Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807046612/lh2487sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807046612/lh2487Isup2.hkl |
CCDC reference: 296773
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.018 Å
- Disorder in solvent or counterion
- R factor = 0.043
- wR factor = 0.095
- Data-to-parameter ratio = 15.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor >O2W - >H1W2 ... ? PLAT420_ALERT_2_B D-H Without Acceptor >O5W - >H3W' ... ? PLAT432_ALERT_2_B Short Inter X...Y Contact O16 .. C2 .. 2.85 Ang.
Author Response: The MeOH molecule is disordered over 2 sites (C5S(H3)-O5S-H and C4S(H3)-O4S-H) with the site occupancy factors of 0.5. The short O16 ... C2 contact (also the short contact O16...N5 2.91 Ang.) probably is due to the secondary attractive interaction between the O16 atom and pi-system of the N4(C2-N3)N5 fragment. |
PLAT432_ALERT_2_B Short Inter X...Y Contact O25 .. C5S .. 2.87 Ang.
Author Response: The MeOH molecule is disordered over 2 sites (C5S(H3)-O5S-H and C4S(H3)-O4S-H) with the site occupancy factors of 0.5. The short O16 ... C2 contact (also the short contact O16...N5 2.91 Ang.) probably is due to the secondary attractive interaction between the O16 atom and pi-system of the N4(C2-N3)N5 fragment. |
Alert level C 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 ............ 0.50 Ratio PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 3 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.05 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.60 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 47.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 18 PLAT355_ALERT_3_C Long O-H Bond (0.82A) O1W - H1W1 ... 1.01 Ang. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O1W - H2W1 ... 1.01 Ang. PLAT415_ALERT_2_C Short Inter D-H..H-X H1N2 .. H5SC .. 2.13 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact N2 .. C5S .. 3.03 Ang.
Author Response: The MeOH molecule is disordered over 2 sites (C5S(H3)-O5S-H and C4S(H3)-O4S-H) with the site occupancy factors of 0.5. The short O16 ... C2 contact (also the short contact O16...N5 2.91 Ang.) probably is due to the secondary attractive interaction between the O16 atom and pi-system of the N4(C2-N3)N5 fragment. |
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 42
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 9960 Count of symmetry unique reflns 5312 Completeness (_total/calc) 187.50% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 4648 Fraction of Friedel pairs measured 0.875 Are heavy atom types Z>Si present yes PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 30
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 13 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 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
2-Gb was prepared by the cyclocondensation of cyanoguanidine and o-phenylenediamine according to the method reported by King and co-worker (King, et al., 1948). Synthesis of [2-gbH][H2PMo12O40].2.5CH3OH.4H2O A solution of 2-gb (0.2 g, 1.15 mmol) in 10 ml CH3OH was added dropwise to a solution of H3PMo12O40 (2.1 g, 1.15 mmol) in CH3CN (60 ml) and stirred (1 h). Filtrating, the solution was kept in a beaker. After a few days, the produced solid was recrystallizes in a mixture of CH3OH—H2O—CH2Cl2 (4:1:1). A dark red crystal was obtained with slow evaporation. All mentioned process was done at room temperature. Elemental analysis (%) calcd. for C10.5H30Mo12N5O46.5P: C 5.86, H 1.40, N 3.25; found: C 5.75, H 1.36, N 3.21. 1H NMR (500.13 MHz, [D6]DMSO, 298 K, TMS): 3.16 (s, CH3, 7.5H), 5.12 (b, NH, OH, H+, 18.5H), 7.12–7.71 (m, C6H4, 4H). 13C NMR (125.77 MHz, [D6]DMSO, 298 K, TMS): 159.10, 150.28, 132.31, 123.03, 112.25, 48.72. IR (KBr, cm-1): 3385, 1687, 1621, 1519, 1451, 1056, 955, 873, 790, 610, 588, 491.
There is a high positive residual density of 1.67 e Å-3 near the Mo8 center (distance 0.87%A) due to considerable absorption effects which could not be completely corrected. All solvent molecules were refind in isotropic approximation becouse of high disorder. The hydrogen atoms of NH2, NH and OH groups, and also H atoms of water molecules were found in difference Fourier synthesis, the H(C) atom positions were calculated. All hydrogen atoms were refined in isotropic approximation in riding model with with the Uiso(H) parameters equal to 1.2 Ueq(Ci), for methyl groups equal to 1.5 Ueq(Ci), where U(Ci) are the equivalent thermal parameters of the carbon atoms to which corresponding H atoms are bonded.
Non-covalent forces play a vital role in crystal packing (Du et al., 2005) which are important for material sciences, supramolecular chemistry and biology (Tan et al., 2005; Duarte et al., 2005; Li et al., 2005; Meot-Ner, 2005; Madhu & Das, 2004; Laberge, 1998). In this subject, some discussions carried out on the electrostatic interactions (Liu et al., 2004), symmetrical aspects and the hydrogen bonds functions (Gholivand, et al., 2006). Hence, we study these interactions in a new polyoxometalate (POM)-based organic/inorganic hybrid containing a polyfunctional molecule 2-gb [N-(1H-1,3-benzimidazol-2-yl)guanidine (2-guanidinobenzimidazole)] as the organic component. Due to the importance of crystal engineering in material studies (Batsanov et al., 2006) and the value of material hybrids based on the polyoxometalates, POMs, (Santos, et al., 2005; Ma, et al., 2005; Coronado, et al., 2004; Coronado & Gómez-García, 1998; Zhang, et al., 1997) this investigation may be useful. The basic unit of title hybrid contains asymmetric [H2PMo12O40]- polyoxoanion (Fig. 1) and 2-gbH+ cation (Fig. 2) besides the solvated H2O and CH3OH molecules (5 CH3OH molecules with the site occupancy factor of 0.5 and 4 H2O). Four different kinds of O atoms occur in bifunctional Keggin acid: a) the 12 terminal, b) the 4 bonded to P and Mo, c) the 12 MoO6 octahedra corner-shared and d) the 12 MoO6 octahedra edge-shared. The phosphorus atom has a tetrahedral configuration (O—P—O angles in the range of 109.1 (3)°-109.9 (3)°) and the Mo atoms are distorted octahedral (152.9 (3)°-170.4 (3)° for trans O—Mo—O angles). The P—O bonds are in the range of P—O single bond (Corbridge, 1995), 1.531 (6)–1.550 (6) Å. Five N atoms are in 2-gb and only one is protonatated (guanidine N(3) atom) to form a C8H10N5+ cation, like previous study on [2-gbH]+ACO-.H2O (Andrade-López, et al., 1997). The C(1)—N(1), C(1)—N(2) and C(1)—N(3) bonds, consistent with the guanidine functional group, are not equivalent in title compound. C(1)—N(1) and C(1)—N(2) bond distances are in the range of "one-and a half bonds" which are strengthened versus to these bonds in free ligand (1.311 (13) Å, 1.326 (12) Å in compare with the 1.350 (4) Å and 1.357 (4) Å (Steel, 1991). This is attributed to contribution of nitrogen atoms lone pair in C(1)—N(1) and C(1)—N(2) bonds. This effect causes that the angle N(1)—C(1)—N(2) become greater in the title compound with compare to the corresponding angle in free ligand (121.5 (9) and 117.7 (3)°). C(1)—N(3) is a single bond in POM-based organic/inorganic hybrid, 1.374 (13) Å (versus 1.321 (4) Å in free ligand). In 2-gbH+ cation, the guanidinium residue is twisted from the nearly planar benzimidazole moiety (torsion angles C(1)—N(3)—C(2)—N(4) and C(1)—N(3)—C(2)—N(5) are 38.3 (15)° and -149.1 (9)°, respectively. Various O—H···O and N—H···O hydrogen bonds (Table 1) in the crystal lattice (and also different O···O and N···O electrostatic interactions) lead to a 3-D supramolecular framework. Via the five nitrogen atoms, 2-gbH+ cation is surrounded by three [H2PMo12O40]- anions (with two N—H···O hydrogen bonds and one electrostatic interaction), and three H2O molecules. Figure 3 shows the location of organic cation between three inorganic anions which the interaction of 2-gbH+ with the left anion in figure is an electrostatic interaction. N(2) and N(5) atoms of 2-gbH+ are hydrogen bonded to terminal O(5) and edge-shared O(36) atoms of POMs (N(2)···O(5) = 2.844 (6) Å and (N(5)···O(36) = 2.974 (5) Å). Besides the solvated CH3OH and H2O molecules, the anion is connected to 3 other neighboring anions via the O···O electrostatic interactions and three 2-gbH+ cations (via N···O electrostatic interactions and two N—H···O hydrogen bonds, N(2)—H(2 N2)···O(5) and N(5)—H(1 N5)···O(36). Crystal packing of polyoxoanions and view of the unit cell packing along b crystal axis are shown in Figs. 4 and 5. Some H2O and CH3OH solvated molecules make infinite zigzag belts around the organic cations and the inorganic anions with the sequence of H2O···CH3OH···CH3OH···CH3OH···H2O···H2O···CH3OH··· in the chains (Fig. 6). All solvated H2O (as well as CH3OH) molecules are symmetrically non-equivalent in case of their various interactions with the other components in crystal lattice.
For related literature, see: Andrade-López et al. (1997); Batsanov et al. (2006); Corbridge (1995); Coronado & Gómez-García (1998); Coronado et al. (2004); Du et al. (2005); Duarte et al. (2005); Gholivand et al. (2006); King et al. (1948); Laberge (1998); Li et al. (2005); Liu et al. (2004); Ma et al. (2005); Madhu & Das (2004); Meot-Ner (2005); Santos et al. (2005); Steel (1991); Tan et al. (2005); Zhang et al. (1997).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 1998b); program(s) used to refine structure: SHELXTL (Sheldrick, 1998b); molecular graphics: SHELXTL (Sheldrick, 1998b); software used to prepare material for publication: SHELXTL (Sheldrick, 1998b).
