Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807021769/bi2185sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807021769/bi2185Isup2.hkl |
CCDC reference: 657556
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.036
- wR factor = 0.061
- Data-to-parameter ratio = 11.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O15 - H15A ... ?
Alert level C PLAT410_ALERT_2_C Short Intra H...H Contact H2A .. H6 .. 1.97 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su .. 0.03
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.49 From the CIF: _reflns_number_total 4257 Count of symmetry unique reflns 2852 Completeness (_total/calc) 149.26% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1405 Fraction of Friedel pairs measured 0.493 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT792_ALERT_1_G Check the Absolute Configuration of N1 = ... S PLAT792_ALERT_1_G Check the Absolute Configuration of N2 = ... R PLAT792_ALERT_1_G Check the Absolute Configuration of C6 = ... R PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1 (5) 5.20 PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2 (5) 5.15 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 14
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 9 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level A PUBL022_ALERT_1_A There is a mismatched ~ on line 68 Poly[tetra-\m~2-aqua-diaqua-\m~2~-chlorido-di-\m~2~-oxo-dioxo[\m~7~-N,N,N',N'- If you require a ~ then it should be escaped with a \, i.e. \~ Otherwise there must be a matching closing ~, e.g. C~2~H~4~ PUBL022_ALERT_1_A There is a mismatched ~ on line 257 Poly[tetra-\m~2-aqua-diaqua-\m~2~-chlorido-di-\m~2~-oxo-dioxo[\m~7~-N,N,N',N'- If you require a ~ then it should be escaped with a \, i.e. \~ Otherwise there must be a matching closing ~, e.g. C~2~H~4~
2 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing
A mixture of H4PDTA (1.58 g, 5 mmol) and Na2MoO4.2H2O (2.42 g, 10 mmol) was dissolved in 10 ml water at room temperature. Na2S2O4 (0.87 g, 5 mmol) was added while stirring, and the color of the solution changed to red. Orange crystals were obtained after standing for several days.
H atoms bound to C atoms were placed in calculated positions and treated using a riding-model approximation (C—H = 0.99 Å for methylene H atoms with Uiso(H) = 1.2Ueq(C), C—H = 0.98 Å for methyl H atoms with Uiso(H) = 1.5Ueq(C) and C—H = 1.00 Å for tertiary H with Uiso(H) = 1.2Ueq(C)). H atoms bound to O atoms were visible in difference Fourier maps and were included in the refinement with O—H distances restrained to 0.90 (2) Å, and with Uiso(H) = 1.5Ueq(O).
Although dinuclear oxomolybdenum(V) compounds of the chelating ligands ethylenediaminetetraacetate (edta) and propylenediaminetetraacetate (PDTA) were widely studied during the late 1950 s and early 1960 s (Pecsok & Sawyer, 1956; Mitchell & Williams, 1962; Blake et al., 1964), the first such crystal structure of a potassium salt did not appear until 1967 (Haynes & Sawyer, 1967). Structures of sodium salts were reported in 1980 (Kimiko et al., 1980) and 1985 (Hong & Liu, 1985). This paper describes the synthesis of a new compound, trisodium bis(µ2-oxo)-(µ2-propylene-1,2-diaminetetra-acetato)-bis(oxo- molybdenum(V)) chloride hexahydrate, (I).
The asymmetric unit of (I) is shown in Fig. 1. The PDTA ligand coordinates to each Mo atom through two carboxylato-O atoms and an N atom, together with one terminal and two bridging O atoms to complete a distorted octahedral environment. Two terminal oxo ligands lie cis to the bridging oxide. The N atom and carboxlato-O atoms occupy the axial (trans to the terminal O) and equatorial positions, respectively. The short Mo···Mo distance (2.5483 (10) Å) indicates a strong interaction between the two Mo atoms.
