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The title compound, [Mn(C12H8N2)3]2[GeW12O40]·2H2O, which was prepared under hydro­thermal conditions, consists of one Keggin [GeW12O40]4− anion disordered over an inversion centre, two isolated [Mn(phen)3]2+ cations (phen is 1,10-phenanthroline) and two solvent water mol­ecules. In each [Mn(phen)3]2+ cation, the MnII ion is coordinated by six N atoms from three phen ligands, completing a distorted octa­hedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807012196/bh2076sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807012196/bh2076Isup2.hkl
Contains datablock I

CCDC reference: 642910

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.028 Å
  • H-atom completeness 93%
  • Disorder in main residue
  • R factor = 0.069
  • wR factor = 0.163
  • Data-to-parameter ratio = 11.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.97 Ratio PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O17 PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 28 PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O1W .. 2.72 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O3 .. 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O2W .. 2.74 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O5 .. C14 .. 2.82 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT213_ALERT_2_C Atom C16 has ADP max/min Ratio ............. 3.40 oblat PLAT213_ALERT_2_C Atom O13 has ADP max/min Ratio ............. 3.10 prola PLAT213_ALERT_2_C Atom O17 has ADP max/min Ratio ............. 3.10 prola PLAT216_ALERT_3_C Disordered O2W (An/Solv) ADP max/min Ratio 5.80 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.76 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C18 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C31 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O8 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O9 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C32 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for W4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for W5 PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact O5 .. C13 .. 2.95 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O13 .. C35 .. 3.01 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 45.00 A   3 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.399(10) ...... 3.00 su-Ra C1 -C2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.39(3), Rep 1.393(10) ...... 3.00 su-Ra C2 -C3 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.41(3), Rep 1.406(10) ...... 3.00 su-Ra C4 -C6 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.400(10) ...... 3.00 su-Ra C6 -C7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.395(10) ...... 3.00 su-Ra C10 -C11 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.39(3), Rep 1.393(10) ...... 3.00 su-Ra C11 -C12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.404(10) ...... 3.00 su-Ra C13 -C14 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.398(10) ...... 3.00 su-Ra C14 -C15 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.400(10) ...... 3.00 su-Ra C15 -C16 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.398(10) ...... 3.00 su-Ra C16 -C18 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.402(10) ...... 3.00 su-Ra C16 -C17 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.39(3), Rep 1.394(10) ...... 3.00 su-Ra C18 -C19 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.399(10) ...... 3.00 su-Ra C19 -C20 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.397(10) ...... 3.00 su-Ra C20 -C22 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.39(3), Rep 1.394(10) ...... 3.00 su-Ra C22 -C23 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.396(10) ...... 3.00 su-Ra C23 -C24 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.400(10) ...... 3.00 su-Ra C25 -C26 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.39(3), Rep 1.393(10) ...... 3.00 su-Ra C26 -C27 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.400(10) ...... 3.00 su-Ra C27 -C28 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.401(10) ...... 3.00 su-Ra C28 -C29 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.41(3), Rep 1.406(10) ...... 3.00 su-Ra C28 -C30 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.395(10) ...... 3.00 su-Ra C30 -C31 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.402(10) ...... 3.00 su-Ra C31 -C32 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.398(10) ...... 3.00 su-Ra C32 -C33 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.398(10) ...... 3.00 su-Ra C34 -C35 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.40(3), Rep 1.399(10) ...... 3.00 su-Ra C35 -C36 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C36 H24 Mn N6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 O
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C72 H52 Ge1 Mn2 N12 O42 W12 Atom count from the _atom_site data: C72 H48 Ge1 Mn2 N12 O42 W12 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_sum C72 H52 Ge Mn2 N12 O42 W12 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 72.00 72.00 0.00 H 52.00 48.00 4.00 Ge 1.00 1.00 0.00 Mn 2.00 2.00 0.00 N 12.00 12.00 0.00 O 42.00 42.00 0.00 W 12.00 12.00 0.00 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 53 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 34 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 23 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 5 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: SMART; data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXTL.

