (3) | 0.0076 (3) | 0.0015 (2) | 0.0028 (2) |
O1 | 0.018 (3) | 0.020 (3) | 0.016 (3) | 0.007 (2) | 0.002 (2) | 0.006 (2) |
O2 | 0.019 (3) | 0.015 (2) | 0.015 (2) | 0.006 (2) | 0.001 (2) | 0.001 (2) |
O3 | 0.014 (2) | 0.016 (2) | 0.016 (2) | 0.004 (2) | 0.001 (2) | −0.002 (2) |
O4 | 0.026 (3) | 0.020 (3) | 0.012 (2) | 0.014 (2) | 0.000 (2) | −0.002 (2) |
O5 | 0.019 (3) | 0.028 (3) | 0.029 (3) | 0.005 (2) | 0.007 (2) | 0.013 (2) |
O6 | 0.034 (3) | 0.018 (3) | 0.020 (3) | 0.013 (2) | 0.005 (2) | −0.002 (2) |
O7 | 0.016 (2) | 0.020 (3) | 0.016 (2) | 0.009 (2) | 0.003 (2) | 0.003 (2) |
O8 | 0.025 (3) | 0.029 (3) | 0.020 (3) | 0.011 (2) | 0.008 (2) | 0.007 (2) |
O9 | 0.024 (3) | 0.027 (3) | 0.016 (3) | 0.008 (2) | 0.001 (2) | −0.001 (2) |
O10 | 0.025 (3) | 0.029 (3) | 0.021 (3) | 0.014 (2) | 0.001 (2) | 0.005 (2) |
O11 | 0.015 (3) | 0.032 (3) | 0.023 (3) | 0.006 (2) | 0.003 (2) | 0.009 (2) |
O12 | 0.022 (3) | 0.020 (3) | 0.018 (3) | 0.011 (2) | 0.005 (2) | 0.004 (2) |
O13 | 0.029 (3) | 0.022 (3) | 0.026 (3) | 0.003 (2) | 0.011 (2) | 0.001 (2) |
O14 | 0.033 (3) | 0.030 (3) | 0.021 (3) | 0.020 (3) | 0.001 (2) | 0.004 (2) |
O15 | 0.029 (3) | 0.024 (3) | 0.053 (4) | 0.009 (3) | 0.011 (3) | 0.011 (3) |
O16 | 0.033 (3) | 0.051 (4) | 0.039 (4) | 0.024 (3) | 0.014 (3) | 0.014 (3) |
O17 | 0.039 (4) | 0.042 (4) | 0.045 (4) | 0.018 (3) | 0.009 (3) | 0.003 (3) |
O18 | 0.072 (5) | 0.050 (4) | 0.039 (4) | 0.040 (4) | 0.025 (4) | 0.014 (3) |
C1 | 0.019 (4) | 0.023 (4) | 0.013 (4) | 0.000 (3) | −0.003 (3) | 0.002 (3) |
C2 | 0.022 (4) | 0.029 (4) | 0.023 (4) | 0.009 (3) | 0.007 (3) | 0.009 (3) |
N1 | 0.027 (4) | 0.029 (4) | 0.032 (4) | 0.008 (3) | 0.002 (3) | 0.007 (3) |
Geometric parameters (Å, º) top
K1—O13i | 2.685 (6) | Mo3—O11 | 1.697 (5) |
K1—O11 | 2.696 (6) | Mo3—O12 | 1.741 (5) |
K1—O16 | 2.733 (7) | Mo3—O3 | 1.900 (5) |
K1—O5i | 2.850 (6) | Mo3—O2 | 1.941 (5) |
K1—O14ii | 2.879 (6) | Mo3—O7 | 2.154 (5) |
K1—O4ii | 2.937 (5) | Mo3—O2iv | 2.431 (5) |
K1—O5 | 2.951 (6) | Mo4—O13 | 1.706 (5) |
K1—O12iii | 3.223 (5) | Mo4—O14 | 1.711 (5) |
K1—O4i | 3.305 (6) | Mo4—O7 | 1.912 (5) |
K1—Mo4ii | 3.614 (2) | Mo4—O4 | 1.931 (5) |
K1—Mo4i | 3.7952 (19) | Mo4—O2 | 2.251 (5) |
K1—Mo1i | 3.829 (2) | Mo4—O12iv | 2.341 (5) |
