Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106051652/ws5044sup1.cif |
Data collection: STOE X-AREA (Stoe & Cie, 2002) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_100, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750. Cell refinement: STOE X-AREA (Stoe & Cie, 2002) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_100, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750. Data reduction: Stoe X-AREA (Stoe & Cie, 2002) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_100, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_100, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750. For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Diamond 3.0 Bradenburg & Berndt 1999) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_100, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750. Software used to prepare material for publication: WinGX 1.70.00 (Farrugia, 1999) for cf5_090, cf5_130, cf5_170, cf5_200, cf5_250, cf5_290, cufege, cf9_050, cf9_200, cf9_300, cf9_550, cf9_600, cf9_650, cf9_750; WinGX 1.70.00 (Farrugia, 1999)' for cf9_100.
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.933 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.090 (2) Å | Cell parameters from 5776 reflections |
b = 8.4901 (9) Å | θ = 2.9–30.0° |
c = 4.8626 (8) Å | µ = 19.06 mm−1 |
β = 96.13 (2)° | T = 90 K |
V = 496.27 (13) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1202 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.060 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −17→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
5776 measured reflections | l = −6→6 |
1527 independent reflections |
Refinement on F2 | 3 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0238P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.032 | (Δ/σ)max = 0.001 |
wR(F2) = 0.058 | Δρmax = 1.51 e Å−3 |
S = 1.02 | Δρmin = −1.16 e Å−3 |
1527 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0024 (3) |
Cu2Fe2Ge4O13 | V = 496.27 (13) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.090 (2) Å | µ = 19.06 mm−1 |
b = 8.4901 (9) Å | T = 90 K |
c = 4.8626 (8) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.13 (2)° |
STOE IPDS-II diffractometer | 1527 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1202 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.060 |
5776 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 110 parameters |
wR(F2) = 0.058 | 3 restraints |
S = 1.02 | Δρmax = 1.51 e Å−3 |
1527 reflections | Δρmin = −1.16 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23969 (5) | 0.25 | 0.49418 (14) | 0.00331 (14) | |
Ge2 | 0.74763 (5) | 0.25 | 0.33894 (14) | 0.00322 (14) | |
Ge3 | −0.00505 (5) | 0.25 | 0.40645 (14) | 0.00369 (14) | |
Ge4 | 0.51221 (5) | 0.25 | 0.60629 (14) | 0.00323 (14) | |
Fe1 | 0.37602 (5) | 0.06144 (7) | 1.04793 (14) | 0.00330 (13) | |
Cu1 | 0.12607 (4) | −0.00344 (7) | 1.04347 (13) | 0.00516 (12) | |
O1 | 0.3319 (3) | 0.25 | 0.7965 (10) | 0.0046 (8) | |
O2 | 0.6537 (3) | 0.25 | 0.5758 (10) | 0.0077 (9) | |
O3 | 0.1133 (4) | 0.25 | 0.6471 (10) | 0.0053 (8) | |
O4 | 0.2478 (2) | 0.0836 (4) | 0.2855 (7) | 0.0059 (6) | |
O5 | 0.8720 (4) | 0.25 | 0.5694 (10) | 0.0055 (8) | |
O6 | 0.50325 (19) | 0.0738 (4) | 0.7917 (5) | 0.0060 (6) | |
O7 | 0.7427 (2) | 0.0804 (4) | 0.1349 (7) | 0.0053 (6) | |
O8 | 0.4361 (3) | 0.25 | 0.2801 (5) | 0.0042 (8) | |
O9 | −0.0027 (2) | 0.0825 (4) | 0.2020 (7) | 0.0071 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0031 (3) | 0.0044 (3) | 0.0025 (4) | 0 | 0.0005 (2) | 0 |
Ge2 | 0.0031 (3) | 0.0040 (3) | 0.0026 (3) | 0 | 0.0006 (2) | 0 |
Ge3 | 0.0032 (3) | 0.0050 (3) | 0.0030 (3) | 0 | 0.0007 (2) | 0 |
Ge4 | 0.0038 (2) | 0.0043 (3) | 0.0017 (3) | 0 | 0.0006 (2) | 0 |
Fe1 | 0.0039 (2) | 0.0040 (2) | 0.0021 (3) | 0.0002 (2) | 0.00076 (19) | −0.0001 (2) |
Cu1 | 0.0032 (2) | 0.0069 (2) | 0.0054 (3) | −0.00046 (17) | 0.00108 (15) | −0.00235 (19) |
O1 | 0.0051 (17) | 0.0075 (19) | 0.001 (2) | 0 | 0.0009 (14) | 0 |
O2 | 0.0055 (19) | 0.012 (2) | 0.006 (2) | 0 | 0.0003 (16) | 0 |
O3 | 0.0044 (17) | 0.0081 (19) | 0.004 (2) | 0 | 0.0024 (15) | 0 |
O4 | 0.0055 (13) | 0.0091 (15) | 0.0033 (15) | −0.0003 (10) | 0.0023 (10) | −0.0013 (12) |
O5 | 0.0047 (17) | 0.0122 (19) | 0.000 (2) | 0 | 0.0017 (15) | 0 |
O6 | 0.0075 (13) | 0.0047 (14) | 0.0059 (17) | 0.0009 (10) | 0.0010 (10) | 0.0006 (12) |
O7 | 0.0043 (12) | 0.0076 (14) | 0.0041 (16) | −0.0012 (10) | 0.0007 (10) | −0.0013 (12) |
O8 | 0.0069 (18) | 0.0036 (18) | 0.002 (2) | 0 | 0.0004 (14) | 0 |
O9 | 0.0041 (12) | 0.0092 (15) | 0.0078 (17) | −0.0012 (11) | −0.0001 (11) | −0.0031 (13) |
Ge1—O1 | 1.747 (4) | Fe1—O8v | 2.0467 (10) |
Ge1—O4 | 1.748 (3) | Fe1—O1 | 2.050 (3) |
Ge1—O4i | 1.748 (3) | Fe1—O6 | 2.0831 (15) |
Ge1—O3 | 1.769 (5) | Cu1—O9vi | 1.929 (3) |
Ge2—O2 | 1.702 (5) | Cu1—O4v | 1.931 (3) |
Ge2—O7 | 1.746 (3) | Cu1—O9v | 1.951 (3) |
Ge2—O7i | 1.746 (3) | Cu1—O7iv | 1.998 (3) |
Ge2—O5 | 1.777 (4) | Cu1—Cu1vii | 3.0331 (12) |
Ge3—O9 | 1.737 (3) | O1—Fe1i | 2.050 (3) |
Ge3—O9i | 1.737 (3) | O4—Cu1viii | 1.931 (3) |
Ge3—O3 | 1.750 (4) | O4—Fe1viii | 2.038 (3) |
Ge3—O5ii | 1.758 (5) | O5—Ge3ix | 1.758 (5) |
Ge4—O2 | 1.733 (4) | O6—Fe1iii | 1.953 (3) |
Ge4—O8 | 1.747 (3) | O7—Cu1iv | 1.998 (3) |
Ge4—O6i | 1.756 (3) | O7—Fe1iv | 2.007 (3) |
Ge4—O6 | 1.756 (3) | O8—Fe1viii | 2.0467 (10) |
Fe1—O6iii | 1.953 (3) | O8—Fe1x | 2.0467 (10) |
