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The title inorganic-organic hybrid, (C10H10N2)(C10H9N2)2[GeMo12O40]·2H2O, is composed of molybdogermanate anions (site symmetry 2), mono- and diprotonated 4,4'-bipyridinium cations (the latter also on a twofold rotation axis), and isolated water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040578/mg2004sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040578/mg2004Isup2.hkl
Contains datablock I

CCDC reference: 628004

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.038
  • wR factor = 0.094
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.77 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT432_ALERT_2_C Short Inter X...Y Contact O9 .. C12 .. 2.95 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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[4,4'-bipyridinium(1+)] 4,4'-bipyridinium(2+) dodecamolybdogermanate(4-) dihydrate top
Crystal data top
(C10H10N2)(C10H9N2)2[GeMo12O40]·2H2OF(000) = 4504
Mr = 2372.51Dx = 2.753 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 8347 reflections
a = 15.214 (2) Åθ = 1.6–27.0°
b = 18.215 (3) ŵ = 3.16 mm1
c = 21.231 (3) ÅT = 296 K
β = 103.370 (3)°Block, yellow
V = 5724.1 (15) Å30.27 × 0.24 × 0.17 mm
Z = 4
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
5612 independent reflections
Radiation source: fine-focus sealed tube4264 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
ω scansθmax = 26.1°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1818
Tmin = 0.452, Tmax = 0.585k = 2122
15147 measured reflectionsl = 2626
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0391P)2 + 10.584P]
where P = (Fo2 + 2Fc2)/3
5612 reflections(Δ/σ)max < 0.001
422 parametersΔρmax = 0.81 e Å3
0 restraintsΔρmin = 0.77 e Å3
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
xyzUiso*/Ueq
Ge0.00000.15053 (4)0.25000.01909 (18)
Mo10.01364 (4)0.01139 (3)0.13524 (3)0.02943 (15)
Mo20.03095 (4)0.28862 (3)0.14134 (3)0.03353 (15)
Mo30.16723 (4)0.01702 (3)0.30026 (3)0.03070 (15)
Mo40.14070 (4)0.14285 (3)0.09167 (3)0.03468 (16)
