Literature DB >> 21579657

Bis{tris-[3-(2-pyrid-yl)-1H-pyrazole]iron(II)} tetra-deca-molybdo(V,VI)silicate.

Peihai Wei, Dong Yuan, Wencai Zhu, Xiutang Zhang, Bo Hu.   

Abstract

The asymmetric unit of the title compound, [Fe(C(8)H(7)N(3))(3)](2)[SiMo(14)O(44)], consists of a complex [Fe(C(8)H(7)N(3))(3)](2+) cation and half of a derivative of an α-Keggin-type anion, [SiMo(14)O(44)](4-). In the mixed-valent Mo(V/VI) anion, the α-Keggin type core is capped on two oppositely disposed tetra-gonal faces by additional (MoO(2)) units. The [SiMo(14)O(44)](4-) anion shows disorder. Two O atoms of the central SiO(4) group ( symmetry) are equally disordered about an inversion centre. Moreover, two of the outer bridging O atoms and the O atoms of the capping (MoO(2)) unit are likewise disordered. The Fe(2+) cation is surrounded in a slightly distorted octa-hedral coordination by six N atoms from three 3-(2-pyrid-yl)-1H-pyrazole ligands. N-H⋯O hydrogen bonding between the cations and anions leads to a consolidation of the structure.

Entities:  

Year:  2010        PMID: 21579657      PMCID: PMC2979929          DOI: 10.1107/S1600536810002412

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For general background to polyoxometalates, see: Pope & Müller (1991 ▶). For polyoxometalates modified with amines, see: Zhang, Dou et al. (2009 ▶); Zhang, Wei, Shi et al. (2010a ▶,b ▶); Zhang, Wei, Sun et al. (2009 ▶); Zhang, Wei, Zhu et al. (2010 ▶); Zhang, Yuan et al. (2010 ▶). For another structure containing the α-Keggin-type derivative [SiMo14O44]4−, see: Dolbecq et al. (1999 ▶). For background to the bond-valence method, see: Brese & O’Keeffe (1991 ▶). For the role of amines in hydro­thermal synthesis, see: Yang et al. (2003 ▶).

Experimental

Crystal data

[Fe(C8H7N3)3]2[SiMo14O44] M = 3057.95 Monoclinic, a = 13.055 (3) Å b = 16.931 (3) Å c = 18.562 (4) Å β = 102.69 (3)° V = 4002.6 (14) Å3 Z = 2 Mo Kα radiation μ = 2.58 mm−1 T = 293 K 0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.747, T max = 0.820 27223 measured reflections 7026 independent reflections 4730 reflections with I > 2σ(I) R int = 0.076