As shown in Fig. 2, the [Mo2O4(PDTA)]2- complexes lie in layers parallel to the (001) planes. Between these layers, Na+ cations, Cl- anions and water molecules form a complex network stabilized by O—H···O and O—H···Cl hydrogen bonds (Table 2).
For related literature, see: Blake et al. (1964); Haynes & Sawyer (1967); Hong & Liu (1985); Kimiko et al. (1980); Mitchell & Williams (1962); Pecsok & Sawyer (1956).
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Na3Mo2(C11H14N2O8)ClO4(H2O)6] | F(000) = 1536 |
Mr = 770.64 | Dx = 2.065 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 3223 reflections |
a = 9.419 (3) Å | θ = 2.4–27.5° |
b = 10.443 (3) Å | µ = 1.26 mm−1 |
c = 25.409 (9) Å | T = 293 K |
β = 97.262 (5)° | Block, orange |
V = 2479.2 (15) Å3 | 0.18 × 0.15 × 0.12 mm |
Z = 4 |
Rigaku Mercury70 CCD diffractometer | 4257 independent reflections |
Radiation source: fine-focus sealed tube | 3894 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω scans | θmax = 27.5°, θmin = 2.9° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000) | h = −12→11 |
Tmin = 0.793, Tmax = 0.866 | k = −13→13 |
9442 measured reflections | l = −27→32 |
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)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.061 | w = 1/[σ2(Fo2) + (0.0125P)2 + 3.2472P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
4257 reflections | Δρmax = 0.64 e Å−3 |
371 parameters | Δρmin = −0.60 e Å−3 |
14 restraints | Absolute structure: Flack (1983), 1408 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (3) |
[Na3Mo2(C11H14N2O8)ClO4(H2O)6] | V = 2479.2 (15) Å3 |
Mr = 770.64 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 9.419 (3) Å | µ = 1.26 mm−1 |
b = 10.443 (3) Å | T = 293 K |
c = 25.409 (9) Å | 0.18 × 0.15 × 0.12 mm |
β = 97.262 (5)° |
Rigaku Mercury70 CCD diffractometer | 4257 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000) | 3894 reflections with I > 2σ(I) |
Tmin = 0.793, Tmax = 0.866 | Rint = 0.039 |
9442 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.061 | Δρmax = 0.64 e Å−3 |
S = 1.07 | Δρmin = −0.60 e Å−3 |
4257 reflections | Absolute structure: Flack (1983), 1408 Friedel pairs |
371 parameters | Absolute structure parameter: 0.00 (3) |
14 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.68634 (4) | 0.27602 (4) | 0.774649 (19) | 0.01927 (10) | |
Mo2 | 0.72208 (4) | 0.17925 (4) | 0.86745 (2) | 0.01976 (10) | |
Cl1 | 1.23667 (17) | 0.05188 (14) | 1.04123 (7) | 0.0373 (4) | |
C1 | 0.8469 (6) | 0.2226 (5) | 0.6825 (2) | 0.0211 (12) | |
C2 | 0.9743 (6) | 0.2587 (5) | 0.7218 (2) | 0.0268 (13) | |
H2A | 1.0244 | 0.1800 | 0.7357 | 0.032* | |
H2B | 1.0420 | 0.3100 | 0.7037 | 0.032* | |
C3 | 0.7845 (6) | 0.5120 (5) | 0.7215 (2) | 0.0227 (12) | |
C4 | 0.9243 (6) | 0.4734 (5) | 0.7522 (2) | 0.0264 (13) | |
H4A | 1.0025 | 0.4918 | 0.7307 | 0.032* | |
H4B | 0.9410 | 0.5255 | 0.7850 | 0.032* | |
C5 | 1.0376 (5) | 0.3277 (5) | 0.81541 (19) | 0.0185 (11) | |
H5A | 1.0049 | 0.3834 | 0.8430 | 0.022* | |
H5B | 1.1286 | 0.3637 | 0.8063 | 0.022* | |
C6 | 1.0684 (5) | 0.1933 (5) | 0.8395 (2) | 0.0224 (12) | |
H6 | 1.0390 | 0.1292 | 0.8110 | 0.027* | |
C7 | 1.2296 (6) | 0.1802 (5) | 0.8547 (2) | 0.0288 (14) | |
H7A | 1.2610 | 0.2382 | 0.8843 | 0.043* | |
H7B | 1.2788 | 0.2023 | 0.8242 | 0.043* | |
H7C | 1.2526 | 0.0918 | 0.8655 | 0.043* | |
C8 | 1.0155 (6) | 0.0285 (5) | 0.9010 (2) | 0.0289 (13) | |
H8A | 1.0308 | −0.0218 | 0.8692 | 0.035* | |
H8B | 1.1049 | 0.0254 | 0.9261 | 0.035* | |
C9 | 0.8976 (6) | −0.0300 (5) | 0.9264 (2) | 0.0251 (12) | |
C10 | 1.0260 (6) | 0.2485 (5) | 0.9324 (2) | 0.0272 (13) | |
H10A | 1.0504 | 0.3350 | 0.9204 | 0.033* | |
H10B | 1.1123 | 0.2122 | 0.9534 | 0.033* | |