Mo50.18899 (4)0.15924 (3)0.17989 (3)0.03004 (15)
Mo60.17229 (4)0.28675 (3)0.28900 (3)0.03377 (15)
O10.0769 (2)0.2061 (2)0.22332 (18)0.0244 (8)
O20.0566 (2)0.09562 (19)0.18710 (17)0.0218 (8)
O30.2101 (3)0.0657 (2)0.38397 (19)0.0309 (9)
O40.1070 (3)0.0897 (2)0.14149 (18)0.0283 (9)
O50.0403 (3)0.2120 (2)0.09784 (19)0.0318 (10)
O60.1826 (3)0.2116 (2)0.3550 (2)0.0326 (10)
O70.0604 (3)0.0683 (2)0.06853 (19)0.0305 (9)
O80.0845 (3)0.0118 (2)0.22265 (19)0.0306 (9)
O90.2446 (3)0.2328 (2)0.2458 (2)0.0349 (10)
O100.0845 (3)0.0377 (2)0.1530 (2)0.0327 (10)
O110.2028 (3)0.1623 (2)0.0174 (2)0.0448 (12)
O120.0559 (3)0.0506 (2)0.0919 (2)0.0412 (11)
O130.1398 (3)0.2364 (2)0.12543 (19)0.0340 (10)
O140.2820 (3)0.1387 (2)0.1528 (2)0.0425 (11)
O150.2454 (3)0.3495 (2)0.3270 (2)0.0453 (12)
O160.2101 (3)0.0914 (2)0.25645 (19)0.0310 (9)
O170.0624 (3)0.3133 (2)0.1808 (2)0.0354 (10)
O180.1178 (3)0.3381 (2)0.2114 (2)0.0351 (10)
O190.2470 (3)0.0483 (2)0.3084 (2)0.0431 (11)
O200.0242 (3)0.3540 (2)0.0851 (2)0.0440 (12)
OW0.1083 (6)0.5186 (5)0.0119 (6)0.213 (7)
HW10.12420.56590.01660.255*
HW20.08710.51310.04880.255*
N10.2504 (4)0.4309 (3)0.0245 (3)0.0489 (16)
HN10.20440.46610.02060.059*
N20.5674 (5)0.1471 (3)0.0677 (3)0.0561 (18)
N30.50000.3460 (4)0.25000.044 (2)
HN30.50000.39870.25000.053*
N40.50000.0364 (5)0.25000.062 (3)
HN40.50000.08900.25000.074*
C10.2412 (5)0.3752 (5)0.0630 (4)0.0501 (19)
H10.19270.37430.08270.060*
C20.3022 (5)0.3200 (4)0.0735 (3)0.0418 (16)
H20.29520.28070.09980.050*
C30.3756 (4)0.3223 (3)0.0447 (3)0.0339 (14)
C40.3826 (4)0.3823 (4)0.0051 (3)0.0372 (15)
H40.43100.38570.01460.045*
C50.3190 (5)0.4351 (4)0.0043 (3)0.0438 (17)
H50.32310.47470.03110.053*
C60.4810 (6)0.1369 (4)0.0733 (4)0.053 (2)
H60.46370.08990.08270.064*
C70.4192 (5)0.1907 (3)0.0659 (3)0.0405 (16)
H70.36050.18050.06900.049*
C80.4435 (4)0.2613 (3)0.0538 (3)0.0332 (14)
C90.5330 (4)0.2742 (4)0.0500 (3)0.0365 (15)
H90.55290.32100.04260.044*
C100.5906 (5)0.2143 (4)0.0578 (4)0.0480 (18)
H100.65020.22270.05590.058*
C110.5561 (5)0.3102 (4)0.2206 (3)0.0426 (17)
H110.59460.33620.20050.051*
