The title compound, (CH
6N
3)
2[Na
2Ni(OH)
6Mo
6O
18]·10H
2O, features inversion-generated hexamolybdonickelate anions (Ni site symmetry
). The anions are linked by octahedrally coordinated Na
+ cations into extended sheets. The guanidinium cations and uncoordinated water molecules link the sheets together
via O—H
O and N—H
O hydrogen bonds to form a three-dimensional network. Two water molecule O atoms have site symmetry 2.
Supporting information
CCDC reference: 629831
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.005 Å
- R factor = 0.023
- wR factor = 0.060
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.09 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.11 Ratio
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B .. O11 .. 2.81 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Bis(guanidinium) hexahydroxooctadecaoxodisodiohexamolybdonickelate decahydrate
top
Crystal data top
(CH6N3)2[Na2Ni(OH)6Mo6O18]·10H2O | F(000) = 2664 |
Mr = 1370.69 | Dx = 2.480 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5347 reflections |
a = 25.2247 (9) Å | θ = 1.8–26.1° |
b = 11.6583 (4) Å | µ = 2.62 mm−1 |
c = 13.7668 (5) Å | T = 293 K |
β = 114.918 (4)° | Prism, green |
V = 3671.6 (3) Å3 | 0.28 × 0.24 × 0.18 mm |
Z = 4 | |
Data collection top
Bruker SMART APEXII CCD area-detector diffractometer | 3557 independent reflections |
Radiation source: fine-focus sealed tube | 3275 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
ω and φ scans | θmax = 26.0°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −31→30 |
Tmin = 0.475, Tmax = 0.630 | k = −14→11 |
9516 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0316P)2 + 13.3478P] where P = (Fo2 + 2Fc2)/3 |
3557 reflections | (Δ/σ)max < 0.001 |
233 parameters | Δρmax = 0.65 e Å−3 |
0 restraints | Δρmin = −0.63 e Å−3 |
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 | |
Ni | 0.7500 | 0.7500 | 0.0000 | 0.01399 (12) | |
Mo1 | 0.875219 (11) | 0.65271 (2) | 0.18571 (2) | 0.01685 (8) | |
Mo2 | 0.627324 (11) | 0.71958 (2) | 0.03086 (2) | 0.01634 (8) | |
Mo3 | 0.752803 (11) | 0.62372 (2) | 0.21791 (2) | 0.01563 (8) | |
Na | 0.83122 (6) | 0.34440 (12) | 0.19303 (11) | 0.0304 (3) | |
O1 | 0.78101 (9) | 0.60580 (18) | 0.08711 (16) | 0.0160 (4) | |