Refinement

R[F 2 > 2σ(F 2)] = 0.059 wR(F 2) = 0.157 S = 1.00 7026 reflections 638 parameters 444 restraints H-atom parameters constrained Δρmax = 1.47 e Å−3 Δρmin = −1.52 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810002412/wm2300sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810002412/wm2300Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Fe(C8H7N3)3]2[SiMo14O44]F(000) = 2924
Mr = 3057.95Dx = 2.537 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7026 reflections
a = 13.055 (3) Åθ = 1.7–25.0°
b = 16.931 (3) ŵ = 2.58 mm1
c = 18.562 (4) ÅT = 293 K
β = 102.69 (3)°Block, brown
V = 4002.6 (14) Å30.12 × 0.10 × 0.08 mm
Z = 2
Bruker APEXII CCD diffractometer7026 independent reflections
Radiation source: fine-focus sealed tube4730 reflections with I > 2σ(I)
graphiteRint = 0.076
phi and ω scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −15→15
Tmin = 0.747, Tmax = 0.820k = −20→20
27223 measured reflectionsl = −21→22
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.157H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.058P)2 + 47.4341P] where P = (Fo2 + 2Fc2)/3
7026 reflections(Δ/σ)max = 0.001
638 parametersΔρmax = 1.47 e Å3
444 restraintsΔρmin = −1.51 e Å3
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.
xyzUiso*/UeqOcc. (<1)
Si10.00000.50000.50000.0193 (8)
Fe10.36074 (14)0.58896 (11)0.17093 (11)0.0497 (5)
Mo10.20889 (7)0.55765 (6)0.41647 (5)0.0364 (3)
Mo2−0.00697 (9)0.46521 (7)0.30342 (6)0.0431 (3)
Mo30.33482 (8)0.44820 (7)0.54989 (6)0.0464 (3)
Mo40.21554 (8)0.59444 (6)0.61448 (6)0.0408 (3)
Mo50.05628 (8)0.70722 (6)0.47289 (6)0.0389 (3)
Mo6−0.16040 (7)0.61555 (6)0.35957 (6)0.0378 (3)
Mo7−0.14918 (7)0.65270 (6)0.55885 (5)0.0339 (3)
C10.5226 (13)0.7541 (10)0.3320 (9)0.080 (5)
H10.58070.78070.35920.096*
C20.4230 (13)0.7709 (10)0.3329 (9)0.074 (4)
H20.39750.80840.36110.088*
C30.3659 (11)0.7178 (8)0.2806 (7)0.055 (3)
C40.2536 (10)0.7064 (8)0.2539 (7)0.048 (3)
C50.1772 (11)0.7481 (9)0.2789 (8)0.060 (4)
H50.19560.78670.31510.072*
C60.0709 (12)0.7310 (10)0.2481 (9)0.069 (4)
H60.01820.75760.26480.082*
C70.0462 (12)0.6771 (10)0.1956 (9)0.070 (4)
H7−0.02400.66610.17520.084*
C80.1236 (11)0.6369 (9)0.1708 (8)0.063 (4)
H80.10440.59950.13360.076*
C90.4257 (14)0.7723 (10)0.0181 (9)0.079 (5)
H90.41530.8194−0.00840.095*
C100.5155 (13)0.7282 (10)0.0337 (8)0.072 (4)
H100.57740.73770.01810.086*
C110.4943 (11)0.6643 (8)0.0791 (7)0.053 (3)
C120.5598 (10)0.6004 (8)0.1139 (7)0.048 (3)
C130.6664 (12)0.5936 (10)0.1094 (8)0.072 (4)
H130.69710.63110.08430.087*
C140.7234 (15)0.5302 (12)0.1431 (10)0.095 (6)
H140.79220.52180.13880.114*
C150.6750 (13)0.4797 (10)0.1834 (9)0.076 (5)
H150.71260.43730.20770.091*
C160.5731 (12)0.4904 (9)0.1886 (8)0.067 (4)
H160.54300.45530.21640.081*
C170.3580 (12)0.3850 (9)0.3102 (9)0.065 (4)
H170.37730.35530.35320.078*
C180.2902 (12)0.3614 (9)0.2482 (8)0.066 (4)
H180.25350.31410.23910.079*
C190.2886 (10)0.4280 (8)0.1993 (8)0.054 (3)
C200.2335 (10)0.4416 (8)0.1235 (7)0.052 (3)
C210.1621 (13)0.3881 (10)0.0809 (10)0.081 (5)
H210.14940.33870.09890.098*
C220.1117 (13)0.4130 (11)0.0105 (9)0.081 (5)
H220.06370.3795−0.01910.097*
C230.1311 (13)0.4857 (10)−0.0161 (9)0.075 (4)
H230.09380.5025−0.06210.090*
C240.2060 (11)0.5332 (9)0.0258 (8)0.059 (4)
H240.22310.58070.00620.070*
N10.3925 (9)0.4562 (7)0.3005 (6)0.060 (3)
H1A0.43680.48130.33380.072*
N20.3507 (8)0.4859 (6)0.2324 (6)0.051 (3)
N30.2551 (9)0.5129 (7)0.0943 (6)0.057 (3)
N40.3541 (10)0.7337 (7)0.0492 (7)0.072 (4)
H40.29020.74900.04490.087*
N50.3958 (9)0.6673 (6)0.0883 (6)0.055 (3)