K2—O15iv | 2.706 (6) | Mo4—K1v | 3.614 (2) |
K2—O16v | 2.742 (7) | Mo4—K1i | 3.7952 (19) |
K2—O17 | 2.795 (7) | O1—Mo1iv | 1.975 (5) |
K2—O3iv | 2.808 (5) | O2—Mo3iv | 2.431 (5) |
K2—O9iv | 2.832 (6) | O3—Mo1iv | 2.251 (5) |
K2—O18 | 2.837 (7) | O3—K2iv | 2.808 (5) |
K2—O6 | 2.855 (6) | O4—K1v | 2.937 (5) |
K2—O18vi | 3.293 (7) | O4—K1i | 3.305 (6) |
K2—Mo2iv | 3.777 (2) | O5—K1i | 2.850 (6) |
K2—Mo1 | 3.819 (2) | O8—C1 | 1.296 (10) |
K2—K2vi | 3.963 (4) | O9—K2iv | 2.832 (6) |
K2—K1v | 4.354 (3) | O12—Mo4iv | 2.341 (5) |
Mo1—O5 | 1.709 (5) | O12—K1iii | 3.223 (5) |
Mo1—O6 | 1.717 (5) | O13—K1i | 2.685 (6) |
Mo1—O4 | 1.933 (5) | O14—K1v | 2.879 (6) |
Mo1—O1iv | 1.975 (5) | O15—C1 | 1.228 (10) |
Mo1—O3iv | 2.251 (5) | O15—K2iv | 2.706 (6) |
Mo1—O2 | 2.264 (5) | O16—K2ii | 2.742 (7) |
Mo1—K1i | 3.829 (2) | O18—K2vi | 3.293 (7) |
Mo2—O10 | 1.711 (5) | C1—C2 | 1.518 (11) |
Mo2—O9 | 1.720 (5) | C2—N1 | 1.497 (10) |
Mo2—O1 | 1.910 (5) | C2—H2A | 0.9700 |
Mo2—O8 | 2.075 (5) | C2—H2B | 0.9700 |
Mo2—O7 | 2.106 (5) | N1—H1A | 0.8900 |
Mo2—O3 | 2.222 (5) | N1—H1B | 0.8900 |
Mo2—K2iv | 3.777 (2) | N1—H1C | 0.8900 |
| | | |
O13i—K1—O11 | 157.01 (19) | O1iv—Mo1—O3iv | 73.11 (19) |
O13i—K1—O16 | 101.9 (2) | O5—Mo1—O2 | 91.1 (2) |
O11—K1—O16 | 84.81 (18) | O6—Mo1—O2 | 162.4 (2) |
O13i—K1—O5i | 75.59 (17) | O4—Mo1—O2 | 73.28 (19) |
O11—K1—O5i | 89.31 (17) | O1iv—Mo1—O2 | 85.67 (19) |
O16—K1—O5i | 155.85 (18) | O3iv—Mo1—O2 | 74.06 (18) |
O13i—K1—O14ii | 118.80 (18) | O5—Mo1—K2 | 150.1 (2) |
O11—K1—O14ii | 74.90 (17) | O6—Mo1—K2 | 44.35 (19) |
O16—K1—O14ii | 118.86 (18) | O4—Mo1—K2 | 85.82 (16) |
O5i—K1—O14ii | 81.78 (17) | O1iv—Mo1—K2 | 91.13 (15) |
O13i—K1—O4ii | 79.92 (17) | O3iv—Mo1—K2 | 46.81 (13) |
O11—K1—O4ii | 122.48 (16) | O2—Mo1—K2 | 118.48 (13) |
O16—K1—O4ii | 89.31 (17) | O5—Mo1—K1i | 43.71 (19) |
O5i—K1—O4ii | 113.40 (16) | O6—Mo1—K1i | 94.95 (18) |
O14ii—K1—O4ii | 58.69 (15) | O4—Mo1—K1i | 59.66 (16) |
O13i—K1—O5 | 72.40 (17) | O1iv—Mo1—K1i | 138.98 (15) |
O11—K1—O5 | 88.35 (17) | O3iv—Mo1—K1i | 145.89 (13) |
O16—K1—O5 | 75.62 (17) | O2—Mo1—K1i | 94.01 (13) |
O5i—K1—O5 | 80.83 (17) | K2—Mo1—K1i | 123.75 (4) |
O14ii—K1—O5 | 155.92 (17) | O10—Mo2—O9 | 105.2 (3) |
O4ii—K1—O5 | 144.63 (15) | O10—Mo2—O1 | 98.5 (2) |