H1 | 0.7719 | 0.5389 | 0.0561 | 0.019* | |
O2 | 0.72033 (9) | 0.78138 (17) | 0.11499 (16) | 0.0151 (4) | |
H2 | 0.7252 | 0.8473 | 0.1452 | 0.018* | |
O3 | 0.83390 (9) | 0.80500 (18) | 0.08610 (17) | 0.0168 (4) | |
H3 | 0.8382 | 0.8667 | 0.1147 | 0.020* | |
O4 | 0.88537 (10) | 0.64101 (18) | 0.05404 (18) | 0.0200 (5) | |
O5 | 0.82963 (10) | 0.69438 (19) | 0.26683 (17) | 0.0191 (4) | |
O6 | 0.77292 (11) | 0.4850 (2) | 0.25988 (19) | 0.0258 (5) | |
O7 | 0.61116 (10) | 0.7807 (2) | 0.12909 (18) | 0.0254 (5) | |
O8 | 0.67600 (9) | 0.59067 (18) | 0.10722 (18) | 0.0195 (4) | |
O9 | 0.89049 (11) | 0.5110 (2) | 0.22220 (19) | 0.0270 (5) | |
O10 | 0.93650 (10) | 0.7243 (2) | 0.26786 (19) | 0.0317 (6) | |
O11 | 0.56614 (11) | 0.6427 (2) | −0.0445 (2) | 0.0301 (6) | |
O12 | 0.73482 (10) | 0.6854 (2) | 0.31356 (18) | 0.0248 (5) | |
OW1 | 0.75490 (12) | 0.3860 (2) | 0.0220 (2) | 0.0315 (6) | |
H1WA | 0.7245 | 0.3661 | 0.0292 | 0.038* | |
H1WB | 0.7474 | 0.3601 | −0.0385 | 0.038* | |
OW2 | 0.65516 (15) | 0.3564 (2) | 0.0716 (2) | 0.0471 (8) | |
H2WA | 0.6636 | 0.4281 | 0.0964 | 0.057* | |
H2WB | 0.6682 | 0.3233 | 0.1355 | 0.057* | |
OW3 | 0.63482 (16) | 0.4915 (3) | 0.2827 (3) | 0.0581 (9) | |
H3WA | 0.6255 | 0.5451 | 0.3154 | 0.070* | |
H3WB | 0.6511 | 0.5313 | 0.2470 | 0.070* | |
OW4 | 0.5000 | 0.4497 (7) | 0.2500 | 0.113 (5) | |
H4W | 0.5300 | 0.4079 | 0.2624 | 0.135* | |
OW5 | 0.5000 | 0.6753 (7) | 0.2500 | 0.142 (4) | |
H5W | 0.4920 | 0.6310 | 0.2969 | 0.171* | |
OW6 | 0.88282 (14) | 0.2150 (3) | 0.1377 (2) | 0.0466 (7) | |
H6WA | 0.9182 | 0.2218 | 0.1812 | 0.056* | |
H6WB | 0.8772 | 0.1987 | 0.0761 | 0.056* | |
N1 | 0.90291 (13) | 0.5722 (3) | 0.4734 (2) | 0.0337 (7) | |
H1A | 0.8817 | 0.6152 | 0.4205 | 0.040* | |
H1B | 0.8887 | 0.5098 | 0.4860 | 0.040* | |
N2 | 0.98862 (15) | 0.5344 (3) | 0.6167 (3) | 0.0459 (9) | |
H2A | 0.9738 | 0.4725 | 0.6286 | 0.055* | |
H2B | 1.0241 | 0.5528 | 0.6577 | 0.055* | |
N3 | 0.97935 (16) | 0.6976 (3) | 0.5166 (3) | 0.0491 (10) | |
H3A | 0.9586 | 0.7413 | 0.4640 | 0.059* | |
H3B | 1.0148 | 0.7161 | 0.5576 | 0.059* | |
C1 | 0.95669 (15) | 0.6017 (3) | 0.5347 (3) | 0.0281 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.0136 (3) | 0.0149 (3) | 0.0125 (3) | 0.0014 (2) | 0.0045 (2) | 0.0013 (2) |