Fe1—O7iv | 2.007 (3) | O9—Cu1vi | 1.929 (3) |
Fe1—O4v | 2.038 (3) | O9—Cu1viii | 1.951 (3) |
O1—Ge1—O4 | 114.70 (12) | O7iv—Fe1—O6 | 107.70 (13) |
O1—Ge1—O4i | 114.70 (12) | O4v—Fe1—O6 | 171.55 (12) |
O4—Ge1—O4i | 107.8 (2) | O8v—Fe1—O6 | 92.84 (15) |
O1—Ge1—O3 | 98.5 (2) | O1—Fe1—O6 | 76.44 (15) |
O4—Ge1—O3 | 110.40 (13) | O9vi—Cu1—O4v | 177.87 (15) |
O4i—Ge1—O3 | 110.40 (13) | O9vi—Cu1—O9v | 77.17 (16) |
O2—Ge2—O7 | 113.56 (13) | O4v—Cu1—O9v | 101.79 (13) |
O2—Ge2—O7i | 113.56 (13) | O9vi—Cu1—O7iv | 102.44 (13) |
O7—Ge2—O7i | 111.1 (2) | O4v—Cu1—O7iv | 78.49 (13) |
O2—Ge2—O5 | 98.8 (2) | O9v—Cu1—O7iv | 176.51 (15) |
O7—Ge2—O5 | 109.50 (12) | O9vi—Cu1—Cu1vii | 38.84 (10) |
O7i—Ge2—O5 | 109.50 (12) | O4v—Cu1—Cu1vii | 140.09 (10) |
O9—Ge3—O9i | 109.9 (2) | O9v—Cu1—Cu1vii | 38.33 (9) |
O9—Ge3—O3 | 108.69 (13) | O7iv—Cu1—Cu1vii | 141.17 (10) |
O9i—Ge3—O3 | 108.69 (13) | Ge1—O1—Fe1i | 127.13 (10) |
O9—Ge3—O5ii | 108.94 (13) | Ge1—O1—Fe1 | 127.13 (10) |
O9i—Ge3—O5ii | 108.94 (13) | Fe1i—O1—Fe1 | 102.7 (2) |
O3—Ge3—O5ii | 111.7 (2) | Ge2—O2—Ge4 | 142.6 (3) |
O2—Ge4—O8 | 110.6 (2) | Ge3—O3—Ge1 | 113.6 (3) |
O2—Ge4—O6i | 99.17 (11) | Ge1—O4—Cu1viii | 125.21 (17) |
O8—Ge4—O6i | 114.25 (11) | Ge1—O4—Fe1viii | 119.79 (17) |
O2—Ge4—O6 | 99.17 (11) | Cu1viii—O4—Fe1viii | 101.28 (15) |
O8—Ge4—O6 | 114.25 (11) | Ge3ix—O5—Ge2 | 114.5 (3) |
O6i—Ge4—O6 | 116.86 (17) | Ge4—O6—Fe1iii | 128.43 (12) |
O6iii—Fe1—O7iv | 107.02 (12) | Ge4—O6—Fe1 | 116.10 (13) |
O6iii—Fe1—O4v | 114.14 (11) | Fe1iii—O6—Fe1 | 107.43 (12) |
O7iv—Fe1—O4v | 75.84 (13) | Ge2—O7—Cu1iv | 122.38 (16) |
O6iii—Fe1—O8v | 91.93 (11) | Ge2—O7—Fe1iv | 136.57 (18) |
O7iv—Fe1—O8v | 155.28 (15) | Cu1iv—O7—Fe1iv | 100.09 (15) |
O4v—Fe1—O8v | 82.05 (15) | Ge4—O8—Fe1viii | 128.48 (4) |
O6iii—Fe1—O1 | 146.41 (14) | Ge4—O8—Fe1x | 128.48 (4) |
O7iv—Fe1—O1 | 94.37 (14) | Fe1viii—O8—Fe1x | 102.92 (7) |
O4v—Fe1—O1 | 95.78 (16) | Ge3—O9—Cu1vi | 125.45 (17) |
O8v—Fe1—O1 | 76.85 (10) | Ge3—O9—Cu1viii | 126.53 (16) |
O6iii—Fe1—O6 | 72.57 (12) | Cu1vi—O9—Cu1viii | 102.83 (16) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1; (vii) −x, −y, −z+2; (viii) x, y, z−1; (ix) x+1, y, z; (x) x, −y+1/2, z−1. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.931 Mg m−3 |
a = 12.0881 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.4914 (5) Å | µ = 19.05 mm−1 |
c = 4.8644 (4) Å | T = 130 K |
β = 96.137 (9)° | Prismatic, pale green |
V = 496.44 (6) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1198 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.056 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −17→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
5770 measured reflections | l = −6→6 |
1530 independent reflections |
Refinement on F2 | 1 restraint |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0229P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.031 | (Δ/σ)max = 0.001 |
wR(F2) = 0.055 | Δρmax = 1.31 e Å−3 |
S = 1.00 | Δρmin = −1.17 e Å−3 |
1530 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0032 (3) |
Cu2Fe2Ge4O13 | V = 496.44 (6) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0881 (9) Å | µ = 19.05 mm−1 |
b = 8.4914 (5) Å | T = 130 K |
c = 4.8644 (4) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.137 (9)° |
STOE IPDS-II diffractometer | 1530 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1198 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.056 |
5770 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 110 parameters |
wR(F2) = 0.055 | 1 restraint |
S = 1.00 | Δρmax = 1.31 e Å−3 |
1530 reflections | Δρmin = −1.17 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23974 (5) | 0.25 | 0.49397 (14) | 0.00374 (14) | |
Ge2 | 0.74765 (5) | 0.25 | 0.33896 (14) | 0.00366 (14) | |
Ge3 | −0.00507 (5) | 0.25 | 0.40634 (14) | 0.00390 (14) | |
Ge4 | 0.51222 (5) | 0.25 | 0.60604 (14) | 0.00335 (14) | |
Fe1 | 0.37605 (5) | 0.06145 (7) | 1.04815 (14) | 0.00354 (12) | |
Cu1 | 0.12593 (4) | −0.00340 (7) | 1.04331 (13) | 0.00600 (12) | |
O1 | 0.3324 (3) | 0.25 | 0.7953 (10) | 0.0053 (8) | |
O2 | 0.6538 (4) | 0.25 | 0.5741 (10) | 0.0095 (9) | |
O3 | 0.1129 (3) | 0.25 | 0.6473 (10) | 0.0050 (8) | |
O4 | 0.2479 (2) | 0.0836 (4) | 0.2866 (7) | 0.0056 (6) | |
O5 | 0.8719 (2) | 0.25 | 0.5683 (9) | 0.0067 (8) | |
O6 | 0.5033 (2) | 0.0742 (4) | 0.7915 (7) | 0.0063 (6) | |
O7 | 0.7423 (2) | 0.0804 (4) | 0.1341 (7) | 0.0060 (6) | |
O8 | 0.4362 (3) | 0.25 | 0.2811 (9) | 0.0053 (8) | |
O9 | −0.0027 (2) | 0.0830 (4) | 0.2017 (7) | 0.0088 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0039 (3) | 0.0046 (3) | 0.0028 (3) | 0 | 0.0004 (2) | 0 |
Ge2 | 0.0034 (3) | 0.0047 (3) | 0.0030 (3) | 0 | 0.0007 (2) | 0 |
Ge3 | 0.0026 (3) | 0.0059 (3) | 0.0033 (3) | 0 | 0.0008 (2) | 0 |
Ge4 | 0.0036 (2) | 0.0044 (3) | 0.0020 (3) | 0 | 0.0001 (2) | 0 |
Fe1 | 0.0036 (2) | 0.0047 (2) | 0.0024 (3) | 0.0004 (2) | 0.00057 (18) | 0.0001 (2) |
Cu1 | 0.0035 (2) | 0.0085 (2) | 0.0060 (2) | −0.00069 (17) | 0.00084 (15) | −0.00336 (19) |
O1 | 0.0048 (17) | 0.0056 (18) | 0.006 (2) | 0 | 0.0005 (15) | 0 |
O2 | 0.0078 (19) | 0.012 (2) | 0.009 (2) | 0 | 0.0016 (16) | 0 |
O3 | 0.0054 (17) | 0.0100 (19) | 0.000 (2) | 0 | 0.0032 (14) | 0 |
O4 | 0.0025 (12) | 0.0080 (14) | 0.0061 (16) | −0.0023 (10) | −0.0004 (10) | −0.0010 (12) |
O5 | 0.0040 (17) | 0.0127 (18) | 0.004 (2) | 0 | 0.0017 (15) | 0 |
O6 | 0.0063 (13) | 0.0081 (14) | 0.0048 (16) | 0.0003 (10) | 0.0019 (10) | −0.0001 (12) |