C120.5563 (4)0.2343 (3)0.2203 (3)0.0364 (15)
H120.59520.20950.19970.044*
C130.50000.1945 (4)0.25000.0263 (18)
C140.50000.1138 (4)0.25000.0288 (19)
C150.4338 (5)0.0737 (3)0.2707 (3)0.0418 (17)
H150.38810.09830.28460.050*
C160.4352 (5)0.0009 (4)0.2707 (4)0.056 (2)
H160.39120.02710.28510.067*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ge0.0199 (4)0.0163 (4)0.0226 (4)0.0000.0080 (3)0.000
Mo10.0327 (3)0.0250 (3)0.0346 (3)0.0008 (2)0.0161 (2)0.0072 (2)
Mo20.0338 (3)0.0305 (3)0.0381 (3)0.0011 (2)0.0119 (2)0.0123 (2)
Mo30.0299 (3)0.0292 (3)0.0364 (3)0.0108 (2)0.0145 (2)0.0067 (2)
Mo40.0367 (3)0.0356 (3)0.0291 (3)0.0016 (2)0.0022 (2)0.0031 (2)
Mo50.0268 (3)0.0296 (3)0.0384 (3)0.0017 (2)0.0170 (2)0.0005 (2)
Mo60.0309 (3)0.0295 (3)0.0415 (3)0.0085 (2)0.0097 (2)0.0057 (2)
O10.0204 (19)0.023 (2)0.032 (2)0.0036 (16)0.0109 (17)0.0005 (16)
O20.022 (2)0.0184 (19)0.026 (2)0.0002 (15)0.0078 (16)0.0018 (15)
O30.028 (2)0.035 (2)0.031 (2)0.0069 (18)0.0075 (18)0.0041 (18)
O40.032 (2)0.028 (2)0.028 (2)0.0043 (18)0.0135 (18)0.0033 (17)
O50.033 (2)0.032 (2)0.031 (2)0.0025 (18)0.0091 (19)0.0028 (18)
O60.033 (2)0.033 (2)0.032 (2)0.0030 (19)0.0083 (19)0.0018 (18)
O70.037 (2)0.031 (2)0.027 (2)0.0025 (19)0.0124 (18)0.0024 (17)
O80.037 (2)0.024 (2)0.034 (2)0.0064 (18)0.0154 (19)0.0028 (17)
O90.030 (2)0.036 (2)0.041 (3)0.0083 (19)0.012 (2)0.0002 (19)
O100.039 (2)0.025 (2)0.036 (2)0.0082 (19)0.012 (2)0.0051 (18)
O110.042 (3)0.052 (3)0.038 (3)0.001 (2)0.004 (2)0.002 (2)
O120.052 (3)0.035 (2)0.042 (3)0.002 (2)0.023 (2)0.007 (2)
O130.035 (2)0.035 (2)0.035 (2)0.0017 (19)0.014 (2)0.0079 (19)
O140.040 (3)0.044 (3)0.052 (3)0.000 (2)0.027 (2)0.006 (2)
O150.045 (3)0.038 (3)0.055 (3)0.018 (2)0.016 (2)0.006 (2)
O160.028 (2)0.034 (2)0.034 (2)0.0026 (18)0.0131 (18)0.0037 (18)
O170.039 (3)0.027 (2)0.043 (3)0.0028 (19)0.015 (2)0.0039 (19)
O180.041 (3)0.021 (2)0.046 (3)0.0071 (18)0.016 (2)0.0012 (18)
O190.043 (3)0.042 (3)0.046 (3)0.019 (2)0.015 (2)0.008 (2)
O200.048 (3)0.042 (3)0.045 (3)0.001 (2)0.017 (2)0.014 (2)
OW0.117 (7)0.110 (7)0.340 (16)0.062 (6)0.090 (9)0.148 (9)