(C8H10N5)[H2PMo12O40]·2.5CH4O·4H2O | F(000) = 2038 |
Mr = 2152.65 | Dx = 2.734 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 7125 reflections |
a = 11.9025 (12) Å | θ = 2.3–30.0° |
b = 18.2497 (19) Å | µ = 2.92 mm−1 |
c = 12.7798 (13) Å | T = 120 K |
β = 109.639 (2)° | Plate, orange |
V = 2614.5 (5) Å3 | 0.40 × 0.30 × 0.15 mm |
Z = 2 |
Bruker SMART 1000 CCD area-detector diffractometer | 9960 independent reflections |
Radiation source: fine-focus sealed tube | 9679 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.093 |
φ and ω scans | θmax = 26.0°, θmin = 2.0° |
Absorption correction: multi scan (SADABS; Sheldrick, 1998a) | h = −14→14 |
Tmin = 0.360, Tmax = 0.648 | k = −22→22 |
22667 measured reflections | l = −15→15 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.043 | H-atom parameters constrained |
wR(F2) = 0.095 | w = 1/[σ2(Fo2) + (0.01P)2 + 25P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.002 |
9960 reflections | Δρmax = 1.68 e Å−3 |
663 parameters | Δρmin = −1.28 e Å−3 |
30 restraints | Absolute structure: Flack (1983), 4793 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (5) |
(C8H10N5)[H2PMo12O40]·2.5CH4O·4H2O | V = 2614.5 (5) Å3 |
Mr = 2152.65 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 11.9025 (12) Å | µ = 2.92 mm−1 |
b = 18.2497 (19) Å | T = 120 K |
c = 12.7798 (13) Å | 0.40 × 0.30 × 0.15 mm |
β = 109.639 (2)° |
Bruker SMART 1000 CCD area-detector diffractometer | 9960 independent reflections |
Absorption correction: multi scan (SADABS; Sheldrick, 1998a) | 9679 reflections with I > 2σ(I) |
Tmin = 0.360, Tmax = 0.648 | Rint = 0.093 |
22667 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | H-atom parameters constrained |
wR(F2) = 0.095 | w = 1/[σ2(Fo2) + (0.01P)2 + 25P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | Δρmax = 1.68 e Å−3 |
9960 reflections | Δρmin = −1.28 e Å−3 |
663 parameters | Absolute structure: Flack (1983), 4793 Friedel pairs |
30 restraints | Absolute structure parameter: 0.04 (5) |
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 | Occ. (<1) | |
Mo1 | 0.43252 (7) | 0.20089 (4) | 0.85557 (6) | 0.01435 (15) | |
Mo2 | 0.29456 (7) | 0.38543 (4) | 0.79544 (6) | 0.01441 (15) | |
Mo3 | 0.21469 (7) | 0.24071 (4) | 0.57690 (6) | 0.01526 (15) | |
Mo4 | 0.79103 (7) | 0.40358 (4) | 0.74839 (6) | 0.01442 (15) | |
Mo5 | 0.71946 (7) | 0.27090 (4) | 0.54842 (6) | 0.01445 (15) | |
Mo6 | 0.58973 (7) | 0.43942 (4) | 0.48978 (6) | 0.01366 (14) | |
Mo7 | 0.72301 (7) | 0.25501 (4) | 0.91725 (6) | 0.01427 (15) | |
Mo8 | 0.59978 (7) | 0.13609 (4) | 0.70229 (6) | 0.01449 (15) | |
Mo9 | 0.40501 (7) | 0.20860 (4) | 0.43064 (6) | 0.01466 (15) | |
Mo10 | 0.27665 (7) | 0.37756 (4) | 0.42193 (6) | 0.01454 (15) | |
Mo11 | 0.40734 (7) | 0.50829 (4) | 0.65420 (6) | 0.01382 (15) | |
Mo12 | 0.58664 (7) | 0.44000 (4) | 0.90565 (6) | 0.01383 (15) | |
P1 | 0.5035 (2) | 0.32237 (12) | 0.67082 (18) | 0.0125 (4) | |
O1 | 0.3700 (6) | 0.1488 (3) | 0.9304 (5) | 0.0212 (14) | |
O2 | 0.1919 (6) | 0.3958 (4) | 0.8580 (6) | 0.0235 (14) | |
H2 | 0.1091 | 0.4047 | 0.8463 | 0.028* | |
O3 | 0.0785 (6) | 0.2075 (4) | 0.5587 (5) | 0.0219 (13) | |
O4 | 0.9269 (6) | 0.4366 (4) | 0.8110 (5) | 0.0204 (13) | |
O5 | 0.8004 (6) | 0.2308 (3) | 0.4782 (5) | 0.0193 (13) | |
O6 | 0.6060 (6) | 0.5045 (3) | 0.4042 (5) | 0.0195 (13) | |
O7 | 0.8325 (6) | 0.2428 (4) | 1.0398 (5) | 0.0210 (13) | |
O8 | 0.6548 (6) | 0.0528 (3) | 0.6932 (5) | 0.0191 (13) | |
H8 | 0.6864 | 0.0087 | 0.7330 | 0.023* | |
O9 | 0.3830 (6) | 0.1458 (3) | 0.3299 (5) | 0.0196 (13) | |
O10 | 0.1877 (6) | 0.4178 (3) | 0.3061 (5) | 0.0198 (13) | |
O11 | 0.3516 (6) | 0.5925 (3) | 0.6152 (5) | 0.0177 (13) | |
O12 | 0.6546 (6) | 0.4913 (3) | 1.0182 (5) | 0.0208 (14) | |
O13 | 0.3113 (6) | 0.1953 (3) | 0.7048 (5) | 0.0171 (12) | |
O14 | 0.2217 (6) | 0.3266 (3) | 0.6772 (5) | 0.0181 (13) | |
O15 | 0.3744 (6) | 0.2915 (3) | 0.8642 (5) | 0.0174 (13) | |
O16 | 0.5853 (6) | 0.2139 (3) | 0.9549 (5) | 0.0160 (12) | |
O17 | 0.5052 (6) | 0.1198 (3) | 0.7902 (5) | 0.0196 (13) | |
O18 | 0.5455 (5) | 0.2576 (3) | 0.7507 (4) | 0.0128 (11) | |
O19 | 0.2874 (6) | 0.4727 (4) | 0.7224 (5) | 0.0181 (13) | |
O20 | 0.4358 (5) | 0.4269 (3) | 0.9164 (5) | 0.0162 (12) | |
O21 | 0.4655 (6) | 0.3861 (3) | 0.7320 (5) | 0.0172 (12) | |
O22 | 0.1704 (6) | 0.3195 (3) | 0.4620 (5) | 0.0200 (13) | |
O23 | 0.2627 (6) | 0.1859 (3) | 0.4784 (5) | 0.0185 (13) | |
O24 | 0.3967 (5) | 0.2980 (3) | 0.5699 (5) | 0.0127 (11) | |
O25 | 0.7379 (6) | 0.4606 (3) | 0.6209 (5) | 0.0201 (14) | |
O26 | 0.8308 (5) | 0.3270 (3) | 0.6541 (5) | 0.0161 (12) | |
O27 | 0.6750 (6) | 0.3628 (4) | 0.4582 (5) | 0.0187 (13) | |
O28 | 0.6055 (6) | 0.3479 (3) | 0.6309 (5) | 0.0152 (12) | |
O29 | 0.4402 (6) | 0.4037 (3) | 0.4229 (5) | 0.0159 (12) | |
O30 | 0.5173 (5) | 0.4958 (3) | 0.5852 (5) | 0.0152 (12) | |
O31 | 0.6474 (6) | 0.3495 (3) | 0.9459 (5) | 0.0162 (12) | |
O32 | 0.7266 (6) | 0.1693 (3) | 0.8436 (5) | 0.0168 (12) | |
O33 | 0.4851 (6) | 0.1510 (3) | 0.5694 (5) | 0.0184 (13) | |
O34 | 0.3147 (6) | 0.2853 (3) | 0.3528 (5) | 0.0153 (12) | |
O35 | 0.3003 (5) | 0.4467 (3) | 0.5275 (5) | 0.0171 (12) | |
O36 | 0.5083 (5) | 0.5228 (3) | 0.7980 (5) | 0.0143 (12) | |
O37 | 0.7012 (6) | 0.1992 (3) | 0.6402 (5) | 0.0170 (12) | |
O38 | 0.7906 (6) | 0.3159 (3) | 0.8407 (5) | 0.0170 (13) | |
O39 | 0.5529 (6) | 0.2441 (3) | 0.4510 (5) | 0.0163 (12) | |
O40 | 0.7004 (6) | 0.4458 (3) | 0.8223 (5) | 0.0165 (12) | |
N1 | 0.9071 (9) | 0.0675 (6) | 0.2019 (8) | 0.037 (2) | |
H1N1 | 0.9820 | 0.0576 | 0.2403 | 0.045* | |
H2N1 | 0.8735 | 0.0479 | 0.1358 | 0.045* | |
N2 | 0.8895 (8) | 0.1424 (5) | 0.3404 (7) | 0.031 (2) | |
H1N2 | 0.9642 | 0.1337 | 0.3812 | 0.037* | |
H2N2 | 0.8454 | 0.1715 | 0.3654 | 0.037* | |
N3 | 0.7277 (7) | 0.1256 (4) | 0.1769 (6) | 0.0232 (17) | |
H1N3 | 0.6929 | 0.0937 | 0.1218 | 0.028* | |
N4 | 0.6957 (8) | 0.2533 (4) | 0.2111 (6) | 0.0218 (17) | |
N5 | 0.5432 (7) | 0.1773 (4) | 0.1600 (6) | 0.0209 (16) | |
H1N5 | 0.4994 | 0.1365 | 0.1365 | 0.025* | |
C1 | 0.8436 (9) | 0.1112 (5) | 0.2414 (7) | 0.0202 (19) | |
C2 | 0.6601 (10) | 0.1846 (5) | 0.1869 (8) | 0.024 (2) | |
C3 | 0.5923 (10) | 0.2948 (6) | 0.1954 (8) | 0.026 (2) | |
C4 | 0.5792 (11) | 0.3697 (6) | 0.2064 (8) | 0.030 (2) | |
H4A | 0.6456 | 0.4020 | 0.2292 | 0.035* | |
C5 | 0.4617 (12) | 0.3947 (7) | 0.1817 (9) | 0.039 (3) | |
H5A | 0.4483 | 0.4453 | 0.1904 | 0.047* | |
C6 | 0.3656 (11) | 0.3484 (7) | 0.1452 (8) | 0.035 (3) | |
H6A | 0.2874 | 0.3679 | 0.1273 | 0.042* | |
C7 | 0.3799 (10) | 0.2729 (6) | 0.1339 (8) | 0.030 (2) | |
H7A | 0.3137 | 0.2405 | 0.1085 | 0.036* | |
C8 | 0.4950 (11) | 0.2487 (6) | 0.1618 (7) | 0.029 (2) | |
C1S | 1.0586 (16) | 0.2459 (9) | 0.8299 (15) | 0.020 (4)* | 0.50 |
H1SA | 1.1420 | 0.2358 | 0.8472 | 0.030* | 0.50 |
H1SB | 1.0222 | 0.2526 | 0.7512 | 0.030* | 0.50 |