O7 | 0.0051 (12) | 0.0065 (14) | 0.0071 (16) | −0.0001 (10) | 0.0030 (10) | −0.0032 (12) |
O8 | 0.0076 (18) | 0.0071 (18) | 0.001 (2) | 0 | 0.0006 (14) | 0 |
O9 | 0.0043 (13) | 0.0130 (15) | 0.0088 (17) | −0.0009 (11) | −0.0004 (11) | −0.0053 (13) |
Ge1—O4 | 1.745 (3) | Ge4—O6i | 1.754 (3) |
Ge1—O4i | 1.745 (3) | Ge4—O6 | 1.754 (3) |
Ge1—O1 | 1.747 (4) | Fe1—O6iii | 1.954 (3) |
Ge1—O3 | 1.775 (4) | Fe1—O7iv | 2.003 (3) |
Ge2—O2 | 1.695 (5) | Fe1—O4v | 2.041 (3) |
Ge2—O7 | 1.748 (3) | Fe1—O8v | 2.049 (3) |
Ge2—O7i | 1.748 (3) | Fe1—O1 | 2.053 (3) |
Ge2—O5 | 1.773 (4) | Fe1—O6 | 2.085 (3) |
Ge3—O9 | 1.734 (3) | Cu1—O9vi | 1.928 (3) |
Ge3—O9i | 1.734 (3) | Cu1—O4v | 1.935 (3) |
Ge3—O3 | 1.747 (4) | Cu1—O9v | 1.951 (3) |
Ge3—O5ii | 1.7559 (19) | Cu1—O7iv | 2.001 (3) |
Ge4—O2 | 1.735 (4) | Cu1—Cu1vii | 3.0292 (10) |
Ge4—O8 | 1.741 (4) | ||
O4—Ge1—O4i | 108.1 (2) | O6i—Ge4—O6 | 116.7 (2) |
O4—Ge1—O1 | 114.48 (12) | O6iii—Fe1—O7iv | 106.84 (12) |
O4i—Ge1—O1 | 114.48 (12) | O6iii—Fe1—O4v | 114.03 (13) |
O4—Ge1—O3 | 110.33 (12) | O7iv—Fe1—O4v | 75.95 (13) |
O4i—Ge1—O3 | 110.33 (12) | O6iii—Fe1—O8v | 91.95 (13) |
O1—Ge1—O3 | 98.8 (2) | O7iv—Fe1—O8v | 155.36 (15) |
O2—Ge2—O7 | 113.46 (13) | O4v—Fe1—O8v | 81.94 (15) |
O2—Ge2—O7i | 113.46 (13) | O6iii—Fe1—O1 | 146.26 (15) |
O7—Ge2—O7i | 110.9 (2) | O7iv—Fe1—O1 | 94.49 (13) |
O2—Ge2—O5 | 99.11 (19) | O4v—Fe1—O1 | 96.11 (15) |
O7—Ge2—O5 | 109.63 (11) | O8v—Fe1—O1 | 77.01 (13) |
O7i—Ge2—O5 | 109.63 (11) | O6iii—Fe1—O6 | 72.70 (15) |
O9—Ge3—O9i | 109.7 (2) | O7iv—Fe1—O6 | 107.68 (13) |
O9—Ge3—O3 | 108.83 (13) | O4v—Fe1—O6 | 171.50 (12) |
O9i—Ge3—O3 | 108.83 (13) | O8v—Fe1—O6 | 92.86 (15) |
O9—Ge3—O5ii | 108.92 (13) | O1—Fe1—O6 | 76.09 (15) |
O9i—Ge3—O5ii | 108.92 (13) | O9vi—Cu1—O4v | 178.09 (14) |
O3—Ge3—O5ii | 111.6 (2) | O9vi—Cu1—O9v | 77.31 (16) |
O2—Ge4—O8 | 110.4 (2) | O4v—Cu1—O9v | 101.65 (13) |
O2—Ge4—O6i | 99.31 (13) | O9vi—Cu1—O7iv | 102.52 (13) |
O8—Ge4—O6i | 114.28 (11) | O4v—Cu1—O7iv | 78.42 (13) |
O2—Ge4—O6 | 99.31 (13) | O9v—Cu1—O7iv | 176.50 (15) |
O8—Ge4—O6 | 114.28 (11) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1; (vii) −x, −y, −z+2. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.962 Mg m−3 |
a = 12.0087 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.4931 (5) Å | µ = 19.17 mm−1 |
c = 4.8657 (4) Å | T = 170 K |
β = 96.139 (9)° | Prismatic, pale green |
V = 493.41 (6) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1171 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.057 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −16→16 |
Tmin = 0.12, Tmax = 0.22 | k = −11→11 |
5729 measured reflections | l = −6→6 |
1518 independent reflections |
Refinement on F2 | 3 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0301P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.031 | (Δ/σ)max = 0.001 |
wR(F2) = 0.062 | Δρmax = 1.03 e Å−3 |
S = 0.98 | Δρmin = −1.15 e Å−3 |
1518 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0058 (4) |
Cu2Fe2Ge4O13 | V = 493.41 (6) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0087 (9) Å | µ = 19.17 mm−1 |
b = 8.4931 (5) Å | T = 170 K |
c = 4.8657 (4) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.139 (9)° |
STOE IPDS-II diffractometer | 1518 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1171 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.22 | Rint = 0.057 |
5729 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 110 parameters |
wR(F2) = 0.062 | 3 restraints |
S = 0.98 | Δρmax = 1.03 e Å−3 |
1518 reflections | Δρmin = −1.15 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23978 (5) | 0.25 | 0.49373 (15) | 0.00453 (15) | |
Ge2 | 0.74752 (5) | 0.25 | 0.33876 (15) | 0.00442 (15) | |
Ge3 | −0.00516 (5) | 0.25 | 0.40619 (15) | 0.00488 (15) | |
Ge4 | 0.51223 (5) | 0.25 | 0.60641 (14) | 0.00396 (15) | |
Fe1 | 0.37589 (5) | 0.06134 (8) | 1.04797 (15) | 0.00438 (14) | |
Cu1 | 0.12583 (4) | −0.00325 (8) | 1.04329 (13) | 0.00727 (13) | |
O1 | 0.3320 (4) | 0.25 | 0.7961 (10) | 0.0075 (9) | |
O2 | 0.65451 (18) | 0.25 | 0.5741 (11) | 0.0084 (9) | |
O3 | 0.1131 (4) | 0.25 | 0.6455 (11) | 0.0074 (9) | |
O4 | 0.2480 (3) | 0.0840 (4) | 0.2860 (7) | 0.0069 (6) | |
O5 | 0.8715 (3) | 0.25 | 0.5699 (9) | 0.0080 (9) | |
O6 | 0.5037 (3) | 0.0752 (4) | 0.7928 (7) | 0.0056 (6) | |
O7 | 0.7426 (3) | 0.0805 (4) | 0.1344 (8) | 0.0068 (6) | |
O8 | 0.4357 (3) | 0.25 | 0.2807 (6) | 0.0054 (8) | |
O9 | −0.0026 (3) | 0.0829 (4) | 0.2032 (8) | 0.0111 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0033 (3) | 0.0059 (3) | 0.0043 (4) | 0 | −0.0003 (2) | 0 |
Ge2 | 0.0032 (3) | 0.0055 (3) | 0.0045 (3) | 0 | 0.0001 (2) | 0 |
Ge3 | 0.0035 (3) | 0.0077 (3) | 0.0034 (4) | 0 | 0.0005 (2) | 0 |
Ge4 | 0.0044 (3) | 0.0051 (3) | 0.0023 (3) | 0 | 0.0002 (2) | 0 |
Fe1 | 0.0039 (2) | 0.0058 (2) | 0.0035 (3) | −0.0001 (2) | 0.0006 (2) | −0.0001 (3) |
Cu1 | 0.0037 (2) | 0.0105 (2) | 0.0076 (3) | −0.00104 (18) | 0.00051 (17) | −0.0034 (2) |
O1 | 0.0088 (19) | 0.009 (2) | 0.005 (2) | 0 | 0.0011 (16) | 0 |
O2 | 0.007 (2) | 0.012 (2) | 0.007 (2) | 0 | 0.0044 (16) | 0 |
O3 | 0.0052 (19) | 0.011 (2) | 0.005 (2) | 0 | −0.0010 (16) | 0 |
O4 | 0.0048 (13) | 0.0098 (16) | 0.0063 (17) | −0.0013 (11) | 0.0018 (11) | −0.0015 (13) |
O5 | 0.0033 (18) | 0.013 (2) | 0.007 (3) | 0 | −0.0003 (16) | 0 |
O6 | 0.0043 (13) | 0.0064 (14) | 0.0064 (17) | 0.0014 (10) | 0.0018 (11) | 0.0015 (12) |