Mo1 | 0.01433 (14) | 0.01939 (14) | 0.01446 (14) | 0.00183 (10) | 0.00376 (10) | 0.00253 (10) |
Mo2 | 0.01388 (14) | 0.01949 (15) | 0.01508 (14) | 0.00034 (10) | 0.00553 (10) | 0.00090 (10) |
Mo3 | 0.01756 (14) | 0.01569 (14) | 0.01377 (14) | 0.00222 (10) | 0.00672 (11) | 0.00250 (10) |
Na | 0.0325 (8) | 0.0282 (7) | 0.0264 (7) | −0.0019 (6) | 0.0084 (6) | 0.0016 (6) |
O1 | 0.0175 (10) | 0.0141 (10) | 0.0152 (10) | 0.0003 (8) | 0.0058 (8) | −0.0017 (8) |
O2 | 0.0172 (11) | 0.0126 (10) | 0.0154 (10) | −0.0005 (8) | 0.0067 (9) | −0.0005 (8) |
O3 | 0.0184 (11) | 0.0142 (10) | 0.0173 (11) | −0.0003 (8) | 0.0070 (9) | −0.0021 (8) |
O4 | 0.0217 (11) | 0.0200 (11) | 0.0196 (11) | 0.0070 (9) | 0.0100 (9) | 0.0030 (9) |
O5 | 0.0207 (11) | 0.0219 (11) | 0.0133 (10) | −0.0001 (9) | 0.0058 (9) | −0.0012 (9) |
O6 | 0.0285 (13) | 0.0205 (12) | 0.0287 (13) | 0.0032 (10) | 0.0124 (11) | 0.0078 (10) |
O7 | 0.0236 (12) | 0.0325 (14) | 0.0225 (12) | 0.0035 (10) | 0.0122 (10) | 0.0013 (10) |
O8 | 0.0191 (11) | 0.0167 (11) | 0.0213 (11) | −0.0020 (9) | 0.0072 (9) | 0.0015 (9) |
O9 | 0.0256 (12) | 0.0277 (13) | 0.0268 (12) | 0.0074 (10) | 0.0102 (10) | 0.0085 (10) |
O10 | 0.0217 (13) | 0.0430 (16) | 0.0248 (13) | −0.0074 (11) | 0.0043 (11) | −0.0016 (11) |
O11 | 0.0212 (12) | 0.0355 (14) | 0.0287 (13) | −0.0068 (10) | 0.0055 (10) | −0.0018 (11) |
O12 | 0.0266 (12) | 0.0309 (13) | 0.0191 (12) | 0.0012 (10) | 0.0118 (10) | −0.0006 (10) |
OW1 | 0.0422 (15) | 0.0270 (13) | 0.0240 (13) | −0.0046 (11) | 0.0126 (12) | −0.0063 (10) |
OW2 | 0.072 (2) | 0.0280 (15) | 0.0297 (15) | −0.0036 (14) | 0.0095 (14) | −0.0001 (12) |
OW3 | 0.079 (3) | 0.0401 (18) | 0.065 (2) | −0.0005 (17) | 0.041 (2) | 0.0114 (16) |
OW4 | 0.118 (9) | 0.025 (4) | 0.082 (7) | 0.000 | −0.068 (6) | 0.000 |
OW5 | 0.066 (5) | 0.101 (6) | 0.171 (8) | 0.000 | −0.038 (5) | 0.000 |
OW6 | 0.0470 (18) | 0.056 (2) | 0.0362 (16) | 0.0046 (15) | 0.0169 (14) | −0.0035 (14) |
N1 | 0.0254 (16) | 0.0385 (18) | 0.0276 (16) | −0.0082 (13) | 0.0019 (13) | 0.0100 (14) |
N2 | 0.0307 (18) | 0.062 (2) | 0.0360 (19) | 0.0033 (17) | 0.0055 (15) | 0.0176 (18) |
N3 | 0.036 (2) | 0.052 (2) | 0.051 (2) | −0.0205 (17) | 0.0101 (17) | 0.0080 (18) |