N60.5155 (8)0.5512 (6)0.1541 (6)0.052 (3)
N70.5271 (10)0.6937 (8)0.2864 (7)0.072 (4)
H7A0.58390.67250.27930.086*
N80.4298 (8)0.6712 (7)0.2534 (6)0.052 (3)
N90.2279 (9)0.6507 (7)0.1994 (6)0.058 (3)
O10.0848 (7)0.8012 (5)0.4612 (5)0.058 (2)
O2−0.2484 (7)0.6655 (6)0.2974 (5)0.061 (2)
O30.3156 (7)0.5797 (6)0.3861 (5)0.061 (2)
O40.3275 (6)0.6295 (5)0.6651 (5)0.052 (2)
O5−0.0141 (7)0.4491 (5)0.2150 (5)0.054 (2)
O6−0.0494 (8)0.7163 (6)0.5323 (5)0.071 (3)
O70.1182 (8)0.5280 (6)0.3314 (5)0.074 (3)
O8−0.0581 (7)0.6902 (6)0.3890 (5)0.071 (3)
O9−0.2306 (7)0.7206 (6)0.5792 (5)0.066 (3)
O100.2238 (9)0.3640 (6)0.5498 (5)0.080 (3)
O11A0.2488 (15)0.5526 (11)0.5273 (10)0.040 (5)0.50
O11B0.2997 (13)0.5646 (10)0.5258 (9)0.033 (4)0.50
O12−0.0731 (8)0.6245 (6)0.6494 (5)0.076 (3)
O130.1592 (8)0.6844 (6)0.5658 (5)0.077 (3)
O140.2189 (12)0.4826 (9)0.6113 (9)0.033 (4)0.50
O14A0.2767 (14)0.4726 (10)0.6443 (9)0.043 (4)0.50
O15−0.0919 (9)0.5605 (6)0.2994 (7)0.090 (3)
O160.2659 (13)0.4376 (10)0.4430 (9)0.036 (4)0.50
O16B0.2127 (12)0.4516 (9)0.4492 (8)0.028 (4)0.50
O17A−0.0469 (10)0.5874 (8)0.4826 (7)0.029 (3)0.50
O17B−0.0747 (10)0.4992 (8)0.4136 (7)0.028 (3)0.50
O18A0.0684 (10)0.4742 (8)0.4390 (7)0.027 (3)0.50
O18B−0.0905 (10)0.4306 (8)0.5014 (7)0.028 (3)0.50
O190.1508 (9)0.6552 (7)0.4225 (6)0.087 (3)
O200.4195 (13)0.4254 (10)0.4906 (10)0.104 (5)0.75
O20A0.412 (2)0.3654 (19)0.5690 (16)0.041 (8)0.25
O21A0.449 (2)0.5140 (17)0.5616 (15)0.034 (7)0.25
O210.4286 (12)0.4547 (10)0.6293 (9)0.100 (5)0.75
O220.1328 (8)0.5930 (6)0.6805 (7)0.085 (3)
U11U22U33U12U13U23
Si10.0201 (18)0.0165 (19)0.0221 (18)0.0002 (15)0.0064 (15)−0.0006 (15)
Fe10.0472 (11)0.0411 (11)0.0604 (12)−0.0018 (9)0.0109 (9)−0.0033 (9)
Mo10.0292 (5)0.0435 (6)0.0374 (6)−0.0003 (4)0.0090 (4)0.0018 (5)
Mo20.0549 (7)0.0418 (7)0.0353 (6)−0.0056 (5)0.0162 (5)−0.0055 (5)
Mo30.0418 (6)0.0427 (7)0.0500 (7)0.0061 (5)−0.0001 (5)−0.0015 (5)
Mo40.0297 (5)0.0392 (6)0.0513 (7)−0.0034 (4)0.0043 (4)−0.0140 (5)
Mo50.0460 (6)0.0235 (5)0.0442 (6)0.0013 (4)0.0036 (5)0.0015 (5)
Mo60.0300 (5)0.0322 (6)0.0487 (6)0.0053 (4)0.0030 (4)0.0082 (5)
Mo70.0296 (5)0.0275 (5)0.0440 (6)0.0044 (4)0.0071 (4)−0.0050 (4)
C10.075 (8)0.079 (8)0.079 (8)−0.011 (7)0.001 (7)−0.005 (7)
C20.080 (8)0.072 (8)0.072 (8)−0.004 (7)0.024 (7)−0.010 (7)
C30.053 (7)0.053 (7)0.058 (7)0.000 (6)0.007 (6)0.011 (6)
C40.051 (6)0.045 (6)0.051 (6)0.010 (5)0.017 (5)0.015 (5)
C50.072 (7)0.053 (7)0.056 (7)0.005 (6)0.019 (6)0.015 (6)
C60.064 (7)0.072 (8)0.074 (8)0.014 (6)0.025 (6)0.023 (7)
C70.060 (7)0.078 (8)0.071 (8)0.003 (7)0.013 (6)0.024 (7)
C80.055 (7)0.068 (8)0.064 (7)0.000 (6)0.006 (6)0.006 (6)
C90.093 (8)0.062 (8)0.080 (8)−0.006 (7)0.012 (7)0.019 (7)
C100.067 (8)0.075 (8)0.069 (7)−0.003 (7)0.008 (6)0.005 (7)
C110.059 (7)0.046 (7)0.049 (6)−0.007 (6)0.003 (5)−0.001 (5)
C120.048 (6)0.051 (7)0.046 (6)0.004 (5)0.010 (5)−0.001 (5)
C130.070 (8)0.080 (8)0.067 (8)0.002 (7)0.015 (6)0.014 (7)
C140.090 (9)0.108 (10)0.093 (9)0.014 (8)0.035 (8)0.011 (8)
C150.081 (8)0.077 (8)0.072 (8)0.022 (7)0.023 (7)0.005 (7)
C160.076 (8)0.063 (8)0.066 (7)0.015 (6)0.023 (6)0.016 (6)
C170.072 (7)0.061 (8)0.063 (7)0.011 (6)0.016 (6)0.008 (6)
C180.075 (8)0.059 (7)0.067 (7)−0.008 (6)0.022 (6)0.000 (6)
C190.053 (7)0.053 (7)0.057 (7)−0.010 (6)0.015 (6)−0.006 (6)
C200.040 (6)0.058 (7)0.059 (7)−0.007 (5)0.016 (5)−0.010 (6)
C210.078 (8)0.074 (8)0.090 (9)−0.024 (7)0.013 (7)−0.005 (7)
C220.078 (8)0.087 (9)0.071 (8)−0.022 (7)0.004 (7)−0.007 (7)
C230.076 (8)0.084 (8)0.067 (8)−0.005 (7)0.018 (6)0.004 (7)
C240.055 (7)0.062 (7)0.058 (7)−0.006 (6)0.010 (6)0.001 (6)