H1SC | 1.0490 | 0.2896 | 0.8678 | 0.030* | 0.50 |
O1S | 1.0024 (16) | 0.1884 (9) | 0.8658 (15) | 0.047 (4)* | 0.50 |
H1OS | 0.9192 | 0.1978 | 0.8447 | 0.056* | 0.50 |
C2S | −0.0769 (16) | 0.0770 (12) | 0.6403 (14) | 0.025 (4)* | 0.50 |
H2SA | −0.1509 | 0.0934 | 0.6470 | 0.038* | 0.50 |
H2SB | −0.0613 | 0.1038 | 0.5821 | 0.038* | 0.50 |
H2SC | −0.0822 | 0.0256 | 0.6230 | 0.038* | 0.50 |
O2S | 0.0166 (16) | 0.0863 (12) | 0.7421 (14) | 0.060 (5)* | 0.50 |
H2OS | 0.0795 | 0.0575 | 0.7917 | 0.072* | 0.50 |
C3S | 0.1712 (15) | 0.0995 (9) | 0.0969 (15) | 0.019 (4)* | 0.50 |
H3SA | 0.1753 | 0.0723 | 0.0340 | 0.029* | 0.50 |
H3SB | 0.2494 | 0.1169 | 0.1395 | 0.029* | 0.50 |
H3SC | 0.1420 | 0.0683 | 0.1425 | 0.029* | 0.50 |
O3S | 0.0958 (16) | 0.1602 (9) | 0.0616 (16) | 0.051 (5)* | 0.50 |
H3OS | 0.0227 | 0.1411 | 0.0106 | 0.061* | 0.50 |
C4S | 0.984 (2) | 0.4172 (16) | 0.5329 (17) | 0.048 (6)* | 0.50 |
H4SA | 1.0535 | 0.4337 | 0.5179 | 0.072* | 0.50 |
H4SB | 0.9639 | 0.4520 | 0.5803 | 0.072* | 0.50 |
H4SC | 0.9996 | 0.3704 | 0.5691 | 0.072* | 0.50 |
O4S | 0.8901 (16) | 0.4078 (10) | 0.4337 (14) | 0.047 (4)* | 0.50 |
H4OS | 0.8047 | 0.4067 | 0.4131 | 0.057* | 0.50 |
C5S | 0.915 (3) | 0.5326 (15) | 0.551 (2) | 0.057 (7)* | 0.50 |
H5SA | 0.8527 | 0.4976 | 0.5188 | 0.086* | 0.50 |
H5SB | 0.9879 | 0.5072 | 0.5894 | 0.086* | 0.50 |
H5SC | 0.9257 | 0.5629 | 0.4941 | 0.086* | 0.50 |
O5S | 0.8835 (14) | 0.5782 (9) | 0.6248 (12) | 0.034 (3)* | 0.50 |
H5OS | 0.8259 | 0.5950 | 0.6568 | 0.041* | 0.50 |
O1W | 0.6451 (6) | 0.0420 (4) | −0.0092 (5) | 0.0226 (14)* | |
H1W1 | 0.5992 | −0.0050 | −0.0125 | 0.027* | |
H2W1 | 0.7186 | 0.0299 | −0.0284 | 0.027* | |
O2W | 0.9124 (9) | 0.3210 (5) | 0.2657 (8) | 0.025 (2)* | 0.70 |
H2W2 | 0.8450 | 0.2856 | 0.2586 | 0.030* | 0.70 |
H1W2 | 0.8814 | 0.3652 | 0.2169 | 0.030* | 0.70 |
O2W' | 0.903 (3) | 0.3913 (17) | 0.181 (2) | 0.045 (7)* | 0.30 |
H1W' | 0.9349 | 0.3825 | 0.1186 | 0.054* | 0.30 |
H2W' | 0.8386 | 0.4299 | 0.1696 | 0.054* | 0.30 |
O3W | 0.0782 (14) | 0.2291 (9) | 0.2349 (13) | 0.035 (4)* | 0.50 |
H1W3 | 0.0989 | 0.2672 | 0.1870 | 0.042* | 0.50 |
H2W3 | 0.0992 | 0.1797 | 0.2111 | 0.042* | 0.50 |
O4W | 0.2188 (17) | 0.0358 (10) | 0.7131 (15) | 0.045 (4)* | 0.50 |
H1W4 | 0.2638 | 0.0604 | 0.6685 | 0.054* | 0.50 |
H2W4 | 0.1340 | 0.0496 | 0.7044 | 0.054* | 0.50 |
O5W | 0.1067 (17) | 0.5645 (11) | 0.0276 (15) | 0.062 (4)* | 0.60 |
H3W' | 0.0623 | 0.5277 | 0.0581 | 0.074* | 0.60 |
H4W' | 0.1503 | 0.6060 | 0.0767 | 0.074* | 0.60 |
O5W' | 0.128 (3) | 0.5022 (17) | 0.058 (2) | 0.066 (7)* | 0.40 |
H5W' | 0.0630 | 0.4744 | 0.0765 | 0.079* | 0.40 |
H6W' | 0.1389 | 0.5414 | 0.1171 | 0.079* | 0.40 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0219 (4) | 0.0110 (3) | 0.0092 (3) | −0.0009 (3) | 0.0040 (3) | 0.0010 (3) |
Mo2 | 0.0199 (4) | 0.0123 (3) | 0.0111 (3) | 0.0000 (3) | 0.0054 (3) | −0.0001 (3) |
Mo3 | 0.0195 (4) | 0.0133 (3) | 0.0109 (3) | −0.0019 (3) | 0.0023 (3) | −0.0005 (3) |
Mo4 | 0.0183 (4) | 0.0125 (3) | 0.0111 (3) | −0.0016 (3) | 0.0032 (3) | −0.0009 (3) |
Mo5 | 0.0212 (4) | 0.0117 (3) | 0.0105 (3) | 0.0022 (3) | 0.0054 (3) | 0.0002 (3) |
Mo6 | 0.0211 (4) | 0.0098 (3) | 0.0102 (3) | 0.0008 (3) | 0.0055 (3) | 0.0015 (3) |
Mo7 | 0.0203 (4) | 0.0118 (3) | 0.0086 (3) | 0.0001 (3) | 0.0021 (3) | 0.0003 (3) |
Mo8 | 0.0230 (4) | 0.0091 (3) | 0.0095 (3) | 0.0007 (3) | 0.0031 (3) | −0.0002 (3) |
Mo9 | 0.0226 (4) | 0.0112 (3) | 0.0080 (3) | 0.0006 (3) | 0.0023 (3) | −0.0012 (3) |
Mo10 | 0.0203 (4) | 0.0120 (3) | 0.0086 (3) | 0.0017 (3) | 0.0011 (3) | 0.0004 (3) |
Mo11 | 0.0204 (4) | 0.0093 (3) | 0.0112 (3) | 0.0007 (3) | 0.0046 (3) | −0.0001 (3) |
Mo12 | 0.0214 (4) | 0.0103 (3) | 0.0089 (3) | −0.0007 (3) | 0.0039 (3) | −0.0024 (3) |
P1 | 0.0203 (10) | 0.0080 (9) | 0.0081 (8) | 0.0004 (8) | 0.0036 (8) | −0.0010 (7) |
O1 | 0.030 (4) | 0.017 (3) | 0.019 (3) | −0.007 (3) | 0.012 (3) | 0.002 (3) |
O2 | 0.028 (3) | 0.020 (3) | 0.025 (3) | 0.000 (3) | 0.012 (3) | 0.001 (3) |
O3 | 0.025 (3) | 0.020 (3) | 0.020 (3) | −0.005 (3) | 0.006 (3) | −0.001 (3) |
O4 | 0.025 (3) | 0.015 (3) | 0.020 (3) | 0.000 (3) | 0.005 (3) | 0.002 (3) |
O5 | 0.025 (3) | 0.019 (3) | 0.017 (3) | 0.005 (3) | 0.010 (3) | −0.004 (2) |
O6 | 0.032 (4) | 0.012 (3) | 0.015 (3) | 0.005 (3) | 0.010 (3) | 0.005 (2) |
O7 | 0.029 (3) | 0.017 (3) | 0.011 (3) | 0.000 (3) | 0.000 (3) | −0.006 (2) |
O8 | 0.028 (3) | 0.011 (3) | 0.018 (3) | 0.006 (3) | 0.007 (3) | 0.004 (2) |
O9 | 0.029 (3) | 0.015 (3) | 0.013 (3) | 0.001 (3) | 0.005 (3) | 0.001 (2) |
O10 | 0.028 (3) | 0.016 (3) | 0.009 (3) | 0.003 (3) | −0.001 (3) | 0.004 (2) |
O11 | 0.027 (3) | 0.010 (3) | 0.015 (3) | 0.001 (2) | 0.007 (3) | 0.004 (2) |
O12 | 0.036 (4) | 0.011 (3) | 0.011 (3) | −0.006 (3) | 0.003 (3) | −0.005 (2) |
O13 | 0.023 (3) | 0.012 (3) | 0.013 (3) | −0.003 (3) | 0.001 (2) | 0.000 (2) |
O14 | 0.021 (3) | 0.017 (3) | 0.013 (3) | −0.002 (3) | 0.002 (3) | 0.005 (2) |
O15 | 0.026 (3) | 0.013 (3) | 0.012 (3) | 0.005 (3) | 0.005 (3) | 0.000 (2) |
O16 | 0.030 (3) | 0.012 (3) | 0.006 (3) | −0.003 (3) | 0.006 (2) | 0.002 (2) |
O17 | 0.032 (4) | 0.010 (3) | 0.015 (3) | −0.002 (3) | 0.007 (3) | 0.003 (2) |
O18 | 0.014 (3) | 0.014 (3) | 0.008 (2) | −0.001 (2) | 0.000 (2) | −0.002 (2) |
O19 | 0.022 (3) | 0.020 (3) | 0.013 (3) | 0.002 (3) | 0.008 (3) | 0.001 (2) |
O20 | 0.022 (3) | 0.019 (3) | 0.007 (3) | 0.000 (3) | 0.003 (2) | 0.001 (2) |
O21 | 0.029 (3) | 0.008 (3) | 0.014 (3) | −0.001 (2) | 0.007 (3) | −0.001 (2) |
O22 | 0.029 (3) | 0.016 (3) | 0.017 (3) | 0.000 (3) | 0.011 (3) | 0.001 (2) |
O23 | 0.028 (3) | 0.013 (3) | 0.015 (3) | 0.000 (3) | 0.007 (3) | 0.000 (2) |
O24 | 0.017 (3) | 0.010 (3) | 0.008 (3) | 0.002 (2) | −0.001 (2) | 0.000 (2) |
O25 | 0.034 (4) | 0.012 (3) | 0.021 (3) | 0.000 (3) | 0.018 (3) | 0.003 (2) |
O26 | 0.016 (3) | 0.016 (3) | 0.017 (3) | 0.001 (2) | 0.005 (3) | −0.001 (2) |
O27 | 0.028 (3) | 0.019 (3) | 0.008 (3) | 0.002 (3) | 0.005 (2) | −0.003 (2) |
O28 | 0.024 (3) | 0.008 (3) | 0.009 (3) | 0.001 (2) | −0.001 (2) | −0.003 (2) |
O29 | 0.028 (3) | 0.011 (3) | 0.011 (3) | 0.001 (3) | 0.009 (3) | 0.002 (2) |
O30 | 0.021 (3) | 0.017 (3) | 0.008 (3) | 0.002 (2) | 0.004 (2) | 0.002 (2) |
O31 | 0.023 (3) | 0.010 (3) | 0.013 (3) | 0.002 (2) | 0.001 (3) | 0.003 (2) |
O32 | 0.021 (3) | 0.014 (3) | 0.014 (3) | 0.010 (2) | 0.004 (3) | 0.005 (2) |
O33 | 0.024 (3) | 0.014 (3) | 0.017 (3) | −0.001 (3) | 0.007 (3) | −0.003 (2) |
O34 | 0.022 (3) | 0.012 (3) | 0.008 (3) | −0.001 (2) | 0.000 (2) | −0.002 (2) |
O35 | 0.020 (3) | 0.016 (3) | 0.015 (3) | 0.003 (3) | 0.006 (3) | 0.004 (2) |
O36 | 0.018 (3) | 0.010 (3) | 0.015 (3) | −0.001 (2) | 0.006 (2) | 0.000 (2) |
O37 | 0.022 (3) | 0.017 (3) | 0.009 (3) | 0.004 (3) | 0.002 (2) | 0.001 (2) |
O38 | 0.022 (3) | 0.017 (3) | 0.013 (3) | 0.005 (3) | 0.006 (3) | 0.006 (2) |