Bis[tris(1,10-phenanthroline-κ2N,N')manganese(II)] dodecatungstogermanate dihydrate top
Crystal data top
[Mn(C12H8N2)3]2[GeW12O40]·2H2OZ = 1
Mr = 4145.93F(000) = 1874
Triclinic, P1Dx = 3.061 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.4210 (15) ÅCell parameters from 320 reflections
b = 13.8640 (16) Åθ = 2.5–25°
c = 14.4979 (17) ŵ = 15.97 mm1
α = 104.642 (2)°T = 293 K
β = 109.256 (1)°Block, brown
γ = 93.877 (2)°0.18 × 0.16 × 0.15 mm
V = 2249.0 (5) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer
7765 independent reflections
Radiation source: fine-focus sealed tube5537 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1414
Tmin = 0.074, Tmax = 0.091k = 916
11641 measured reflectionsl = 1715
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)] = 0.069Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.163H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0545P)2 + 86.3193P]
where P = (Fo2 + 2Fc2)/3
7765 reflections(Δ/σ)max = 0.001
665 parametersΔρmax = 3.17 e Å3
213 restraintsΔρmin = 2.26 e Å3
Special details top

Experimental. Spectroscopic analysis, IR (KBr disk, cm-1): 1634, 1521, 1424, 1342, 1224, 1147, 1106, 958, 881, 845, 814, 773.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mn10.28874 (19)0.64849 (18)0.30838 (18)0.0167 (5)
Ge10.00000.00000.00000.0226 (5)
W10.22922 (8)0.09678 (7)0.06487 (7)0.0450 (3)
W20.19250 (9)0.11786 (7)0.15972 (7)0.0521 (3)
W30.28856 (8)0.12065 (7)0.14183 (7)0.0504 (3)
W40.09786 (7)0.23549 (6)0.02109 (8)0.0451 (3)
W50.06115 (7)0.21903 (6)0.20648 (6)0.0389 (2)
W60.03464 (8)0.01671 (8)0.22932 (7)0.0478 (3)
O10.3346 (12)0.1437 (12)0.0981 (14)0.061 (5)
O20.2810 (12)0.1729 (10)0.2358 (10)0.041 (3)
O30.4217 (11)0.1776 (12)0.2082 (11)0.054 (4)
O40.1451 (14)0.3482 (11)0.0263 (13)0.058 (4)
O50.0913 (17)0.3221 (12)0.3065 (13)0.086 (6)
O60.0541 (15)0.0226 (14)0.3347 (13)0.068 (5)
O70.2904 (15)0.0134 (13)0.2045 (13)0.065 (3)
O80.2438 (15)0.1519 (13)0.0447 (13)0.066 (3)
O90.3177 (15)0.0273 (14)0.0305 (13)0.069 (3)
O100.0622 (14)0.2224 (13)0.0873 (12)0.062 (3)
O110.1106 (14)0.0598 (14)0.2462 (14)0.081 (5)
O120.2122 (14)0.1858 (18)0.2271 (14)0.088 (7)
O130.2386 (14)0.2019 (17)0.0548 (14)0.079 (6)
O140.1080 (14)0.1518 (14)0.1389 (15)0.087 (5)
O150.0413 (13)0.1190 (12)0.2721 (12)0.058 (3)
O160.1750 (13)0.0260 (12)0.1641 (12)0.058 (3)
O170.0683 (13)0.2733 (16)0.1027 (14)0.073 (6)
O180.1011 (13)0.2046 (12)0.1502 (12)0.054 (3)
O190.150 (2)0.018 (2)0.046 (2)0.043 (3)0.50
O200.083 (2)0.1120 (18)0.0667 (19)0.031 (4)0.50
O210.004 (2)0.079 (2)0.0834 (18)0.036 (4)0.50
O220.0336 (19)0.0619 (16)0.0979 (16)0.0224 (9)0.50
N10.1146 (13)0.7046 (12)0.3468 (11)0.034 (4)
N20.2450 (15)0.5364 (13)0.2041 (13)0.041 (4)