C1 | 0.0232 (17) | 0.040 (2) | 0.0226 (17) | −0.0016 (15) | 0.0110 (14) | −0.0006 (15) |
Geometric parameters (Å, º) top
Ni—O1 | 2.021 (2) | Na—O9 | 2.379 (3) |
Ni—O3 | 2.045 (2) | Na—OW1 | 2.380 (3) |
Ni—O2 | 2.049 (2) | Na—O12ii | 2.468 (3) |
Ni—O1i | 2.021 (2) | Na—O6 | 2.615 (3) |
Ni—O3i | 2.045 (2) | O1—H1 | 0.8723 |
Ni—O2i | 2.049 (2) | O2—H2 | 0.8574 |
Mo1—O10 | 1.701 (2) | O3—H3 | 0.8049 |
Mo1—O9 | 1.723 (2) | OW1—H1WA | 0.8460 |
Mo1—O4 | 1.939 (2) | OW1—H1WB | 0.8295 |
Mo1—O5 | 1.972 (2) | OW2—H2WA | 0.8948 |
Mo1—O3 | 2.217 (2) | OW2—H2WB | 0.8877 |
Mo1—O1 | 2.252 (2) | OW3—H3WA | 0.8583 |
Mo2—O11 | 1.707 (2) | OW3—H3WB | 0.8918 |
Mo2—O7 | 1.723 (2) | OW4—H4W | 0.8542 |
Mo2—O8 | 1.945 (2) | OW5—H5W | 0.9141 |
Mo2—O4i | 1.948 (2) | OW6—H6WA | 0.8430 |
Mo2—O3i | 2.227 (2) | OW6—H6WB | 0.8211 |
Mo2—O2 | 2.253 (2) | N1—C1 | 1.306 (5) |
Mo3—O6 | 1.720 (2) | N1—H1A | 0.8600 |
Mo3—O12 | 1.721 (2) | N1—H1B | 0.8600 |
Mo3—O8 | 1.933 (2) | N2—C1 | 1.331 (5) |
Mo3—O5 | 1.946 (2) | N2—H2A | 0.8600 |
Mo3—O1 | 2.207 (2) | N2—H2B | 0.8600 |
Mo3—O2 | 2.254 (2) | N3—C1 | 1.327 (5) |
Na—OW6 | 2.321 (3) | N3—H3A | 0.8600 |
Na—O7ii | 2.379 (3) | N3—H3B | 0.8600 |
| | | |
O1i—Ni—O1 | 180.0 | OW6—Na—O7ii | 87.20 (11) |
O1i—Ni—O3i | 82.51 (8) | OW6—Na—O9 | 100.76 (11) |
O1—Ni—O3i | 97.49 (8) | O7ii—Na—O9 | 90.75 (9) |
O1i—Ni—O3 | 97.49 (8) | OW6—Na—OW1 | 98.03 (11) |
O1—Ni—O3 | 82.51 (8) | O7ii—Na—OW1 | 166.02 (11) |
O3i—Ni—O3 | 180.0 | O9—Na—OW1 | 100.92 (10) |
O1i—Ni—O2i | 82.31 (8) | OW6—Na—O12ii | 87.87 (11) |
O1—Ni—O2i | 97.69 (8) | O7ii—Na—O12ii | 85.05 (9) |
O3i—Ni—O2i | 97.00 (8) | O9—Na—O12ii | 170.22 (10) |
O3—Ni—O2i | 83.00 (8) | OW1—Na—O12ii | 82.21 (9) |
O1i—Ni—O2 | 97.69 (8) | OW6—Na—O6 | 178.07 (11) |
O1—Ni—O2 | 82.31 (8) | O7ii—Na—O6 | 91.35 (9) |
O3i—Ni—O2 | 83.00 (8) | O9—Na—O6 | 80.53 (9) |
O3—Ni—O2 | 97.00 (8) | OW1—Na—O6 | 83.09 (9) |
O2i—Ni—O2 | 180.0 | O12ii—Na—O6 | 90.73 (9) |
O10—Mo1—O9 | 104.36 (12) | Ni—O1—Mo3 | 103.18 (9) |
O10—Mo1—O4 | 102.42 (11) | Ni—O1—Mo1 | 101.65 (9) |
O9—Mo1—O4 | 95.95 (10) | Mo3—O1—Mo1 | 96.10 (8) |
O10—Mo1—O5 | 94.94 (11) | Ni—O1—H1 | 119.8 |
O9—Mo1—O5 | 100.56 (10) | Mo3—O1—H1 | 112.1 |
O4—Mo1—O5 | 152.24 (9) | Mo1—O1—H1 | 120.3 |