N10.055 (6)0.062 (7)0.063 (6)−0.004 (5)0.014 (5)−0.004 (5)
N20.050 (5)0.050 (6)0.052 (6)0.000 (5)0.011 (5)0.007 (5)
N30.062 (6)0.055 (6)0.055 (6)−0.006 (5)0.016 (5)−0.002 (5)
N40.073 (7)0.058 (7)0.077 (7)0.015 (6)−0.002 (6)−0.007 (6)
N50.059 (6)0.046 (6)0.056 (6)0.010 (5)0.000 (5)0.003 (5)
N60.057 (6)0.042 (6)0.055 (6)0.010 (5)0.011 (5)0.004 (5)
N70.060 (6)0.078 (7)0.075 (7)−0.001 (6)0.010 (6)0.006 (6)
N80.040 (5)0.061 (6)0.053 (6)−0.004 (5)0.004 (5)0.006 (5)
N90.056 (6)0.058 (6)0.060 (6)−0.003 (5)0.012 (5)0.010 (5)
O10.058 (3)0.057 (3)0.058 (3)−0.0004 (10)0.0125 (11)0.0000 (10)
O20.061 (3)0.062 (3)0.061 (3)0.0006 (10)0.0132 (11)0.0009 (10)
O30.061 (3)0.061 (3)0.062 (3)−0.0001 (10)0.0139 (11)0.0009 (10)
O40.051 (2)0.052 (2)0.052 (2)0.0003 (10)0.0108 (11)−0.0007 (10)
O50.055 (2)0.054 (2)0.053 (2)−0.0001 (10)0.0118 (11)−0.0002 (10)
O60.072 (6)0.092 (6)0.053 (5)−0.038 (5)0.019 (4)−0.017 (5)
O70.086 (6)0.056 (5)0.061 (5)−0.020 (5)−0.026 (5)0.019 (4)
O80.070 (5)0.101 (6)0.044 (5)−0.038 (5)0.017 (4)−0.002 (5)
O90.066 (3)0.066 (3)0.067 (3)0.0009 (10)0.0142 (11)−0.0014 (10)
O100.105 (7)0.073 (6)0.062 (6)−0.049 (5)0.018 (5)−0.014 (5)
O11A0.041 (8)0.035 (8)0.043 (8)−0.001 (7)0.010 (7)0.005 (6)
O11B0.028 (7)0.030 (7)0.038 (7)0.003 (6)0.000 (6)0.002 (6)
O120.087 (6)0.052 (5)0.070 (6)−0.028 (5)−0.026 (5)0.013 (5)
O130.092 (6)0.076 (6)0.053 (5)0.050 (5)−0.005 (5)−0.017 (5)
O140.033 (7)0.031 (7)0.036 (7)−0.003 (6)0.007 (6)0.007 (6)
O14A0.042 (7)0.039 (8)0.044 (8)0.003 (6)0.002 (6)−0.003 (6)
O150.093 (6)0.059 (6)0.138 (8)0.002 (5)0.069 (6)−0.010 (6)
O160.035 (7)0.038 (8)0.036 (7)0.008 (7)0.009 (6)0.000 (6)
O16B0.023 (7)0.033 (7)0.029 (7)0.004 (6)0.008 (6)−0.008 (6)
O17A0.025 (6)0.028 (6)0.033 (6)0.003 (5)0.004 (5)0.000 (5)
O17B0.030 (6)0.024 (6)0.034 (6)0.008 (5)0.013 (5)0.005 (5)
O18A0.027 (6)0.027 (6)0.023 (6)0.003 (5)0.000 (5)−0.003 (5)
O18B0.030 (6)0.023 (6)0.028 (6)0.001 (5)0.001 (5)−0.011 (5)
O190.101 (6)0.094 (6)0.060 (5)0.044 (5)0.006 (5)0.001 (5)
O200.096 (8)0.105 (9)0.114 (9)0.008 (7)0.031 (7)−0.007 (7)
O20A0.040 (11)0.048 (11)0.036 (11)0.020 (9)0.007 (8)0.000 (9)
O21A0.024 (9)0.043 (10)0.031 (10)−0.008 (8)0.001 (8)0.005 (8)
O210.079 (8)0.096 (9)0.111 (9)0.003 (7)−0.008 (7)−0.001 (7)
O220.086 (6)0.051 (6)0.136 (7)−0.005 (5)0.062 (6)−0.020 (5)
Si1—O17Ai1.606 (13)C1—H10.9300
Si1—O17A1.606 (13)C2—C31.410 (19)
Si1—O18A1.648 (13)C2—H20.9300
Si1—O18Ai1.648 (13)C3—N81.325 (16)
Si1—O18B1.670 (13)C3—C41.455 (18)
Si1—O18Bi1.670 (13)C4—N91.370 (16)
Si1—O17B1.684 (13)C4—C51.383 (18)
Si1—O17Bi1.684 (13)C5—C61.409 (19)
Fe1—N22.105 (11)C5—H50.9300
Fe1—N82.119 (11)C6—C71.32 (2)
Fe1—N52.153 (11)C6—H60.9300
Fe1—N32.173 (11)C7—C81.38 (2)
Fe1—N92.186 (12)C7—H70.9300
Fe1—N62.206 (11)C8—N91.369 (17)
Mo1—O31.657 (9)C8—H80.9300
Mo1—O71.823 (9)C9—C101.37 (2)
Mo1—O191.832 (11)C9—N41.368 (19)
Mo1—O16B1.892 (16)C9—H90.9300
Mo1—O11A2.010 (19)C10—C111.435 (19)
Mo1—O11B2.117 (17)C10—H100.9300
Mo1—O162.183 (17)C11—N51.335 (16)
Mo1—O18Bi2.406 (13)C11—C121.440 (18)
Mo1—O18A2.423 (13)C12—N61.332 (16)
Mo2—O51.646 (9)C12—C131.417 (19)
Mo2—O71.923 (9)C13—C141.38 (2)
Mo2—O12i1.940 (10)C13—H130.9300
Mo2—O151.950 (11)C14—C151.38 (2)
Mo2—O22i1.993 (10)C14—H140.9300
Mo2—O17B2.468 (13)C15—C161.37 (2)
Mo2—O18A2.498 (12)C15—H150.9300
Mo3—O211.700 (15)C16—N61.351 (17)
Mo3—O20A1.72 (3)C16—H160.9300
Mo3—O201.765 (17)C17—N11.313 (17)
Mo3—O21A1.84 (3)C17—C181.349 (19)
Mo3—O161.998 (16)C17—H170.9300
Mo3—O102.033 (9)C18—C191.444 (19)
Mo3—O11B2.051 (17)C18—H180.9300
Mo3—O11A2.086 (19)C19—N21.333 (16)