N10.033 (3)0.048 (4)0.061 (4)0.006 (3)0.003 (3)0.024 (3)
N20.068 (5)0.038 (4)0.058 (4)0.013 (3)0.004 (4)0.005 (3)
N30.056 (5)0.017 (4)0.056 (5)0.0000.010 (4)0.000
N40.054 (6)0.027 (4)0.112 (8)0.0000.036 (6)0.000
C10.039 (4)0.061 (5)0.055 (5)0.009 (4)0.021 (4)0.027 (4)
C20.039 (4)0.045 (4)0.046 (4)0.004 (3)0.019 (3)0.007 (3)
C30.035 (4)0.033 (3)0.033 (3)0.003 (3)0.008 (3)0.008 (3)
C40.038 (4)0.045 (4)0.032 (4)0.003 (3)0.016 (3)0.000 (3)
C50.043 (4)0.045 (4)0.044 (4)0.005 (3)0.012 (3)0.011 (3)
C60.076 (6)0.030 (4)0.049 (5)0.002 (4)0.006 (4)0.001 (3)
C70.053 (4)0.032 (4)0.037 (4)0.013 (3)0.011 (3)0.001 (3)
C80.039 (4)0.038 (4)0.026 (3)0.001 (3)0.013 (3)0.000 (3)
C90.042 (4)0.038 (4)0.030 (3)0.004 (3)0.011 (3)0.001 (3)
C100.041 (4)0.050 (5)0.055 (5)0.007 (3)0.014 (4)0.004 (4)
C110.045 (4)0.024 (3)0.063 (5)0.004 (3)0.020 (4)0.006 (3)
C120.033 (4)0.031 (3)0.049 (4)0.002 (3)0.018 (3)0.006 (3)
C130.021 (4)0.018 (4)0.037 (5)0.0000.001 (4)0.000
C140.024 (4)0.021 (4)0.038 (5)0.0000.002 (4)0.000
C150.038 (4)0.026 (3)0.067 (5)0.004 (3)0.024 (4)0.002 (3)
C160.043 (4)0.028 (4)0.102 (7)0.003 (3)0.028 (4)0.004 (4)
Geometric parameters (Å, º) top
Ge—O21.730 (4)OW—HW10.8951
Ge—O11.737 (4)OW—HW20.9176
Mo1—O121.675 (4)N1—C11.328 (10)
Mo1—O101.853 (4)N1—C51.329 (9)
Mo1—O71.900 (4)N1—HN10.9400
Mo1—O81.964 (4)N2—C101.305 (9)
Mo1—O41.995 (4)N2—C61.360 (11)
Mo1—O22.292 (3)N3—C111.338 (7)
Mo2—O201.673 (4)N3—HN30.9594
Mo2—O171.863 (4)N4—C161.337 (8)
Mo2—O51.875 (4)N4—HN40.9575
Mo2—O181.965 (4)C1—C21.352 (10)
Mo2—O132.005 (4)C1—H10.9300
Mo2—O12.284 (4)C2—C31.392 (9)
Mo3—O191.679 (4)C2—H20.9300
Mo3—O161.845 (4)C3—C41.397 (9)
Mo3—O81.901 (4)C3—C81.499 (9)
Mo3—O31.958 (4)C4—C51.346 (9)
Mo3—O10i2.035 (4)C4—H40.9300
Mo3—O2i2.272 (4)C5—H50.9300
Mo4—O111.677 (4)C6—C71.342 (10)
Mo4—O6i1.895 (4)C6—H60.9300
Mo4—O3i1.901 (4)C7—C81.379 (9)
Mo4—O51.960 (4)C7—H70.9300
Mo4—O71.964 (4)C8—C91.402 (9)
Mo4—O22.298 (4)C9—C101.385 (9)
Mo5—O141.688 (4)C9—H90.9300
Mo5—O41.832 (4)C10—H100.9300
Mo5—O131.863 (4)C11—C121.383 (9)
Mo5—O91.980 (4)C11—H110.9300
Mo5—O162.008 (4)C12—C131.381 (7)