N30.2585 (14)0.5614 (11)0.4115 (12)0.036 (4)
N40.4595 (14)0.5743 (11)0.2680 (12)0.034 (4)
N50.3118 (12)0.7776 (11)0.4079 (11)0.029 (3)
N60.3439 (14)0.7326 (14)0.2057 (13)0.040 (4)
C10.0528 (13)0.7874 (16)0.4194 (16)0.041 (5)
H1A0.08690.82480.46170.049*
C20.0624 (13)0.8203 (14)0.4343 (15)0.051 (6)
H2A0.10410.87850.48600.061*
C30.1138 (14)0.7648 (12)0.3709 (13)0.043 (5)
H3A0.19030.78520.37980.051*
C40.0481 (12)0.6779 (11)0.2937 (12)0.034 (5)
C50.0664 (12)0.6513 (15)0.2850 (14)0.031 (4)
C60.0926 (16)0.6138 (13)0.2284 (14)0.046 (6)
H6A0.16800.63230.23310.056*
C70.0276 (12)0.5232 (14)0.1566 (15)0.044 (5)
H7A0.06030.48160.11590.053*
C80.0873 (13)0.4956 (11)0.1466 (12)0.036 (5)
C90.1336 (15)0.5606 (13)0.2093 (13)0.029 (4)
C100.1581 (13)0.4064 (12)0.0753 (14)0.039 (5)
H10A0.13040.36290.03140.047*
C110.2709 (14)0.3850 (13)0.0720 (14)0.040 (5)
H11A0.31910.32540.02770.048*
C120.3100 (17)0.4545 (14)0.1363 (15)0.045 (5)
H12A0.38680.44170.13040.055*
C130.1608 (19)0.5534 (13)0.4793 (14)0.042 (5)
H13A0.09290.59210.48630.050*
C140.1544 (15)0.4894 (14)0.5414 (15)0.048 (6)
H14A0.08480.48640.59020.058*
C150.2581 (14)0.4305 (15)0.5261 (16)0.064 (8)
H15A0.25630.38500.56390.077*
C160.3645 (13)0.4371 (13)0.4564 (14)0.036 (5)
C170.3580 (16)0.5020 (12)0.3976 (13)0.031 (4)
C180.4684 (14)0.3791 (15)0.4421 (15)0.057 (7)
H18A0.46950.33730.48290.068*
C190.5703 (16)0.3843 (14)0.3666 (14)0.045 (5)
H19A0.63930.34410.35520.053*
C200.5681 (12)0.4503 (13)0.3083 (13)0.041 (5)
C210.4635 (12)0.5076 (13)0.3228 (14)0.029 (4)
C220.6660 (14)0.4579 (15)0.2297 (14)0.048 (6)
H22A0.73640.41870.21580.057*
C230.6604 (14)0.5231 (15)0.1717 (15)0.049 (6)
H23A0.72490.52970.11980.059*
C240.5508 (13)0.5776 (16)0.1971 (15)0.041 (5)
H24A0.54420.62040.15850.050*
C250.2938 (18)0.7953 (14)0.5059 (15)0.045 (5)
H25A0.27140.74530.53720.054*
C260.308 (2)0.8876 (13)0.5639 (14)0.058 (7)
H26A0.29500.89820.63290.070*
C270.341 (2)0.9639 (17)0.5190 (14)0.064 (7)
H27A0.34901.02580.55750.077*
C280.3615 (19)0.9452 (14)0.4147 (14)0.057 (7)
C290.3470 (15)0.8501 (13)0.3623 (13)0.039 (5)
C300.398 (2)1.0145 (17)0.3595 (18)0.076 (9)
H30A0.40811.07790.39300.091*
C310.419 (2)0.9893 (16)0.2549 (18)0.077 (9)
H31A0.44371.03610.21990.092*
C320.4031 (17)0.8951 (13)0.2014 (12)0.041 (5)
C330.3663 (14)0.8257 (15)0.2555 (15)0.037 (5)
C340.428 (2)0.8709 (18)0.0966 (13)0.064 (8)
H34A0.45620.91550.05970.077*
C350.4077 (17)0.7763 (17)0.0496 (16)0.060 (7)
H35A0.42150.75600.02000.071*
C360.3662 (18)0.7126 (18)0.1098 (15)0.052 (6)
H36A0.35380.64990.07680.062*
O1W0.367 (3)0.291 (3)0.246 (3)0.094 (16)0.50
O2W0.404 (4)0.236 (4)0.398 (4)0.112 (18)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0136 (12)0.0169 (12)0.0191 (12)0.0043 (10)0.0046 (10)0.0057 (10)