Mo3—O14A2.099 (16)C19—C201.452 (18)
Mo3—O142.164 (15)C20—N31.378 (16)
Mo3—O16B2.174 (15)C20—C211.411 (19)
Mo4—O41.663 (8)C21—C221.39 (2)
Mo4—O221.803 (10)C21—H210.9300
Mo4—O131.839 (9)C22—C231.37 (2)
Mo4—O141.895 (15)C22—H220.9300
Mo4—O11A1.903 (19)C23—C241.37 (2)
Mo4—O11B2.228 (18)C23—H230.9300
Mo4—O14A2.237 (17)C24—N31.335 (16)
Mo4—O17Bi2.397 (14)C24—H240.9300
Mo4—O18Bi2.435 (13)N1—N21.359 (14)
Mo5—O11.659 (9)N1—H1A0.8600
Mo5—O191.918 (11)N4—N51.382 (15)
Mo5—O81.928 (9)N4—H40.8600
Mo5—O61.952 (9)N7—N81.339 (14)
Mo5—O131.978 (9)N7—H7A0.8600
Mo5—O18Bi2.404 (13)O10—Mo7i2.058 (10)
Mo5—O17A2.463 (14)O10—Mo6i2.061 (11)
Mo6—O21.668 (9)O11A—O11B0.701 (18)
Mo6—O81.833 (9)O12—Mo2i1.940 (10)
Mo6—O151.832 (10)O14—O14A0.878 (17)
Mo6—O14i1.954 (15)O14—Mo6i1.954 (15)
Mo6—O10i2.061 (11)O14A—Mo6i2.119 (17)
Mo6—O14Ai2.119 (17)O16—O16B0.766 (16)
Mo6—O17B2.375 (13)O16—Mo7i2.154 (17)
Mo6—O17A2.480 (13)O16B—Mo7i1.943 (16)
Mo7—O91.664 (10)O17A—O18Bi1.778 (18)
Mo7—O121.818 (9)O17B—Mo4i2.397 (14)
Mo7—O61.840 (9)O18A—Mo7i2.389 (13)
Mo7—O16Bi1.943 (16)O18B—O17Ai1.778 (18)
Mo7—O10i2.058 (10)O18B—Mo5i2.404 (13)
Mo7—O16i2.154 (17)O18B—Mo1i2.406 (13)
Mo7—O18Ai2.389 (13)O18B—Mo4i2.435 (13)
Mo7—O17A2.417 (13)O20—O20A1.79 (4)
C1—C21.34 (2)O21A—O211.68 (3)
C1—N71.337 (19)O22—Mo2i1.993 (10)
O17Ai—Si1—O17A180.0 (10)O14i—Mo6—O14Ai24.5 (5)
O17Ai—Si1—O18A69.8 (7)O10i—Mo6—O14Ai74.5 (5)
O17A—Si1—O18A110.2 (7)O2—Mo6—O17B154.3 (5)
O17Ai—Si1—O18Ai110.2 (7)O8—Mo6—O17B101.6 (5)
O17A—Si1—O18Ai69.8 (7)O15—Mo6—O17B65.6 (5)
O18A—Si1—O18Ai180.000 (3)O14i—Mo6—O17B49.8 (6)
O17Ai—Si1—O18B65.7 (6)O10i—Mo6—O17B91.8 (4)
O17A—Si1—O18B114.3 (6)O14Ai—Mo6—O17B72.4 (6)
O18A—Si1—O18B108.4 (6)O2—Mo6—O17A156.3 (4)
O18Ai—Si1—O18B71.6 (6)O8—Mo6—O17A67.0 (4)
O17Ai—Si1—O18Bi114.3 (6)O15—Mo6—O17A101.0 (5)
O17A—Si1—O18Bi65.7 (6)O14i—Mo6—O17A76.8 (6)
O18A—Si1—O18Bi71.6 (6)O10i—Mo6—O17A63.1 (4)
O18Ai—Si1—O18Bi108.4 (6)O14Ai—Mo6—O17A100.1 (6)
O18B—Si1—O18Bi180.0 (6)O17B—Mo6—O17A47.2 (5)
O17Ai—Si1—O17B107.4 (7)O9—Mo7—O12102.6 (5)
O17A—Si1—O17B72.6 (7)O9—Mo7—O6100.4 (5)
O18A—Si1—O17B68.4 (6)O12—Mo7—O697.2 (4)
O18Ai—Si1—O17B111.6 (6)O9—Mo7—O16Bi111.2 (6)
O18B—Si1—O17B75.3 (6)O12—Mo7—O16Bi88.3 (5)
O18Bi—Si1—O17B104.7 (6)O6—Mo7—O16Bi145.8 (6)
O17Ai—Si1—O17Bi72.6 (7)O9—Mo7—O10i97.4 (5)
O17A—Si1—O17Bi107.4 (7)O12—Mo7—O10i156.2 (5)
O18A—Si1—O17Bi111.6 (6)O6—Mo7—O10i91.6 (4)
O18Ai—Si1—O17Bi68.4 (6)O16Bi—Mo7—O10i72.4 (5)
O18B—Si1—O17Bi104.7 (6)O9—Mo7—O16i90.5 (6)
O18Bi—Si1—O17Bi75.3 (6)O12—Mo7—O16i94.0 (5)
O17B—Si1—O17Bi180.000 (3)O6—Mo7—O16i162.2 (5)
N2—Fe1—N8102.7 (4)O16Bi—Mo7—O16i20.7 (5)
N2—Fe1—N5161.1 (4)O10i—Mo7—O16i72.9 (5)
N8—Fe1—N589.3 (4)O9—Mo7—O18Ai156.7 (5)
N2—Fe1—N376.0 (4)O12—Mo7—O18Ai66.4 (5)
N8—Fe1—N3166.1 (4)O6—Mo7—O18Ai101.3 (5)
N5—Fe1—N395.8 (4)O16Bi—Mo7—O18Ai50.4 (6)
N2—Fe1—N996.8 (4)O10i—Mo7—O18Ai90.3 (4)
N8—Fe1—N975.2 (4)O16i—Mo7—O18Ai70.7 (5)
N5—Fe1—N9100.5 (4)O9—Mo7—O17A155.7 (5)
N3—Fe1—N991.1 (4)O12—Mo7—O17A99.3 (5)
N2—Fe1—N690.3 (4)O6—Mo7—O17A66.2 (5)
N8—Fe1—N692.0 (4)O16Bi—Mo7—O17A79.6 (6)
N5—Fe1—N674.5 (4)O10i—Mo7—O17A64.3 (5)
N3—Fe1—N6101.8 (4)O16i—Mo7—O17A98.4 (6)
N9—Fe1—N6166.5 (4)O18Ai—Mo7—O17A45.6 (4)
O3—Mo1—O7101.6 (5)C2—C1—N7110.5 (15)
O3—Mo1—O19102.0 (5)C2—C1—H1124.7
O7—Mo1—O1995.9 (5)N7—C1—H1124.8
O3—Mo1—O16B111.0 (6)C1—C2—C3102.9 (15)
O7—Mo1—O16B89.0 (5)C1—C2—H2128.5
O19—Mo1—O16B144.9 (6)C3—C2—H2128.6
O3—Mo1—O11A108.1 (6)N8—C3—C2111.1 (13)
O7—Mo1—O11A147.9 (6)N8—C3—C4117.5 (13)
O19—Mo1—O11A89.7 (6)C2—C3—C4131.4 (14)
O16B—Mo1—O11A69.4 (7)N9—C4—C5121.5 (13)
O3—Mo1—O11B88.8 (6)N9—C4—C3114.1 (12)
O7—Mo1—O11B165.0 (6)C5—C4—C3124.4 (13)