Mo5—O12.284 (4)C12—H120.9300
Mo6—O151.668 (4)C13—C141.471 (11)
Mo6—O91.866 (4)C14—C151.395 (7)
Mo6—O181.909 (4)C15—C161.359 (9)
Mo6—O61.939 (4)C15—H150.9300
Mo6—O17i1.984 (4)C16—H160.9300
Mo6—O12.297 (4)
O2—Ge—O2i109.4 (2)O15—Mo6—O1171.78 (19)
O2—Ge—O1109.73 (17)O9—Mo6—O174.13 (15)
O2i—Ge—O1109.61 (17)O18—Mo6—O172.69 (15)
O1i—Ge—O1108.8 (2)O6—Mo6—O185.45 (15)
O12—Mo1—O10102.4 (2)O17i—Mo6—O183.74 (16)
O12—Mo1—O7101.2 (2)Ge—O1—Mo5122.43 (19)
O10—Mo1—O792.75 (18)Ge—O1—Mo2121.44 (18)
O12—Mo1—O8100.23 (19)Mo5—O1—Mo293.64 (14)
O10—Mo1—O889.79 (17)Ge—O1—Mo6123.59 (19)
O7—Mo1—O8157.28 (16)Mo5—O1—Mo693.31 (13)
O12—Mo1—O499.28 (19)Mo2—O1—Mo694.60 (13)
O10—Mo1—O4157.87 (16)Ge—O2—Mo3i121.56 (18)
O7—Mo1—O487.12 (16)Ge—O2—Mo1123.59 (18)
O8—Mo1—O482.19 (16)Mo3i—O2—Mo194.32 (13)
O12—Mo1—O2174.57 (18)Ge—O2—Mo4122.70 (18)
O10—Mo1—O274.82 (15)Mo3i—O2—Mo493.65 (13)
O7—Mo1—O274.39 (15)Mo1—O2—Mo493.06 (13)
O8—Mo1—O284.54 (15)Mo4i—O3—Mo3119.49 (19)
O4—Mo1—O283.87 (14)Mo5—O4—Mo1157.7 (2)
O20—Mo2—O17102.8 (2)Mo2—O5—Mo4149.8 (2)
O20—Mo2—O5104.2 (2)Mo4i—O6—Mo6156.4 (2)
O17—Mo2—O589.25 (18)Mo1—O7—Mo4119.1 (2)
O20—Mo2—O1897.7 (2)Mo3—O8—Mo1150.3 (2)
O17—Mo2—O1889.90 (18)Mo6—O9—Mo5120.0 (2)
O5—Mo2—O18157.76 (16)Mo1—O10—Mo3i118.75 (19)
O20—Mo2—O1397.7 (2)Mo5—O13—Mo2118.9 (2)
O17—Mo2—O13159.31 (17)Mo3—O16—Mo5148.3 (2)
O5—Mo2—O1388.25 (17)Mo2—O17—Mo6i150.9 (2)
O18—Mo2—O1384.75 (18)Mo6—O18—Mo2120.66 (19)
O20—Mo2—O1165.99 (19)HW1—OW—HW298.6
O17—Mo2—O186.98 (16)C1—N1—C5122.2 (6)
O5—Mo2—O185.71 (15)C1—N1—HN1113.2
O18—Mo2—O172.05 (15)C5—N1—HN1124.7
O13—Mo2—O172.36 (15)C10—N2—C6116.5 (7)
O19—Mo3—O16103.9 (2)C11ii—N3—C11121.7 (7)
O19—Mo3—O8102.2 (2)C11ii—N3—HN3119.1
O16—Mo3—O890.33 (18)C11—N3—HN3119.1
O19—Mo3—O398.4 (2)C16—N4—C16ii122.0 (9)
O16—Mo3—O392.47 (17)C16—N4—HN4119.0
O8—Mo3—O3157.87 (16)C16ii—N4—HN4119.0
O19—Mo3—O10i96.65 (19)N1—C1—C2120.2 (7)
O16—Mo3—O10i159.41 (16)N1—C1—H1119.9
O8—Mo3—O10i85.85 (17)C2—C1—H1119.9
O3—Mo3—O10i83.84 (17)C1—C2—C3119.7 (7)
O19—Mo3—O2i166.24 (18)C1—C2—H2120.2
O16—Mo3—O2i87.42 (15)C3—C2—H2120.2
O8—Mo3—O2i85.19 (15)C2—C3—C4117.9 (6)
O3—Mo3—O2i73.03 (14)C2—C3—C8121.4 (6)