O7 | 0.0072 (13) | 0.0047 (14) | 0.0086 (17) | −0.0005 (10) | 0.0010 (11) | −0.0024 (12) |
O8 | 0.009 (2) | 0.0050 (19) | 0.002 (2) | 0 | 0.0001 (15) | 0 |
O9 | 0.0045 (14) | 0.0159 (17) | 0.0122 (19) | −0.0020 (12) | −0.0017 (12) | −0.0076 (14) |
Ge1—O4 | 1.744 (3) | Ge4—O8 | 1.7451 (19) |
Ge1—O4i | 1.744 (3) | Ge4—O6i | 1.749 (3) |
Ge1—O1 | 1.744 (5) | Ge4—O6 | 1.749 (3) |
Ge1—O3 | 1.761 (5) | Fe1—O6iii | 1.948 (3) |
Ge2—O2 | 1.683 (4) | Fe1—O7iv | 1.998 (3) |
Ge2—O7 | 1.747 (3) | Fe1—O4v | 2.030 (3) |
Ge2—O7i | 1.747 (3) | Fe1—O8v | 2.0472 (14) |
Ge2—O5 | 1.768 (5) | Fe1—O1 | 2.052 (3) |
Ge3—O9i | 1.731 (3) | Fe1—O6 | 2.078 (3) |
Ge3—O9 | 1.731 (3) | Cu1—O9vi | 1.925 (3) |
Ge3—O3 | 1.737 (5) | Cu1—O4v | 1.930 (3) |
Ge3—O5ii | 1.755 (4) | Cu1—O9v | 1.944 (4) |
Ge4—O2 | 1.7325 (19) | Cu1—O7iv | 1.992 (3) |
O4—Ge1—O4i | 107.9 (2) | O6i—Ge4—O6 | 116.2 (2) |
O4—Ge1—O1 | 114.76 (13) | O6iii—Fe1—O7iv | 106.30 (13) |
O4i—Ge1—O1 | 114.76 (13) | O6iii—Fe1—O4v | 113.85 (14) |
O4—Ge1—O3 | 110.35 (13) | O7iv—Fe1—O4v | 76.36 (14) |
O4i—Ge1—O3 | 110.35 (13) | O6iii—Fe1—O8v | 92.54 (12) |
O1—Ge1—O3 | 98.4 (2) | O7iv—Fe1—O8v | 155.29 (16) |
O2—Ge2—O7 | 113.74 (13) | O4v—Fe1—O8v | 81.51 (16) |
O2—Ge2—O7i | 113.74 (13) | O6iii—Fe1—O1 | 146.58 (17) |
O7—Ge2—O7i | 111.0 (2) | O7iv—Fe1—O1 | 94.61 (14) |
O2—Ge2—O5 | 98.18 (18) | O4v—Fe1—O1 | 96.04 (17) |
O7—Ge2—O5 | 109.71 (12) | O8v—Fe1—O1 | 76.80 (12) |
O7i—Ge2—O5 | 109.71 (12) | O6iii—Fe1—O6 | 72.96 (15) |
O9i—Ge3—O9 | 110.1 (3) | O7iv—Fe1—O6 | 107.75 (14) |
O9i—Ge3—O3 | 108.64 (14) | O4v—Fe1—O6 | 171.15 (12) |
O9—Ge3—O3 | 108.64 (14) | O8v—Fe1—O6 | 92.79 (16) |
O9i—Ge3—O5ii | 109.03 (14) | O1—Fe1—O6 | 75.99 (16) |
O9—Ge3—O5ii | 109.03 (14) | O9vi—Cu1—O4v | 177.99 (16) |
O3—Ge3—O5ii | 111.4 (2) | O9vi—Cu1—O9v | 77.98 (17) |
O2—Ge4—O8 | 110.3 (2) | O4v—Cu1—O9v | 101.20 (14) |
O2—Ge4—O6i | 99.21 (14) | O9vi—Cu1—O7iv | 101.90 (14) |
O8—Ge4—O6i | 114.62 (12) | O4v—Cu1—O7iv | 78.81 (14) |
O2—Ge4—O6 | 99.21 (14) | O9v—Cu1—O7iv | 176.68 (16) |
O8—Ge4—O6 | 114.62 (12) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.928 Mg m−3 |
a = 12.0859 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.4947 (5) Å | µ = 19.04 mm−1 |
c = 4.8667 (4) Å | T = 200 K |
β = 96.143 (9)° | Prismatic, pale green |
V = 496.78 (6) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1196 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.059 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −17→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
5779 measured reflections | l = −6→6 |
1530 independent reflections |
Refinement on F2 | 4 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0234P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.031 | (Δ/σ)max = 0.001 |
wR(F2) = 0.055 | Δρmax = 0.92 e Å−3 |
S = 0.97 | Δρmin = −1.09 e Å−3 |
1530 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0063 (4) |
Cu2Fe2Ge4O13 | V = 496.78 (6) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0859 (9) Å | µ = 19.04 mm−1 |
b = 8.4947 (5) Å | T = 200 K |
c = 4.8667 (4) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.143 (9)° |
STOE IPDS-II diffractometer | 1530 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1196 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.059 |
5779 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 110 parameters |
wR(F2) = 0.055 | 4 restraints |
S = 0.97 | Δρmax = 0.92 e Å−3 |
1530 reflections | Δρmin = −1.09 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23976 (5) | 0.25 | 0.49366 (14) | 0.00450 (14) | |
Ge2 | 0.74750 (5) | 0.25 | 0.33851 (14) | 0.00461 (14) | |
Ge3 | −0.00513 (5) | 0.25 | 0.40630 (14) | 0.00530 (14) | |
Ge4 | 0.51223 (5) | 0.25 | 0.60629 (13) | 0.00416 (14) | |
Fe1 | 0.37604 (5) | 0.06131 (7) | 1.04822 (14) | 0.00478 (13) | |
Cu1 | 0.12574 (4) | −0.00325 (7) | 1.04322 (13) | 0.00795 (12) | |
O1 | 0.3328 (3) | 0.25 | 0.7953 (10) | 0.0075 (8) | |
O2 | 0.6536 (3) | 0.25 | 0.5744 (10) | 0.0084 (8) | |
O3 | 0.1131 (4) | 0.25 | 0.6456 (10) | 0.0068 (8) | |
O4 | 0.2477 (2) | 0.0837 (3) | 0.2854 (7) | 0.0069 (6) | |
O5 | 0.8724 (4) | 0.25 | 0.5695 (10) | 0.0070 (8) | |
O6 | 0.5034 (2) | 0.0749 (2) | 0.7923 (6) | 0.0061 (6) | |
O7 | 0.7428 (2) | 0.0805 (4) | 0.1348 (7) | 0.0074 (6) | |
O8 | 0.4358 (3) | 0.25 | 0.2810 (6) | 0.0070 (8) | |
O9 | −0.00267 (17) | 0.0827 (3) | 0.2031 (6) | 0.0115 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0041 (3) | 0.0063 (3) | 0.0031 (3) | 0 | 0.0002 (2) | 0 |
Ge2 | 0.0043 (3) | 0.0056 (3) | 0.0041 (3) | 0 | 0.0009 (2) | 0 |
Ge3 | 0.0036 (3) | 0.0080 (3) | 0.0044 (3) | 0 | 0.0004 (2) | 0 |
Ge4 | 0.0048 (2) | 0.0052 (3) | 0.0023 (3) | 0 | −0.0001 (2) | 0 |
Fe1 | 0.0044 (2) | 0.0059 (2) | 0.0041 (3) | 0.0002 (2) | 0.00075 (19) | −0.0003 (2) |
Cu1 | 0.0043 (2) | 0.0112 (2) | 0.0083 (3) | −0.00087 (17) | 0.00064 (16) | −0.0042 (2) |
O1 | 0.0087 (18) | 0.0068 (18) | 0.007 (2) | 0 | −0.0002 (15) | 0 |
O2 | 0.0070 (19) | 0.013 (2) | 0.006 (2) | 0 | 0.0047 (15) | 0 |
O3 | 0.0072 (18) | 0.0107 (19) | 0.003 (2) | 0 | 0.0018 (14) | 0 |
O4 | 0.0060 (12) | 0.0085 (14) | 0.0065 (16) | −0.0022 (10) | 0.0017 (10) | −0.0005 (12) |
O5 | 0.0062 (16) | 0.0120 (18) | 0.002 (2) | 0 | −0.0008 (14) | 0 |
O6 | 0.0073 (13) | 0.0056 (13) | 0.0059 (16) | 0.0017 (10) | 0.0030 (10) | 0.0006 (11) |
O7 | 0.0068 (12) | 0.0089 (14) | 0.0066 (16) | −0.0012 (10) | 0.0013 (10) | −0.0016 (12) |
O8 | 0.0099 (19) | 0.0053 (18) | 0.005 (2) | 0 | −0.0007 (15) | 0 |