O19—Mo1—O11B92.5 (6)C4—C5—C6118.5 (14)
O16B—Mo1—O11B77.0 (6)C4—C5—H5120.7
O11A—Mo1—O11B19.3 (5)C6—C5—H5120.8
O3—Mo1—O1690.9 (6)C7—C6—C5119.9 (15)
O7—Mo1—O1693.6 (5)C7—C6—H6120.1
O19—Mo1—O16162.0 (6)C5—C6—H6120.0
O16B—Mo1—O1620.1 (5)C6—C7—C8120.6 (16)
O11A—Mo1—O1674.4 (7)C6—C7—H7119.6
O11B—Mo1—O1675.2 (6)C8—C7—H7119.8
O3—Mo1—O18Bi154.5 (4)N9—C8—C7121.8 (15)
O7—Mo1—O18Bi100.7 (5)N9—C8—H8119.1
O19—Mo1—O18Bi63.6 (5)C7—C8—H8119.1
O16B—Mo1—O18Bi81.4 (6)C10—C9—N4106.4 (14)
O11A—Mo1—O18Bi54.1 (6)C10—C9—H9126.8
O11B—Mo1—O18Bi71.9 (6)N4—C9—H9126.7
O16—Mo1—O18Bi99.7 (5)C9—C10—C11105.6 (14)
O3—Mo1—O18A156.2 (5)C9—C10—H10127.1
O7—Mo1—O18A67.5 (4)C11—C10—H10127.2
O19—Mo1—O18A100.2 (5)N5—C11—C10111.2 (13)
O16B—Mo1—O18A50.1 (6)N5—C11—C12117.7 (12)
O11A—Mo1—O18A80.4 (6)C10—C11—C12131.1 (13)
O11B—Mo1—O18A98.8 (6)N6—C12—C13122.3 (13)
O16—Mo1—O18A69.6 (5)N6—C12—C11115.7 (11)
O18Bi—Mo1—O18A47.4 (4)C13—C12—C11121.9 (13)
O5—Mo2—O7102.7 (4)C14—C13—C12118.5 (16)
O5—Mo2—O12i103.1 (4)C14—C13—H13120.7
O7—Mo2—O12i88.3 (4)C12—C13—H13120.7
O5—Mo2—O15101.1 (5)C13—C14—C15117.6 (17)
O7—Mo2—O1589.7 (5)C13—C14—H14121.1
O12i—Mo2—O15155.6 (5)C15—C14—H14121.3
O5—Mo2—O22i101.5 (5)C16—C15—C14121.8 (17)
O7—Mo2—O22i155.8 (5)C16—C15—H15119.2
O12i—Mo2—O22i85.7 (4)C14—C15—H15119.1
O15—Mo2—O22i86.2 (4)N6—C16—C15121.1 (15)
O5—Mo2—O17B155.9 (4)N6—C16—H16119.5
O7—Mo2—O17B94.9 (5)C15—C16—H16119.4
O12i—Mo2—O17B93.7 (4)N1—C17—C18109.6 (14)
O15—Mo2—O17B62.2 (5)N1—C17—H17125.2
O22i—Mo2—O17B62.2 (4)C18—C17—H17125.2
O5—Mo2—O18A159.8 (4)C17—C18—C19102.8 (14)
O7—Mo2—O18A64.6 (4)C17—C18—H18128.7
O12i—Mo2—O18A62.6 (4)C19—C18—H18128.5
O15—Mo2—O18A94.8 (5)N2—C19—C18111.2 (12)
O22i—Mo2—O18A92.0 (5)N2—C19—C20116.9 (12)
O17B—Mo2—O18A44.3 (4)C18—C19—C20131.9 (13)
O21—Mo3—O20A66.1 (11)N3—C20—C21120.6 (13)
O21—Mo3—O2097.1 (8)N3—C20—C19114.9 (11)
O20A—Mo3—O2061.9 (12)C21—C20—C19124.5 (14)
O21—Mo3—O21A56.4 (10)C22—C21—C20116.7 (16)
O20A—Mo3—O21A92.6 (14)C22—C21—H21121.6
O20—Mo3—O21A66.6 (11)C20—C21—H21121.8
O21—Mo3—O16161.4 (8)C23—C22—C21121.5 (16)
O20A—Mo3—O16104.3 (11)C23—C22—H22119.2
O20—Mo3—O1664.5 (7)C21—C22—H22119.2
O21A—Mo3—O16110.4 (10)C24—C23—C22119.2 (16)
O21—Mo3—O10115.0 (7)C24—C23—H23120.4
O20A—Mo3—O1079.4 (11)C22—C23—H23120.4
O20—Mo3—O10113.0 (7)N3—C24—C23121.5 (14)
O21A—Mo3—O10170.5 (9)N3—C24—H24119.2
O16—Mo3—O1076.8 (6)C23—C24—H24119.2
O21—Mo3—O11B102.1 (7)C17—N1—N2112.8 (12)
O20A—Mo3—O11B157.2 (12)C17—N1—H1A123.5
O20—Mo3—O11B102.4 (8)N2—N1—H1A123.7
O21A—Mo3—O11B65.1 (10)C19—N2—N1103.6 (11)
O16—Mo3—O11B80.8 (7)C19—N2—Fe1117.6 (9)
O10—Mo3—O11B123.3 (6)N1—N2—Fe1138.7 (9)
O21—Mo3—O11A111.9 (8)C24—N3—C20120.2 (12)
O20A—Mo3—O11A176.6 (12)C24—N3—Fe1125.0 (10)
O20—Mo3—O11A116.3 (8)C20—N3—Fe1114.6 (8)
O21A—Mo3—O11A84.1 (10)C9—N4—N5112.5 (13)
O16—Mo3—O11A76.8 (7)C9—N4—H4123.8
O10—Mo3—O11A104.0 (6)N5—N4—H4123.7
O11B—Mo3—O11A19.5 (5)C11—N5—N4104.1 (12)
O21—Mo3—O14A65.6 (8)C11—N5—Fe1115.4 (9)
O20A—Mo3—O14A107.0 (11)N4—N5—Fe1138.9 (10)
O20—Mo3—O14A162.7 (7)C12—N6—C16118.5 (12)
O21A—Mo3—O14A102.4 (10)C12—N6—Fe1114.9 (8)
O16—Mo3—O14A132.9 (7)C16—N6—Fe1125.8 (10)
O10—Mo3—O14A75.5 (5)C1—N7—N8109.7 (13)
O11B—Mo3—O14A83.6 (7)C1—N7—H7A125.1
O11A—Mo3—O14A74.0 (7)N8—N7—H7A125.2
O21—Mo3—O1488.8 (7)C3—N8—N7105.7 (12)
O20A—Mo3—O14124.0 (11)C3—N8—Fe1117.6 (9)
O20—Mo3—O14173.2 (7)N7—N8—Fe1136.6 (10)
O21A—Mo3—O14114.7 (10)C8—N9—C4117.6 (12)
O16—Mo3—O14109.4 (7)C8—N9—Fe1126.9 (10)
O10—Mo3—O1466.9 (5)C4—N9—Fe1115.4 (8)
O11B—Mo3—O1473.0 (6)Mo7—O6—Mo5137.3 (6)
O11A—Mo3—O1458.0 (6)Mo1—O7—Mo2137.5 (6)
O14A—Mo3—O1423.7 (5)Mo6—O8—Mo5136.7 (5)