O10i—Mo3—O2i72.11 (14)C4—C3—C8120.7 (6)
O11—Mo4—O6i103.2 (2)C5—C4—C3119.7 (6)
O11—Mo4—O3i100.6 (2)C5—C4—H4120.1
O6i—Mo4—O3i92.37 (17)C3—C4—H4120.1
O11—Mo4—O5100.8 (2)N1—C5—C4120.3 (7)
O6i—Mo4—O584.26 (17)N1—C5—H5119.8
O3i—Mo4—O5158.49 (17)C4—C5—H5119.8
O11—Mo4—O799.1 (2)C7—C6—N2123.6 (7)
O6i—Mo4—O7157.09 (17)C7—C6—H6118.2
O3i—Mo4—O788.46 (17)N2—C6—H6118.2
O5—Mo4—O786.62 (17)C6—C7—C8119.6 (7)
O11—Mo4—O2170.08 (18)C6—C7—H7120.2
O6i—Mo4—O285.16 (15)C8—C7—H7120.2
O3i—Mo4—O273.39 (15)C7—C8—C9118.2 (6)
O5—Mo4—O285.15 (14)C7—C8—C3120.6 (6)
O7—Mo4—O273.14 (14)C9—C8—C3121.2 (6)
O14—Mo5—O4103.5 (2)C10—C9—C8117.2 (6)
O14—Mo5—O13101.8 (2)C10—C9—H9121.4
O4—Mo5—O1396.33 (18)C8—C9—H9121.4
O14—Mo5—O997.8 (2)N2—C10—C9124.8 (7)
O4—Mo5—O9156.63 (17)N2—C10—H10117.6
O13—Mo5—O988.48 (18)C9—C10—H10117.6
O14—Mo5—O1698.62 (19)N3—C11—C12119.4 (6)
O4—Mo5—O1684.24 (16)N3—C11—H11120.3
O13—Mo5—O16158.87 (17)C12—C11—H11120.3
O9—Mo5—O1683.22 (17)C13—C12—C11121.4 (6)
O14—Mo5—O1169.64 (18)C13—C12—H12119.3
O4—Mo5—O186.68 (15)C11—C12—H12119.3
O13—Mo5—O174.83 (16)C12ii—C13—C12116.7 (7)
O9—Mo5—O172.48 (15)C12ii—C13—C14121.6 (4)
O16—Mo5—O184.14 (15)C12—C13—C14121.6 (4)
O15—Mo6—O9101.3 (2)C15—C14—C15ii116.9 (8)
O15—Mo6—O18100.9 (2)C15—C14—C13121.5 (4)
O9—Mo6—O1891.27 (19)C15ii—C14—C13121.5 (4)
O15—Mo6—O6101.6 (2)C16—C15—C14120.7 (7)
O9—Mo6—O691.40 (17)C16—C15—H15119.7
O18—Mo6—O6156.32 (17)C14—C15—H15119.7
O15—Mo6—O17i101.2 (2)N4—C16—C15119.8 (7)
O9—Mo6—O17i157.49 (17)N4—C16—H16120.1
O18—Mo6—O17i85.96 (18)C15—C16—H16120.1
O6—Mo6—O17i82.64 (18)
O2—Ge—O1—Mo557.8 (2)O13—Mo5—O4—Mo1125.3 (6)
O2i—Ge—O1—Mo562.3 (2)O9—Mo5—O4—Mo124.3 (9)
O1i—Ge—O1—Mo5177.7 (3)O16—Mo5—O4—Mo133.5 (6)
O2—Ge—O1—Mo260.7 (2)O1—Mo5—O4—Mo150.9 (6)
O2i—Ge—O1—Mo2179.22 (19)O12—Mo1—O4—Mo5132.4 (6)
O1i—Ge—O1—Mo259.24 (16)O10—Mo1—O4—Mo536.5 (9)
O2—Ge—O1—Mo6178.08 (19)O7—Mo1—O4—Mo5126.7 (6)
O2i—Ge—O1—Mo657.9 (3)O8—Mo1—O4—Mo533.2 (6)
O1i—Ge—O1—Mo662.02 (17)O2—Mo1—O4—Mo552.1 (6)
O14—Mo5—O1—Ge152.9 (10)O20—Mo2—O5—Mo4124.9 (4)
O4—Mo5—O1—Ge37.7 (2)O17—Mo2—O5—Mo421.9 (4)
O13—Mo5—O1—Ge135.1 (3)O18—Mo2—O5—Mo466.0 (7)
