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A new three-dimensional open-framework germanate, namely ethylenediamine bis(ethylenediammonium) tetra­hydro­xo­octadecaoxononagermanate, (C2H8N2)(C2H10N2)2[Ge9O18(OH)4], has been synthesized hydro­thermally and its structure determined by single-crystal X-ray diffraction. The framework is built of [Ge9O22(OH)4] units formed by four-, five- and six-oxy­gen-coordinated germanium and templated by ethyl­enedi­amine. Three types of intersecting channels are formed in the framework, one by eight-membered rings running along the b axis and the other two by ten-membered rings running parallel to the a and c axes, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009057/os1114sup1.cif
Contains datablocks I, default

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009057/os1114Isup2.hkl
Contains datablock I

CCDC reference: 150768

Computing details top

Data collection: EXPOSE (Stoe & Cie, 1997b); cell refinement: CELL (Stoe & Cie, 1997b); data reduction: INTEGRATE (Stoe & Cie, 1997b); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996).

(I) top
Crystal data top
(C2H8N2)(C2H10N2)2[H4Ge9O22]F(000) = 1148
Mr = 1193.68Dx = 2.961 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.1958 (15) ÅCell parameters from 5000 reflections
b = 9.9753 (10) Åθ = 2.9–26.0°
c = 13.1655 (19) ŵ = 10.06 mm1
β = 90.695 (17)°T = 293 K
V = 1338.9 (3) Å3Prism, colourless
Z = 20.06 × 0.04 × 0.04 mm
Data collection top
STOE IPDS
diffractometer
2598 independent reflections
Radiation source: fine-focus sealed tube2077 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
Detector resolution: 6.0 pixels mm-1θmax = 26.0°, θmin = 2.9°
φ–oscill., φ–incr. = 1.5°; 133 exposures scansh = 1212
Absorption correction: numerical
(XRED; Stoe & Cie, 1997a)
k = 1112
Tmin = 0.577, Tmax = 0.721l = 1616
10190 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.058 w = 1/[σ2(Fo2) + (0.0315P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.96(Δ/σ)max = 0.041
2598 reflectionsΔρmax = 0.80 e Å3
204 parametersΔρmin = 0.63 e Å3
3 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00047 (18)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ge10.50000.00000.00000.00530 (14)
Ge20.66385 (4)0.11685 (4)0.22083 (3)0.00670 (12)
Ge30.38181 (4)0.16338 (4)0.22955 (3)0.00800 (12)
Ge40.37016 (4)0.17895 (4)0.16785 (3)0.00633 (12)
Ge50.66835 (4)0.13366 (4)0.16933 (3)0.00673 (12)
O10.3862 (3)0.1442 (3)0.0388 (2)0.0099 (6)
O20.5145 (3)0.0677 (3)0.1338 (2)0.0073 (6)
O30.7882 (3)0.1684 (3)0.3194 (2)0.0113 (6)
O40.6463 (3)0.1004 (3)0.0407 (2)0.0102 (6)
O50.2897 (3)0.0122 (3)0.2377 (2)0.0143 (7)
O60.7432 (3)0.2095 (3)0.1243 (2)0.0139 (7)
H10.71630.18460.06850.017*
O70.5342 (3)0.1864 (3)0.2947 (2)0.0129 (7)
O80.5254 (3)0.2072 (3)0.2226 (2)0.0128 (6)
O90.3406 (3)0.2767 (3)0.1307 (2)0.0173 (7)
H20.34540.23830.07580.021*
O100.2939 (3)0.2503 (3)0.3284 (2)0.0132 (7)
O110.7151 (3)0.0528 (3)0.2336 (2)0.0127 (7)