O39 | 0.020 (3) | 0.015 (3) | 0.009 (3) | 0.001 (2) | −0.002 (2) | −0.002 (2) |
O40 | 0.023 (3) | 0.015 (3) | 0.011 (3) | 0.003 (3) | 0.005 (2) | 0.000 (2) |
N1 | 0.031 (5) | 0.047 (6) | 0.037 (5) | −0.006 (4) | 0.015 (4) | −0.021 (5) |
N2 | 0.025 (4) | 0.039 (5) | 0.025 (4) | 0.008 (4) | 0.004 (4) | −0.014 (4) |
N3 | 0.031 (4) | 0.023 (4) | 0.013 (4) | 0.008 (4) | 0.003 (3) | 0.001 (3) |
N4 | 0.040 (5) | 0.008 (3) | 0.015 (4) | 0.001 (3) | 0.006 (3) | −0.002 (3) |
N5 | 0.021 (4) | 0.023 (4) | 0.011 (4) | −0.007 (3) | −0.003 (3) | −0.005 (3) |
C1 | 0.028 (4) | 0.024 (4) | 0.010 (4) | −0.009 (3) | 0.008 (3) | −0.008 (3) |
C2 | 0.044 (6) | 0.017 (5) | 0.018 (4) | 0.000 (4) | 0.020 (4) | 0.002 (4) |
C3 | 0.049 (6) | 0.021 (5) | 0.012 (4) | −0.006 (4) | 0.015 (4) | −0.001 (4) |
C4 | 0.049 (6) | 0.026 (5) | 0.014 (4) | 0.004 (5) | 0.011 (4) | 0.005 (4) |
C5 | 0.064 (6) | 0.034 (5) | 0.020 (4) | 0.014 (5) | 0.015 (4) | 0.007 (4) |
C6 | 0.040 (5) | 0.047 (5) | 0.017 (4) | 0.012 (4) | 0.009 (4) | 0.004 (4) |
C7 | 0.037 (6) | 0.037 (6) | 0.014 (4) | 0.011 (5) | 0.006 (4) | 0.006 (4) |
C8 | 0.052 (7) | 0.026 (5) | 0.011 (4) | −0.003 (5) | 0.014 (4) | 0.003 (4) |
Mo1—O1 | 1.689 (6) | P1—O18 | 1.531 (6) |
Mo1—O15 | 1.811 (6) | P1—O28 | 1.539 (7) |
Mo1—O16 | 1.850 (6) | P1—O24 | 1.541 (6) |
Mo1—O13 | 1.984 (6) | P1—O21 | 1.550 (6) |
Mo1—O17 | 2.030 (6) | O2—H2 | 0.9600 |
Mo1—O18 | 2.427 (6) | O8—H8 | 0.9601 |
Mo2—O2 | 1.680 (6) | N1—C1 | 1.311 (13) |
Mo2—O14 | 1.818 (6) | N1—H1N1 | 0.8803 |
Mo2—O19 | 1.833 (6) | N1—H2N1 | 0.8798 |
Mo2—O20 | 2.010 (6) | N2—C1 | 1.326 (12) |
Mo2—O15 | 2.012 (6) | N2—H1N2 | 0.8799 |
Mo2—O21 | 2.431 (6) | N2—H2N2 | 0.8799 |
Mo3—O3 | 1.672 (7) | N3—C1 | 1.374 (13) |
Mo3—O23 | 1.843 (6) | N3—C2 | 1.375 (12) |
Mo3—O13 | 1.848 (6) | N3—H1N3 | 0.8999 |
Mo3—O22 | 1.995 (6) | N4—C2 | 1.327 (12) |
Mo3—O14 | 2.009 (6) | N4—C3 | 1.401 (14) |
Mo3—O24 | 2.434 (6) | N5—C2 | 1.324 (14) |
Mo4—O4 | 1.658 (7) | N5—C8 | 1.426 (14) |
Mo4—O40 | 1.826 (6) | N5—H1N5 | 0.9011 |
Mo4—O25 | 1.856 (6) | C3—C8 | 1.378 (15) |
Mo4—O38 | 1.989 (6) | C3—C4 | 1.388 (15) |
Mo4—O26 | 2.004 (6) | C4—C5 | 1.402 (17) |
Mo4—O28 | 2.436 (6) | C4—H4A | 0.9500 |
Mo5—O5 | 1.688 (6) | C5—C6 | 1.372 (18) |
Mo5—O37 | 1.818 (6) | C5—H5A | 0.9500 |
Mo5—O26 | 1.851 (6) | C6—C7 | 1.401 (17) |
Mo5—O27 | 2.003 (6) | C6—H6A | 0.9500 |
Mo5—O39 | 2.015 (6) | C7—C8 | 1.368 (16) |
Mo5—O28 | 2.426 (6) | C7—H7A | 0.9500 |
Mo6—O6 | 1.670 (6) | C1S—O1S | 1.402 (10) |
Mo6—O29 | 1.816 (6) | C1S—H1SA | 0.9598 |
Mo6—O27 | 1.850 (6) | C1S—H1SB | 0.9603 |
Mo6—O30 | 1.998 (6) | C1S—H1SC | 0.9601 |
Mo6—O25 | 2.021 (7) | O1S—H1OS | 0.9499 |
Mo6—O28 | 2.419 (6) | C2S—O2S | 1.410 (10) |
Mo7—O7 | 1.682 (6) | C2S—H2SA | 0.9605 |
Mo7—O32 | 1.834 (6) | C2S—H2SB | 0.9601 |
Mo7—O38 | 1.835 (6) | C2S—H2SC | 0.9596 |
Mo7—O16 | 2.003 (6) | O2S—H2OS | 0.9598 |
Mo7—O31 | 2.035 (6) | C3S—O3S | 1.401 (10) |
Mo7—O18 | 2.444 (6) | C3S—H3SA | 0.9601 |
Mo8—O8 | 1.674 (6) | C3S—H3SB | 0.9602 |
Mo8—O33 | 1.806 (6) | C3S—H3SC | 0.9596 |
Mo8—O17 | 1.862 (6) | O3S—H3OS | 0.9598 |
Mo8—O37 | 2.015 (6) | C4S—O4S | 1.390 (10) |
Mo8—O32 | 2.018 (6) | C4S—H4SA | 0.9599 |
Mo8—O18 | 2.447 (6) | C4S—H4SB | 0.9601 |
Mo9—O9 | 1.677 (6) | C4S—H4SC | 0.9600 |
Mo9—O39 | 1.810 (6) | O4S—H4OS | 0.9599 |
Mo9—O34 | 1.840 (6) | C5S—O5S | 1.395 (10) |
Mo9—O33 | 2.006 (6) | C5S—H5SA | 0.9600 |
Mo9—O23 | 2.026 (6) | C5S—H5SB | 0.9601 |
Mo9—O24 | 2.440 (6) | C5S—H5SC | 0.9600 |
Mo10—O10 | 1.673 (6) | O5S—H5OS | 0.9599 |
Mo10—O35 | 1.799 (6) | O1W—H1W1 | 1.0101 |
Mo10—O22 | 1.849 (6) | O1W—H2W1 | 1.0095 |
Mo10—O29 | 2.001 (6) | O2W—H2W2 | 1.0101 |
Mo10—O34 | 2.023 (6) | O2W—H1W2 | 1.0101 |
Mo10—O24 | 2.431 (6) | O2W'—H1W2 | 0.7595 |
Mo11—O11 | 1.681 (6) | O2W'—H1W' | 1.0098 |
Mo11—O30 | 1.822 (6) | O2W'—H2W' | 1.0102 |
Mo11—O36 | 1.845 (6) | O3W—H1W3 | 1.0099 |
Mo11—O19 | 2.014 (6) | O3W—H2W3 | 1.0099 |
Mo11—O35 | 2.030 (6) | O4W—H1W4 | 1.0099 |
Mo11—O21 | 2.446 (6) | O4W—H2W4 | 1.0100 |
Mo12—O12 | 1.679 (6) | O5W—H3W' | 1.0097 |
Mo12—O31 | 1.806 (6) | O5W—H4W' | 1.0102 |
Mo12—O20 | 1.862 (6) | O5W—H6W' | 1.1570 |
Mo12—O40 | 1.987 (6) | O5W'—H3W' | 0.9128 |
Mo12—O36 | 2.046 (6) | O5W'—H5W' | 1.0200 |
Mo12—O21 | 2.413 (6) | O5W'—H6W' | 1.0201 |
O1—Mo1—O15 | 103.3 (3) | O36—Mo11—O21 | 74.1 (2) |
O1—Mo1—O16 | 101.7 (3) | O19—Mo11—O21 | 71.0 (2) |
O15—Mo1—O16 | 98.5 (3) | O35—Mo11—O21 | 80.5 (2) |
O1—Mo1—O13 | 101.9 (3) | O12—Mo12—O31 | 103.6 (3) |
O15—Mo1—O13 | 86.4 (3) | O12—Mo12—O20 | 102.0 (3) |
O16—Mo1—O13 | 154.1 (3) | O31—Mo12—O20 | 99.5 (3) |
O1—Mo1—O17 | 98.8 (3) | O12—Mo12—O40 | 102.1 (3) |
O15—Mo1—O17 | 156.2 (3) | O31—Mo12—O40 | 85.5 (3) |
O16—Mo1—O17 | 85.4 (3) | O20—Mo12—O40 | 153.4 (3) |
O13—Mo1—O17 | 80.5 (3) | O12—Mo12—O36 | 98.3 (3) |
O1—Mo1—O18 | 170.0 (3) | O31—Mo12—O36 | 156.2 (2) |
O15—Mo1—O18 | 86.4 (2) | O20—Mo12—O36 | 84.9 (2) |
O16—Mo1—O18 | 74.1 (2) | O40—Mo12—O36 | 80.7 (2) |
O13—Mo1—O18 | 80.9 (2) | O12—Mo12—O21 | 169.3 (3) |
O17—Mo1—O18 | 72.1 (2) | O31—Mo12—O21 | 87.0 (2) |
O2—Mo2—O14 | 104.0 (3) | O20—Mo12—O21 | 73.9 (2) |
O2—Mo2—O19 | 103.1 (3) | O40—Mo12—O21 | 80.4 (2) |
O14—Mo2—O19 | 99.3 (3) | O36—Mo12—O21 | 71.7 (2) |
O2—Mo2—O20 | 98.4 (3) | O18—P1—O28 | 109.7 (3) |
O14—Mo2—O20 | 154.6 (3) | O18—P1—O24 | 109.1 (3) |
O19—Mo2—O20 | 87.0 (3) | O28—P1—O24 | 109.3 (3) |
O2—Mo2—O15 | 101.6 (3) | O18—P1—O21 | 109.1 (3) |
O14—Mo2—O15 | 83.3 (3) | O28—P1—O21 | 109.6 (3) |
O19—Mo2—O15 | 153.7 (3) | O24—P1—O21 | 109.9 (3) |
O20—Mo2—O15 | 80.5 (3) | Mo2—O2—H2 | 144.9 |
O2—Mo2—O21 | 169.2 (3) | Mo8—O8—H8 | 144.9 |
O14—Mo2—O21 | 86.8 (2) | Mo3—O13—Mo1 | 150.4 (3) |
O19—Mo2—O21 | 74.1 (2) | Mo2—O14—Mo3 | 153.8 (4) |
O20—Mo2—O21 | 71.2 (2) | Mo1—O15—Mo2 | 152.3 (3) |
O15—Mo2—O21 | 79.9 (2) | Mo1—O16—Mo7 | 125.3 (3) |
O3—Mo3—O23 | 102.6 (3) | Mo8—O17—Mo1 | 124.0 (3) |
O3—Mo3—O13 | 104.3 (3) | P1—O18—Mo1 | 125.5 (3) |
O23—Mo3—O13 | 96.7 (3) | P1—O18—Mo7 | 126.1 (3) |
O3—Mo3—O22 | 98.9 (3) | Mo1—O18—Mo7 | 89.30 (18) |
O23—Mo3—O22 | 87.4 (3) | P1—O18—Mo8 | 125.8 (3) |
O13—Mo3—O22 | 154.9 (3) | Mo1—O18—Mo8 | 89.7 (2) |
O3—Mo3—O14 | 101.7 (3) | Mo7—O18—Mo8 | 88.73 (19) |
O23—Mo3—O14 | 154.6 (3) | Mo2—O19—Mo11 | 125.6 (3) |
O13—Mo3—O14 | 84.6 (3) | Mo12—O20—Mo2 | 124.7 (3) |
O22—Mo3—O14 | 81.4 (2) | P1—O21—Mo12 | 125.8 (4) |
O3—Mo3—O24 | 169.7 (3) | P1—O21—Mo2 | 125.7 (3) |
O23—Mo3—O24 | 73.9 (2) | Mo12—O21—Mo2 | 90.19 (19) |
O13—Mo3—O24 | 85.9 (2) | P1—O21—Mo11 | 124.7 (3) |
O22—Mo3—O24 | 71.4 (2) | Mo12—O21—Mo11 | 90.1 (2) |
O14—Mo3—O24 | 80.9 (2) | Mo2—O21—Mo11 | 89.2 (2) |
O4—Mo4—O40 | 104.3 (3) | Mo10—O22—Mo3 | 125.5 (4) |
O4—Mo4—O25 | 102.1 (3) | Mo3—O23—Mo9 | 125.3 (3) |
O40—Mo4—O25 | 97.5 (3) | P1—O24—Mo10 | 125.6 (3) |
O4—Mo4—O38 | 101.7 (3) | P1—O24—Mo3 | 125.9 (3) |
O40—Mo4—O38 | 85.0 (3) | Mo10—O24—Mo3 | 89.3 (2) |
O25—Mo4—O38 | 154.7 (3) | P1—O24—Mo9 | 125.4 (3) |
O4—Mo4—O26 | 98.9 (3) | Mo10—O24—Mo9 | 89.39 (19) |