Ge10.0245 (13)0.0190 (13)0.0215 (13)0.0073 (11)0.0025 (10)0.0080 (11)
W10.0601 (6)0.0382 (5)0.0475 (5)0.0199 (4)0.0290 (5)0.0149 (4)
W20.0708 (7)0.0327 (5)0.0349 (5)0.0253 (5)0.0058 (4)0.0083 (4)
W30.0481 (6)0.0405 (5)0.0453 (5)0.0135 (4)0.0040 (4)0.0162 (4)
W40.0340 (5)0.0245 (4)0.0695 (6)0.0032 (4)0.0090 (4)0.0146 (4)
W50.0431 (5)0.0286 (5)0.0377 (5)0.0055 (4)0.0104 (4)0.0030 (4)
W60.0487 (5)0.0679 (7)0.0346 (5)0.0254 (5)0.0185 (4)0.0193 (5)
O10.024 (8)0.055 (10)0.102 (13)0.003 (7)0.027 (8)0.013 (9)
O20.043 (8)0.040 (8)0.046 (8)0.021 (7)0.011 (7)0.026 (7)
O30.028 (7)0.069 (11)0.051 (9)0.003 (7)0.017 (7)0.007 (8)
O40.076 (11)0.028 (8)0.082 (12)0.018 (8)0.036 (10)0.025 (8)
O50.108 (12)0.041 (9)0.057 (9)0.040 (9)0.021 (9)0.012 (8)
O60.077 (12)0.073 (12)0.061 (11)0.006 (10)0.020 (9)0.041 (10)
O70.066 (3)0.065 (3)0.065 (3)0.0104 (12)0.0231 (14)0.0191 (13)
O80.067 (3)0.065 (3)0.065 (3)0.0107 (12)0.0233 (14)0.0192 (13)
O90.070 (3)0.068 (3)0.068 (3)0.0109 (12)0.0241 (15)0.0200 (13)
O100.061 (3)0.061 (3)0.062 (3)0.0110 (11)0.0215 (14)0.0165 (13)
O110.049 (7)0.082 (8)0.071 (8)0.027 (7)0.000 (7)0.022 (7)
O120.052 (10)0.18 (2)0.096 (14)0.053 (12)0.045 (10)0.112 (15)
O130.060 (11)0.148 (19)0.080 (12)0.064 (12)0.038 (10)0.091 (13)
O140.044 (7)0.072 (8)0.093 (8)0.019 (7)0.007 (7)0.027 (8)
O150.049 (6)0.059 (6)0.063 (6)0.008 (5)0.007 (5)0.031 (5)
O160.053 (6)0.060 (6)0.061 (6)0.012 (5)0.007 (5)0.035 (5)
O170.038 (9)0.132 (17)0.099 (13)0.051 (10)0.039 (9)0.090 (13)
O180.052 (6)0.049 (6)0.063 (6)0.006 (5)0.012 (5)0.029 (5)
O190.043 (3)0.042 (3)0.042 (3)0.0071 (11)0.0152 (14)0.0127 (13)
O200.028 (6)0.022 (6)0.045 (6)0.008 (6)0.017 (6)0.007 (6)
O210.038 (8)0.055 (9)0.030 (8)0.016 (8)0.020 (7)0.024 (7)
O220.0243 (17)0.0190 (16)0.0214 (16)0.0072 (15)0.0027 (15)0.0080 (15)
N10.026 (8)0.035 (9)0.026 (8)0.002 (7)0.003 (7)0.004 (7)
N20.042 (10)0.037 (10)0.045 (10)0.004 (8)0.014 (8)0.016 (9)
N30.041 (10)0.020 (8)0.046 (10)0.007 (7)0.018 (8)0.005 (7)
N40.039 (9)0.025 (8)0.039 (9)0.006 (7)0.017 (8)0.007 (7)
N50.024 (8)0.033 (9)0.026 (8)0.007 (7)0.001 (6)0.013 (7)
N60.032 (9)0.048 (11)0.040 (10)0.002 (8)0.009 (8)0.018 (9)
C10.029 (11)0.041 (12)0.049 (13)0.009 (10)0.005 (9)0.019 (11)
C20.032 (12)0.028 (11)0.062 (15)0.007 (9)0.014 (10)0.005 (11)
C30.016 (9)0.038 (12)0.080 (16)0.005 (9)0.011 (10)0.038 (12)
C40.037 (11)0.029 (11)0.041 (11)0.008 (9)0.006 (9)0.027 (9)
C50.022 (9)0.041 (12)0.037 (11)0.011 (9)0.012 (8)0.019 (9)
C60.031 (11)0.051 (14)0.079 (16)0.014 (10)0.027 (11)0.043 (13)
C70.034 (11)0.048 (13)0.060 (14)0.020 (10)0.016 (10)0.031 (12)
C80.045 (12)0.035 (11)0.046 (12)0.014 (10)0.027 (10)0.027 (10)