O10—Mo1—O3 | 94.42 (11) | Ni—O2—Mo2 | 100.72 (8) |
O9—Mo1—O3 | 159.65 (10) | Ni—O2—Mo3 | 100.70 (8) |
O4—Mo1—O3 | 72.00 (8) | Mo2—O2—Mo3 | 94.95 (8) |
O5—Mo1—O3 | 85.34 (8) | Ni—O2—H2 | 120.7 |
O10—Mo1—O1 | 162.32 (11) | Mo2—O2—H2 | 116.2 |
O9—Mo1—O1 | 89.56 (10) | Mo3—O2—H2 | 119.1 |
O4—Mo1—O1 | 86.61 (9) | Ni—O3—Mo1 | 102.09 (9) |
O5—Mo1—O1 | 71.46 (8) | Ni—O3—Mo2i | 101.72 (9) |
O3—Mo1—O1 | 73.73 (8) | Mo1—O3—Mo2i | 96.26 (8) |
O11—Mo2—O7 | 104.01 (12) | Ni—O3—H3 | 117.2 |
O11—Mo2—O8 | 97.25 (11) | Mo1—O3—H3 | 118.8 |
O7—Mo2—O8 | 101.53 (10) | Mo2i—O3—H3 | 117.4 |
O11—Mo2—O4i | 101.26 (11) | Mo1—O4—Mo2i | 116.68 (11) |
O7—Mo2—O4i | 95.29 (10) | Mo3—O5—Mo1 | 115.66 (10) |
O8—Mo2—O4i | 151.12 (9) | Mo3—O6—Na | 126.96 (12) |
O11—Mo2—O3i | 93.03 (10) | Mo2—O7—Naiii | 133.87 (13) |
O7—Mo2—O3i | 160.42 (10) | Mo3—O8—Mo2 | 117.83 (11) |
O8—Mo2—O3i | 85.52 (9) | Mo1—O9—Na | 133.33 (13) |
O4i—Mo2—O3i | 71.62 (8) | Mo3—O12—Naiii | 132.64 (13) |
O11—Mo2—O2 | 163.68 (10) | Na—OW1—H1WA | 103.0 |
O7—Mo2—O2 | 90.21 (10) | Na—OW1—H1WB | 131.7 |
O8—Mo2—O2 | 71.68 (8) | H1WA—OW1—H1WB | 100.6 |
O4i—Mo2—O2 | 85.06 (9) | H2WA—OW2—H2WB | 95.6 |
O3i—Mo2—O2 | 74.53 (8) | H3WA—OW3—H3WB | 101.5 |
O6—Mo3—O12 | 105.76 (11) | Na—OW6—H6WA | 106.1 |
O6—Mo3—O8 | 97.66 (11) | Na—OW6—H6WB | 127.7 |
O12—Mo3—O8 | 100.76 (10) | H6WA—OW6—H6WB | 115.3 |
O6—Mo3—O5 | 99.89 (10) | C1—N1—H1A | 120.0 |
O12—Mo3—O5 | 95.93 (10) | C1—N1—H1B | 120.0 |
O8—Mo3—O5 | 151.44 (9) | H1A—N1—H1B | 120.0 |
O6—Mo3—O1 | 91.96 (10) | C1—N2—H2A | 120.0 |
O12—Mo3—O1 | 160.64 (10) | C1—N2—H2B | 120.0 |
O8—Mo3—O1 | 84.18 (9) | H2A—N2—H2B | 120.0 |
O5—Mo3—O1 | 72.91 (8) | C1—N3—H3A | 120.0 |
O6—Mo3—O2 | 162.84 (10) | C1—N3—H3B | 120.0 |
O12—Mo3—O2 | 89.82 (10) | H3A—N3—H3B | 120.0 |
O8—Mo3—O2 | 71.87 (8) | N1—C1—N3 | 120.9 (4) |
O5—Mo3—O2 | 85.27 (8) | N1—C1—N2 | 119.0 (4) |
O1—Mo3—O2 | 73.80 (7) | N3—C1—N2 | 120.1 (4) |
| | | |
O3i—Ni—O1—Mo3 | −81.79 (9) | O10—Mo1—O3—Ni | −167.57 (11) |
O3—Ni—O1—Mo3 | 98.21 (9) | O9—Mo1—O3—Ni | 35.0 (3) |
O2i—Ni—O1—Mo3 | −179.95 (8) | O4—Mo1—O3—Ni | 90.79 (10) |
O2—Ni—O1—Mo3 | 0.05 (8) | O5—Mo1—O3—Ni | −72.96 (9) |
O3i—Ni—O1—Mo1 | 179.02 (8) | O1—Mo1—O3—Ni | −0.93 (7) |
O3—Ni—O1—Mo1 | −0.98 (8) | O10—Mo1—O3—Mo2i | 88.99 (10) |