O13i—K1—O12iii | 129.43 (17) | O9—Mo2—O1 | 97.9 (2) |
O11—K1—O12iii | 73.45 (15) | O10—Mo2—O8 | 95.9 (2) |
O16—K1—O12iii | 66.27 (16) | O9—Mo2—O8 | 91.1 (2) |
O5i—K1—O12iii | 133.94 (16) | O1—Mo2—O8 | 160.3 (2) |
O14ii—K1—O12iii | 52.77 (14) | O10—Mo2—O7 | 94.0 (2) |
O4ii—K1—O12iii | 52.33 (14) | O9—Mo2—O7 | 159.0 (2) |
O5—K1—O12iii | 138.74 (15) | O1—Mo2—O7 | 87.4 (2) |
O13i—K1—O4i | 53.79 (15) | O8—Mo2—O7 | 78.3 (2) |
O11—K1—O4i | 128.85 (15) | O10—Mo2—O3 | 163.0 (2) |
O16—K1—O4i | 143.42 (17) | O9—Mo2—O3 | 91.3 (2) |
O5i—K1—O4i | 53.46 (14) | O1—Mo2—O3 | 74.97 (19) |
O14ii—K1—O4i | 66.95 (15) | O8—Mo2—O3 | 87.5 (2) |
O4ii—K1—O4i | 61.98 (16) | O7—Mo2—O3 | 70.37 (18) |
O5—K1—O4i | 114.11 (14) | O10—Mo2—K2iv | 149.36 (19) |
O12iii—K1—O4i | 105.97 (13) | O9—Mo2—K2iv | 44.90 (18) |
O13i—K1—Mo4ii | 106.33 (14) | O1—Mo2—K2iv | 93.45 (15) |
O11—K1—Mo4ii | 93.63 (13) | O8—Mo2—K2iv | 80.67 (15) |
O16—K1—Mo4ii | 101.43 (14) | O7—Mo2—K2iv | 114.78 (13) |
O5i—K1—Mo4ii | 102.31 (13) | O3—Mo2—K2iv | 47.60 (13) |
O14ii—K1—Mo4ii | 27.70 (11) | O11—Mo3—O12 | 103.9 (2) |
O4ii—K1—Mo4ii | 32.22 (9) | O11—Mo3—O3 | 104.0 (2) |
O5—K1—Mo4ii | 176.30 (12) | O12—Mo3—O3 | 100.0 (2) |
O12iii—K1—Mo4ii | 39.52 (9) | O11—Mo3—O2 | 101.9 (2) |
O4i—K1—Mo4ii | 66.91 (9) | O12—Mo3—O2 | 99.6 (2) |
O13i—K1—Mo4i | 23.42 (12) | O3—Mo3—O2 | 142.4 (2) |
O11—K1—Mo4i | 154.38 (13) | O11—Mo3—O7 | 99.1 (2) |
O16—K1—Mo4i | 120.09 (15) | O12—Mo3—O7 | 156.9 (2) |
O5i—K1—Mo4i | 65.53 (12) | O3—Mo3—O7 | 75.7 (2) |
O14ii—K1—Mo4i | 95.74 (12) | O2—Mo3—O7 | 73.7 (2) |
O4ii—K1—Mo4i | 67.83 (10) | O11—Mo3—O2iv | 177.8 (2) |
O5—K1—Mo4i | 92.09 (11) | O12—Mo3—O2iv | 78.0 (2) |
O12iii—K1—Mo4i | 120.09 (11) | O3—Mo3—O2iv | 76.67 (19) |
O4i—K1—Mo4i | 30.58 (8) | O2—Mo3—O2iv | 76.5 (2) |
Mo4ii—K1—Mo4i | 87.49 (4) | O7—Mo3—O2iv | 78.99 (18) |
O13i—K1—Mo1i | 68.87 (13) | O11—Mo3—K1 | 33.62 (18) |
O11—K1—Mo1i | 103.79 (12) | O12—Mo3—K1 | 85.86 (17) |
O16—K1—Mo1i | 170.73 (15) | O3—Mo3—K1 | 135.84 (15) |
O5i—K1—Mo1i | 24.48 (11) | O2—Mo3—K1 | 77.26 (15) |
O14ii—K1—Mo1i | 67.56 (12) | O7—Mo3—K1 | 113.26 (13) |
O4ii—K1—Mo1i | 88.92 (11) | O2iv—Mo3—K1 | 146.27 (12) |
O5—K1—Mo1i | 100.85 (11) | O13—Mo4—O14 | 103.8 (3) |
O12iii—K1—Mo1i | 119.14 (10) | O13—Mo4—O7 | 98.2 (2) |
O4i—K1—Mo1i | 30.32 (9) | O14—Mo4—O7 | 103.5 (2) |