C90.028 (10)0.027 (10)0.036 (10)0.011 (8)0.009 (8)0.016 (9)
C100.052 (13)0.030 (11)0.044 (12)0.023 (10)0.023 (10)0.013 (10)
C110.057 (14)0.020 (10)0.036 (11)0.013 (10)0.012 (10)0.000 (9)
C120.033 (11)0.031 (12)0.065 (15)0.010 (10)0.014 (11)0.005 (11)
C130.049 (13)0.029 (11)0.036 (11)0.020 (10)0.004 (10)0.002 (9)
C140.044 (13)0.043 (13)0.047 (13)0.026 (11)0.004 (10)0.018 (11)
C150.11 (2)0.019 (11)0.056 (15)0.003 (13)0.029 (16)0.013 (11)
C160.049 (12)0.029 (11)0.046 (12)0.013 (9)0.018 (10)0.033 (10)
C170.038 (11)0.021 (9)0.032 (10)0.009 (8)0.005 (8)0.010 (8)
C180.09 (2)0.033 (12)0.055 (15)0.002 (13)0.047 (15)0.005 (11)
C190.041 (12)0.042 (13)0.044 (13)0.015 (10)0.014 (10)0.009 (10)
C200.053 (13)0.029 (11)0.040 (12)0.001 (10)0.023 (10)0.003 (9)
C210.017 (9)0.030 (10)0.035 (10)0.002 (8)0.005 (8)0.008 (9)
C220.022 (10)0.055 (14)0.046 (13)0.011 (10)0.001 (9)0.003 (11)
C230.045 (13)0.062 (15)0.040 (12)0.022 (12)0.012 (10)0.013 (11)
C240.019 (10)0.058 (14)0.037 (11)0.015 (9)0.001 (9)0.019 (10)
C250.047 (13)0.046 (13)0.034 (12)0.003 (11)0.016 (10)0.002 (10)
C260.067 (16)0.059 (16)0.022 (11)0.012 (13)0.008 (11)0.017 (11)
C270.073 (18)0.059 (17)0.061 (17)0.034 (14)0.031 (14)0.003 (14)
C280.041 (13)0.048 (14)0.075 (17)0.027 (11)0.020 (12)0.000 (13)
C290.016 (9)0.072 (15)0.034 (11)0.014 (10)0.005 (8)0.029 (11)
C300.09 (2)0.039 (15)0.12 (3)0.029 (14)0.039 (19)0.038 (16)
C310.067 (18)0.09 (2)0.10 (2)0.030 (16)0.025 (17)0.06 (2)
C320.041 (5)0.041 (5)0.041 (5)0.0068 (13)0.015 (2)0.0124 (18)
C330.015 (9)0.054 (14)0.041 (11)0.009 (9)0.003 (8)0.026 (10)
C340.050 (15)0.10 (2)0.055 (16)0.004 (15)0.017 (12)0.047 (16)
C350.028 (12)0.10 (2)0.033 (12)0.013 (13)0.004 (9)0.016 (14)
C360.055 (14)0.074 (17)0.030 (12)0.006 (13)0.023 (10)0.015 (11)
O1W0.06 (2)0.06 (2)0.15 (4)0.020 (19)0.08 (3)0.04 (2)
O2W0.10 (3)0.17 (5)0.13 (4)0.08 (3)0.05 (3)0.14 (4)
Geometric parameters (Å, º) top
Ge1—O191.81 (3)N2—C121.30 (2)
Ge1—O201.67 (2)N2—C91.37 (2)
Ge1—O211.81 (2)N3—C131.32 (2)
Ge1—O221.66 (2)N3—C171.36 (2)
Ge1—O19i1.81 (3)N4—C241.27 (2)
Ge1—O20i1.67 (2)N4—C211.37 (2)
Ge1—O21i1.81 (2)N5—C251.32 (2)
Ge1—O22i1.66 (2)N5—C291.36 (2)
W1—O11.656 (14)N6—C361.28 (2)
W2—O21.657 (12)N6—C331.41 (3)
W3—O31.635 (13)C1—C21.399 (10)
W4—O41.661 (14)C1—H1A0.9300
W5—O51.675 (15)C2—C31.393 (10)
W6—O61.644 (16)C2—H2A0.9300
W1—O81.893 (17)C3—C41.398 (10)
W1—O91.902 (18)C3—H3A0.9300
W1—O161.911 (14)C4—C51.400 (10)
W1—O181.934 (15)C4—C61.406 (10)
W2—O71.947 (17)C5—C91.43 (2)
W2—O81.938 (17)C6—C71.400 (10)
W2—O101.901 (17)C6—H6A0.9300
W2—O11i1.923 (17)C7—C81.402 (10)
W3—O71.926 (17)C7—H7A0.9300
W3—O91.951 (18)C8—C91.403 (10)
W3—O12i1.889 (19)C8—C101.406 (10)
W3—O13i1.882 (15)C10—C111.395 (10)