C11 | 0.9067 (6) | 0.2585 (5) | 0.9668 (2) | 0.0226 (12) | |
N1 | 0.9287 (5) | 0.3343 (4) | 0.76691 (17) | 0.0190 (10) | |
N2 | 0.9832 (5) | 0.1654 (4) | 0.88510 (17) | 0.0187 (9) | |
O1 | 0.8635 (5) | 0.1945 (4) | 0.63630 (16) | 0.0370 (11) | |
O2 | 0.7257 (4) | 0.2154 (3) | 0.69963 (15) | 0.0285 (9) | |
O3 | 0.7812 (5) | 0.5935 (4) | 0.68608 (16) | 0.0374 (11) | |
O4 | 0.6737 (4) | 0.4579 (3) | 0.73618 (16) | 0.0281 (9) | |
O5 | 0.5061 (4) | 0.2665 (3) | 0.76182 (16) | 0.0278 (9) | |
O6 | 0.7564 (4) | 0.1099 (3) | 0.79953 (14) | 0.0208 (8) | |
O7 | 0.7362 (4) | 0.3533 (3) | 0.84310 (15) | 0.0253 (9) | |
O8 | 0.5492 (4) | 0.1545 (4) | 0.87545 (15) | 0.0288 (9) | |
O9 | 0.7688 (4) | 0.0026 (4) | 0.90722 (16) | 0.0310 (10) | |
O10 | 0.9228 (4) | −0.1099 (4) | 0.96216 (16) | 0.0338 (10) | |
O11 | 0.9301 (5) | 0.2746 (4) | 1.01484 (15) | 0.0351 (11) | |
O12 | 0.7777 (4) | 0.2559 (4) | 0.94321 (16) | 0.0311 (10) | |
O13 | 1.0124 (5) | −0.3908 (5) | 0.9867 (2) | 0.0425 (11) | |
H13A | 0.997 (8) | −0.390 (7) | 0.9509 (8) | 0.064* | |
H13B | 0.930 (5) | −0.413 (7) | 0.998 (3) | 0.064* | |
O14 | 1.1359 (5) | −0.2467 (4) | 1.10336 (17) | 0.0342 (10) | |
H14B | 1.183 (6) | −0.195 (5) | 1.127 (2) | 0.051* | |
H14A | 1.046 (3) | −0.268 (6) | 1.105 (3) | 0.051* | |
O15 | 1.0060 (5) | 0.0945 (4) | 1.12619 (18) | 0.0406 (11) | |
H15A | 1.047 (7) | 0.048 (6) | 1.103 (2) | 0.061* | |
H15B | 1.051 (7) | 0.062 (6) | 1.1551 (17) | 0.061* | |
O16 | 1.2246 (5) | 0.4494 (4) | 1.03599 (18) | 0.0367 (11) | |
H16B | 1.292 (6) | 0.423 (6) | 1.017 (2) | 0.055* | |
H16A | 1.172 (7) | 0.484 (6) | 1.008 (2) | 0.055* | |
O17 | 1.0118 (5) | 0.4499 (4) | 1.11941 (16) | 0.0356 (10) | |
H17B | 0.978 (7) | 0.417 (6) | 1.1470 (18) | 0.053* | |
H17A | 0.962 (7) | 0.487 (5) | 1.0915 (18) | 0.053* | |
O18 | 1.2844 (5) | 0.5725 (4) | 1.21464 (19) | 0.0413 (12) | |
H18A | 1.301 (8) | 0.510 (5) | 1.239 (2) | 0.062* | |
H18B | 1.361 (5) | 0.615 (6) | 1.231 (3) | 0.062* | |
Na1 | 1.1254 (3) | 0.2723 (2) | 1.08039 (9) | 0.0319 (6) | |
Na2 | 1.1410 (3) | −0.1912 (2) | 1.01298 (9) | 0.0318 (5) | |
Na3 | 1.2537 (3) | 0.5442 (2) | 1.12192 (10) | 0.0366 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0151 (2) | 0.0204 (2) | 0.0218 (2) | 0.00048 (19) | 0.00022 (17) | 0.0006 (2) |
Mo2 | 0.0139 (2) | 0.0257 (2) | 0.0195 (2) | 0.0006 (2) | 0.00159 (17) | −0.0003 (2) |
Cl1 | 0.0354 (9) | 0.0337 (8) | 0.0426 (9) | 0.0054 (6) | 0.0043 (7) | −0.0019 (7) |
C1 | 0.025 (3) | 0.018 (3) | 0.020 (3) | 0.000 (2) | 0.000 (2) | 0.001 (2) |
C2 | 0.024 (3) | 0.035 (3) | 0.021 (3) | −0.001 (2) | 0.004 (2) | −0.004 (2) |
C3 | 0.028 (3) | 0.016 (3) | 0.024 (3) | 0.000 (2) | 0.001 (2) | 0.000 (2) |
C4 | 0.028 (3) | 0.021 (3) | 0.029 (3) | −0.007 (2) | −0.001 (2) | 0.005 (2) |
C5 | 0.018 (3) | 0.025 (3) | 0.013 (2) | −0.004 (2) | 0.002 (2) | 0.001 (2) |
C6 | 0.015 (3) | 0.032 (3) | 0.021 (3) | −0.001 (2) | 0.004 (2) | −0.002 (2) |
C7 | 0.016 (3) | 0.034 (3) | 0.037 (4) | 0.001 (2) | 0.005 (3) | 0.001 (3) |
C8 | 0.026 (3) | 0.031 (3) | 0.031 (3) | 0.011 (2) | 0.010 (3) | 0.009 (3) |
C9 | 0.028 (3) | 0.023 (3) | 0.026 (3) | 0.006 (2) | 0.009 (2) | 0.001 (2) |
C10 | 0.023 (3) | 0.043 (3) | 0.015 (3) | 0.000 (2) | 0.001 (2) | 0.002 (2) |
C11 | 0.021 (3) | 0.025 (3) | 0.021 (3) | 0.002 (2) | 0.002 (2) | −0.002 (2) |
N1 | 0.019 (3) | 0.022 (2) | 0.016 (2) | −0.0031 (18) | −0.0005 (18) | 0.0039 (18) |
N2 | 0.014 (2) | 0.021 (2) | 0.020 (2) | −0.0009 (17) | 0.0020 (18) | 0.0043 (18) |
O1 | 0.043 (3) | 0.049 (3) | 0.019 (2) | 0.001 (2) | 0.0041 (19) | −0.0085 (19) |
O2 | 0.024 (2) | 0.041 (2) | 0.020 (2) | −0.0071 (19) | −0.0004 (17) | −0.0055 (17) |
O3 | 0.044 (3) | 0.038 (2) | 0.031 (2) | 0.002 (2) | 0.006 (2) | 0.0136 (19) |
O4 | 0.024 (2) | 0.027 (2) | 0.033 (2) | 0.0016 (17) | 0.0004 (18) | 0.0102 (17) |