O9 | 0.0051 (13) | 0.0168 (16) | 0.0119 (18) | 0.0013 (11) | −0.0016 (11) | −0.0091 (14) |
Ge1—O4 | 1.747 (3) | Ge4—O8 | 1.7455 (19) |
Ge1—O4i | 1.747 (3) | Ge4—O6i | 1.7505 (17) |
Ge1—O1 | 1.751 (4) | Ge4—O6 | 1.7505 (17) |
Ge1—O3 | 1.770 (5) | Fe1—O6iii | 1.955 (2) |
Ge2—O2 | 1.698 (5) | Fe1—O7iv | 2.008 (3) |
Ge2—O7 | 1.746 (3) | Fe1—O4v | 2.039 (3) |
Ge2—O7i | 1.746 (3) | Fe1—O8v | 2.0491 (13) |
Ge2—O5 | 1.783 (4) | Fe1—O1 | 2.054 (3) |
Ge3—O9 | 1.7332 (17) | Fe1—O6 | 2.084 (3) |
Ge3—O9i | 1.7332 (17) | Cu1—O9vi | 1.930 (3) |
Ge3—O3 | 1.744 (4) | Cu1—O4v | 1.932 (3) |
Ge3—O5ii | 1.754 (5) | Cu1—O9v | 1.951 (3) |
Ge4—O2 | 1.732 (4) | Cu1—O7iv | 2.000 (3) |
O4—Ge1—O4i | 107.9 (2) | O6i—Ge4—O6 | 116.4 (2) |
O4—Ge1—O1 | 114.61 (12) | O6iii—Fe1—O7iv | 106.76 (11) |
O4i—Ge1—O1 | 114.61 (12) | O6iii—Fe1—O4v | 114.24 (12) |
O4—Ge1—O3 | 110.23 (12) | O7iv—Fe1—O4v | 75.86 (13) |
O4i—Ge1—O3 | 110.23 (12) | O6iii—Fe1—O8v | 92.28 (11) |
O1—Ge1—O3 | 99.0 (2) | O7iv—Fe1—O8v | 155.15 (15) |
O2—Ge2—O7 | 113.60 (13) | O4v—Fe1—O8v | 81.87 (15) |
O2—Ge2—O7i | 113.60 (13) | O6iii—Fe1—O1 | 146.17 (14) |
O7—Ge2—O7i | 111.1 (2) | O7iv—Fe1—O1 | 94.49 (13) |
O2—Ge2—O5 | 98.9 (2) | O4v—Fe1—O1 | 96.09 (16) |
O7—Ge2—O5 | 109.40 (13) | O8v—Fe1—O1 | 76.88 (11) |
O7i—Ge2—O5 | 109.40 (13) | O6iii—Fe1—O6 | 72.74 (10) |
O9—Ge3—O9i | 110.1 (2) | O7iv—Fe1—O6 | 107.88 (13) |
O9—Ge3—O3 | 108.56 (10) | O4v—Fe1—O6 | 171.21 (10) |
O9i—Ge3—O3 | 108.56 (10) | O8v—Fe1—O6 | 92.75 (15) |
O9—Ge3—O5ii | 108.98 (12) | O1—Fe1—O6 | 75.85 (14) |
O9i—Ge3—O5ii | 108.98 (12) | O9vi—Cu1—O4v | 177.99 (14) |
O3—Ge3—O5ii | 111.6 (2) | O9vi—Cu1—O9v | 77.61 (9) |
O2—Ge4—O8 | 110.5 (2) | O4v—Cu1—O9v | 101.59 (11) |
O2—Ge4—O6i | 99.32 (13) | O9vi—Cu1—O7iv | 102.20 (12) |
O8—Ge4—O6i | 114.41 (11) | O4v—Cu1—O7iv | 78.48 (13) |
O2—Ge4—O6 | 99.32 (13) | O9v—Cu1—O7iv | 176.70 (15) |
O8—Ge4—O6 | 114.41 (11) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.924 Mg m−3 |
a = 12.0858 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.4979 (5) Å | µ = 19.02 mm−1 |
c = 4.8691 (4) Å | T = 250 K |
β = 96.161 (9)° | Prismatic, pale green |
V = 497.19 (6) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1172 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.065 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −17→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
5751 measured reflections | l = −6→6 |
1523 independent reflections |
Refinement on F2 | 8 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0231P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.033 | (Δ/σ)max = 0.002 |
wR(F2) = 0.059 | Δρmax = 1.38 e Å−3 |
S = 1.00 | Δρmin = −1.09 e Å−3 |
1523 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0057 (4) |
Cu2Fe2Ge4O13 | V = 497.19 (6) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0858 (9) Å | µ = 19.02 mm−1 |
b = 8.4979 (5) Å | T = 250 K |
c = 4.8691 (4) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.161 (9)° |
STOE IPDS-II diffractometer | 1523 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1172 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.065 |
5751 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 110 parameters |
wR(F2) = 0.059 | 8 restraints |
S = 1.00 | Δρmax = 1.38 e Å−3 |
1523 reflections | Δρmin = −1.09 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23989 (5) | 0.25 | 0.49361 (15) | 0.00497 (15) | |
Ge2 | 0.74750 (5) | 0.25 | 0.33802 (15) | 0.00480 (15) | |
Ge3 | −0.00516 (5) | 0.25 | 0.40595 (15) | 0.00585 (15) | |
Ge4 | 0.51221 (5) | 0.25 | 0.60630 (15) | 0.00446 (15) | |
Fe1 | 0.37598 (5) | 0.06137 (7) | 1.04807 (15) | 0.00472 (13) | |
Cu1 | 0.12558 (4) | −0.00339 (8) | 1.04322 (14) | 0.00871 (13) | |
O1 | 0.3324 (3) | 0.25 | 0.7953 (11) | 0.0067 (9) | |
O2 | 0.6535 (3) | 0.25 | 0.5733 (8) | 0.0127 (10) | |
O3 | 0.1129 (4) | 0.25 | 0.6457 (11) | 0.0092 (9) | |
O4 | 0.24758 (19) | 0.0836 (4) | 0.2850 (6) | 0.0071 (6) | |
O5 | 0.8720 (2) | 0.25 | 0.5684 (9) | 0.0072 (9) | |
O6 | 0.5034 (2) | 0.0747 (3) | 0.7919 (7) | 0.0078 (6) | |
O7 | 0.74258 (13) | 0.0805 (3) | 0.1336 (6) | 0.0086 (6) | |
O8 | 0.4354 (4) | 0.25 | 0.2817 (10) | 0.0066 (9) | |
O9 | −0.0025 (3) | 0.0831 (3) | 0.2023 (7) | 0.0130 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0048 (3) | 0.0059 (3) | 0.0040 (4) | 0 | −0.0002 (2) | 0 |
Ge2 | 0.0047 (3) | 0.0052 (3) | 0.0047 (4) | 0 | 0.0014 (2) | 0 |
Ge3 | 0.0044 (3) | 0.0086 (3) | 0.0047 (4) | 0 | 0.0011 (2) | 0 |
Ge4 | 0.0055 (3) | 0.0053 (3) | 0.0026 (4) | 0 | 0.0004 (2) | 0 |
Fe1 | 0.0053 (2) | 0.0053 (2) | 0.0037 (3) | 0.0003 (2) | 0.0012 (2) | −0.0005 (3) |
Cu1 | 0.0051 (2) | 0.0121 (2) | 0.0090 (3) | −0.00076 (18) | 0.00115 (17) | −0.0050 (2) |
O1 | 0.0072 (17) | 0.0061 (19) | 0.006 (2) | 0 | −0.0005 (16) | 0 |
O2 | 0.0043 (19) | 0.021 (2) | 0.013 (3) | 0 | 0.0022 (17) | 0 |
O3 | 0.0064 (19) | 0.014 (2) | 0.007 (3) | 0 | 0.0038 (16) | 0 |
O4 | 0.0064 (13) | 0.0080 (15) | 0.0073 (18) | −0.0029 (10) | 0.0022 (11) | −0.0010 (12) |
O5 | 0.0066 (17) | 0.014 (2) | 0.000 (2) | 0 | −0.0009 (15) | 0 |
O6 | 0.0080 (13) | 0.0080 (15) | 0.0076 (18) | 0.0012 (11) | 0.0024 (11) | 0.0012 (13) |
O7 | 0.0076 (13) | 0.0094 (15) | 0.0091 (18) | −0.0007 (11) | 0.0021 (11) | −0.0045 (13) |
O8 | 0.0099 (19) | 0.010 (2) | 0.000 (2) | 0 | −0.0009 (15) | 0 |
O9 | 0.0073 (14) | 0.0177 (18) | 0.014 (2) | 0.0010 (12) | −0.0014 (12) | −0.0127 (15) |