O21—Mo3—O16B174.7 (7)Mo3—O10—Mo7i106.3 (4)
O20A—Mo3—O16B119.1 (11)Mo3—O10—Mo6i107.2 (4)
O20—Mo3—O16B84.9 (7)Mo7i—O10—Mo6i129.4 (6)
O21A—Mo3—O16B120.5 (9)O11B—O11A—Mo4109 (3)
O16—Mo3—O16B20.6 (5)O11B—O11A—Mo189 (3)
O10—Mo3—O16B68.3 (5)Mo4—O11A—Mo1143.0 (10)
O11B—Mo3—O16B72.6 (6)O11B—O11A—Mo377 (2)
O11A—Mo3—O16B62.9 (7)Mo4—O11A—Mo3111.0 (9)
O14A—Mo3—O16B112.4 (6)Mo1—O11A—Mo3104.4 (8)
O14—Mo3—O16B88.8 (6)O11A—O11B—Mo383 (2)
O4—Mo4—O22101.8 (5)O11A—O11B—Mo172 (2)
O4—Mo4—O13100.9 (5)Mo3—O11B—Mo1101.9 (7)
O22—Mo4—O1396.4 (5)O11A—O11B—Mo454 (2)
O4—Mo4—O14110.5 (6)Mo3—O11B—Mo4100.4 (7)
O22—Mo4—O1491.7 (6)Mo1—O11B—Mo4117.2 (7)
O13—Mo4—O14145.2 (6)Mo7—O12—Mo2i138.9 (6)
O4—Mo4—O11A106.1 (6)Mo4—O13—Mo5135.4 (6)
O22—Mo4—O11A148.9 (7)O14A—O14—Mo4101.1 (17)
O13—Mo4—O11A91.8 (6)O14A—O14—Mo6i88.3 (16)
O14—Mo4—O11A65.8 (7)Mo4—O14—Mo6i145.8 (9)
O4—Mo4—O11B89.0 (5)O14A—O14—Mo373.9 (15)
O22—Mo4—O11B164.8 (6)Mo4—O14—Mo3108.0 (7)
O13—Mo4—O11B91.9 (5)Mo6i—O14—Mo3106.1 (7)
O14—Mo4—O11B74.4 (6)O14—O14A—Mo382.4 (16)
O11A—Mo4—O11B17.4 (6)O14—O14A—Mo6i67.2 (15)
O4—Mo4—O14A88.1 (5)Mo3—O14A—Mo6i102.7 (7)
O22—Mo4—O14A93.1 (5)O14—O14A—Mo456.2 (15)
O13—Mo4—O14A165.3 (5)Mo3—O14A—Mo498.6 (7)
O14—Mo4—O14A22.7 (5)Mo6i—O14A—Mo4115.3 (8)
O11A—Mo4—O14A74.4 (7)Mo6—O15—Mo2138.4 (7)
O11B—Mo4—O14A76.5 (6)O16B—O16—Mo392.8 (19)
O4—Mo4—O17Bi153.6 (4)O16B—O16—Mo7i63.9 (19)
O22—Mo4—O17Bi66.0 (5)Mo3—O16—Mo7i104.0 (7)
O13—Mo4—O17Bi103.7 (5)O16B—O16—Mo158.0 (18)
O14—Mo4—O17Bi49.8 (6)Mo3—O16—Mo1101.4 (7)
O11A—Mo4—O17Bi82.9 (6)Mo7i—O16—Mo1116.9 (8)
O11B—Mo4—O17Bi99.7 (5)O16—O16B—Mo1102 (2)
O14A—Mo4—O17Bi70.0 (5)O16—O16B—Mo7i95 (2)
O4—Mo4—O18Bi153.7 (4)Mo1—O16B—Mo7i149.0 (9)
O22—Mo4—O18Bi102.3 (5)O16—O16B—Mo366.6 (18)
O13—Mo4—O18Bi66.0 (4)Mo1—O16B—Mo3105.3 (7)
O14—Mo4—O18Bi79.3 (6)Mo7i—O16B—Mo3105.2 (7)
O11A—Mo4—O18Bi54.4 (6)Si1—O17A—O18Bi58.9 (6)
O11B—Mo4—O18Bi69.6 (5)Si1—O17A—Mo7122.6 (7)
O14A—Mo4—O18Bi101.0 (5)O18Bi—O17A—Mo7130.3 (8)
O17Bi—Mo4—O18Bi50.1 (5)Si1—O17A—Mo5125.7 (7)
O1—Mo5—O19100.9 (5)O18Bi—O17A—Mo566.8 (6)
O1—Mo5—O8101.2 (4)Mo7—O17A—Mo592.7 (5)
O19—Mo5—O890.3 (4)Si1—O17A—Mo6119.1 (7)
O1—Mo5—O6101.8 (4)O18Bi—O17A—Mo6124.3 (8)
O19—Mo5—O6157.2 (5)Mo7—O17A—Mo699.0 (5)
O8—Mo5—O687.2 (4)Mo5—O17A—Mo690.0 (4)
O1—Mo5—O1399.9 (4)Si1—O17B—Mo6121.1 (7)
O19—Mo5—O1387.1 (4)Si1—O17B—Mo4i117.9 (6)
O8—Mo5—O13158.8 (4)Mo6—O17B—Mo4i100.9 (5)
O6—Mo5—O1387.2 (4)Si1—O17B—Mo2123.6 (6)
O1—Mo5—O18Bi156.9 (4)Mo6—O17B—Mo293.7 (4)
O19—Mo5—O18Bi62.6 (5)Mo4i—O17B—Mo293.6 (5)
O8—Mo5—O18Bi95.3 (4)Si1—O18A—Mo7i122.1 (7)
O6—Mo5—O18Bi95.0 (5)Si1—O18A—Mo1120.6 (7)
O13—Mo5—O18Bi64.9 (4)Mo7i—O18A—Mo1100.3 (5)
O1—Mo5—O17A160.3 (4)Si1—O18A—Mo2123.7 (6)
O19—Mo5—O17A94.5 (5)Mo7i—O18A—Mo292.1 (4)
O8—Mo5—O17A66.2 (4)Mo1—O18A—Mo290.4 (4)
O6—Mo5—O17A63.8 (4)Si1—O18B—O17Ai55.4 (6)
O13—Mo5—O17A93.0 (5)Si1—O18B—Mo5i125.8 (7)
O18Bi—Mo5—O17A42.8 (4)O17Ai—O18B—Mo5i70.4 (6)
O2—Mo6—O8101.7 (5)Si1—O18B—Mo1i120.5 (6)
O2—Mo6—O15101.0 (5)O17Ai—O18B—Mo1i132.3 (8)
O8—Mo6—O1596.4 (5)Mo5i—O18B—Mo1i94.1 (5)
O2—Mo6—O14i111.8 (6)Si1—O18B—Mo4i116.6 (7)
O8—Mo6—O14i143.8 (6)O17Ai—O18B—Mo4i125.0 (8)
O15—Mo6—O14i90.5 (6)Mo5i—O18B—Mo4i93.7 (4)
O2—Mo6—O10i98.0 (5)Mo1i—O18B—Mo4i100.1 (5)
O8—Mo6—O10i92.2 (4)Mo1—O19—Mo5139.7 (7)
O15—Mo6—O10i157.0 (5)Mo3—O20—O20A57.8 (11)
O14i—Mo6—O10i70.5 (5)Mo3—O20A—O2060.3 (11)
O2—Mo6—O14Ai87.4 (6)O21—O21A—Mo357.7 (10)
O8—Mo6—O14Ai165.0 (5)O21A—O21—Mo365.9 (11)
O15—Mo6—O14Ai93.6 (6)Mo4—O22—Mo2i138.2 (6)
D—H···AD—HH···AD···AD—H···A
N4—H4···O13ii0.862.152.973 (17)159
N1—H1A···O21Aiii0.862.172.96 (3)152
N1—H1A···O21iii0.862.052.844 (19)153
Table 1