O40—Mo4—O26 | 154.9 (3) | Mo3—O24—Mo9 | 89.7 (2) |
O25—Mo4—O26 | 86.7 (3) | Mo4—O25—Mo6 | 124.4 (3) |
O38—Mo4—O26 | 81.0 (2) | Mo5—O26—Mo4 | 124.7 (3) |
O4—Mo4—O28 | 169.8 (3) | Mo6—O27—Mo5 | 124.5 (3) |
O40—Mo4—O28 | 85.7 (2) | P1—O28—Mo6 | 125.7 (3) |
O25—Mo4—O28 | 73.9 (3) | P1—O28—Mo5 | 126.0 (3) |
O38—Mo4—O28 | 81.2 (2) | Mo6—O28—Mo5 | 89.5 (2) |
O26—Mo4—O28 | 71.7 (2) | P1—O28—Mo4 | 125.1 (3) |
O5—Mo5—O37 | 104.1 (3) | Mo6—O28—Mo4 | 89.9 (2) |
O5—Mo5—O26 | 103.3 (3) | Mo5—O28—Mo4 | 89.2 (2) |
O37—Mo5—O26 | 98.0 (3) | Mo6—O29—Mo10 | 152.3 (3) |
O5—Mo5—O27 | 98.3 (3) | Mo11—O30—Mo6 | 152.6 (4) |
O37—Mo5—O27 | 155.2 (3) | Mo12—O31—Mo7 | 151.9 (3) |
O26—Mo5—O27 | 86.7 (3) | Mo7—O32—Mo8 | 125.2 (3) |
O5—Mo5—O39 | 100.7 (3) | Mo8—O33—Mo9 | 153.5 (4) |
O37—Mo5—O39 | 85.3 (3) | Mo9—O34—Mo10 | 124.9 (3) |
O26—Mo5—O39 | 154.1 (3) | Mo10—O35—Mo11 | 152.2 (4) |
O27—Mo5—O39 | 80.4 (3) | Mo11—O36—Mo12 | 124.1 (3) |
O5—Mo5—O28 | 169.8 (3) | Mo5—O37—Mo8 | 152.0 (4) |
O37—Mo5—O28 | 86.1 (2) | Mo7—O38—Mo4 | 153.2 (4) |
O26—Mo5—O28 | 74.4 (2) | Mo9—O39—Mo5 | 152.0 (3) |
O27—Mo5—O28 | 71.7 (2) | Mo4—O40—Mo12 | 151.9 (4) |
O39—Mo5—O28 | 80.3 (2) | C1—N1—H1N1 | 121.2 |
O6—Mo6—O29 | 104.9 (3) | C1—N1—H2N1 | 118.8 |
O6—Mo6—O27 | 101.7 (3) | H1N1—N1—H2N1 | 120.0 |
O29—Mo6—O27 | 98.6 (3) | C1—N2—H1N2 | 119.9 |
O6—Mo6—O30 | 101.7 (3) | C1—N2—H2N2 | 120.1 |
O29—Mo6—O30 | 85.2 (3) | H1N2—N2—H2N2 | 120.0 |
O27—Mo6—O30 | 154.5 (3) | C1—N3—C2 | 126.5 (9) |
O6—Mo6—O25 | 98.4 (3) | C1—N3—H1N3 | 116.8 |
O29—Mo6—O25 | 154.6 (2) | C2—N3—H1N3 | 116.7 |
O27—Mo6—O25 | 86.3 (3) | C2—N4—C3 | 106.3 (9) |
O30—Mo6—O25 | 80.3 (2) | C2—N5—C8 | 107.3 (8) |
O6—Mo6—O28 | 169.4 (3) | C2—N5—H1N5 | 127.5 |
O29—Mo6—O28 | 85.5 (2) | C8—N5—H1N5 | 124.8 |
O27—Mo6—O28 | 74.3 (2) | N1—C1—N2 | 121.5 (9) |
O30—Mo6—O28 | 80.9 (2) | N1—C1—N3 | 118.5 (8) |
O25—Mo6—O28 | 71.7 (2) | N2—C1—N3 | 120.0 (8) |
O7—Mo7—O32 | 102.8 (3) | N5—C2—N4 | 112.4 (9) |
O7—Mo7—O38 | 103.6 (3) | N5—C2—N3 | 119.7 (9) |
O32—Mo7—O38 | 98.8 (3) | N4—C2—N3 | 127.6 (10) |
O7—Mo7—O16 | 99.6 (3) | C8—C3—C4 | 121.4 (11) |
O32—Mo7—O16 | 88.0 (3) | C8—C3—N4 | 108.7 (9) |
O38—Mo7—O16 | 153.6 (3) | C4—C3—N4 | 129.9 (10) |
O7—Mo7—O31 | 101.3 (3) | C3—C4—C5 | 115.8 (11) |
O32—Mo7—O31 | 154.6 (3) | C3—C4—H4A | 122.1 |
O38—Mo7—O31 | 83.2 (3) | C5—C4—H4A | 122.1 |
O16—Mo7—O31 | 80.0 (2) | C6—C5—C4 | 122.1 (11) |
O7—Mo7—O18 | 170.4 (3) | C6—C5—H5A | 119.0 |
O32—Mo7—O18 | 74.5 (2) | C4—C5—H5A | 119.0 |
O38—Mo7—O18 | 85.9 (2) | C5—C6—C7 | 121.6 (11) |
O16—Mo7—O18 | 71.3 (2) | C5—C6—H6A | 119.2 |
O31—Mo7—O18 | 80.5 (2) | C7—C6—H6A | 119.2 |
O8—Mo8—O33 | 105.1 (3) | C8—C7—C6 | 115.8 (11) |
O8—Mo8—O17 | 103.1 (3) | C8—C7—H7A | 122.1 |
O33—Mo8—O17 | 99.9 (3) | C6—C7—H7A | 122.1 |
O8—Mo8—O37 | 101.0 (3) | C7—C8—C3 | 123.2 (11) |
O33—Mo8—O37 | 84.7 (3) | C7—C8—N5 | 131.5 (10) |
O17—Mo8—O37 | 153.2 (3) | C3—C8—N5 | 105.2 (9) |
O8—Mo8—O32 | 98.2 (3) | O1S—C1S—H1SA | 110.6 |
O33—Mo8—O32 | 153.8 (3) | O1S—C1S—H1SB | 110.0 |
O17—Mo8—O32 | 86.0 (3) | H1SA—C1S—H1SB | 109.5 |
O37—Mo8—O32 | 79.3 (2) | O1S—C1S—H1SC | 107.8 |
O8—Mo8—O18 | 169.4 (3) | H1SA—C1S—H1SC | 109.5 |
O33—Mo8—O18 | 85.4 (2) | H1SB—C1S—H1SC | 109.5 |
O17—Mo8—O18 | 74.2 (2) | C1S—O1S—H1OS | 109.7 |
O37—Mo8—O18 | 80.0 (2) | O2S—C2S—H2SA | 110.1 |
O32—Mo8—O18 | 71.6 (2) | O2S—C2S—H2SB | 110.8 |
O9—Mo9—O39 | 104.4 (3) | H2SA—C2S—H2SB | 109.4 |
O9—Mo9—O34 | 101.1 (3) | O2S—C2S—H2SC | 107.6 |
O39—Mo9—O34 | 99.7 (3) | H2SA—C2S—H2SC | 109.5 |
O9—Mo9—O33 | 103.1 (3) | H2SB—C2S—H2SC | 109.5 |
O39—Mo9—O33 | 84.8 (3) | C2S—O2S—H2OS | 137.9 |
O34—Mo9—O33 | 153.4 (2) | O3S—C3S—H3SA | 110.3 |
O9—Mo9—O23 | 99.3 (3) | O3S—C3S—H3SB | 108.3 |
O39—Mo9—O23 | 154.2 (3) | H3SA—C3S—H3SB | 109.5 |
O34—Mo9—O23 | 85.6 (3) | O3S—C3S—H3SC | 109.9 |
O33—Mo9—O23 | 79.8 (3) | H3SA—C3S—H3SC | 109.5 |
O9—Mo9—O24 | 169.2 (3) | H3SB—C3S—H3SC | 109.4 |
O39—Mo9—O24 | 86.1 (2) | C3S—O3S—H3OS | 105.6 |
O34—Mo9—O24 | 74.1 (2) | O4S—C4S—H4SA | 109.9 |
O33—Mo9—O24 | 80.2 (2) | O4S—C4S—H4SB | 111.4 |
O23—Mo9—O24 | 71.0 (2) | H4SA—C4S—H4SB | 109.5 |
O10—Mo10—O35 | 104.4 (3) | O4S—C4S—H4SC | 107.2 |
O10—Mo10—O22 | 102.1 (3) | H4SA—C4S—H4SC | 109.5 |
O35—Mo10—O22 | 98.2 (3) | H4SB—C4S—H4SC | 109.5 |
O10—Mo10—O29 | 103.0 (3) | C4S—O4S—H4OS | 134.8 |
O35—Mo10—O29 | 85.5 (3) | O5S—C5S—H4SB | 124.0 |
O22—Mo10—O29 | 152.9 (3) | O5S—C5S—H5SA | 110.3 |
O10—Mo10—O34 | 98.4 (3) | H4SB—C5S—H5SA | 69.7 |
O35—Mo10—O34 | 155.5 (3) | O5S—C5S—H5SB | 110.4 |
O22—Mo10—O34 | 85.3 (3) | H5SA—C5S—H5SB | 109.5 |
O29—Mo10—O34 | 80.9 (2) | O5S—C5S—H5SC | 107.7 |
O10—Mo10—O24 | 169.2 (3) | H4SB—C5S—H5SC | 125.5 |
O35—Mo10—O24 | 86.2 (2) | H5SA—C5S—H5SC | 109.5 |
O22—Mo10—O24 | 73.7 (3) | H5SB—C5S—H5SC | 109.5 |
O29—Mo10—O24 | 79.7 (2) | C5S—O5S—H5OS | 150.4 |
O34—Mo10—O24 | 71.5 (2) | H1W1—O1W—H2W1 | 107.8 |
O11—Mo11—O30 | 104.3 (3) | H2W2—O2W—H1W2 | 109.9 |
O11—Mo11—O36 | 102.9 (3) | H1W2—O2W'—H1W' | 131.8 |
O30—Mo11—O36 | 99.6 (3) | H1W2—O2W'—H2W' | 97.0 |
O11—Mo11—O19 | 99.0 (3) | H1W'—O2W'—H2W' | 117.7 |
O30—Mo11—O19 | 153.9 (3) | H1W3—O3W—H2W3 | 107.2 |
O36—Mo11—O19 | 86.2 (3) | H1W4—O4W—H2W4 | 121.8 |
O11—Mo11—O35 | 101.0 (3) | H3W'—O5W—H4W' | 119.0 |
O30—Mo11—O35 | 84.5 (3) | H3W'—O5W—H6W' | 54.4 |
O36—Mo11—O35 | 153.9 (3) | H4W'—O5W—H6W' | 74.3 |
O19—Mo11—O35 | 79.7 (2) | H3W'—O5W'—H5W' | 62.1 |
O11—Mo11—O21 | 169.6 (3) | H3W'—O5W'—H6W' | 62.0 |
O30—Mo11—O21 | 86.0 (2) | H5W'—O5W'—H6W' | 95.1 |
O3—Mo3—O13—Mo1 | −127.8 (7) | O23—Mo9—O24—P1 | 133.8 (4) |
O23—Mo3—O13—Mo1 | 127.4 (7) | O9—Mo9—O24—Mo10 | −65.4 (14) |
O22—Mo3—O13—Mo1 | 29.1 (12) | O39—Mo9—O24—Mo10 | 100.8 (2) |
O14—Mo3—O13—Mo1 | −27.1 (7) | O34—Mo9—O24—Mo10 | −0.5 (2) |
O24—Mo3—O13—Mo1 | 54.1 (7) | O33—Mo9—O24—Mo10 | −173.8 (2) |
O1—Mo1—O13—Mo3 | 130.2 (7) | O23—Mo9—O24—Mo10 | −91.2 (2) |
O15—Mo1—O13—Mo3 | 27.3 (7) | O9—Mo9—O24—Mo3 | 23.9 (14) |
O16—Mo1—O13—Mo3 | −74.9 (10) | O39—Mo9—O24—Mo3 | −169.9 (2) |
O17—Mo1—O13—Mo3 | −132.8 (7) | O34—Mo9—O24—Mo3 | 88.8 (2) |
O18—Mo1—O13—Mo3 | −59.6 (7) | O33—Mo9—O24—Mo3 | −84.5 (2) |
O2—Mo2—O14—Mo3 | −133.1 (8) | O23—Mo9—O24—Mo3 | −2.0 (2) |
O19—Mo2—O14—Mo3 | 120.7 (8) | O4—Mo4—O25—Mo6 | 168.2 (4) |
O20—Mo2—O14—Mo3 | 17.9 (12) | O40—Mo4—O25—Mo6 | −85.3 (4) |
O15—Mo2—O14—Mo3 | −32.8 (8) | O38—Mo4—O25—Mo6 | 8.9 (8) |
O21—Mo2—O14—Mo3 | 47.4 (8) | O26—Mo4—O25—Mo6 | 69.8 (4) |
O3—Mo3—O14—Mo2 | 137.1 (8) | O28—Mo4—O25—Mo6 | −2.1 (3) |
O23—Mo3—O14—Mo2 | −60.7 (11) | O6—Mo6—O25—Mo4 | −173.8 (4) |
O13—Mo3—O14—Mo2 | 33.6 (8) | O29—Mo6—O25—Mo4 | 29.7 (8) |
O22—Mo3—O14—Mo2 | −125.5 (8) | O27—Mo6—O25—Mo4 | −72.6 (4) |
O24—Mo3—O14—Mo2 | −53.1 (8) | O30—Mo6—O25—Mo4 | 85.7 (4) |
O1—Mo1—O15—Mo2 | −129.9 (8) | O28—Mo6—O25—Mo4 | 2.1 (3) |
O16—Mo1—O15—Mo2 | 125.9 (8) | O5—Mo5—O26—Mo4 | 168.2 (4) |
O13—Mo1—O15—Mo2 | −28.5 (8) | O37—Mo5—O26—Mo4 | −85.2 (4) |
O17—Mo1—O15—Mo2 | 27.9 (13) | O27—Mo5—O26—Mo4 | 70.4 (4) |