O5 | 0.016 (2) | 0.027 (2) | 0.039 (2) | −0.0007 (16) | −0.0031 (18) | 0.0042 (18) |
O6 | 0.019 (2) | 0.0199 (18) | 0.023 (2) | −0.0016 (15) | 0.0012 (15) | −0.0052 (15) |
O7 | 0.022 (2) | 0.0191 (18) | 0.035 (2) | 0.0009 (15) | 0.0028 (18) | 0.0003 (16) |
O8 | 0.015 (2) | 0.044 (2) | 0.028 (2) | 0.0015 (17) | 0.0058 (17) | 0.0010 (18) |
O9 | 0.019 (2) | 0.034 (2) | 0.039 (3) | −0.0023 (16) | −0.0009 (18) | 0.0154 (18) |
O10 | 0.034 (3) | 0.032 (2) | 0.035 (2) | 0.0065 (18) | 0.0038 (19) | 0.0159 (19) |
O11 | 0.035 (3) | 0.048 (3) | 0.021 (2) | 0.007 (2) | −0.0019 (19) | −0.010 (2) |
O12 | 0.016 (2) | 0.047 (3) | 0.030 (2) | 0.0011 (18) | −0.0013 (17) | −0.0090 (19) |
O13 | 0.036 (3) | 0.049 (3) | 0.043 (3) | 0.002 (2) | 0.008 (2) | 0.012 (2) |
O14 | 0.038 (3) | 0.039 (3) | 0.026 (2) | −0.011 (2) | 0.007 (2) | −0.0063 (18) |
O15 | 0.040 (3) | 0.048 (3) | 0.034 (3) | −0.001 (2) | 0.005 (2) | 0.005 (2) |
O16 | 0.034 (3) | 0.049 (3) | 0.028 (2) | 0.005 (2) | 0.007 (2) | 0.003 (2) |
O17 | 0.033 (3) | 0.050 (3) | 0.024 (3) | 0.003 (2) | 0.0031 (19) | 0.000 (2) |
O18 | 0.040 (3) | 0.045 (3) | 0.036 (3) | −0.016 (2) | −0.005 (2) | 0.003 (2) |
Na1 | 0.0319 (14) | 0.0294 (12) | 0.0328 (13) | −0.0010 (10) | −0.0016 (11) | −0.0003 (10) |
Na2 | 0.0358 (15) | 0.0351 (13) | 0.0266 (13) | 0.0055 (11) | 0.0117 (11) | 0.0021 (10) |
Na3 | 0.0347 (15) | 0.0404 (14) | 0.0336 (14) | −0.0030 (11) | −0.0001 (11) | −0.0021 (11) |
Mo1—O5 | 1.690 (4) | C9—O9 | 1.295 (6) |
Mo1—O7 | 1.921 (4) | C10—N2 | 1.495 (7) |
Mo1—O6 | 1.933 (3) | C10—C11 | 1.513 (8) |
Mo1—O2 | 2.086 (4) | C10—H10A | 0.990 |
Mo1—O4 | 2.133 (4) | C10—H10B | 0.990 |
Mo1—N1 | 2.395 (4) | C11—O11 | 1.224 (6) |
Mo1—Mo2 | 2.5483 (10) | C11—O12 | 1.285 (7) |
Mo2—O8 | 1.686 (4) | O1—Na1i | 2.522 (5) |
Mo2—O7 | 1.930 (4) | O1—Na3i | 2.706 (5) |
Mo2—O6 | 1.936 (4) | O10—Na2 | 2.437 (4) |
Mo2—O12 | 2.089 (4) | O11—Na1 | 2.320 (4) |
Mo2—O9 | 2.122 (4) | O11—Na2ii | 2.742 (5) |
Mo2—N2 | 2.448 (4) | O12—Na2ii | 2.384 (5) |
Cl1—Na2 | 2.758 (3) | O13—Na2 | 2.460 (5) |
Cl1—Na1 | 2.766 (3) | O13—H13A | 0.90 (2) |
C1—O1 | 1.238 (7) | O13—H13B | 0.89 (5) |
C1—O2 | 1.275 (7) | O14—Na2 | 2.375 (5) |
C1—C2 | 1.508 (7) | O14—Na3iii | 2.468 (5) |
C2—N1 | 1.499 (7) | O14—H14B | 0.88 (5) |
C2—H2A | 0.990 | O14—H14A | 0.88 (2) |
C2—H2B | 0.990 | O15—Na3iv | 2.422 (6) |
C3—O3 | 1.236 (6) | O15—Na1 | 2.529 (5) |
C3—O4 | 1.282 (7) | O15—H15A | 0.89 (6) |
C3—C4 | 1.499 (7) | O15—H15B | 0.87 (5) |
C4—N1 | 1.499 (6) | O16—Na3 | 2.381 (5) |
C4—H4A | 0.990 | O16—Na1 | 2.415 (5) |
C4—H4B | 0.990 | O16—H16B | 0.89 (6) |
C5—N1 | 1.502 (6) | O16—H16A | 0.89 (6) |
C5—C6 | 1.543 (7) | O17—Na1 | 2.416 (5) |
C5—H5A | 0.990 | O17—Na3 | 2.475 (5) |
C5—H5B | 0.990 | O17—H17B | 0.88 (5) |
C6—N2 | 1.519 (7) | O17—H17A | 0.89 (5) |
C6—C7 | 1.525 (7) | O18—Na3 | 2.356 (5) |
C6—H6 | 1.000 | O18—H18A | 0.90 (5) |
C7—H7A | 0.980 | O18—H18B | 0.90 (6) |
C7—H7B | 0.980 | Na1—O1v | 2.522 (5) |
C7—H7C | 0.980 | Na2—O12vi | 2.384 (5) |
C8—C9 | 1.484 (8) | Na2—O11vi | 2.742 (5) |
C8—N2 | 1.506 (6) | Na3—O15vii | 2.422 (6) |
C8—H8A | 0.990 | Na3—O14viii | 2.468 (5) |
C8—H8B | 0.990 | Na3—O1v | 2.706 (5) |
C9—O10 | 1.235 (6) | ||
O5—Mo1—O7 | 108.89 (18) | C4—N1—C5 | 104.1 (4) |
O5—Mo1—O6 | 107.66 (16) | C2—N1—C5 | 111.8 (4) |
O7—Mo1—O6 | 92.66 (15) | C4—N1—Mo1 | 105.6 (3) |
O5—Mo1—O2 | 95.52 (18) | C2—N1—Mo1 | 107.3 (3) |
O7—Mo1—O2 | 154.64 (16) | C5—N1—Mo1 | 118.7 (3) |
O6—Mo1—O2 | 86.20 (15) | C10—N2—C8 | 108.1 (4) |
O5—Mo1—O4 | 88.14 (16) | C10—N2—C6 | 112.7 (4) |
O7—Mo1—O4 | 91.95 (15) | C8—N2—C6 | 106.2 (4) |
O6—Mo1—O4 | 161.05 (16) | C10—N2—Mo2 | 106.0 (3) |
O2—Mo1—O4 | 81.81 (16) | C8—N2—Mo2 | 105.6 (3) |
O5—Mo1—N1 | 160.66 (16) | C6—N2—Mo2 | 117.7 (3) |