W4—O101.873 (16)C10—H10A0.9300
W4—O131.894 (15)C11—C121.393 (10)
W4—O141.854 (18)C11—H11A0.9300
W4—O171.902 (17)C12—H12A0.9300
W5—O121.907 (16)C13—C141.404 (10)
W5—O151.914 (15)C13—H13A0.9300
W5—O171.868 (15)C14—C151.398 (10)
W5—O181.884 (15)C14—H14A0.9300
W6—O111.897 (16)C15—C161.400 (10)
W6—O14i1.949 (17)C15—H15A0.9300
W6—O151.897 (16)C16—C181.398 (10)
W6—O161.903 (15)C16—C171.402 (10)
W1—O192.25 (3)C17—C211.42 (2)
W1—O22i2.42 (2)C18—C191.394 (10)
W2—O192.37 (3)C18—H18A0.9300
W2—O21i2.40 (2)C19—C201.399 (10)
W3—O192.28 (3)C19—H19A0.9300
W3—O20i2.41 (2)C20—C221.397 (10)
W4—O202.41 (2)C20—C211.400 (10)
W4—O21i2.24 (3)C22—C231.394 (10)
W5—O202.30 (2)C22—H22A0.9300
W5—O22i2.30 (2)C23—C241.396 (10)
W6—O212.29 (2)C23—H23A0.9300
W6—O22i2.42 (2)C24—H24A0.9300
O11—W2i1.923 (17)C25—C261.400 (10)
O12—W3i1.889 (19)C25—H25A0.9300
O13—W3i1.882 (15)C26—C271.393 (10)
O14—W6i1.949 (17)C26—H26A0.9300
O20—O22i1.80 (3)C27—C281.400 (10)
O20—W3i2.41 (2)C27—H27A0.9300
O21—W4i2.24 (3)C28—C291.401 (10)
O21—W2i2.40 (2)C28—C301.406 (10)
O22—O20i1.80 (3)C29—C331.43 (3)
O22—W5i2.30 (2)C30—C311.395 (10)
O22—W1i2.42 (2)C30—H30A0.9300
O22—W6i2.42 (2)C31—C321.402 (10)
Mn1—N12.086 (15)C31—H31A0.9300
Mn1—N22.113 (17)C32—C341.391 (10)
Mn1—N32.107 (17)C32—C331.398 (10)
Mn1—N42.117 (16)C34—C351.398 (10)
Mn1—N52.099 (15)C34—H34A0.9300
Mn1—N62.088 (17)C35—C361.399 (10)
N1—C11.32 (2)C35—H35A0.9300
N1—C51.34 (2)C36—H36A0.9300
N1—Mn1—N692.9 (6)W1—O8—W2133.0 (10)
N1—Mn1—N592.4 (6)W1—O9—W3130.9 (9)
N6—Mn1—N581.2 (6)W4—O10—W2138.6 (10)
N1—Mn1—N395.2 (6)W6—O11—W2i137.1 (10)
N6—Mn1—N3171.5 (6)W3i—O12—W5135.4 (11)
N5—Mn1—N395.9 (6)W3i—O13—W4138.3 (10)
N1—Mn1—N279.3 (6)W4—O14—W6i135.8 (13)
N6—Mn1—N293.4 (7)W6—O15—W5136.0 (9)
N5—Mn1—N2169.9 (6)W6—O16—W1137.3 (9)
N3—Mn1—N290.7 (6)W5—O17—W4139.4 (11)
N1—Mn1—N4173.1 (6)W5—O18—W1137.1 (9)
N6—Mn1—N491.8 (6)Ge1—O19—W1120.0 (13)
N5—Mn1—N493.2 (6)Ge1—O19—W3118.7 (14)
N3—Mn1—N480.3 (6)W1—O19—W3101.4 (11)
N2—Mn1—N495.5 (6)Ge1—O19—W2115.0 (13)
O22—Ge1—O22i180 (2)W1—O19—W299.0 (11)
O22—Ge1—O20i65.5 (11)W3—O19—W299.2 (10)
O22i—Ge1—O20i114.5 (11)Ge1—O20—O22i57.0 (10)
O22—Ge1—O20114.5 (11)Ge1—O20—W5124.2 (12)
O22i—Ge1—O2065.5 (11)O22i—O20—W567.2 (10)
O20i—Ge1—O20180 (3)Ge1—O20—W3i119.2 (12)
O22—Ge1—O21i70.7 (11)O22i—O20—W3i131.0 (15)
O22i—Ge1—O21i109.3 (11)W5—O20—W3i96.6 (9)
O20i—Ge1—O21i110.0 (12)Ge1—O20—W4118.8 (13)
O20—Ge1—O21i70.0 (12)O22i—O20—W4132.2 (14)
O22—Ge1—O21109.3 (11)W5—O20—W497.4 (9)
O22i—Ge1—O2170.7 (11)W3i—O20—W494.2 (8)
O20i—Ge1—O2170.0 (12)Ge1—O21—W4i120.5 (13)
O20—Ge1—O21110.0 (12)Ge1—O21—W6119.2 (13)
O21i—Ge1—O21180.0 (12)W4i—O21—W6101.9 (9)
O22—Ge1—O19109.2 (11)Ge1—O21—W2i113.8 (11)