Selected bond lengths (Å)

Si1—O17A1.606 (13)
Si1—O18A1.648 (13)
Si1—O18B1.670 (13)
Si1—O17B1.684 (13)
Fe1—N22.105 (11)
Fe1—N82.119 (11)
Fe1—N52.153 (11)
Fe1—N32.173 (11)
Fe1—N92.186 (12)
Fe1—N62.206 (11)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
N4—H4⋯O13i0.862.152.973 (17)159
N1—H1A⋯O21Aii0.862.172.96 (3)152
N1—H1A⋯O21ii0.862.052.844 (19)153

Symmetry codes: (i) ; (ii) .

  5 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Tris{aqua-bis[3-(2-pyrid-yl)-1H-pyrazole]copper(II)} di-μ(9)-arsenato-hexa-triaconta-μ(2)-oxido-octa-deca-oxidoocta-deca-molybdate(VI).

Authors:  Xiutang Zhang; Peihai Wei; Congwen Shi; Bin Li; Bo Hu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-16

3.  Diaqua-1κO,2κO-(2,2'-bi-1H-imidazole-1κN,N)(oxalato-2κO,O)di-μ-oxido-κO:O-dioxido-1κO,2κO-dimolyb-denum(V) trihydrate.

Authors:  Xiutang Zhang; Peihai Wei; Congwen Shi; Bin Li; Bo Hu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-12-09

4.  Bis{tris-[3-(2-pyrid-yl)-1H-pyrazole]nickel(II)} dodeca-molybdosilicate tetra-hydrate.

Authors:  Xiutang Zhang; Dong Yuan; Peihai Wei; Bin Li; Bo Hu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-13

5.  Bis{tris-[3-(2-pyrid-yl)-1H-pyrazole]zinc(II)} dodeca-molybdosilicate hexa-hydrate.

Authors:  Xiutang Zhang; Peihai Wei; Wencai Zhu; Bin Li; Bo Hu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-09
  5 in total

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