O18—Mo1—O15—Mo2 | 52.7 (8) | O39—Mo5—O26—Mo4 | 10.4 (8) |
O2—Mo2—O15—Mo1 | 132.6 (8) | O28—Mo5—O26—Mo4 | −1.6 (3) |
O14—Mo2—O15—Mo1 | 29.6 (8) | O4—Mo4—O26—Mo5 | −174.2 (4) |
O19—Mo2—O15—Mo1 | −67.9 (11) | O40—Mo4—O26—Mo5 | 28.3 (8) |
O20—Mo2—O15—Mo1 | −130.7 (8) | O25—Mo4—O26—Mo5 | −72.5 (4) |
O21—Mo2—O15—Mo1 | −58.3 (8) | O38—Mo4—O26—Mo5 | 85.2 (4) |
O1—Mo1—O16—Mo7 | 168.2 (4) | O28—Mo4—O26—Mo5 | 1.6 (3) |
O15—Mo1—O16—Mo7 | −86.3 (4) | O6—Mo6—O27—Mo5 | 168.8 (4) |
O13—Mo1—O16—Mo7 | 13.2 (8) | O29—Mo6—O27—Mo5 | −84.0 (4) |
O17—Mo1—O16—Mo7 | 70.2 (4) | O30—Mo6—O27—Mo5 | 12.9 (9) |
O18—Mo1—O16—Mo7 | −2.5 (3) | O25—Mo6—O27—Mo5 | 70.9 (4) |
O7—Mo7—O16—Mo1 | −174.4 (4) | O28—Mo6—O27—Mo5 | −1.1 (3) |
O32—Mo7—O16—Mo1 | −71.7 (4) | O5—Mo5—O27—Mo6 | −176.5 (4) |
O38—Mo7—O16—Mo1 | 34.2 (8) | O37—Mo5—O27—Mo6 | 28.5 (9) |
O31—Mo7—O16—Mo1 | 85.8 (4) | O26—Mo5—O27—Mo6 | −73.5 (4) |
O18—Mo7—O16—Mo1 | 2.5 (3) | O39—Mo5—O27—Mo6 | 84.0 (4) |
O8—Mo8—O17—Mo1 | 169.6 (4) | O28—Mo5—O27—Mo6 | 1.1 (3) |
O33—Mo8—O17—Mo1 | −82.2 (4) | O18—P1—O28—Mo6 | 173.4 (3) |
O37—Mo8—O17—Mo1 | 15.7 (8) | O24—P1—O28—Mo6 | 53.7 (5) |
O32—Mo8—O17—Mo1 | 72.1 (4) | O21—P1—O28—Mo6 | −66.8 (4) |
O18—Mo8—O17—Mo1 | 0.2 (3) | O18—P1—O28—Mo5 | 52.9 (5) |
O1—Mo1—O17—Mo8 | −176.0 (4) | O24—P1—O28—Mo5 | −66.8 (5) |
O15—Mo1—O17—Mo8 | 25.9 (9) | O21—P1—O28—Mo5 | 172.7 (3) |
O16—Mo1—O17—Mo8 | −74.9 (4) | O18—P1—O28—Mo4 | −66.4 (4) |
O13—Mo1—O17—Mo8 | 83.3 (4) | O24—P1—O28—Mo4 | 173.9 (3) |
O18—Mo1—O17—Mo8 | −0.2 (3) | O21—P1—O28—Mo4 | 53.4 (5) |
O28—P1—O18—Mo1 | 173.6 (3) | O6—Mo6—O28—P1 | 155.8 (13) |
O24—P1—O18—Mo1 | −66.6 (4) | O29—Mo6—O28—P1 | −34.8 (4) |
O21—P1—O18—Mo1 | 53.5 (5) | O27—Mo6—O28—P1 | −135.0 (4) |
O28—P1—O18—Mo7 | 53.6 (5) | O30—Mo6—O28—P1 | 51.0 (4) |
O24—P1—O18—Mo7 | 173.4 (3) | O25—Mo6—O28—P1 | 133.7 (4) |
O21—P1—O18—Mo7 | −66.5 (5) | O6—Mo6—O28—Mo5 | −68.4 (14) |
O28—P1—O18—Mo8 | −65.9 (5) | O29—Mo6—O28—Mo5 | 100.9 (2) |
O24—P1—O18—Mo8 | 53.9 (5) | O27—Mo6—O28—Mo5 | 0.7 (2) |
O21—P1—O18—Mo8 | 174.0 (3) | O30—Mo6—O28—Mo5 | −173.2 (2) |
O1—Mo1—O18—P1 | 160.2 (14) | O25—Mo6—O28—Mo5 | −90.5 (2) |
O15—Mo1—O18—P1 | −34.0 (4) | O6—Mo6—O28—Mo4 | 20.8 (14) |
O16—Mo1—O18—P1 | −133.9 (4) | O29—Mo6—O28—Mo4 | −169.8 (2) |
O13—Mo1—O18—P1 | 53.0 (4) | O27—Mo6—O28—Mo4 | 90.0 (3) |
O17—Mo1—O18—P1 | 135.8 (4) | O30—Mo6—O28—Mo4 | −84.0 (2) |
O1—Mo1—O18—Mo7 | −64.2 (15) | O25—Mo6—O28—Mo4 | −1.3 (2) |
O15—Mo1—O18—Mo7 | 101.6 (2) | O5—Mo5—O28—P1 | 148.4 (14) |
O16—Mo1—O18—Mo7 | 1.7 (2) | O37—Mo5—O28—P1 | −34.0 (4) |
O13—Mo1—O18—Mo7 | −171.5 (2) | O26—Mo5—O28—P1 | −133.4 (4) |
O17—Mo1—O18—Mo7 | −88.6 (2) | O27—Mo5—O28—P1 | 134.9 (5) |
O1—Mo1—O18—Mo8 | 24.5 (16) | O39—Mo5—O28—P1 | 51.9 (4) |
O15—Mo1—O18—Mo8 | −169.7 (2) | O5—Mo5—O28—Mo6 | 12.8 (16) |
O16—Mo1—O18—Mo8 | 90.4 (2) | O37—Mo5—O28—Mo6 | −169.6 (2) |
O13—Mo1—O18—Mo8 | −82.7 (2) | O26—Mo5—O28—Mo6 | 91.0 (2) |
O17—Mo1—O18—Mo8 | 0.1 (2) | O27—Mo5—O28—Mo6 | −0.7 (2) |
O32—Mo7—O18—P1 | −133.1 (4) | O39—Mo5—O28—Mo6 | −83.7 (2) |
O38—Mo7—O18—P1 | −32.8 (4) | O5—Mo5—O28—Mo4 | −77.1 (15) |
O16—Mo7—O18—P1 | 133.6 (4) | O37—Mo5—O28—Mo4 | 100.5 (2) |
O31—Mo7—O18—P1 | 51.0 (4) | O26—Mo5—O28—Mo4 | 1.1 (2) |
O32—Mo7—O18—Mo1 | 91.7 (2) | O27—Mo5—O28—Mo4 | −90.6 (2) |
O38—Mo7—O18—Mo1 | −168.0 (2) | O39—Mo5—O28—Mo4 | −173.6 (2) |
O16—Mo7—O18—Mo1 | −1.6 (2) | O4—Mo4—O28—P1 | 158.0 (13) |
O31—Mo7—O18—Mo1 | −84.2 (2) | O40—Mo4—O28—P1 | −34.9 (4) |
O32—Mo7—O18—Mo8 | 2.0 (2) | O25—Mo4—O28—P1 | −134.0 (4) |
O38—Mo7—O18—Mo8 | 102.3 (2) | O38—Mo4—O28—P1 | 50.7 (4) |
O16—Mo7—O18—Mo8 | −91.3 (2) | O26—Mo4—O28—P1 | 134.1 (4) |
O31—Mo7—O18—Mo8 | −173.9 (2) | O4—Mo4—O28—Mo6 | −66.5 (15) |
O8—Mo8—O18—P1 | 147.7 (13) | O40—Mo4—O28—Mo6 | 100.6 (2) |
O33—Mo8—O18—P1 | −33.9 (4) | O25—Mo4—O28—Mo6 | 1.4 (2) |
O17—Mo8—O18—P1 | −135.5 (5) | O38—Mo4—O28—Mo6 | −173.8 (2) |
O37—Mo8—O18—P1 | 51.5 (4) | O26—Mo4—O28—Mo6 | −90.5 (2) |
O32—Mo8—O18—P1 | 133.4 (4) | O4—Mo4—O28—Mo5 | 22.9 (15) |
O8—Mo8—O18—Mo1 | −76.9 (14) | O40—Mo4—O28—Mo5 | −170.0 (2) |
O33—Mo8—O18—Mo1 | 101.5 (2) | O25—Mo4—O28—Mo5 | 90.9 (2) |
O17—Mo8—O18—Mo1 | −0.1 (2) | O38—Mo4—O28—Mo5 | −84.4 (2) |
O37—Mo8—O18—Mo1 | −173.1 (2) | O26—Mo4—O28—Mo5 | −1.0 (2) |
O32—Mo8—O18—Mo1 | −91.1 (2) | O6—Mo6—O29—Mo10 | −126.2 (7) |
O8—Mo8—O18—Mo7 | 12.4 (15) | O27—Mo6—O29—Mo10 | 129.2 (7) |
O33—Mo8—O18—Mo7 | −169.2 (2) | O30—Mo6—O29—Mo10 | −25.4 (7) |
O17—Mo8—O18—Mo7 | 89.2 (2) | O25—Mo6—O29—Mo10 | 29.7 (12) |
O37—Mo8—O18—Mo7 | −83.8 (2) | O28—Mo6—O29—Mo10 | 55.8 (7) |
O32—Mo8—O18—Mo7 | −1.8 (2) | O10—Mo10—O29—Mo6 | 129.6 (7) |
O2—Mo2—O19—Mo11 | 167.0 (4) | O35—Mo10—O29—Mo6 | 25.8 (7) |
O14—Mo2—O19—Mo11 | −86.1 (4) | O22—Mo10—O29—Mo6 | −73.4 (10) |
O20—Mo2—O19—Mo11 | 69.1 (4) | O34—Mo10—O29—Mo6 | −133.8 (8) |
O15—Mo2—O19—Mo11 | 7.7 (9) | O24—Mo10—O29—Mo6 | −61.1 (7) |
O21—Mo2—O19—Mo11 | −2.2 (3) | O11—Mo11—O30—Mo6 | −128.5 (7) |
O11—Mo11—O19—Mo2 | −174.8 (4) | O36—Mo11—O30—Mo6 | 125.4 (7) |
O30—Mo11—O19—Mo2 | 32.0 (8) | O19—Mo11—O30—Mo6 | 24.2 (12) |
O36—Mo11—O19—Mo2 | −72.3 (4) | O35—Mo11—O30—Mo6 | −28.6 (7) |
O35—Mo11—O19—Mo2 | 85.6 (4) | O21—Mo11—O30—Mo6 | 52.3 (7) |
O21—Mo11—O19—Mo2 | 2.2 (3) | O6—Mo6—O30—Mo11 | 133.1 (7) |
O12—Mo12—O20—Mo2 | 168.7 (4) | O29—Mo6—O30—Mo11 | 28.9 (7) |
O31—Mo12—O20—Mo2 | −85.2 (4) | O27—Mo6—O30—Mo11 | −71.0 (10) |
O40—Mo12—O20—Mo2 | 14.0 (8) | O25—Mo6—O30—Mo11 | −130.2 (8) |
O36—Mo12—O20—Mo2 | 71.3 (4) | O28—Mo6—O30—Mo11 | −57.3 (7) |
O21—Mo12—O20—Mo2 | −1.1 (3) | O12—Mo12—O31—Mo7 | −131.9 (8) |
O2—Mo2—O20—Mo12 | −176.0 (4) | O20—Mo12—O31—Mo7 | 123.3 (8) |
O14—Mo2—O20—Mo12 | 32.4 (8) | O40—Mo12—O31—Mo7 | −30.4 (8) |
O19—Mo2—O20—Mo12 | −73.1 (4) | O36—Mo12—O31—Mo7 | 24.2 (13) |
O15—Mo2—O20—Mo12 | 83.6 (4) | O21—Mo12—O31—Mo7 | 50.1 (8) |
O21—Mo2—O20—Mo12 | 1.1 (3) | O7—Mo7—O31—Mo12 | 134.6 (8) |
O18—P1—O21—Mo12 | 54.0 (5) | O32—Mo7—O31—Mo12 | −64.3 (11) |
O28—P1—O21—Mo12 | −66.1 (5) | O38—Mo7—O31—Mo12 | 32.0 (8) |
O24—P1—O21—Mo12 | 173.7 (3) | O16—Mo7—O31—Mo12 | −127.5 (8) |
O18—P1—O21—Mo2 | −67.4 (5) | O18—Mo7—O31—Mo12 | −55.0 (8) |
O28—P1—O21—Mo2 | 172.4 (3) | O7—Mo7—O32—Mo8 | 167.6 (4) |
O24—P1—O21—Mo2 | 52.2 (5) | O38—Mo7—O32—Mo8 | −86.2 (4) |
O18—P1—O21—Mo11 | 174.2 (3) | O16—Mo7—O32—Mo8 | 68.2 (4) |
O28—P1—O21—Mo11 | 54.0 (5) | O31—Mo7—O32—Mo8 | 6.6 (8) |
O24—P1—O21—Mo11 | −66.2 (5) | O18—Mo7—O32—Mo8 | −2.9 (3) |
O12—Mo12—O21—P1 | 156.0 (13) | O8—Mo8—O32—Mo7 | −174.4 (4) |
O31—Mo12—O21—P1 | −34.6 (4) | O33—Mo8—O32—Mo7 | 32.7 (8) |
O20—Mo12—O21—P1 | −135.4 (4) | O17—Mo8—O32—Mo7 | −71.7 (4) |
O40—Mo12—O21—P1 | 51.4 (4) | O37—Mo8—O32—Mo7 | 85.9 (4) |
O36—Mo12—O21—P1 | 134.7 (4) | O18—Mo8—O32—Mo7 | 3.0 (3) |
O12—Mo12—O21—Mo2 | −67.9 (15) | O8—Mo8—O33—Mo9 | −127.3 (8) |
O31—Mo12—O21—Mo2 | 101.6 (2) | O17—Mo8—O33—Mo9 | 126.1 (8) |
O20—Mo12—O21—Mo2 | 0.8 (2) | O37—Mo8—O33—Mo9 | −27.3 (8) |
O40—Mo12—O21—Mo2 | −172.4 (2) | O32—Mo8—O33—Mo9 | 24.9 (12) |