O7—Mo1—N1 | 80.86 (16) | C1—O1—Na1i | 106.9 (4) |
O6—Mo1—N1 | 88.01 (15) | C1—O1—Na3i | 104.7 (4) |
O2—Mo1—N1 | 73.79 (15) | Na1i—O1—Na3i | 75.70 (13) |
O4—Mo1—N1 | 74.59 (15) | C1—O2—Mo1 | 124.4 (3) |
O5—Mo1—Mo2 | 99.62 (14) | C3—O4—Mo1 | 121.7 (3) |
O7—Mo1—Mo2 | 48.71 (11) | Mo1—O6—Mo2 | 82.38 (13) |
O6—Mo1—Mo2 | 48.85 (11) | Mo1—O7—Mo2 | 82.88 (14) |
O2—Mo1—Mo2 | 135.02 (11) | C9—O9—Mo2 | 122.4 (3) |
O4—Mo1—Mo2 | 140.39 (11) | C9—O10—Na2 | 134.1 (4) |
N1—Mo1—Mo2 | 99.26 (10) | C11—O11—Na1 | 137.8 (4) |
O8—Mo2—O7 | 106.84 (18) | C11—O11—Na2ii | 87.0 (3) |
O8—Mo2—O6 | 108.83 (17) | Na1—O11—Na2ii | 135.18 (19) |
O7—Mo2—O6 | 92.30 (15) | C11—O12—Mo2 | 123.4 (4) |
O8—Mo2—O12 | 94.66 (18) | C11—O12—Na2ii | 102.5 (3) |
O7—Mo2—O12 | 85.14 (16) | Mo2—O12—Na2ii | 132.7 (2) |
O6—Mo2—O12 | 156.04 (16) | Na2—O13—H13A | 106 (5) |
O8—Mo2—O9 | 87.41 (17) | Na2—O13—H13B | 123 (5) |
O7—Mo2—O9 | 162.28 (15) | H13A—O13—H13B | 107 (7) |
O6—Mo2—O9 | 92.95 (15) | Na2—O14—Na3iii | 109.70 (19) |
O12—Mo2—O9 | 83.19 (16) | Na2—O14—H14B | 116 (5) |
O8—Mo2—N2 | 158.75 (16) | Na3iii—O14—H14B | 104 (4) |
O7—Mo2—N2 | 90.35 (15) | Na2—O14—H14A | 104 (4) |
O6—Mo2—N2 | 82.19 (15) | Na3iii—O14—H14A | 100 (4) |
O12—Mo2—N2 | 74.02 (15) | H14B—O14—H14A | 122 (6) |
O9—Mo2—N2 | 73.63 (14) | Na3iv—O15—Na1 | 129.0 (2) |
O8—Mo2—Mo1 | 98.96 (13) | Na3iv—O15—H15A | 111 (5) |
O7—Mo2—Mo1 | 48.41 (11) | Na1—O15—H15A | 81 (5) |
O6—Mo2—Mo1 | 48.76 (10) | Na3iv—O15—H15B | 109 (5) |
O12—Mo2—Mo1 | 133.55 (12) | Na1—O15—H15B | 118 (5) |
O9—Mo2—Mo1 | 141.29 (12) | H15A—O15—H15B | 99 (6) |
N2—Mo2—Mo1 | 101.84 (10) | Na3—O16—Na1 | 84.05 (17) |
Na2—Cl1—Na1 | 137.16 (10) | Na3—O16—H16B | 128 (5) |
O1—C1—O2 | 122.4 (5) | Na1—O16—H16B | 111 (4) |
O1—C1—C2 | 120.1 (5) | Na3—O16—H16A | 123 (5) |
O2—C1—C2 | 117.4 (5) | Na1—O16—H16A | 118 (5) |
O1—C1—Na1i | 50.7 (3) | H16B—O16—H16A | 93 (6) |
O2—C1—Na1i | 75.6 (3) | Na1—O17—Na3 | 82.06 (17) |
C2—C1—Na1i | 160.0 (4) | Na1—O17—H17B | 105 (5) |
N1—C2—C1 | 110.9 (5) | Na3—O17—H17B | 124 (5) |
N1—C2—H2A | 109.5 | Na1—O17—H17A | 103 (4) |
C1—C2—H2A | 109.5 | Na3—O17—H17A | 104 (5) |
N1—C2—H2B | 109.5 | H17B—O17—H17A | 127 (7) |
C1—C2—H2B | 109.5 | Na3—O18—H18A | 125 (5) |
H2A—C2—H2B | 108.0 | Na3—O18—H18B | 120 (5) |
O3—C3—O4 | 124.7 (5) | H18A—O18—H18B | 90 (6) |
O3—C3—C4 | 120.2 (5) | O11—Na1—O16 | 88.59 (17) |
O4—C3—C4 | 115.0 (5) | O11—Na1—O17 | 86.27 (16) |
N1—C4—C3 | 112.7 (4) | O16—Na1—O17 | 79.71 (17) |
N1—C4—H4A | 109.1 | O11—Na1—O1v | 166.07 (18) |
C3—C4—H4A | 109.1 | O16—Na1—O1v | 77.81 (16) |
N1—C4—H4B | 109.1 | O17—Na1—O1v | 94.12 (17) |
C3—C4—H4B | 109.1 | O11—Na1—O15 | 88.83 (17) |
H4A—C4—H4B | 107.8 | O16—Na1—O15 | 176.26 (19) |
N1—C5—C6 | 116.2 (4) | O17—Na1—O15 | 97.42 (18) |
N1—C5—H5A | 108.2 | O1v—Na1—O15 | 104.90 (16) |
C6—C5—H5A | 108.2 | O11—Na1—Cl1 | 93.00 (13) |
N1—C5—H5B | 108.2 | O16—Na1—Cl1 | 106.41 (15) |
C6—C5—H5B | 108.2 | O17—Na1—Cl1 | 173.83 (16) |
H5A—C5—H5B | 107.4 | O1v—Na1—Cl1 | 88.07 (13) |
N2—C6—C7 | 113.2 (4) | O15—Na1—Cl1 | 76.43 (13) |
N2—C6—C5 | 112.7 (4) | O14—Na2—O12vi | 137.83 (18) |
C7—C6—C5 | 108.3 (4) | O14—Na2—O10 | 118.61 (18) |
N2—C6—H6 | 107.4 | O12vi—Na2—O10 | 100.68 (16) |
C7—C6—H6 | 107.4 | O14—Na2—O13 | 89.24 (17) |
C5—C6—H6 | 107.4 | O12vi—Na2—O13 | 83.98 (17) |
C6—C7—H7A | 109.5 | O10—Na2—O13 | 78.34 (16) |
C6—C7—H7B | 109.5 | O14—Na2—O11vi | 95.33 (16) |
H7A—C7—H7B | 109.5 | O12vi—Na2—O11vi | 49.73 (13) |
C6—C7—H7C | 109.5 | O10—Na2—O11vi | 145.47 (16) |
H7A—C7—H7C | 109.5 | O13—Na2—O11vi | 110.36 (17) |
H7B—C7—H7C | 109.5 | O14—Na2—Cl1 | 91.07 (13) |
C9—C8—N2 | 111.7 (4) | O12vi—Na2—Cl1 | 102.55 (13) |
C9—C8—H8A | 109.3 | O10—Na2—Cl1 | 92.49 (12) |
N2—C8—H8A | 109.3 | O13—Na2—Cl1 | 169.69 (16) |
C9—C8—H8B | 109.3 | O11vi—Na2—Cl1 | 79.88 (12) |