Mo4ii—K1—Mo1i | 81.73 (4) | O13—Mo4—O4 | 98.8 (2) |
Mo4i—K1—Mo1i | 51.00 (3) | O14—Mo4—O4 | 102.9 (2) |
O15iv—K2—O16v | 77.8 (2) | O7—Mo4—O4 | 144.0 (2) |
O15iv—K2—O17 | 87.8 (2) | O13—Mo4—O2 | 101.7 (2) |
O16v—K2—O17 | 84.3 (2) | O14—Mo4—O2 | 154.5 (2) |
O15iv—K2—O3iv | 74.99 (18) | O7—Mo4—O2 | 72.03 (19) |
O16v—K2—O3iv | 71.36 (17) | O4—Mo4—O2 | 73.62 (19) |
O17—K2—O3iv | 152.52 (19) | O13—Mo4—O12iv | 173.0 (2) |
O15iv—K2—O9iv | 67.63 (18) | O14—Mo4—O12iv | 83.1 (2) |
O16v—K2—O9iv | 125.86 (18) | O7—Mo4—O12iv | 80.57 (19) |
O17—K2—O9iv | 132.1 (2) | O4—Mo4—O12iv | 78.8 (2) |
O3iv—K2—O9iv | 60.47 (15) | O2—Mo4—O12iv | 71.36 (18) |
O15iv—K2—O18 | 160.4 (2) | O13—Mo4—K1v | 122.7 (2) |
O16v—K2—O18 | 111.8 (2) | O14—Mo4—K1v | 51.48 (19) |
O17—K2—O18 | 76.6 (2) | O7—Mo4—K1v | 134.48 (15) |
O3iv—K2—O18 | 123.80 (19) | O4—Mo4—K1v | 54.20 (15) |
O9iv—K2—O18 | 114.7 (2) | O2—Mo4—K1v | 113.33 (13) |
O15iv—K2—O6 | 127.75 (18) | O12iv—Mo4—K1v | 61.19 (13) |
O16v—K2—O6 | 108.65 (18) | O13—Mo4—K1i | 38.72 (19) |
O17—K2—O6 | 143.52 (19) | O14—Mo4—K1i | 105.12 (19) |
O3iv—K2—O6 | 60.05 (15) | O7—Mo4—K1i | 132.87 (15) |
O9iv—K2—O6 | 67.78 (16) | O4—Mo4—K1i | 60.54 (16) |
O18—K2—O6 | 66.92 (18) | O2—Mo4—K1i | 95.15 (13) |
O15iv—K2—O18vi | 64.14 (19) | O12iv—Mo4—K1i | 139.29 (13) |
O16v—K2—O18vi | 136.6 (2) | K1v—Mo4—K1i | 92.51 (4) |
O17—K2—O18vi | 74.7 (2) | Mo2—O1—Mo1iv | 115.0 (2) |
O3iv—K2—O18vi | 114.67 (17) | Mo3—O2—Mo4 | 102.1 (2) |
O9iv—K2—O18vi | 57.76 (17) | Mo3—O2—Mo1 | 154.6 (3) |
O18—K2—O18vi | 99.81 (18) | Mo4—O2—Mo1 | 93.29 (18) |
O6—K2—O18vi | 110.78 (19) | Mo3—O2—Mo3iv | 103.5 (2) |
O15iv—K2—Mo2iv | 63.07 (14) | Mo4—O2—Mo3iv | 95.33 (18) |
O16v—K2—Mo2iv | 101.65 (14) | Mo1—O2—Mo3iv | 94.99 (18) |
O17—K2—Mo2iv | 147.63 (16) | Mo3—O3—Mo2 | 108.3 (2) |
O3iv—K2—Mo2iv | 35.75 (10) | Mo3—O3—Mo1iv | 112.8 (2) |
O9iv—K2—Mo2iv | 25.38 (11) | Mo2—O3—Mo1iv | 94.25 (18) |
O18—K2—Mo2iv | 127.77 (17) | Mo3—O3—K2iv | 138.4 (2) |
O6—K2—Mo2iv | 64.90 (11) | Mo2—O3—K2iv | 96.65 (17) |
O18vi—K2—Mo2iv | 79.70 (13) | Mo1iv—O3—K2iv | 97.43 (17) |
O15iv—K2—Mo1 | 108.62 (15) | Mo4—O4—Mo1 | 116.3 (2) |
O16v—K2—Mo1 | 90.23 (14) | Mo4—O4—K1v | 93.57 (18) |
O17—K2—Mo1 | 161.22 (16) | Mo1—O4—K1v | 140.0 (2) |