O2i—Ni—O1—Mo1 | 80.86 (9) | O9—Mo1—O3—Mo2i | −68.4 (3) |
O2—Ni—O1—Mo1 | −99.14 (9) | O4—Mo1—O3—Mo2i | −12.65 (8) |
O6—Mo3—O1—Ni | 170.23 (11) | O5—Mo1—O3—Mo2i | −176.40 (9) |
O12—Mo3—O1—Ni | −33.3 (3) | O1—Mo1—O3—Mo2i | −104.37 (9) |
O8—Mo3—O1—Ni | 72.73 (10) | O10—Mo1—O4—Mo2i | −74.48 (15) |
O5—Mo3—O1—Ni | −90.02 (10) | O9—Mo1—O4—Mo2i | 179.37 (13) |
O2—Mo3—O1—Ni | −0.05 (8) | O5—Mo1—O4—Mo2i | 52.9 (3) |
O6—Mo3—O1—Mo1 | −86.26 (10) | O3—Mo1—O4—Mo2i | 16.17 (11) |
O12—Mo3—O1—Mo1 | 70.2 (3) | O1—Mo1—O4—Mo2i | 90.16 (12) |
O8—Mo3—O1—Mo1 | 176.24 (9) | O6—Mo3—O5—Mo1 | 71.91 (13) |
O5—Mo3—O1—Mo1 | 13.49 (8) | O12—Mo3—O5—Mo1 | 179.09 (12) |
O2—Mo3—O1—Mo1 | 103.46 (8) | O8—Mo3—O5—Mo1 | −55.2 (2) |
O10—Mo1—O1—Ni | 50.3 (4) | O1—Mo3—O5—Mo1 | −17.09 (10) |
O9—Mo1—O1—Ni | −167.28 (11) | O2—Mo3—O5—Mo1 | −91.58 (12) |
O4—Mo1—O1—Ni | −71.29 (9) | O10—Mo1—O5—Mo3 | −174.68 (13) |
O5—Mo1—O1—Ni | 91.42 (10) | O9—Mo1—O5—Mo3 | −69.06 (14) |
O3—Mo1—O1—Ni | 0.94 (7) | O4—Mo1—O5—Mo3 | 56.4 (2) |
O10—Mo1—O1—Mo3 | −54.6 (3) | O3—Mo1—O5—Mo3 | 91.28 (12) |
O9—Mo1—O1—Mo3 | 87.87 (10) | O1—Mo1—O5—Mo3 | 16.88 (10) |
O4—Mo1—O1—Mo3 | −176.14 (9) | O12—Mo3—O6—Na | −163.37 (14) |
O5—Mo1—O1—Mo3 | −13.42 (8) | O8—Mo3—O6—Na | 93.11 (15) |
O3—Mo1—O1—Mo3 | −103.91 (9) | O5—Mo3—O6—Na | −64.26 (16) |
O1i—Ni—O2—Mo2 | 82.76 (9) | O1—Mo3—O6—Na | 8.73 (15) |
O1—Ni—O2—Mo2 | −97.24 (9) | O2—Mo3—O6—Na | 42.1 (4) |
O3i—Ni—O2—Mo2 | 1.34 (8) | O7ii—Na—O6—Mo3 | 137.67 (16) |
O3—Ni—O2—Mo2 | −178.66 (8) | O9—Na—O6—Mo3 | 47.14 (16) |
O1i—Ni—O2—Mo3 | 179.95 (8) | OW1—Na—O6—Mo3 | −55.20 (16) |
O1—Ni—O2—Mo3 | −0.05 (8) | O12ii—Na—O6—Mo3 | −137.26 (16) |
O3i—Ni—O2—Mo3 | 98.53 (9) | O11—Mo2—O7—Naiii | 153.45 (17) |
O3—Ni—O2—Mo3 | −81.47 (9) | O8—Mo2—O7—Naiii | 52.86 (18) |
O11—Mo2—O2—Ni | 40.2 (4) | O4i—Mo2—O7—Naiii | −103.54 (17) |
O7—Mo2—O2—Ni | −168.83 (10) | O3i—Mo2—O7—Naiii | −56.7 (4) |
O8—Mo2—O2—Ni | 89.09 (10) | O2—Mo2—O7—Naiii | −18.48 (17) |
O4i—Mo2—O2—Ni | −73.54 (9) | O6—Mo3—O8—Mo2 | 177.07 (13) |
O3i—Mo2—O2—Ni | −1.26 (8) | O12—Mo3—O8—Mo2 | 69.34 (14) |
O11—Mo2—O2—Mo3 | −61.7 (4) | O5—Mo3—O8—Mo2 | −55.4 (2) |
O7—Mo2—O2—Mo3 | 89.27 (10) | O1—Mo3—O8—Mo2 | −91.74 (12) |
O8—Mo2—O2—Mo3 | −12.81 (8) | O2—Mo3—O8—Mo2 | −16.90 (10) |