N2—C8—H8B | 109.3 | O18—Na3—O16 | 162.65 (19) |
H8A—C8—H8B | 107.9 | O18—Na3—O15vii | 86.12 (18) |
O10—C9—O9 | 122.6 (5) | O16—Na3—O15vii | 97.47 (19) |
O10—C9—C8 | 120.9 (5) | O18—Na3—O14viii | 94.32 (17) |
O9—C9—C8 | 116.5 (5) | O16—Na3—O14viii | 101.28 (17) |
N2—C10—C11 | 111.1 (4) | O15vii—Na3—O14viii | 103.37 (17) |
N2—C10—H10A | 109.4 | O18—Na3—O17 | 94.12 (17) |
C11—C10—H10A | 109.4 | O16—Na3—O17 | 79.18 (17) |
N2—C10—H10B | 109.4 | O15vii—Na3—O17 | 169.07 (18) |
C11—C10—H10B | 109.4 | O14viii—Na3—O17 | 87.51 (17) |
H10A—C10—H10B | 108.0 | O18—Na3—O1v | 89.09 (16) |
O11—C11—O12 | 120.6 (6) | O16—Na3—O1v | 74.85 (15) |
O11—C11—C10 | 122.2 (5) | O15vii—Na3—O1v | 80.68 (17) |
O12—C11—C10 | 117.1 (5) | O14viii—Na3—O1v | 174.85 (16) |
C4—N1—C2 | 108.8 (4) | O17—Na3—O1v | 88.40 (16) |
O5—Mo1—Mo2—O8 | −2.14 (18) | O3—C3—O4—Mo1 | 156.8 (4) |
O7—Mo1—Mo2—O8 | 104.6 (2) | C4—C3—O4—Mo1 | −25.7 (6) |
O6—Mo1—Mo2—O8 | −107.24 (19) | O5—Mo1—O4—C3 | −164.8 (4) |
O2—Mo1—Mo2—O8 | −110.1 (2) | O7—Mo1—O4—C3 | 86.4 (4) |
O4—Mo1—Mo2—O8 | 96.7 (2) | O6—Mo1—O4—C3 | −17.6 (7) |
N1—Mo1—Mo2—O8 | 173.66 (17) | O2—Mo1—O4—C3 | −68.9 (4) |
O5—Mo1—Mo2—O7 | −106.8 (2) | N1—Mo1—O4—C3 | 6.4 (4) |
O6—Mo1—Mo2—O7 | 148.2 (2) | Mo2—Mo1—O4—C3 | 92.4 (4) |
O2—Mo1—Mo2—O7 | 145.3 (2) | O5—Mo1—O6—Mo2 | −87.40 (18) |
O4—Mo1—Mo2—O7 | −7.9 (2) | O7—Mo1—O6—Mo2 | 23.38 (15) |
N1—Mo1—Mo2—O7 | 69.05 (19) | O2—Mo1—O6—Mo2 | 178.01 (15) |
O5—Mo1—Mo2—O6 | 105.10 (19) | O4—Mo1—O6—Mo2 | 127.3 (4) |
O7—Mo1—Mo2—O6 | −148.2 (2) | N1—Mo1—O6—Mo2 | 104.13 (14) |
O2—Mo1—Mo2—O6 | −2.8 (2) | O8—Mo2—O6—Mo1 | 85.40 (17) |
O4—Mo1—Mo2—O6 | −156.1 (2) | O7—Mo2—O6—Mo1 | −23.27 (15) |
N1—Mo1—Mo2—O6 | −79.10 (17) | O12—Mo2—O6—Mo1 | −106.5 (3) |
O5—Mo1—Mo2—O12 | −107.4 (2) | O9—Mo2—O6—Mo1 | 173.66 (13) |
O7—Mo1—Mo2—O12 | −0.7 (2) | N2—Mo2—O6—Mo1 | −113.31 (14) |
O6—Mo1—Mo2—O12 | 147.5 (2) | O5—Mo1—O7—Mo2 | 86.24 (17) |
O2—Mo1—Mo2—O12 | 144.7 (2) | O6—Mo1—O7—Mo2 | −23.44 (15) |
O4—Mo1—Mo2—O12 | −8.6 (2) | O2—Mo1—O7—Mo2 | −110.2 (3) |
N1—Mo1—Mo2—O12 | 68.40 (19) | O4—Mo1—O7—Mo2 | 174.95 (15) |
O5—Mo1—Mo2—O9 | 94.9 (2) | N1—Mo1—O7—Mo2 | −111.00 (15) |
O7—Mo1—Mo2—O9 | −158.3 (2) | O8—Mo2—O7—Mo1 | −87.07 (18) |
O6—Mo1—Mo2—O9 | −10.2 (2) | O6—Mo2—O7—Mo1 | 23.40 (15) |
O2—Mo1—Mo2—O9 | −13.0 (2) | O12—Mo2—O7—Mo1 | 179.52 (16) |
O4—Mo1—Mo2—O9 | −166.2 (2) | O9—Mo2—O7—Mo1 | 130.6 (5) |
N1—Mo1—Mo2—O9 | −89.2 (2) | N2—Mo2—O7—Mo1 | 105.60 (15) |
O5—Mo1—Mo2—N2 | 173.48 (16) | O10—C9—O9—Mo2 | 157.7 (4) |
O7—Mo1—Mo2—N2 | −79.77 (19) | C8—C9—O9—Mo2 | −25.5 (7) |
O6—Mo1—Mo2—N2 | 68.38 (17) | O8—Mo2—O9—C9 | −164.3 (5) |
O2—Mo1—Mo2—N2 | 65.57 (18) | O7—Mo2—O9—C9 | −20.2 (8) |
O4—Mo1—Mo2—N2 | −87.7 (2) | O6—Mo2—O9—C9 | 86.9 (4) |
N1—Mo1—Mo2—N2 | −10.71 (14) | O12—Mo2—O9—C9 | −69.3 (4) |
O1—C1—C2—N1 | 158.7 (5) | N2—Mo2—O9—C9 | 5.9 (4) |
O2—C1—C2—N1 | −25.2 (7) | Mo1—Mo2—O9—C9 | 94.5 (4) |
Na1i—C1—C2—N1 | 101.9 (11) | O9—C9—O10—Na2 | −175.9 (4) |
O3—C3—C4—N1 | −144.9 (5) | C8—C9—O10—Na2 | 7.4 (8) |
O4—C3—C4—N1 | 37.4 (7) | O12—C11—O11—Na1 | 173.6 (4) |
N1—C5—C6—N2 | −96.4 (5) | C10—C11—O11—Na1 | −9.9 (9) |
N1—C5—C6—C7 | 137.6 (5) | O12—C11—O11—Na2ii | −4.8 (5) |
N2—C8—C9—O10 | −146.2 (5) | C10—C11—O11—Na2ii | 171.7 (5) |
N2—C8—C9—O9 | 37.0 (7) | O11—C11—O12—Mo2 | −162.0 (4) |
N2—C10—C11—O11 | 150.2 (5) | C10—C11—O12—Mo2 | 21.3 (6) |
N2—C10—C11—O12 | −33.2 (6) | O11—C11—O12—Na2ii | 5.6 (6) |
N2—C10—C11—Na2ii | −66.3 (17) | C10—C11—O12—Na2ii | −171.1 (4) |
C3—C4—N1—C2 | 85.8 (6) | O8—Mo2—O12—C11 | 158.2 (4) |
C3—C4—N1—C5 | −154.8 (5) | O7—Mo2—O12—C11 | −95.3 (4) |
C3—C4—N1—Mo1 | −29.0 (5) | O6—Mo2—O12—C11 | −10.6 (7) |
C1—C2—N1—C4 | −87.8 (5) | O9—Mo2—O12—C11 | 71.3 (4) |
C1—C2—N1—C5 | 157.7 (4) | N2—Mo2—O12—C11 | −3.5 (4) |
C1—C2—N1—Mo1 | 26.0 (5) | Mo1—Mo2—O12—C11 | −94.8 (4) |