Ge1—O1 | 1.748 (5) | Ge4—O8 | 1.745 (5) |
Ge1—O4 | 1.749 (3) | Ge4—O6i | 1.751 (4) |
Ge1—O4i | 1.749 (3) | Ge4—O6 | 1.751 (4) |
Ge1—O3 | 1.774 (5) | Fe1—O6iii | 1.956 (3) |
Ge2—O2 | 1.698 (4) | Fe1—O7iv | 2.004 (4) |
Ge2—O7 | 1.748 (3) | Fe1—O4v | 2.039 (4) |
Ge2—O7i | 1.748 (3) | Fe1—O8v | 2.050 (3) |
Ge2—O5 | 1.777 (4) | Fe1—O1 | 2.055 (3) |
Ge3—O9 | 1.733 (4) | Fe1—O6 | 2.086 (3) |
Ge3—O9i | 1.733 (4) | Cu1—O9vi | 1.928 (3) |
Ge3—O3 | 1.744 (5) | Cu1—O4v | 1.932 (3) |
Ge3—O5ii | 1.756 (4) | Cu1—O9v | 1.948 (3) |
Ge4—O2 | 1.733 (3) | Cu1—O7iv | 2.001 (3) |
O1—Ge1—O4 | 114.76 (13) | O6iii—Fe1—O4v | 114.15 (13) |
O1—Ge1—O4i | 114.76 (13) | O7iv—Fe1—O4v | 75.76 (10) |
O4—Ge1—O4i | 107.9 (2) | O6iii—Fe1—O8v | 92.26 (14) |
O1—Ge1—O3 | 98.8 (2) | O7iv—Fe1—O8v | 155.00 (13) |
O4—Ge1—O3 | 110.15 (11) | O4v—Fe1—O8v | 81.73 (16) |
O4i—Ge1—O3 | 110.15 (11) | O6iii—Fe1—O1 | 146.31 (15) |
O2—Ge2—O7 | 113.58 (11) | O7iv—Fe1—O1 | 94.57 (14) |
O2—Ge2—O7i | 113.58 (10) | O4v—Fe1—O1 | 96.02 (16) |
O7—Ge2—O7i | 111.0 (2) | O8v—Fe1—O1 | 76.97 (14) |
O2—Ge2—O5 | 98.98 (19) | O6iii—Fe1—O6 | 72.79 (11) |
O7—Ge2—O5 | 109.52 (10) | O7iv—Fe1—O6 | 107.91 (11) |
O7i—Ge2—O5 | 109.52 (10) | O4v—Fe1—O6 | 171.30 (11) |
O9—Ge3—O9i | 109.9 (3) | O8v—Fe1—O6 | 92.99 (16) |
O9—Ge3—O3 | 108.61 (14) | O1—Fe1—O6 | 75.97 (15) |
O9i—Ge3—O3 | 108.61 (14) | O9vi—Cu1—O4v | 178.07 (15) |
O9—Ge3—O5ii | 109.03 (14) | O9vi—Cu1—O9v | 77.65 (11) |
O9i—Ge3—O5ii | 109.03 (14) | O4v—Cu1—O9v | 101.56 (10) |
O3—Ge3—O5ii | 111.7 (2) | O9vi—Cu1—O7iv | 102.41 (10) |
O2—Ge4—O8 | 110.5 (2) | O4v—Cu1—O7iv | 78.27 (8) |
O2—Ge4—O6i | 99.38 (12) | O9v—Cu1—O7iv | 176.58 (17) |
O8—Ge4—O6i | 114.29 (12) | O9vi—Cu1—Cu1vii | 39.07 (8) |
O2—Ge4—O6 | 99.38 (12) | O4v—Cu1—Cu1vii | 140.12 (8) |
O8—Ge4—O6 | 114.29 (12) | O9v—Cu1—Cu1vii | 38.59 (8) |
O6i—Ge4—O6 | 116.5 (2) | O7iv—Cu1—Cu1vii | 141.37 (7) |
O6iii—Fe1—O7iv | 106.69 (12) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1; (vii) −x, −y, −z+2. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.922 Mg m−3 |
a = 12.0861 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.5008 (8) Å | µ = 19.00 mm−1 |
c = 4.8704 (5) Å | T = 290 K |
β = 96.167 (9)° | Prismatic, pale green |
V = 497.50 (9) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-II diffractometer | 1256 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.055 |
rotation method, ω scans | θmax = 30.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −17→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
7188 measured reflections | l = −6→6 |
1524 independent reflections |
Refinement on F2 | 4 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0282P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.026 | (Δ/σ)max = 0.001 |
wR(F2) = 0.054 | Δρmax = 0.91 e Å−3 |
S = 1.02 | Δρmin = −1.04 e Å−3 |
1524 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0179 (7) |
Cu2Fe2Ge4O13 | V = 497.50 (9) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0861 (12) Å | µ = 19.00 mm−1 |
b = 8.5008 (8) Å | T = 290 K |
c = 4.8704 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.167 (9)° |
STOE IPDS-II diffractometer | 1524 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1256 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.055 |
7188 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 110 parameters |
wR(F2) = 0.054 | 4 restraints |
S = 1.02 | Δρmax = 0.91 e Å−3 |
1524 reflections | Δρmin = −1.04 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23992 (4) | 0.25 | 0.49323 (11) | 0.00581 (12) | |
Ge2 | 0.74747 (4) | 0.25 | 0.33797 (11) | 0.00590 (12) | |
Ge3 | −0.00509 (4) | 0.25 | 0.40560 (11) | 0.00689 (12) | |
Ge4 | 0.51227 (4) | 0.25 | 0.60648 (11) | 0.00523 (12) | |
Fe1 | 0.37596 (4) | 0.06134 (6) | 1.04827 (11) | 0.00578 (11) | |
Cu1 | 0.12563 (4) | −0.00343 (6) | 1.04340 (10) | 0.01038 (11) | |
O1 | 0.3322 (3) | 0.25 | 0.7946 (6) | 0.0081 (7) | |
O2 | 0.6532 (3) | 0.25 | 0.5715 (9) | 0.0132 (7) | |
O3 | 0.1132 (3) | 0.25 | 0.6456 (8) | 0.0096 (7) | |
O4 | 0.24766 (17) | 0.0836 (3) | 0.2849 (5) | 0.0091 (5) | |
O5 | 0.8718 (2) | 0.25 | 0.5663 (7) | 0.0095 (7) | |
O6 | 0.5034 (2) | 0.0750 (2) | 0.7918 (5) | 0.0087 (5) | |
O7 | 0.7426 (2) | 0.0802 (3) | 0.1335 (6) | 0.0094 (5) | |
O8 | 0.4360 (3) | 0.25 | 0.2815 (7) | 0.0067 (6) | |
O9 | −0.0029 (2) | 0.0832 (3) | 0.2017 (6) | 0.0143 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0050 (2) | 0.0079 (2) | 0.0044 (3) | 0 | −0.00011 (18) | 0 |
Ge2 | 0.0052 (2) | 0.0070 (2) | 0.0056 (2) | 0 | 0.00095 (17) | 0 |
Ge3 | 0.0042 (2) | 0.0105 (2) | 0.0060 (3) | 0 | 0.00068 (18) | 0 |
Ge4 | 0.0055 (2) | 0.0066 (2) | 0.0035 (2) | 0 | 0.00021 (17) | 0 |
Fe1 | 0.0052 (2) | 0.00690 (19) | 0.0054 (2) | 0.00022 (16) | 0.00109 (16) | −0.00021 (18) |
Cu1 | 0.00548 (18) | 0.0143 (2) | 0.0114 (2) | −0.00102 (14) | 0.00125 (14) | −0.00620 (17) |
O1 | 0.0085 (15) | 0.0069 (14) | 0.0085 (17) | 0 | −0.0004 (13) | 0 |
O2 | 0.0070 (16) | 0.0234 (19) | 0.0099 (19) | 0 | 0.0039 (14) | 0 |
O3 | 0.0076 (15) | 0.0160 (16) | 0.0056 (17) | 0 | 0.0021 (13) | 0 |
O4 | 0.0058 (10) | 0.0133 (12) | 0.0087 (12) | −0.0030 (8) | 0.0025 (9) | −0.0021 (10) |
O5 | 0.0060 (14) | 0.0156 (16) | 0.0068 (17) | 0 | 0.0005 (13) | 0 |
O6 | 0.0091 (11) | 0.0083 (11) | 0.0091 (13) | 0.0020 (8) | 0.0028 (9) | 0.0035 (9) |
O7 | 0.0061 (10) | 0.0107 (11) | 0.0116 (13) | −0.0012 (8) | 0.0018 (9) | −0.0029 (10) |