O9—Mo5—O1—Ge131.6 (3)O13—Mo2—O5—Mo4137.5 (4)
O16—Mo5—O1—Ge46.9 (2)O1—Mo2—O5—Mo465.1 (4)
O14—Mo5—O1—Mo275.8 (11)O6i—Mo4—O5—Mo222.0 (4)
O4—Mo5—O1—Mo293.62 (15)O3i—Mo4—O5—Mo259.8 (7)
O13—Mo5—O1—Mo23.86 (15)O7—Mo4—O5—Mo2136.9 (5)
O9—Mo5—O1—Mo297.12 (16)O2—Mo4—O5—Mo263.6 (4)
O16—Mo5—O1—Mo2178.16 (15)O15—Mo6—O6—Mo4i131.2 (6)
O14—Mo5—O1—Mo619.0 (11)O9—Mo6—O6—Mo4i127.0 (6)
O4—Mo5—O1—Mo6171.55 (15)O18—Mo6—O6—Mo4i30.7 (9)
O13—Mo5—O1—Mo690.97 (17)O17i—Mo6—O6—Mo4i31.2 (6)
O9—Mo5—O1—Mo62.29 (14)O1—Mo6—O6—Mo4i53.1 (6)
O16—Mo5—O1—Mo687.01 (15)O12—Mo1—O7—Mo4171.9 (2)
O20—Mo2—O1—Ge178.2 (7)O10—Mo1—O7—Mo468.7 (2)
O17—Mo2—O1—Ge43.4 (2)O8—Mo1—O7—Mo427.4 (6)
O5—Mo2—O1—Ge46.1 (2)O4—Mo1—O7—Mo489.2 (2)
O18—Mo2—O1—Ge134.3 (3)O2—Mo1—O7—Mo44.74 (19)
O13—Mo2—O1—Ge135.6 (3)O6i—Mo4—O7—Mo124.1 (6)
O20—Mo2—O1—Mo549.8 (8)O3i—Mo4—O7—Mo168.3 (2)
O17—Mo2—O1—Mo5175.37 (16)O5—Mo4—O7—Mo190.7 (2)
O5—Mo2—O1—Mo585.89 (16)O2—Mo4—O7—Mo14.75 (19)
O18—Mo2—O1—Mo593.75 (17)O19—Mo3—O8—Mo1126.9 (5)
O13—Mo2—O1—Mo53.63 (14)O16—Mo3—O8—Mo122.6 (5)
O20—Mo2—O1—Mo643.8 (8)O3—Mo3—O8—Mo174.8 (7)
O17—Mo2—O1—Mo691.01 (17)O10i—Mo3—O8—Mo1137.2 (5)
O5—Mo2—O1—Mo6179.51 (16)O2i—Mo3—O8—Mo164.8 (4)
O18—Mo2—O1—Mo60.13 (15)O12—Mo1—O8—Mo3120.3 (5)
O13—Mo2—O1—Mo689.99 (16)O10—Mo1—O8—Mo3137.1 (5)
O9—Mo6—O1—Ge130.7 (3)O7—Mo1—O8—Mo340.5 (7)
O18—Mo6—O1—Ge132.8 (3)O4—Mo1—O8—Mo322.2 (4)
O6—Mo6—O1—Ge37.9 (2)O2—Mo1—O8—Mo362.3 (4)
O17i—Mo6—O1—Ge45.1 (2)O15—Mo6—O9—Mo5169.8 (2)
O9—Mo6—O1—Mo52.41 (15)O18—Mo6—O9—Mo568.4 (2)
O18—Mo6—O1—Mo594.06 (17)O6—Mo6—O9—Mo588.1 (2)
O6—Mo6—O1—Mo595.16 (16)O17i—Mo6—O9—Mo514.1 (6)
O17i—Mo6—O1—Mo5178.23 (16)O14—Mo5—O9—Mo6173.0 (2)
O9—Mo6—O1—Mo296.33 (17)O4—Mo5—O9—Mo631.2 (6)
O18—Mo6—O1—Mo20.14 (16)O13—Mo5—O9—Mo671.3 (2)
O6—Mo6—O1—Mo2170.91 (16)O16—Mo5—O9—Mo689.2 (2)
O17i—Mo6—O1—Mo287.84 (16)O12—Mo1—O10—Mo3i175.3 (2)
O2i—Ge—O2—Mo3i61.89 (16)O7—Mo1—O10—Mo3i73.2 (2)
O1i—Ge—O2—Mo3i58.5 (2)O8—Mo1—O10—Mo3i84.2 (2)
O1—Ge—O2—Mo3i177.84 (18)O4—Mo1—O10—Mo3i15.9 (6)
O2i—Ge—O2—Mo159.06 (16)O2—Mo1—O10—Mo3i0.15 (19)
O1i—Ge—O2—Mo1179.40 (19)O14—Mo5—O13—Mo2174.9 (2)
O1—Ge—O2—Mo161.2 (2)O4—Mo5—O13—Mo279.8 (2)