C10.5575 (5)0.4524 (5)0.0077 (4)0.0273 (12)
H1A0.53680.36530.02090.033*
H1B0.63460.48710.02580.033*
N10.5825 (5)0.4405 (5)0.1180 (3)0.0293 (11)
H1C0.61780.51640.14110.035*
H1D0.63760.37290.12970.035*
H1E0.50730.42510.14950.035*
C20.4830 (7)0.0688 (7)0.5199 (5)0.0409 (16)
H2A0.41360.10640.47770.049*
H2B0.44940.05980.58820.049*
N20.5918 (6)0.1605 (6)0.4781 (4)0.0471 (15)
H2C0.65570.12740.43880.057*
H2D0.56580.23900.45330.057*
H2E0.62140.17190.54080.057*
C30.5232 (13)0.5073 (10)0.4518 (6)0.092 (4)
H3A0.46990.57470.41880.110*
H3B0.61140.54320.45580.110*
N30.5281 (6)0.3920 (7)0.3866 (5)0.0487 (15)
H3C0.449 (3)0.366 (7)0.366 (4)0.058*
H3D0.580 (5)0.402 (8)0.331 (3)0.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ge10.0061 (3)0.0048 (3)0.0050 (3)0.0004 (2)0.0009 (2)0.0004 (2)
Ge20.0065 (2)0.0050 (2)0.0086 (2)0.00009 (16)0.00103 (16)0.00059 (17)
Ge30.0073 (2)0.0067 (2)0.0100 (2)0.00070 (16)0.00015 (17)0.00085 (18)
Ge40.0077 (2)0.0043 (2)0.0069 (2)0.00008 (16)0.00225 (16)0.00046 (17)
Ge50.0071 (2)0.0062 (2)0.0069 (2)0.00028 (16)0.00108 (17)0.00076 (17)
O10.0113 (15)0.0091 (16)0.0092 (15)0.0027 (12)0.0003 (12)0.0030 (12)
O20.0066 (14)0.0101 (16)0.0052 (14)0.0014 (11)0.0007 (11)0.0004 (12)
O30.0124 (15)0.0070 (16)0.0144 (15)0.0017 (12)0.0084 (12)0.0020 (12)
O40.0098 (15)0.0119 (16)0.0088 (15)0.0044 (12)0.0020 (12)0.0027 (12)
O50.0145 (16)0.0105 (17)0.0180 (16)0.0040 (12)0.0078 (13)0.0047 (13)
O60.0185 (16)0.0157 (17)0.0075 (15)0.0092 (13)0.0025 (12)0.0005 (13)
O70.0079 (14)0.0180 (18)0.0126 (15)0.0019 (13)0.0019 (12)0.0091 (13)
O80.0125 (15)0.0146 (17)0.0113 (15)0.0004 (13)0.0005 (12)0.0055 (13)
O90.0241 (18)0.0136 (18)0.0143 (16)0.0096 (14)0.0009 (14)0.0010 (13)
O100.0154 (16)0.0126 (17)0.0115 (16)0.0047 (12)0.0006 (13)0.0015 (13)
O110.0126 (16)0.0088 (16)0.0165 (16)0.0007 (12)0.0090 (13)0.0010 (13)
C10.030 (3)0.018 (3)0.033 (3)0.004 (2)0.013 (2)0.001 (2)
N10.036 (3)0.017 (2)0.035 (3)0.0064 (19)0.020 (2)0.006 (2)
C20.046 (4)0.048 (4)0.029 (3)0.003 (3)0.004 (3)0.006 (3)
N20.057 (4)0.053 (4)0.031 (3)0.008 (3)0.008 (3)0.004 (3)
C30.178 (12)0.058 (6)0.040 (4)0.013 (7)0.011 (6)0.015 (4)
N30.036 (3)0.062 (4)0.048 (3)0.004 (3)0.003 (3)0.015 (3)
Geometric parameters (Å, º) top
Ge1—O41.880 (3)O5—Ge5i1.766 (3)
Ge1—O4i1.880 (3)O6—H10.8200
Ge1—O2i1.890 (3)O9—H20.8200
Ge1—O21.890 (3)O10—Ge5v1.726 (3)
Ge1—O1i1.914 (3)O11—Ge4i1.752 (3)
Ge1—O11.914 (3)C1—N11.475 (7)
Ge2—O61.774 (3)C1—C1vi1.520 (10)
Ge2—O111.778 (3)C1—H1A0.9700
Ge2—O71.790 (3)C1—H1B0.9700
Ge2—O31.874 (3)N1—H1C0.8900
Ge2—O21.957 (3)N1—H1D0.8900
Ge2—Ge32.9165 (7)N1—H1E0.8900
Ge3—O91.770 (3)C2—N2vii1.438 (9)
Ge3—O71.781 (3)C2—C2viii1.511 (14)
Ge3—O51.781 (3)C2—H2A0.9700
Ge3—O101.810 (3)C2—H2B0.9700
Ge3—O22.091 (3)N2—C2ix1.438 (9)
Ge4—O11.739 (3)N2—H2C0.8900
Ge4—O3ii1.744 (3)N2—H2D0.8900
Ge4—O11i1.752 (3)N2—H2E0.8900
Ge4—O81.770 (3)C3—C3x1.357 (16)
Ge5—O10iii1.726 (3)C3—N31.436 (10)
Ge5—O41.743 (3)C3—H3A0.9700