O8 | 0.0087 (15) | 0.0093 (15) | 0.0016 (15) | 0 | −0.0014 (12) | 0 |
O9 | 0.0074 (11) | 0.0204 (14) | 0.0151 (14) | −0.0003 (10) | 0.0008 (10) | −0.0106 (11) |
Ge1—O1 | 1.746 (3) | Ge4—O8 | 1.744 (3) |
Ge1—O4 | 1.750 (2) | Ge4—O6i | 1.749 (3) |
Ge1—O4i | 1.750 (2) | Ge4—O6 | 1.749 (3) |
Ge1—O3 | 1.772 (4) | Fe1—O6iii | 1.957 (2) |
Ge2—O2 | 1.694 (4) | Fe1—O7iv | 2.004 (3) |
Ge2—O7 | 1.751 (3) | Fe1—O4v | 2.038 (3) |
Ge2—O7i | 1.751 (3) | Fe1—O8v | 2.052 (2) |
Ge2—O5 | 1.771 (3) | Fe1—O1 | 2.059 (3) |
Ge3—O9 | 1.733 (3) | Fe1—O6 | 2.088 (3) |
Ge3—O9i | 1.733 (3) | Cu1—O9vi | 1.925 (3) |
Ge3—O3 | 1.747 (4) | Cu1—O4v | 1.932 (3) |
Ge3—O5ii | 1.7541 (19) | Cu1—O9v | 1.951 (3) |
Ge4—O2 | 1.730 (4) | Cu1—O7iv | 1.999 (3) |
O1—Ge1—O4 | 114.75 (9) | O6i—Ge4—O6 | 116.51 (18) |
O1—Ge1—O4i | 114.75 (9) | O6iii—Fe1—O7iv | 106.69 (10) |
O4—Ge1—O4i | 107.94 (18) | O6iii—Fe1—O4v | 114.17 (10) |
O1—Ge1—O3 | 98.67 (18) | O7iv—Fe1—O4v | 75.74 (10) |
O4—Ge1—O3 | 110.21 (10) | O6iii—Fe1—O8v | 92.21 (10) |
O4i—Ge1—O3 | 110.21 (10) | O7iv—Fe1—O8v | 155.17 (13) |
O2—Ge2—O7 | 113.46 (11) | O4v—Fe1—O8v | 81.95 (12) |
O2—Ge2—O7i | 113.46 (11) | O6iii—Fe1—O1 | 146.34 (12) |
O7—Ge2—O7i | 111.03 (18) | O7iv—Fe1—O1 | 94.44 (10) |
O2—Ge2—O5 | 99.50 (16) | O4v—Fe1—O1 | 96.04 (13) |
O7—Ge2—O5 | 109.35 (9) | O8v—Fe1—O1 | 77.06 (9) |
O7i—Ge2—O5 | 109.35 (9) | O6iii—Fe1—O6 | 72.85 (9) |
O9—Ge3—O9i | 109.8 (2) | O7iv—Fe1—O6 | 107.93 (11) |
O9—Ge3—O3 | 108.75 (11) | O4v—Fe1—O6 | 171.22 (9) |
O9i—Ge3—O3 | 108.75 (11) | O8v—Fe1—O6 | 92.75 (13) |
O9—Ge3—O5ii | 108.77 (11) | O1—Fe1—O6 | 75.88 (12) |
O9i—Ge3—O5ii | 108.77 (11) | O9vi—Cu1—O4v | 178.10 (13) |
O3—Ge3—O5ii | 111.97 (18) | O9vi—Cu1—O9v | 77.56 (13) |
O2—Ge4—O8 | 109.90 (19) | O4v—Cu1—O9v | 101.72 (11) |
O2—Ge4—O6i | 99.58 (11) | O9vi—Cu1—O7iv | 102.37 (11) |
O8—Ge4—O6i | 114.37 (9) | O4v—Cu1—O7iv | 78.24 (11) |
O2—Ge4—O6 | 99.58 (11) | O9v—Cu1—O7iv | 176.43 (13) |
O8—Ge4—O6 | 114.37 (9) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.920 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.088 (2) Å | Cell parameters from 4906 reflections |
b = 8.5019 (9) Å | θ = 2.9–28.1° |
c = 4.8703 (8) Å | µ = 18.99 mm−1 |
β = 96.17 (2)° | T = 298 K |
V = 497.61 (13) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 1087 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.039 |
rotation method, ϕ scans | θmax = 28.1°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4906 measured reflections | l = −6→6 |
1267 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0291P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.021 | (Δ/σ)max = 0.001 |
wR(F2) = 0.048 | Δρmax = 1.45 e Å−3 |
S = 1.02 | Δρmin = −1.59 e Å−3 |
1267 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
107 parameters | Extinction coefficient: 0.0332 (9) |
Cu2Fe2Ge4O13 | V = 497.61 (13) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.088 (2) Å | µ = 18.99 mm−1 |
b = 8.5019 (9) Å | T = 298 K |
c = 4.8703 (8) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.17 (2)° |
STOE IPDS-I diffractometer | 1267 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 1087 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.039 |
4906 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 107 parameters |
wR(F2) = 0.048 | 0 restraints |
S = 1.02 | Δρmax = 1.45 e Å−3 |
1267 reflections | Δρmin = −1.59 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23997 (3) | 0.25 | 0.49324 (9) | 0.00252 (11) | |
Ge2 | 0.74733 (4) | 0.25 | 0.33753 (9) | 0.00285 (12) | |
Ge3 | −0.00505 (3) | 0.25 | 0.40568 (9) | 0.00396 (12) | |
Ge4 | 0.51225 (3) | 0.25 | 0.60653 (9) | 0.00236 (11)* | |
Fe1 | 0.37588 (3) | 0.06131 (5) | 1.04818 (9) | 0.00279 (12) | |
Cu1 | 0.12561 (3) | −0.00333 (5) | 1.04327 (9) | 0.00796 (11) | |
O1 | 0.3310 (2) | 0.25 | 0.7954 (6) | 0.0042 (6) | |
O2 | 0.6530 (3) | 0.25 | 0.5723 (7) | 0.0112 (7) | |
O3 | 0.1132 (3) | 0.25 | 0.6456 (7) | 0.0065 (6) | |
O4 | 0.24768 (17) | 0.0838 (3) | 0.2847 (5) | 0.0061 (4) | |
O5 | 0.8725 (2) | 0.25 | 0.5667 (7) | 0.0064 (6) | |
O6 | 0.50347 (17) | 0.0745 (2) | 0.7919 (4) | 0.0052 (4) | |
O7 | 0.74245 (18) | 0.0803 (3) | 0.1347 (5) | 0.0068 (4) | |
O8 | 0.4356 (2) | 0.25 | 0.2820 (6) | 0.0048 (6) | |
O9 | −0.00298 (18) | 0.0829 (3) | 0.2022 (5) | 0.0120 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0027 (2) | 0.0040 (2) | 0.0006 (2) | 0 | −0.00080 (16) | 0 |
Ge2 | 0.0031 (2) | 0.0036 (2) | 0.0018 (2) | 0 | −0.00012 (16) | 0 |
Ge3 | 0.0024 (2) | 0.0070 (2) | 0.0024 (2) | 0 | 0.00002 (17) | 0 |
Fe1 | 0.0033 (2) | 0.0032 (2) | 0.0019 (2) | 0.00020 (14) | −0.00004 (15) | 0.00009 (16) |
Cu1 | 0.00344 (18) | 0.0118 (2) | 0.0086 (2) | −0.00106 (14) | 0.00057 (13) | −0.00667 (16) |
O1 | 0.0066 (14) | 0.0035 (14) | 0.0023 (14) | 0 | −0.0011 (11) | 0 |
O2 | 0.0103 (16) | 0.0187 (18) | 0.0051 (16) | 0 | 0.0033 (13) | 0 |
O3 | 0.0031 (13) | 0.0110 (15) | 0.0051 (15) | 0 | −0.0013 (11) | 0 |
O4 | 0.0056 (10) | 0.0072 (11) | 0.0054 (10) | −0.0005 (8) | 0.0006 (8) | −0.0039 (9) |
O5 | 0.0031 (13) | 0.0118 (16) | 0.0042 (15) | 0 | −0.0001 (11) | 0 |
O6 | 0.0069 (10) | 0.0052 (10) | 0.0040 (10) | 0.0016 (8) | 0.0026 (8) | 0.0026 (9) |
O7 | 0.0064 (10) | 0.0055 (10) | 0.0087 (11) | −0.0009 (8) | 0.0023 (8) | −0.0031 (9) |
O8 | 0.0037 (14) | 0.0062 (14) | 0.0041 (15) | 0 | −0.0019 (11) | 0 |
O9 | 0.0059 (10) | 0.0182 (13) | 0.0119 (12) | 0.0004 (9) | 0.0009 (9) | −0.0110 (11) |
Ge1—O1 | 1.740 (3) | Ge4—O8 | 1.744 (3) |