C6—C5—N1—C4 | −178.8 (5) | O8—Mo2—O12—Na2ii | −5.3 (3) |
C6—C5—N1—C2 | −61.5 (6) | O7—Mo2—O12—Na2ii | 101.3 (3) |
C6—C5—N1—Mo1 | 64.2 (5) | O6—Mo2—O12—Na2ii | −174.0 (2) |
O5—Mo1—N1—C4 | 40.7 (7) | O9—Mo2—O12—Na2ii | −92.1 (3) |
O7—Mo1—N1—C4 | −81.4 (3) | N2—Mo2—O12—Na2ii | −167.0 (3) |
O6—Mo1—N1—C4 | −174.4 (3) | Mo1—Mo2—O12—Na2ii | 101.8 (3) |
O2—Mo1—N1—C4 | 99.0 (3) | C11—O11—Na1—O16 | 62.4 (6) |
O4—Mo1—N1—C4 | 13.2 (3) | Na2ii—O11—Na1—O16 | −120.0 (3) |
Mo2—Mo1—N1—C4 | −126.7 (3) | C11—O11—Na1—O17 | 142.2 (6) |
O5—Mo1—N1—C2 | −75.2 (6) | Na2ii—O11—Na1—O17 | −40.2 (3) |
O7—Mo1—N1—C2 | 162.7 (3) | C11—O11—Na1—O1v | 50.1 (11) |
O6—Mo1—N1—C2 | 69.7 (3) | Na2ii—O11—Na1—O1v | −132.3 (7) |
O2—Mo1—N1—C2 | −16.9 (3) | C11—O11—Na1—O15 | −120.3 (6) |
O4—Mo1—N1—C2 | −102.7 (3) | Na2ii—O11—Na1—O15 | 57.3 (3) |
Mo2—Mo1—N1—C2 | 117.4 (3) | C11—O11—Na1—Cl1 | −44.0 (6) |
O5—Mo1—N1—C5 | 157.0 (5) | Na2ii—O11—Na1—Cl1 | 133.7 (2) |
O7—Mo1—N1—C5 | 34.9 (3) | Na3—O16—Na1—O11 | 130.10 (17) |
O6—Mo1—N1—C5 | −58.2 (3) | Na3—O16—Na1—O17 | 43.64 (15) |
O2—Mo1—N1—C5 | −144.8 (4) | Na3—O16—Na1—O1v | −52.90 (15) |
O4—Mo1—N1—C5 | 129.5 (4) | Na3—O16—Na1—Cl1 | −137.19 (12) |
Mo2—Mo1—N1—C5 | −10.4 (3) | Na3—O16—Na1—C1v | −41.02 (16) |
C11—C10—N2—C8 | −86.0 (5) | Na3—O17—Na1—O11 | −131.05 (16) |
C11—C10—N2—C6 | 156.9 (4) | Na3—O17—Na1—O16 | −41.81 (14) |
C11—C10—N2—Mo2 | 26.9 (5) | Na3—O17—Na1—O1v | 35.00 (15) |
C9—C8—N2—C10 | 84.6 (6) | Na3—O17—Na1—O15 | 140.62 (15) |
C9—C8—N2—C6 | −154.3 (5) | Na3—O17—Na1—C1v | 55.82 (15) |
C9—C8—N2—Mo2 | −28.6 (5) | Na3iv—O15—Na1—O11 | −25.5 (3) |
C7—C6—N2—C10 | 56.9 (6) | Na3iv—O15—Na1—O17 | 60.6 (3) |
C5—C6—N2—C10 | −66.4 (5) | Na3iv—O15—Na1—O1v | 156.8 (2) |
C7—C6—N2—C8 | −61.3 (5) | Na3iv—O15—Na1—Cl1 | −118.9 (3) |
C5—C6—N2—C8 | 175.4 (4) | Na3iv—O15—Na1—C1v | 145.9 (3) |
C7—C6—N2—Mo2 | −179.3 (3) | Na3iv—O15—Na1—Na3 | 101.2 (3) |
C5—C6—N2—Mo2 | 57.4 (5) | Na2—Cl1—Na1—O11 | −51.88 (19) |
O8—Mo2—N2—C10 | −73.6 (6) | Na2—Cl1—Na1—O16 | −141.29 (16) |
O7—Mo2—N2—C10 | 71.0 (3) | Na2—Cl1—Na1—O1v | 142.02 (16) |
O6—Mo2—N2—C10 | 163.3 (3) | Na2—Cl1—Na1—O15 | 36.19 (17) |
O12—Mo2—N2—C10 | −13.9 (3) | Na2—Cl1—Na1—C1v | 120.46 (16) |
O9—Mo2—N2—C10 | −101.3 (3) | Na2—Cl1—Na1—Na3 | 173.35 (12) |
Mo1—Mo2—N2—C10 | 118.4 (3) | Na3iii—O14—Na2—O12vi | −22.2 (3) |
O8—Mo2—N2—C8 | 40.9 (6) | Na3iii—O14—Na2—O10 | 134.23 (19) |
O7—Mo2—N2—C8 | −174.5 (3) | Na3iii—O14—Na2—O13 | 58.0 (2) |
O6—Mo2—N2—C8 | −82.2 (3) | Na3iii—O14—Na2—O11vi | −52.4 (2) |
O12—Mo2—N2—C8 | 100.7 (4) | Na3iii—O14—Na2—Cl1 | −132.34 (17) |
O9—Mo2—N2—C8 | 13.2 (3) | C9—O10—Na2—O14 | 145.3 (5) |
Mo1—Mo2—N2—C8 | −127.1 (3) | C9—O10—Na2—O12vi | −50.5 (5) |
O8—Mo2—N2—C6 | 159.2 (4) | C9—O10—Na2—O13 | −132.0 (5) |
O7—Mo2—N2—C6 | −56.2 (3) | C9—O10—Na2—O11vi | −22.9 (7) |
O6—Mo2—N2—C6 | 36.1 (3) | C9—O10—Na2—Cl1 | 52.7 (5) |
O12—Mo2—N2—C6 | −141.0 (4) | Na1—Cl1—Na2—O14 | −71.71 (18) |
O9—Mo2—N2—C6 | 131.5 (4) | Na1—Cl1—Na2—O12vi | 148.50 (15) |
Mo1—Mo2—N2—C6 | −8.8 (3) | Na1—Cl1—Na2—O10 | 46.98 (18) |
O2—C1—O1—Na1i | 25.9 (6) | Na1—Cl1—Na2—O13 | 20.0 (9) |
C2—C1—O1—Na1i | −158.2 (4) | Na1—Cl1—Na2—O11vi | −166.93 (14) |
O2—C1—O1—Na3i | −53.3 (6) | Na1—O16—Na3—O18 | 26.0 (7) |
C2—C1—O1—Na3i | 122.5 (4) | Na1—O16—Na3—O15vii | 127.04 (17) |
Na1i—C1—O1—Na3i | −79.2 (2) | Na1—O16—Na3—O14viii | −127.65 (17) |
O1—C1—O2—Mo1 | −174.4 (4) | Na1—O16—Na3—O17 | −42.42 (15) |
C2—C1—O2—Mo1 | 9.6 (6) | Na1—O16—Na3—O1v | 48.85 (14) |
Na1i—C1—O2—Mo1 | −154.0 (3) | Na1—O16—Na3—Na2viii | −142.31 (16) |
O5—Mo1—O2—C1 | 168.3 (4) | Na1—O17—Na3—O18 | −121.22 (16) |
O7—Mo1—O2—C1 | 3.8 (6) | Na1—O17—Na3—O16 | 42.64 (15) |
O6—Mo1—O2—C1 | −84.4 (4) | Na1—O17—Na3—O15vii | −30.4 (10) |
O4—Mo1—O2—C1 | 80.9 (4) | Na1—O17—Na3—O14viii | 144.63 (16) |