Ge5—O5i1.766 (3)C3—H3B0.9700
Ge5—O81.769 (3)N3—H3C0.90 (2)
O3—Ge4iv1.744 (3)N3—H3D0.90 (2)
O4—Ge1—O4i180.0 (2)O10iii—Ge5—O5i111.06 (15)
O4—Ge1—O2i88.74 (13)O4—Ge5—O5i111.91 (15)
O4i—Ge1—O2i91.26 (13)O10iii—Ge5—O8108.81 (15)
O4—Ge1—O291.26 (13)O4—Ge5—O8110.41 (14)
O4i—Ge1—O288.74 (13)O5i—Ge5—O8110.05 (15)
O2i—Ge1—O2180.00 (6)Ge4—O1—Ge1117.40 (16)
O4—Ge1—O1i89.76 (13)Ge1—O2—Ge2133.36 (15)
O4i—Ge1—O1i90.24 (13)Ge1—O2—Ge3132.93 (15)
O2i—Ge1—O1i91.18 (12)Ge2—O2—Ge392.13 (11)
O2—Ge1—O1i88.82 (12)Ge4iv—O3—Ge2128.73 (17)
O4—Ge1—O190.24 (13)Ge5—O4—Ge1119.40 (16)
O4i—Ge1—O189.76 (13)Ge5i—O5—Ge3122.40 (17)
O2i—Ge1—O188.82 (12)Ge2—O6—H1109.5
O2—Ge1—O191.18 (12)Ge3—O7—Ge2109.51 (15)
O1i—Ge1—O1180.0 (2)Ge4—O8—Ge5120.59 (17)
O6—Ge2—O11115.28 (15)Ge3—O9—H2109.5
O6—Ge2—O7122.21 (15)Ge5v—O10—Ge3135.03 (18)
O11—Ge2—O7122.41 (15)Ge4i—O11—Ge2119.56 (16)
O6—Ge2—O392.42 (14)N1—C1—C1vi107.8 (6)
O11—Ge2—O390.02 (13)N1—C1—H1A110.1
O7—Ge2—O390.87 (13)C1vi—C1—H1A110.1
O6—Ge2—O293.97 (13)N1—C1—H1B110.1
O11—Ge2—O292.45 (13)C1vi—C1—H1B110.1
O7—Ge2—O280.84 (12)H1A—C1—H1B108.5
O3—Ge2—O2171.39 (13)C1—N1—H1C109.5
O6—Ge2—Ge3113.80 (11)C1—N1—H1D109.5
O11—Ge2—Ge3115.89 (10)H1C—N1—H1D109.5
O7—Ge2—Ge335.14 (9)C1—N1—H1E109.5
O3—Ge2—Ge3126.00 (10)H1C—N1—H1E109.5
O2—Ge2—Ge345.76 (8)H1D—N1—H1E109.5
O9—Ge3—O7118.00 (16)N2vii—C2—C2viii113.8 (7)
O9—Ge3—O5117.69 (16)N2vii—C2—H2A108.8
O7—Ge3—O5122.55 (15)C2viii—C2—H2A108.8
O9—Ge3—O1096.15 (14)N2vii—C2—H2B108.8
O7—Ge3—O1091.65 (14)C2viii—C2—H2B108.8
O5—Ge3—O1095.52 (14)H2A—C2—H2B107.7
O9—Ge3—O289.87 (13)C2ix—N2—H2C109.5
O7—Ge3—O277.42 (12)C2ix—N2—H2D109.5
O5—Ge3—O289.74 (13)H2C—N2—H2D109.5
O10—Ge3—O2169.04 (12)C2ix—N2—H2E109.5
O9—Ge3—Ge2107.35 (11)H2C—N2—H2E109.5
O7—Ge3—Ge235.35 (10)H2D—N2—H2E109.5
O5—Ge3—Ge2112.86 (10)C3x—C3—N3118.8 (11)
O10—Ge3—Ge2126.99 (10)C3x—C3—H3A107.6
O2—Ge3—Ge242.12 (8)N3—C3—H3A107.6
O1—Ge4—O3ii107.91 (14)C3x—C3—H3B107.6
O1—Ge4—O11i112.28 (14)N3—C3—H3B107.6
O3ii—Ge4—O11i110.18 (14)H3A—C3—H3B107.0
O1—Ge4—O8110.84 (14)C3—N3—H3C113 (5)
O3ii—Ge4—O8104.57 (14)C3—N3—H3D115 (5)
O11i—Ge4—O8110.75 (15)H3C—N3—H3D107 (3)
O10iii—Ge5—O4104.43 (14)
Symmetry codes: (i) x+1, y, z; (ii) x1/2, y+1/2, z1/2; (iii) x+1/2, y+1/2, z1/2; (iv) x+1/2, y+1/2, z+1/2; (v) x1/2, y+1/2, z+1/2; (vi) x+1, y+1, z; (vii) x, y, z+1; (viii) x+1, y, z+1; (ix) x, y, z1; (x) x+1, y+1, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H1···O40.821.812.614 (4)169
O9—H2···O10.821.832.641 (4)170
N1—H1C···O3xi0.891.872.750 (5)172
N1—H1E···O90.892.272.965 (6)135
N1—H1D···O60.891.962.828 (6)166
N1—H1D···O11xi0.892.452.826 (5)106
N2—H2C···O9iii0.892.292.965 (7)132
N2—H2D···N30.891.802.687 (9)171
N2—H2E···O7ix0.892.343.053 (6)138
N2—H2E···O3ix0.892.523.355 (6)156
N3—H3C···O6ii0.90 (2)2.23 (3)3.081 (7)158 (5)
N3—H3D···O5iii0.90 (2)2.47 (4)3.256 (7)146 (5)
Symmetry codes: (ii) x1/2, y+1/2, z1/2; (iii) x+1/2, y+1/2, z1/2; (ix) x, y, z1; (xi) x+3/2, y+1/2, z+1/2.
 

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