O36—Mo12—O21—Mo2 | −89.1 (2) | O18—Mo8—O33—Mo9 | 53.0 (8) |
O12—Mo12—O21—Mo11 | 21.2 (15) | O9—Mo9—O33—Mo8 | 131.8 (8) |
O31—Mo12—O21—Mo11 | −169.3 (2) | O39—Mo9—O33—Mo8 | 28.2 (8) |
O20—Mo12—O21—Mo11 | 89.9 (2) | O34—Mo9—O33—Mo8 | −73.2 (10) |
O40—Mo12—O21—Mo11 | −83.3 (2) | O23—Mo9—O33—Mo8 | −130.9 (8) |
O36—Mo12—O21—Mo11 | 0.03 (19) | O24—Mo9—O33—Mo8 | −58.7 (8) |
O2—Mo2—O21—P1 | 150.8 (13) | O9—Mo9—O34—Mo10 | 170.8 (4) |
O14—Mo2—O21—P1 | −31.6 (4) | O39—Mo9—O34—Mo10 | −82.3 (4) |
O19—Mo2—O21—P1 | −132.3 (5) | O33—Mo9—O34—Mo10 | 15.6 (8) |
O20—Mo2—O21—P1 | 135.5 (5) | O23—Mo9—O34—Mo10 | 72.2 (4) |
O15—Mo2—O21—P1 | 52.2 (4) | O24—Mo9—O34—Mo10 | 0.7 (3) |
O2—Mo2—O21—Mo12 | 14.6 (15) | O10—Mo10—O34—Mo9 | −176.7 (4) |
O14—Mo2—O21—Mo12 | −167.8 (2) | O35—Mo10—O34—Mo9 | 24.5 (8) |
O19—Mo2—O21—Mo12 | 91.5 (3) | O22—Mo10—O34—Mo9 | −75.2 (4) |
O20—Mo2—O21—Mo12 | −0.7 (2) | O29—Mo10—O34—Mo9 | 81.4 (4) |
O15—Mo2—O21—Mo12 | −84.0 (2) | O24—Mo10—O34—Mo9 | −0.7 (3) |
O2—Mo2—O21—Mo11 | −75.5 (15) | O10—Mo10—O35—Mo11 | −128.9 (7) |
O14—Mo2—O21—Mo11 | 102.1 (2) | O22—Mo10—O35—Mo11 | 126.4 (7) |
O19—Mo2—O21—Mo11 | 1.4 (2) | O29—Mo10—O35—Mo11 | −26.6 (7) |
O20—Mo2—O21—Mo11 | −90.8 (2) | O34—Mo10—O35—Mo11 | 29.5 (12) |
O15—Mo2—O21—Mo11 | −174.1 (2) | O24—Mo10—O35—Mo11 | 53.4 (7) |
O11—Mo11—O21—P1 | 149.9 (13) | O11—Mo11—O35—Mo10 | 131.6 (7) |
O30—Mo11—O21—P1 | −34.3 (4) | O30—Mo11—O35—Mo10 | 28.0 (7) |
O36—Mo11—O21—P1 | −135.5 (5) | O36—Mo11—O35—Mo10 | −72.7 (10) |
O19—Mo11—O21—P1 | 133.0 (5) | O19—Mo11—O35—Mo10 | −131.2 (8) |
O35—Mo11—O21—P1 | 50.8 (4) | O21—Mo11—O35—Mo10 | −58.9 (7) |
O11—Mo11—O21—Mo12 | −74.6 (15) | O11—Mo11—O36—Mo12 | 169.8 (3) |
O30—Mo11—O21—Mo12 | 101.1 (2) | O30—Mo11—O36—Mo12 | −83.0 (4) |
O36—Mo11—O21—Mo12 | 0.0 (2) | O19—Mo11—O36—Mo12 | 71.4 (4) |
O19—Mo11—O21—Mo12 | −91.5 (2) | O35—Mo11—O36—Mo12 | 14.2 (8) |
O35—Mo11—O21—Mo12 | −173.8 (2) | O21—Mo11—O36—Mo12 | 0.0 (3) |
O11—Mo11—O21—Mo2 | 15.6 (16) | O12—Mo12—O36—Mo11 | −176.1 (4) |
O30—Mo11—O21—Mo2 | −168.7 (2) | O31—Mo12—O36—Mo11 | 27.4 (8) |
O36—Mo11—O21—Mo2 | 90.1 (2) | O20—Mo12—O36—Mo11 | −74.7 (4) |
O19—Mo11—O21—Mo2 | −1.3 (2) | O40—Mo12—O36—Mo11 | 82.8 (4) |
O35—Mo11—O21—Mo2 | −83.6 (2) | O21—Mo12—O36—Mo11 | 0.0 (3) |
O10—Mo10—O22—Mo3 | 167.9 (4) | O5—Mo5—O37—Mo8 | −126.5 (7) |
O35—Mo10—O22—Mo3 | −85.4 (4) | O26—Mo5—O37—Mo8 | 127.5 (7) |
O29—Mo10—O22—Mo3 | 10.8 (8) | O27—Mo5—O37—Mo8 | 28.0 (12) |
O34—Mo10—O22—Mo3 | 70.3 (4) | O39—Mo5—O37—Mo8 | −26.6 (7) |
O24—Mo10—O22—Mo3 | −1.8 (3) | O28—Mo5—O37—Mo8 | 53.9 (7) |
O3—Mo3—O22—Mo10 | −174.4 (4) | O8—Mo8—O37—Mo5 | 131.5 (7) |
O23—Mo3—O22—Mo10 | −72.1 (4) | O33—Mo8—O37—Mo5 | 27.0 (7) |
O13—Mo3—O22—Mo10 | 28.2 (8) | O17—Mo8—O37—Mo5 | −74.4 (10) |
O14—Mo3—O22—Mo10 | 85.1 (4) | O32—Mo8—O37—Mo5 | −132.2 (8) |
O24—Mo3—O22—Mo10 | 1.9 (3) | O18—Mo8—O37—Mo5 | −59.3 (7) |
O3—Mo3—O23—Mo9 | 166.9 (4) | O7—Mo7—O38—Mo4 | −131.9 (8) |
O13—Mo3—O23—Mo9 | −86.8 (4) | O32—Mo7—O38—Mo4 | 122.6 (8) |
O22—Mo3—O23—Mo9 | 68.3 (4) | O16—Mo7—O38—Mo4 | 19.1 (12) |
O14—Mo3—O23—Mo9 | 4.7 (9) | O31—Mo7—O38—Mo4 | −31.8 (8) |
O24—Mo3—O23—Mo9 | −3.1 (3) | O18—Mo7—O38—Mo4 | 49.0 (8) |
O9—Mo9—O23—Mo3 | −172.1 (4) | O4—Mo4—O38—Mo7 | 135.1 (8) |
O39—Mo9—O23—Mo3 | 31.6 (8) | O40—Mo4—O38—Mo7 | 31.5 (8) |
O34—Mo9—O23—Mo3 | −71.6 (4) | O25—Mo4—O38—Mo7 | −65.6 (11) |
O33—Mo9—O23—Mo3 | 86.2 (4) | O26—Mo4—O38—Mo7 | −127.7 (8) |
O24—Mo9—O23—Mo3 | 3.2 (3) | O28—Mo4—O38—Mo7 | −54.9 (8) |
O18—P1—O24—Mo10 | 173.7 (3) | O9—Mo9—O39—Mo5 | −129.3 (7) |
O28—P1—O24—Mo10 | −66.3 (5) | O34—Mo9—O39—Mo5 | 126.5 (7) |
O21—P1—O24—Mo10 | 54.1 (5) | O33—Mo9—O39—Mo5 | −27.1 (7) |
O18—P1—O24—Mo3 | 53.7 (5) | O23—Mo9—O39—Mo5 | 26.5 (12) |
O28—P1—O24—Mo3 | 173.7 (3) | O24—Mo9—O39—Mo5 | 53.3 (7) |
O21—P1—O24—Mo3 | −66.0 (5) | O5—Mo5—O39—Mo9 | 131.5 (8) |
O18—P1—O24—Mo9 | −66.8 (4) | O37—Mo5—O39—Mo9 | 28.0 (8) |
O28—P1—O24—Mo9 | 53.2 (5) | O26—Mo5—O39—Mo9 | −70.5 (10) |
O21—P1—O24—Mo9 | 173.6 (3) | O27—Mo5—O39—Mo9 | −131.7 (8) |
O10—Mo10—O24—P1 | 157.3 (13) | O28—Mo5—O39—Mo9 | −58.8 (7) |
O35—Mo10—O24—P1 | −34.5 (4) | O4—Mo4—O40—Mo12 | −126.7 (7) |
O22—Mo10—O24—P1 | −134.3 (4) | O25—Mo4—O40—Mo12 | 128.7 (7) |
O29—Mo10—O24—P1 | 51.6 (4) | O38—Mo4—O40—Mo12 | −25.9 (7) |
O34—Mo10—O24—P1 | 135.3 (5) | O26—Mo4—O40—Mo12 | 30.3 (12) |
O10—Mo10—O24—Mo3 | −67.2 (15) | O28—Mo4—O40—Mo12 | 55.6 (7) |
O35—Mo10—O24—Mo3 | 101.0 (2) | O12—Mo12—O40—Mo4 | 129.8 (7) |
O22—Mo10—O24—Mo3 | 1.2 (2) | O31—Mo12—O40—Mo4 | 26.9 (7) |
O29—Mo10—O24—Mo3 | −172.9 (2) | O20—Mo12—O40—Mo4 | −75.5 (10) |
O34—Mo10—O24—Mo3 | −89.2 (2) | O36—Mo12—O40—Mo4 | −133.7 (8) |
O10—Mo10—O24—Mo9 | 22.5 (15) | O21—Mo12—O40—Mo4 | −60.8 (7) |
O35—Mo10—O24—Mo9 | −169.4 (2) | C2—N3—C1—N1 | −159.0 (10) |
O22—Mo10—O24—Mo9 | 90.9 (2) | C2—N3—C1—N2 | 20.0 (15) |
O29—Mo10—O24—Mo9 | −83.2 (2) | C8—N5—C2—N4 | 2.6 (10) |
O34—Mo10—O24—Mo9 | 0.5 (2) | C8—N5—C2—N3 | −171.1 (8) |
O3—Mo3—O24—P1 | 155.3 (14) | C3—N4—C2—N5 | −1.7 (10) |
O23—Mo3—O24—P1 | −133.2 (4) | C3—N4—C2—N3 | 171.3 (9) |
O13—Mo3—O24—P1 | −35.0 (4) | C1—N3—C2—N5 | −149.1 (9) |
O22—Mo3—O24—P1 | 134.1 (4) | C1—N3—C2—N4 | 38.3 (15) |
O14—Mo3—O24—P1 | 50.1 (4) | C2—N4—C3—C8 | 0.2 (10) |
O3—Mo3—O24—Mo10 | 20.0 (16) | C2—N4—C3—C4 | −178.1 (9) |
O23—Mo3—O24—Mo10 | 91.5 (2) | C8—C3—C4—C5 | 0.3 (13) |
O13—Mo3—O24—Mo10 | −170.3 (2) | N4—C3—C4—C5 | 178.4 (9) |
O22—Mo3—O24—Mo10 | −1.1 (2) | C3—C4—C5—C6 | −2.2 (14) |
O14—Mo3—O24—Mo10 | −85.1 (2) | C4—C5—C6—C7 | 1.9 (16) |
O3—Mo3—O24—Mo9 | −69.4 (16) | C5—C6—C7—C8 | 0.3 (15) |
O23—Mo3—O24—Mo9 | 2.1 (2) | C6—C7—C8—C3 | −2.2 (14) |
O13—Mo3—O24—Mo9 | 100.3 (2) | C6—C7—C8—N5 | −179.4 (9) |
O22—Mo3—O24—Mo9 | −90.5 (2) | C4—C3—C8—C7 | 2.0 (14) |
O14—Mo3—O24—Mo9 | −174.5 (2) | N4—C3—C8—C7 | −176.5 (8) |
O9—Mo9—O24—P1 | 159.7 (12) | C4—C3—C8—N5 | 179.8 (8) |
O39—Mo9—O24—P1 | −34.2 (4) | N4—C3—C8—N5 | 1.3 (9) |
O34—Mo9—O24—P1 | −135.5 (5) | C2—N5—C8—C7 | 175.2 (9) |
O33—Mo9—O24—P1 | 51.2 (4) | C2—N5—C8—C3 | −2.3 (10) |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O4i | 0.96 | 2.14 | 3.097 (9) | 173 |
O8—H8···O10ii | 0.96 | 2.40 | 3.093 (5) | 129 |
N1—H1N1···O5Siii | 0.88 | 1.95 | 2.728 (6) | 146 |
N1—H2N1···O5Wiv | 0.88 | 2.20 | 2.883 (6) | 134 |
N2—H1N2···O5Siii | 0.88 | 2.10 | 2.839 (6) | 141 |
N2—H2N2···O5 | 0.88 | 2.01 | 2.844 (6) | 157 |
N3—H1N3···O1W | 0.90 | 1.84 | 2.717 (6) | 165 |
N5—H1N5···O36ii | 0.90 | 2.25 | 2.974 (5) | 137 |
O1S—H1OS···O32 | 0.95 | 2.35 | 3.218 (5) | 152 |
O3S—H3OS···O5Wv | 0.96 | 2.01 | 2.881 (7) | 149 |
O4S—H4OS···O27 | 0.96 | 1.99 | 2.805 (6) | 141 |
O1W—H1W1···O20ii | 1.01 | 1.89 | 2.740 (6) | 140 |
O1W—H2W1···O5W′iv | 1.01 | 2.05 | 3.057 (7) | 176 |
O1W—H2W1···O5Wiv | 1.01 | 2.17 | 3.067 (7) | 148 |
O2W—H2W2···N4 | 1.01 | 1.78 | 2.731 (6) | 157 |
O3W—H2W3···O3S | 1.01 | 1.93 | 2.618 (8) | 123 |
O4W—H1W4···O6ii | 1.01 | 2.30 | 3.004 (7) | 126 |