O3iv—K2—Mo1 | 35.76 (10) | Mo4—O4—K1i | 88.89 (18) |
O9iv—K2—Mo1 | 64.89 (12) | Mo1—O4—K1i | 90.02 (18) |
O18—K2—Mo1 | 88.89 (15) | K1v—O4—K1i | 118.02 (16) |
O6—K2—Mo1 | 24.86 (10) | Mo1—O5—K1i | 111.8 (3) |
O18vi—K2—Mo1 | 120.21 (14) | Mo1—O5—K1 | 133.4 (3) |
Mo2iv—K2—Mo1 | 51.12 (3) | K1i—O5—K1 | 99.17 (17) |
O15iv—K2—K2vi | 108.19 (17) | Mo1—O6—K2 | 110.8 (2) |
O16v—K2—K2vi | 150.40 (16) | Mo4—O7—Mo2 | 148.4 (3) |
O17—K2—K2vi | 67.34 (15) | Mo4—O7—Mo3 | 106.7 (2) |
O3iv—K2—K2vi | 138.16 (13) | Mo2—O7—Mo3 | 103.5 (2) |
O9iv—K2—K2vi | 81.69 (12) | C1—O8—Mo2 | 133.0 (5) |
O18—K2—K2vi | 54.95 (15) | Mo2—O9—K2iv | 109.7 (2) |
O6—K2—K2vi | 90.81 (12) | Mo3—O11—K1 | 126.0 (3) |
O18vi—K2—K2vi | 44.86 (13) | Mo3—O12—Mo4iv | 115.3 (2) |
Mo2iv—K2—K2vi | 106.84 (8) | Mo3—O12—K1iii | 131.2 (2) |
Mo1—K2—K2vi | 113.84 (8) | Mo4iv—O12—K1iii | 79.29 (14) |
O15iv—K2—K1v | 112.85 (15) | Mo4—O13—K1i | 117.9 (3) |
O16v—K2—K1v | 37.26 (14) | Mo4—O14—K1v | 100.8 (2) |
O17—K2—K1v | 97.69 (16) | C1—O15—K2iv | 131.5 (5) |
O3iv—K2—K1v | 70.63 (11) | K1—O16—K2ii | 105.3 (2) |
O9iv—K2—K1v | 129.31 (12) | K2—O18—K2vi | 80.19 (18) |
O18—K2—K1v | 81.37 (15) | O15—C1—O8 | 127.2 (7) |
O6—K2—K1v | 77.33 (12) | O15—C1—C2 | 120.1 (7) |
O18vi—K2—K1v | 171.66 (15) | O8—C1—C2 | 112.7 (7) |
Mo2iv—K2—K1v | 106.21 (5) | N1—C2—C1 | 111.6 (7) |
Mo1—K2—K1v | 67.96 (4) | N1—C2—H2A | 109.3 |
K2vi—K2—K1v | 135.61 (8) | C1—C2—H2A | 109.3 |
O5—Mo1—O6 | 105.8 (3) | N1—C2—H2B | 109.3 |
O5—Mo1—O4 | 100.2 (2) | C1—C2—H2B | 109.3 |
O6—Mo1—O4 | 98.4 (2) | H2A—C2—H2B | 108.0 |
O5—Mo1—O1iv | 95.3 (2) | C2—N1—H1A | 109.5 |
O6—Mo1—O1iv | 97.4 (2) | C2—N1—H1B | 109.5 |
O4—Mo1—O1iv | 154.0 (2) | H1A—N1—H1B | 109.5 |
O5—Mo1—O3iv | 161.6 (2) | C2—N1—H1C | 109.5 |
O6—Mo1—O3iv | 90.1 (2) | H1A—N1—H1C | 109.5 |
O4—Mo1—O3iv | 86.2 (2) | H1B—N1—H1C | 109.5 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x+1, y, z; (iii) −x+1, −y, −z; (iv) −x, −y, −z; (v) x−1, y, z; (vi) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O6i | 0.89 | 2.15 | 2.936 (9) | 147 |
N1—H1B···O10vii | 0.89 | 2.25 | 3.000 (9) | 142 |
N1—H1C···O14ii | 0.89 | 2.26 | 2.851 (9) | 124 |
N1—H1C···O10ii | 0.89 | 2.39 | 3.064 (9) | 133 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x+1, y, z; (vii) −x, −y, −z−1. |