O22i—Ge1—O1970.8 (11)W4i—O21—W2i99.1 (10)
O20i—Ge1—O1971.0 (12)W6—O21—W2i98.5 (9)
O20—Ge1—O19109.0 (12)Ge1—O22—O20i57.4 (10)
O21i—Ge1—O1975.6 (12)Ge1—O22—W5i124.2 (12)
O21—Ge1—O19104.4 (12)O20i—O22—W5i66.8 (10)
O22—Ge1—O19i70.8 (11)Ge1—O22—W1i118.3 (10)
O22i—Ge1—O19i109.2 (11)O20i—O22—W1i131.5 (13)
O20i—Ge1—O19i109.0 (12)W5i—O22—W1i97.4 (8)
O20—Ge1—O19i71.0 (12)Ge1—O22—W6i119.7 (11)
O21i—Ge1—O19i104.4 (12)O20i—O22—W6i131.7 (13)
O21—Ge1—O19i75.6 (12)W5i—O22—W6i96.7 (8)
O19—Ge1—O19i180 (2)W1i—O22—W6i94.2 (8)
O1—W1—O898.1 (8)C1—N1—C5119.2 (16)
O1—W1—O997.9 (8)C1—N1—Mn1127.3 (13)
O8—W1—O989.5 (8)C5—N1—Mn1113.4 (11)
O1—W1—O16100.0 (8)C12—N2—C9119.2 (17)
O8—W1—O16161.9 (7)C12—N2—Mn1128.8 (13)
O9—W1—O1688.8 (7)C9—N2—Mn1111.9 (12)
O1—W1—O18100.0 (7)C13—N3—C17118.8 (16)
O8—W1—O1888.5 (7)C13—N3—Mn1130.0 (13)
O9—W1—O18162.1 (7)C17—N3—Mn1111.1 (11)
O16—W1—O1887.6 (6)C24—N4—C21119.0 (16)
O1—W1—O19154.8 (9)C24—N4—Mn1129.0 (13)
O8—W1—O1965.6 (9)C21—N4—Mn1111.7 (11)
O9—W1—O1964.5 (9)C25—N5—C29119.0 (16)
O16—W1—O1997.6 (9)C25—N5—Mn1127.9 (13)
O18—W1—O1998.6 (9)C29—N5—Mn1113.1 (11)
O1—W1—O22i154.2 (8)C36—N6—C33117.3 (18)
O8—W1—O22i98.6 (7)C36—N6—Mn1132.6 (16)
O9—W1—O22i101.7 (7)C33—N6—Mn1110.0 (11)
O16—W1—O22i64.2 (7)N1—C1—C2121.9 (19)
O18—W1—O22i61.1 (7)N1—C1—H1A119.0
O19—W1—O22i50.9 (9)C2—C1—H1A119.0
O2—W2—O10101.7 (7)C3—C2—C1119.3 (17)
O2—W2—O11i99.6 (8)C3—C2—H2A120.3
O10—W2—O11i87.8 (7)C1—C2—H2A120.3
O2—W2—O899.5 (7)C2—C3—C4118.7 (15)
O10—W2—O889.9 (7)C2—C3—H3A120.7
O11i—W2—O8160.9 (8)C4—C3—H3A120.7
O2—W2—O798.3 (7)C3—C4—C5117.7 (15)
O10—W2—O7160.0 (7)C3—C4—C6123.5 (14)
O11i—W2—O788.4 (8)C5—C4—C6118.8 (15)
O8—W2—O787.4 (7)N1—C5—C4123.2 (16)
O2—W2—O19153.3 (8)N1—C5—C9118.2 (13)
O10—W2—O1998.0 (8)C4—C5—C9118.6 (15)
O11i—W2—O1999.1 (9)C7—C6—C4122.5 (17)
O8—W2—O1962.5 (8)C7—C6—H6A118.8
O7—W2—O1963.3 (8)C4—C6—H6A118.8
O2—W2—O21i151.1 (7)C6—C7—C8119.5 (17)
O10—W2—O21i59.3 (8)C6—C7—H7A120.2
O11i—W2—O21i60.9 (8)C8—C7—H7A120.2
O8—W2—O21i101.8 (8)C7—C8—C9118.4 (15)
O7—W2—O21i101.9 (8)C7—C8—C10122.6 (14)
O19—W2—O21i55.6 (9)C9—C8—C10119.0 (14)
O3—W3—O13i100.9 (9)N2—C9—C8120.9 (16)
O3—W3—O12i100.4 (8)N2—C9—C5116.8 (14)
O13i—W3—O12i90.8 (7)C8—C9—C5122.2 (15)
O3—W3—O797.7 (8)C11—C10—C8118.3 (15)
O13i—W3—O7161.4 (8)C11—C10—H10A120.9
O12i—W3—O787.0 (7)C8—C10—H10A120.9
O3—W3—O998.1 (7)C12—C11—C10118.8 (17)
O13i—W3—O987.8 (8)C12—C11—H11A120.6
O12i—W3—O9161.4 (8)C10—C11—H11A120.6
O7—W3—O988.5 (7)N2—C12—C11123.6 (18)
O3—W3—O19153.8 (9)N2—C12—H12A118.2
O13i—W3—O1996.7 (10)C11—C12—H12A118.2
O12i—W3—O1998.7 (10)N3—C13—C14123.2 (19)
O7—W3—O1965.5 (9)N3—C13—H13A118.4
O9—W3—O1963.2 (9)C14—C13—H13A118.4
O3—W3—O20i155.1 (8)C15—C14—C13116.5 (18)
O13i—W3—O20i63.8 (8)C15—C14—H14A121.8