O4W—H2W4···O2S | 1.01 | 1.76 | 2.716 (7) | 157 |
O5W—H4W′···O32vi | 1.01 | 1.87 | 2.847 (7) | 161 |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, y−1/2, −z+1; (iii) −x+2, y−1/2, −z+1; (iv) −x+1, y−1/2, −z; (v) −x, y−1/2, −z; (vi) −x+1, y+1/2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C8H10N5)[H2PMo12O40]·2.5CH4O·4H2O |
Mr | 2152.65 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 120 |
a, b, c (Å) | 11.9025 (12), 18.2497 (19), 12.7798 (13) |
β (°) | 109.639 (2) |
V (Å3) | 2614.5 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.92 |
Crystal size (mm) | 0.40 × 0.30 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD area-detector |
Absorption correction | Multi scan (SADABS; Sheldrick, 1998a) |
Tmin, Tmax | 0.360, 0.648 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22667, 9960, 9679 |
Rint | 0.093 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.095, 1.05 |
No. of reflections | 9960 |
No. of parameters | 663 |
No. of restraints | 30 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.01P)2 + 25P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.68, −1.28 |
Absolute structure | Flack (1983), 4793 Friedel pairs |
Absolute structure parameter | 0.04 (5) |
Computer programs: SMART (Bruker, 1998), SAINT-Plus (Bruker, 1998), SHELXTL (Sheldrick, 1998b).
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O4i | 0.960 | 2.142 | 3.097 (9) | 173.13 |
O8—H8···O10ii | 0.960 | 2.397 | 3.093 (5) | 129.12 |
N1—H1N1···O5Siii | 0.880 | 1.954 | 2.728 (6) | 145.87 |
N1—H2N1···O5Wiv | 0.880 | 2.200 | 2.883 (6) | 134.16 |
N2—H1N2···O5Siii | 0.880 | 2.101 | 2.839 (6) | 140.96 |
N2—H2N2···O5 | 0.880 | 2.014 | 2.844 (6) | 156.93 |
N3—H1N3···O1W | 0.900 | 1.838 | 2.717 (6) | 164.83 |
N5—H1N5···O36ii | 0.901 | 2.252 | 2.974 (5) | 136.86 |
O1S—H1OS···O32 | 0.950 | 2.347 | 3.218 (5) | 152.11 |
O3S—H3OS···O5Wv | 0.960 | 2.013 | 2.881 (7) | 149.28 |
O4S—H4OS···O27 | 0.960 | 1.990 | 2.805 (6) | 141.37 |
O1W—H1W1···O20ii | 1.010 | 1.888 | 2.740 (6) | 140.00 |
O1W—H2W1···O5W'iv | 1.010 | 2.049 | 3.057 (7) | 176.42 |
O1W—H2W1···O5Wiv | 1.010 | 2.167 | 3.067 (7) | 147.46 |
O2W—H2W2···N4 | 1.010 | 1.775 | 2.731 (6) | 156.55 |
O3W—H2W3···O3S | 1.010 | 1.932 | 2.618 (8) | 122.59 |
O4W—H1W4···O6ii | 1.010 | 2.296 | 3.004 (7) | 126.05 |
O4W—H2W4···O2S | 1.010 | 1.756 | 2.716 (7) | 157.34 |
O5W—H4W'···O32vi | 1.010 | 1.873 | 2.847 (7) | 160.94 |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, y−1/2, −z+1; (iii) −x+2, y−1/2, −z+1; (iv) −x+1, y−1/2, −z; (v) −x, y−1/2, −z; (vi) −x+1, y+1/2, −z+1. |
Non-covalent forces play a vital role in crystal packing (Du et al., 2005) which are important for material sciences, supramolecular chemistry and biology (Tan et al., 2005; Duarte et al., 2005; Li et al., 2005; Meot-Ner, 2005; Madhu & Das, 2004; Laberge, 1998). In this subject, some discussions carried out on the electrostatic interactions (Liu et al., 2004), symmetrical aspects and the hydrogen bonds functions (Gholivand, et al., 2006). Hence, we study these interactions in a new polyoxometalate (POM)-based organic/inorganic hybrid containing a polyfunctional molecule 2-gb [N-(1H-1,3-benzimidazol-2-yl)guanidine (2-guanidinobenzimidazole)] as the organic component. Due to the importance of crystal engineering in material studies (Batsanov et al., 2006) and the value of material hybrids based on the polyoxometalates, POMs, (Santos, et al., 2005; Ma, et al., 2005; Coronado, et al., 2004; Coronado & Gómez-García, 1998; Zhang, et al., 1997) this investigation may be useful. The basic unit of title hybrid contains asymmetric [H2PMo12O40]- polyoxoanion (Fig. 1) and 2-gbH+ cation (Fig. 2) besides the solvated H2O and CH3OH molecules (5 CH3OH molecules with the site occupancy factor of 0.5 and 4 H2O). Four different kinds of O atoms occur in bifunctional Keggin acid: a) the 12 terminal, b) the 4 bonded to P and Mo, c) the 12 MoO6 octahedra corner-shared and d) the 12 MoO6 octahedra edge-shared. The phosphorus atom has a tetrahedral configuration (O—P—O angles in the range of 109.1 (3)°-109.9 (3)°) and the Mo atoms are distorted octahedral (152.9 (3)°-170.4 (3)° for trans O—Mo—O angles). The P—O bonds are in the range of P—O single bond (Corbridge, 1995), 1.531 (6)–1.550 (6) Å. Five N atoms are in 2-gb and only one is protonatated (guanidine N(3) atom) to form a C8H10N5+ cation, like previous study on [2-gbH]+ACO-.H2O (Andrade-López, et al., 1997). The C(1)—N(1), C(1)—N(2) and C(1)—N(3) bonds, consistent with the guanidine functional group, are not equivalent in title compound. C(1)—N(1) and C(1)—N(2) bond distances are in the range of "one-and a half bonds" which are strengthened versus to these bonds in free ligand (1.311 (13) Å, 1.326 (12) Å in compare with the 1.350 (4) Å and 1.357 (4) Å (Steel, 1991). This is attributed to contribution of nitrogen atoms lone pair in C(1)—N(1) and C(1)—N(2) bonds. This effect causes that the angle N(1)—C(1)—N(2) become greater in the title compound with compare to the corresponding angle in free ligand (121.5 (9) and 117.7 (3)°). C(1)—N(3) is a single bond in POM-based organic/inorganic hybrid, 1.374 (13) Å (versus 1.321 (4) Å in free ligand). In 2-gbH+ cation, the guanidinium residue is twisted from the nearly planar benzimidazole moiety (torsion angles C(1)—N(3)—C(2)—N(4) and C(1)—N(3)—C(2)—N(5) are 38.3 (15)° and -149.1 (9)°, respectively. Various O—H···O and N—H···O hydrogen bonds (Table 1) in the crystal lattice (and also different O···O and N···O electrostatic interactions) lead to a 3-D supramolecular framework. Via the five nitrogen atoms, 2-gbH+ cation is surrounded by three [H2PMo12O40]- anions (with two N—H···O hydrogen bonds and one electrostatic interaction), and three H2O molecules. Figure 3 shows the location of organic cation between three inorganic anions which the interaction of 2-gbH+ with the left anion in figure is an electrostatic interaction. N(2) and N(5) atoms of 2-gbH+ are hydrogen bonded to terminal O(5) and edge-shared O(36) atoms of POMs (N(2)···O(5) = 2.844 (6) Å and (N(5)···O(36) = 2.974 (5) Å). Besides the solvated CH3OH and H2O molecules, the anion is connected to 3 other neighboring anions via the O···O electrostatic interactions and three 2-gbH+ cations (via N···O electrostatic interactions and two N—H···O hydrogen bonds, N(2)—H(2 N2)···O(5) and N(5)—H(1 N5)···O(36). Crystal packing of polyoxoanions and view of the unit cell packing along b crystal axis are shown in Figs. 4 and 5. Some H2O and CH3OH solvated molecules make infinite zigzag belts around the organic cations and the inorganic anions with the sequence of H2O···CH3OH···CH3OH···CH3OH···H2O···H2O···CH3OH··· in the chains (Fig. 6). All solvated H2O (as well as CH3OH) molecules are symmetrically non-equivalent in case of their various interactions with the other components in crystal lattice.