O2i—Ge—O2—Mo4179.2 (3)O9—Mo5—O13—Mo277.3 (2)
O1i—Ge—O2—Mo460.4 (2)O16—Mo5—O13—Mo210.6 (6)
O1—Ge—O2—Mo459.0 (2)O1—Mo5—O13—Mo25.01 (19)
O10—Mo1—O2—Ge133.0 (3)O20—Mo2—O13—Mo5174.9 (3)
O7—Mo1—O2—Ge129.7 (3)O5—Mo2—O13—Mo581.0 (2)
O8—Mo1—O2—Ge41.7 (2)O18—Mo2—O13—Mo577.9 (2)
O4—Mo1—O2—Ge41.0 (2)O1—Mo2—O13—Mo55.1 (2)
O10—Mo1—O2—Mo3i0.12 (15)O19—Mo3—O16—Mo5124.9 (4)
O7—Mo1—O2—Mo3i97.43 (16)O8—Mo3—O16—Mo522.2 (4)
O8—Mo1—O2—Mo3i91.15 (16)O3—Mo3—O16—Mo5135.9 (4)
O4—Mo1—O2—Mo3i173.85 (15)O10i—Mo3—O16—Mo556.9 (7)
O10—Mo1—O2—Mo493.78 (16)O2i—Mo3—O16—Mo563.0 (4)
O7—Mo1—O2—Mo43.54 (14)O14—Mo5—O16—Mo3125.8 (4)
O8—Mo1—O2—Mo4174.95 (15)O4—Mo5—O16—Mo323.0 (4)
O4—Mo1—O2—Mo492.25 (14)O13—Mo5—O16—Mo369.7 (7)
O6i—Mo4—O2—Ge42.2 (2)O9—Mo5—O16—Mo3137.3 (4)
O3i—Mo4—O2—Ge136.1 (3)O1—Mo5—O16—Mo364.3 (4)
O5—Mo4—O2—Ge42.5 (2)O20—Mo2—O17—Mo6i128.2 (5)
O7—Mo4—O2—Ge130.4 (2)O5—Mo2—O17—Mo6i23.8 (5)
O6i—Mo4—O2—Mo3i89.46 (15)O18—Mo2—O17—Mo6i133.9 (5)
O3i—Mo4—O2—Mo3i4.47 (14)O13—Mo2—O17—Mo6i59.2 (8)
O5—Mo4—O2—Mo3i174.09 (15)O1—Mo2—O17—Mo6i61.9 (5)
O7—Mo4—O2—Mo3i97.98 (16)O15—Mo6—O18—Mo2174.5 (3)
O6i—Mo4—O2—Mo1176.00 (15)O9—Mo6—O18—Mo272.8 (3)
O3i—Mo4—O2—Mo190.06 (16)O6—Mo6—O18—Mo223.6 (6)
O5—Mo4—O2—Mo191.37 (15)O17i—Mo6—O18—Mo284.9 (3)
O7—Mo4—O2—Mo13.44 (14)O1—Mo6—O18—Mo20.2 (2)
O19—Mo3—O3—Mo4i175.0 (2)O20—Mo2—O18—Mo6170.1 (3)
O16—Mo3—O3—Mo4i80.5 (2)O17—Mo2—O18—Mo687.0 (3)
O8—Mo3—O3—Mo4i16.5 (6)O5—Mo2—O18—Mo60.8 (6)
O10i—Mo3—O3—Mo4i79.2 (2)O13—Mo2—O18—Mo672.9 (3)
O2i—Mo3—O3—Mo4i6.04 (19)O1—Mo2—O18—Mo60.2 (2)
O14—Mo5—O4—Mo1131.0 (6)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW—HW1···N2iii0.902.132.759 (9)126
N1—HN1···OW0.941.722.652 (9)171
N3—HN3···O10iv0.962.453.026 (6)118
N3—HN3···O8iv0.962.243.008 (7)137
N4—HN4···O17v0.962.363.147 (8)139
C7—H7···O140.932.483.230 (8)138
C12—H12···O9ii0.932.482.947 (7)111
C16—H16···O18vi0.932.463.088 (8)125
C16—H16···O190.932.393.263 (9)156
Symmetry codes: (ii) x+1, y, z+1/2; (iii) x1/2, y+1/2, z; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1/2, y1/2, z+1/2.
 

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