O12i—W3—O20i62.4 (8)C13—C14—H14A121.8
O7—W3—O20i99.1 (8)C14—C15—C16122.7 (17)
O9—W3—O20i100.7 (8)C14—C15—H15A118.7
O19—W3—O20i51.1 (9)C16—C15—H15A118.7
O4—W4—O14101.1 (9)C18—C16—C15122.7 (14)
O4—W4—O10102.0 (8)C18—C16—C17122.5 (16)
O14—W4—O1089.9 (7)C15—C16—C17114.8 (16)
O4—W4—O13100.3 (8)N3—C17—C16123.8 (16)
O14—W4—O1388.7 (8)N3—C17—C21119.6 (13)
O10—W4—O13157.4 (8)C16—C17—C21116.6 (15)
O4—W4—O17100.4 (8)C19—C18—C16119.8 (18)
O14—W4—O17158.5 (9)C19—C18—H18A120.1
O10—W4—O1786.0 (7)C16—C18—H18A120.1
O13—W4—O1787.1 (7)C18—C19—C20119.5 (17)
O4—W4—O21i155.7 (8)C18—C19—H19A120.3
O14—W4—O21i62.2 (9)C20—C19—H19A120.3
O10—W4—O21i62.9 (8)C22—C20—C19122.9 (15)
O13—W4—O21i96.9 (9)C22—C20—C21116.8 (14)
O17—W4—O21i97.5 (8)C19—C20—C21120.2 (15)
O4—W4—O20153.5 (8)N4—C21—C20121.3 (15)
O14—W4—O2099.5 (9)N4—C21—C17117.3 (13)
O10—W4—O2094.5 (8)C20—C21—C17121.4 (15)
O13—W4—O2063.6 (8)C23—C22—C20121.4 (16)
O17—W4—O2060.0 (8)C23—C22—H22A119.3
O21i—W4—O2050.7 (8)C20—C22—H22A119.3
O5—W5—O17102.7 (10)C22—C23—C24115.1 (18)
O5—W5—O18100.8 (8)C22—C23—H23A122.4
O17—W5—O1888.3 (6)C24—C23—H23A122.4
O5—W5—O12100.2 (10)N4—C24—C23126.1 (19)
O17—W5—O1290.5 (6)N4—C24—H24A116.9
O18—W5—O12158.7 (9)C23—C24—H24A116.9
O5—W5—O1598.4 (9)N5—C25—C26121 (2)
O17—W5—O15158.9 (8)N5—C25—H25A119.3
O18—W5—O1587.9 (6)C26—C25—H25A119.3
O12—W5—O1585.6 (7)C27—C26—C25120.5 (19)
O5—W5—O20157.3 (10)C27—C26—H26A119.8
O17—W5—O2062.8 (9)C25—C26—H26A119.8
O18—W5—O2096.3 (8)C26—C27—C28118.5 (19)
O12—W5—O2064.5 (9)C26—C27—H27A120.8
O15—W5—O2097.0 (8)C28—C27—H27A120.8
O5—W5—O22i156.6 (10)C27—C28—C29117.2 (17)
O17—W5—O22i94.9 (9)C27—C28—C30124.3 (18)
O18—W5—O22i64.2 (7)C29—C28—C30118.5 (18)
O12—W5—O22i94.8 (9)N5—C29—C28123.5 (16)
O15—W5—O22i64.8 (7)N5—C29—C33116.1 (15)
O20—W5—O22i46.0 (8)C28—C29—C33120.4 (17)
O6—W6—O11102.4 (9)C31—C30—C28121 (2)
O6—W6—O1599.9 (8)C31—C30—H30A119.6
O11—W6—O1588.9 (8)C28—C30—H30A119.6
O6—W6—O1699.5 (8)C30—C31—C32122 (2)
O11—W6—O16158.1 (8)C30—C31—H31A119.2
O15—W6—O1688.8 (7)C32—C31—H31A119.2
O6—W6—O14i101.1 (9)C34—C32—C33121.4 (18)
O11—W6—O14i88.2 (7)C34—C32—C31120.3 (18)
O15—W6—O14i159.0 (9)C33—C32—C31118.2 (18)
O16—W6—O14i86.2 (7)C32—C33—N6119.9 (17)
O6—W6—O21154.9 (9)C32—C33—C29120.5 (18)
O11—W6—O2163.4 (8)N6—C33—C29119.6 (14)
O15—W6—O21100.3 (9)C32—C34—C35117 (2)
O16—W6—O2195.7 (8)C32—C34—H34A121.7
O14i—W6—O2160.0 (10)C35—C34—H34A121.7
O6—W6—O22i154.6 (8)C34—C35—C36119 (2)
O11—W6—O22i95.6 (8)C34—C35—H35A120.7
O15—W6—O22i62.4 (7)C36—C35—H35A120.7
O16—W6—O22i64.2 (7)N6—C36—C35126 (2)
O14i—W6—O22i97.2 (9)N6—C36—H36A116.9
O21—W6—O22i50.4 (8)C35—C36—H36A116.9
W3—O7—W2132.0 (9)
Symmetry code: (i) x, y, z.
 

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