N1—Mo1—O2—C1 | 4.7 (4) | Na1—O17—Na3—O1v | −32.25 (14) |
Mo2—Mo1—O2—C1 | −82.2 (4) | Na1—O17—Na3—Na2viii | 111.14 (11) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x−1/2, y+1/2, z; (iii) x, y−1, z; (iv) x−1/2, y−1/2, z; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, y−1/2, z; (vii) x+1/2, y+1/2, z; (viii) x, y+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O13—H13A···O8vi | 0.90 (2) | 2.09 (4) | 2.929 (6) | 154 (7) |
O13—H13B···Cl1iv | 0.89 (5) | 2.27 (6) | 3.152 (5) | 169 (7) |
O14—H14B···O3v | 0.88 (5) | 1.97 (5) | 2.850 (6) | 173 (6) |
O14—H14A···O1ix | 0.88 (2) | 2.13 (5) | 2.850 (7) | 139 (6) |
O15—H15A···Cl1 | 0.89 (6) | 2.52 (4) | 3.281 (5) | 144 (6) |
O15—H15B···O4v | 0.87 (5) | 2.24 (3) | 3.081 (6) | 163 (6) |
O16—H16B···O10vii | 0.89 (6) | 2.00 (3) | 2.876 (6) | 168 (7) |
O16—H16A···O13viii | 0.89 (6) | 2.02 (5) | 2.778 (6) | 143 (7) |
O17—H17B···O3x | 0.88 (5) | 2.22 (5) | 2.953 (7) | 142 (6) |
O17—H17A···Cl1ii | 0.89 (5) | 2.43 (4) | 3.239 (5) | 152 (7) |
O18—H18A···O6v | 0.90 (5) | 2.08 (4) | 2.914 (6) | 156 (7) |
O18—H18B···O5xi | 0.90 (6) | 1.93 (6) | 2.827 (6) | 170 (7) |
Symmetry codes: (ii) x−1/2, y+1/2, z; (iv) x−1/2, y−1/2, z; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, y−1/2, z; (vii) x+1/2, y+1/2, z; (viii) x, y+1, z; (ix) x, −y, z+1/2; (x) x, −y+1, z+1/2; (xi) x+1, −y+1, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Na3Mo2(C11H14N2O8)ClO4(H2O)6] |
Mr | 770.64 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 293 |
a, b, c (Å) | 9.419 (3), 10.443 (3), 25.409 (9) |
β (°) | 97.262 (5) |
V (Å3) | 2479.2 (15) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.26 |
Crystal size (mm) | 0.18 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Rigaku Mercury70 CCD |
Absorption correction | Multi-scan (CrystalClear; Rigaku, 2000) |
Tmin, Tmax | 0.793, 0.866 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9442, 4257, 3894 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.061, 1.07 |
No. of reflections | 4257 |
No. of parameters | 371 |
No. of restraints | 14 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.64, −0.60 |
Absolute structure | Flack (1983), 1408 Friedel pairs |
Absolute structure parameter | 0.00 (3) |
Computer programs: CrystalClear (Rigaku, 2000), CrystalClear, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXTL.
Although dinuclear oxomolybdenum(V) compounds of the chelating ligands ethylenediaminetetraacetate (edta) and propylenediaminetetraacetate (PDTA) were widely studied during the late 1950 s and early 1960 s (Pecsok & Sawyer, 1956; Mitchell & Williams, 1962; Blake et al., 1964), the first such crystal structure of a potassium salt did not appear until 1967 (Haynes & Sawyer, 1967). Structures of sodium salts were reported in 1980 (Kimiko et al., 1980) and 1985 (Hong & Liu, 1985). This paper describes the synthesis of a new compound, trisodium bis(µ2-oxo)-(µ2-propylene-1,2-diaminetetra-acetato)-bis(oxo- molybdenum(V)) chloride hexahydrate, (I).
The asymmetric unit of (I) is shown in Fig. 1. The PDTA ligand coordinates to each Mo atom through two carboxylato-O atoms and an N atom, together with one terminal and two bridging O atoms to complete a distorted octahedral environment. Two terminal oxo ligands lie cis to the bridging oxide. The N atom and carboxlato-O atoms occupy the axial (trans to the terminal O) and equatorial positions, respectively. The short Mo···Mo distance (2.5483 (10) Å) indicates a strong interaction between the two Mo atoms.
As shown in Fig. 2, the [Mo2O4(PDTA)]2- complexes lie in layers parallel to the (001) planes. Between these layers, Na+ cations, Cl- anions and water molecules form a complex network stabilized by O—H···O and O—H···Cl hydrogen bonds (Table 2).