O4i—Mo2—O2—Mo3 | −175.44 (9) | O11—Mo2—O8—Mo3 | −175.39 (13) |
O3i—Mo2—O2—Mo3 | −103.16 (8) | O7—Mo2—O8—Mo3 | −69.43 (14) |
O6—Mo3—O2—Ni | −34.8 (4) | O4i—Mo2—O8—Mo3 | 54.9 (2) |
O12—Mo3—O2—Ni | 169.58 (11) | O3i—Mo2—O8—Mo3 | 92.11 (12) |
O8—Mo3—O2—Ni | −89.03 (10) | O2—Mo2—O8—Mo3 | 16.93 (10) |
O5—Mo3—O2—Ni | 73.61 (9) | O10—Mo1—O9—Na | 162.78 (17) |
O1—Mo3—O2—Ni | 0.05 (8) | O4—Mo1—O9—Na | −92.75 (18) |
O6—Mo3—O2—Mo2 | 67.1 (3) | O5—Mo1—O9—Na | 64.84 (18) |
O12—Mo3—O2—Mo2 | −88.52 (10) | O3—Mo1—O9—Na | −40.5 (4) |
O8—Mo3—O2—Mo2 | 12.88 (8) | O1—Mo1—O9—Na | −6.20 (17) |
O5—Mo3—O2—Mo2 | 175.52 (9) | OW6—Na—O9—Mo1 | 132.98 (18) |
O1—Mo3—O2—Mo2 | 101.96 (8) | O7ii—Na—O9—Mo1 | −139.73 (18) |
O1i—Ni—O3—Mo1 | −179.00 (8) | OW1—Na—O9—Mo1 | 32.5 (2) |
O1—Ni—O3—Mo1 | 1.00 (8) | O6—Na—O9—Mo1 | −48.48 (18) |
O2i—Ni—O3—Mo1 | −97.75 (9) | O6—Mo3—O12—Naiii | −153.45 (16) |
O2—Ni—O3—Mo1 | 82.25 (9) | O8—Mo3—O12—Naiii | −52.23 (18) |
O1i—Ni—O3—Mo2i | −79.89 (9) | O5—Mo3—O12—Naiii | 104.50 (17) |
O1—Ni—O3—Mo2i | 100.11 (9) | O1—Mo3—O12—Naiii | 51.0 (4) |
O2i—Ni—O3—Mo2i | 1.36 (8) | O2—Mo3—O12—Naiii | 19.27 (17) |
O2—Ni—O3—Mo2i | −178.64 (8) | | |
Symmetry codes: (i) −x+3/2, −y+3/2, −z; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···OW1 | 0.87 | 1.85 | 2.703 (3) | 167 |
O2—H2···O6iii | 0.86 | 2.06 | 2.896 (3) | 165 |
O3—H3···OW3iii | 0.80 | 1.94 | 2.722 (4) | 164 |
OW1—H1WB···O12iv | 0.83 | 2.00 | 2.822 (3) | 173 |
OW1—H1WA···OW2 | 0.85 | 2.07 | 2.892 (4) | 165 |
OW2—H2WA···O8 | 0.89 | 1.92 | 2.786 (4) | 164 |
OW2—H2WB···O5ii | 0.89 | 2.00 | 2.818 (3) | 152 |
OW3—H3WA···OW6iii | 0.86 | 2.12 | 2.932 (4) | 158 |
OW5—H5W···OW4 | 0.91 | 2.24 | 2.630 (11) | 105 |
OW6—H6WA···OW5ii | 0.84 | 1.95 | 2.736 (4) | 155 |
OW6—H6WB···OW2v | 0.82 | 1.95 | 2.754 (4) | 165 |
OW6—H6WA···OW5vi | 0.84 | 1.95 | 2.736 (4) | 155 |
N1—H1A···O5 | 0.86 | 2.17 | 3.017 (4) | 168 |
N1—H1B···O4vii | 0.86 | 2.01 | 2.832 (4) | 159 |
N2—H2B···O9viii | 0.86 | 2.22 | 2.966 (4) | 145 |
N3—H3B···O7ix | 0.86 | 2.20 | 3.029 (4) | 161 |
N3—H3B···O11ix | 0.86 | 2.81 | 3.243 (4) | 113 |
Symmetry codes: (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x+3/2, −y+1/2, −z; (vi) x+1/2, y−1/2, z; (vii) x, −y+1, z+1/2; (viii) −x+2, −y+1, −z+1; (ix) x+1/2, −y+3/2, z+1/2. |