Ge1—O4 | 1.748 (2) | Ge4—O6i | 1.753 (2) |
Ge1—O4i | 1.748 (2) | Ge4—O6 | 1.753 (2) |
Ge1—O3 | 1.772 (3) | Fe1—O6iii | 1.955 (2) |
Ge2—O2 | 1.699 (3) | Fe1—O7iv | 2.004 (2) |
Ge2—O7 | 1.746 (2) | Fe1—O4v | 2.037 (2) |
Ge2—O7i | 1.746 (2) | Fe1—O8v | 2.0529 (19) |
Ge2—O5 | 1.781 (3) | Fe1—O1 | 2.0592 (19) |
Ge3—O9 | 1.734 (2) | Fe1—O6 | 2.089 (2) |
Ge3—O9i | 1.734 (2) | Cu1—O9vi | 1.925 (2) |
Ge3—O3 | 1.747 (3) | Cu1—O4v | 1.933 (2) |
Ge3—O5ii | 1.748 (3) | Cu1—O9v | 1.952 (2) |
Ge4—O2 | 1.727 (3) | Cu1—O7iv | 2.005 (2) |
O1—Ge1—O4 | 115.02 (8) | O6i—Ge4—O6 | 116.67 (15) |
O1—Ge1—O4i | 115.02 (8) | O6iii—Fe1—O7iv | 106.77 (9) |
O4—Ge1—O4i | 107.82 (15) | O6iii—Fe1—O4v | 114.24 (9) |
O1—Ge1—O3 | 98.19 (15) | O7iv—Fe1—O4v | 75.97 (9) |
O4—Ge1—O3 | 110.22 (9) | O6iii—Fe1—O8v | 92.17 (9) |
O4i—Ge1—O3 | 110.22 (9) | O7iv—Fe1—O8v | 155.18 (11) |
O2—Ge2—O7 | 113.36 (9) | O4v—Fe1—O8v | 81.73 (11) |
O2—Ge2—O7i | 113.36 (9) | O6iii—Fe1—O1 | 146.68 (11) |
O7—Ge2—O7i | 111.44 (15) | O7iv—Fe1—O1 | 94.17 (9) |
O2—Ge2—O5 | 99.47 (16) | O4v—Fe1—O1 | 95.59 (11) |
O7—Ge2—O5 | 109.23 (9) | O8v—Fe1—O1 | 77.13 (9) |
O7i—Ge2—O5 | 109.23 (9) | O6iii—Fe1—O6 | 72.70 (10) |
O9—Ge3—O9i | 110.02 (17) | O7iv—Fe1—O6 | 107.72 (9) |
O9—Ge3—O3 | 108.74 (10) | O4v—Fe1—O6 | 171.27 (9) |
O9i—Ge3—O3 | 108.74 (10) | O8v—Fe1—O6 | 92.95 (11) |
O9—Ge3—O5ii | 108.75 (9) | O1—Fe1—O6 | 76.40 (10) |
O9i—Ge3—O5ii | 108.75 (9) | O9vi—Cu1—O4v | 178.02 (11) |
O3—Ge3—O5ii | 111.83 (15) | O9vi—Cu1—O9v | 77.61 (11) |
O2—Ge4—O8 | 110.22 (16) | O4v—Cu1—O9v | 101.72 (9) |
O2—Ge4—O6i | 99.46 (9) | O9vi—Cu1—O7iv | 102.25 (10) |
O8—Ge4—O6i | 114.27 (8) | O4v—Cu1—O7iv | 78.31 (9) |
O2—Ge4—O6 | 99.46 (9) | O9v—Cu1—O7iv | 176.51 (10) |
O8—Ge4—O6 | 114.27 (8) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.917 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.0876 (8) Å | Cell parameters from 4432 reflections |
b = 8.5043 (7) Å | θ = 2.9–28.1° |
c = 4.8715 (5) Å | µ = 18.99 mm−1 |
β = 96.19 (2)° | T = 320 K |
V = 497.86 (7) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 955 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.038 |
rotation method, ϕ scans | θmax = 28.1°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4481 measured reflections | l = −5→5 |
1162 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0272P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max = 0.001 |
wR(F2) = 0.051 | Δρmax = 0.75 e Å−3 |
S = 1.01 | Δρmin = −0.81 e Å−3 |
1162 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0268 (8) |
Cu2Fe2Ge4O13 | V = 497.86 (7) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0876 (8) Å | µ = 18.99 mm−1 |
b = 8.5043 (7) Å | T = 320 K |
c = 4.8715 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.19 (2)° |
STOE IPDS-I diffractometer | 1162 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 955 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.038 |
4481 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 110 parameters |
wR(F2) = 0.051 | 0 restraints |
S = 1.01 | Δρmax = 0.75 e Å−3 |
1162 reflections | Δρmin = −0.81 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23988 (5) | 0.25 | 0.49305 (14) | 0.00620 (16) | |
Ge2 | 0.74738 (5) | 0.25 | 0.33752 (15) | 0.00633 (16) | |
Ge3 | −0.00508 (5) | 0.25 | 0.40544 (15) | 0.00758 (16) | |
Ge4 | 0.51226 (5) | 0.25 | 0.60642 (14) | 0.00566 (15) | |
Fe1 | 0.37596 (5) | 0.06135 (7) | 1.04831 (14) | 0.00639 (15) | |
Cu1 | 0.12556 (4) | −0.00334 (7) | 1.04342 (13) | 0.01159 (15) | |
O1 | 0.3322 (3) | 0.25 | 0.7949 (10) | 0.0079 (9) | |
O2 | 0.6532 (3) | 0.25 | 0.5721 (11) | 0.0132 (10) | |
O3 | 0.1129 (3) | 0.25 | 0.6458 (11) | 0.0098 (9) | |
O4 | 0.2481 (2) | 0.0836 (4) | 0.2853 (7) | 0.0095 (6) | |
O5 | 0.8717 (3) | 0.25 | 0.5671 (11) | 0.0098 (9) | |
O6 | 0.5034 (2) | 0.0745 (3) | 0.7915 (7) | 0.0091 (6) | |
O7 | 0.7429 (2) | 0.0800 (4) | 0.1339 (7) | 0.0105 (6) | |
O8 | 0.4359 (3) | 0.25 | 0.2825 (10) | 0.0078 (9) | |
O9 | −0.0030 (2) | 0.0830 (4) | 0.2016 (8) | 0.0171 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0033 (3) | 0.0056 (3) | 0.0095 (4) | 0 | 0.0000 (2) | 0 |
Ge2 | 0.0028 (3) | 0.0049 (3) | 0.0112 (4) | 0 | 0.0006 (2) | 0 |
Ge3 | 0.0027 (3) | 0.0094 (3) | 0.0107 (4) | 0 | 0.0006 (2) | 0 |
Ge4 | 0.0039 (3) | 0.0047 (3) | 0.0082 (4) | 0 | −0.0002 (2) | 0 |
Fe1 | 0.0035 (2) | 0.0048 (3) | 0.0110 (4) | 0.0002 (2) | 0.0010 (2) | −0.0002 (2) |
Cu1 | 0.0032 (2) | 0.0140 (3) | 0.0175 (3) | −0.00094 (18) | 0.00106 (17) | −0.0067 (2) |
O1 | 0.0063 (18) | 0.0038 (18) | 0.013 (3) | 0 | 0.0001 (15) | 0 |
O2 | 0.0034 (19) | 0.019 (2) | 0.018 (3) | 0 | 0.0041 (17) | 0 |
O3 | 0.0019 (17) | 0.016 (2) | 0.012 (3) | 0 | 0.0031 (15) | 0 |
O4 | 0.0039 (12) | 0.0094 (15) | 0.015 (2) | −0.0037 (10) | 0.0024 (11) | −0.0030 (12) |
O5 | 0.0053 (17) | 0.014 (2) | 0.010 (3) | 0 | 0.0022 (16) | 0 |
O6 | 0.0061 (13) | 0.0074 (14) | 0.014 (2) | 0.0040 (11) | 0.0024 (11) | 0.0035 (12) |
O7 | 0.0062 (13) | 0.0077 (14) | 0.018 (2) | −0.0007 (11) | 0.0007 (11) | −0.0051 (12) |
O8 | 0.0061 (18) | 0.0064 (19) | 0.011 (3) | 0 | 0.0000 (15) | 0 |
O9 | 0.0045 (13) | 0.0216 (18) | 0.025 (2) | 0.0026 (12) | −0.0008 (12) | −0.0130 (15) |
Ge1—O1 | 1.748 (5) | Ge4—O8 | 1.740 (5) |
Ge1—O4 | 1.749 (3) | Ge4—O6i | 1.753 (3) |
Ge1—O4i | 1.749 (3) | Ge4—O6 | 1.753 (3) |
Ge1—O3 | 1.776 (4) | Fe1—O6iii | 1.956 (3) |
Ge2—O2 | 1.698 (5) | Fe1—O7iv | 2.005 (3) |
Ge2—O7 | 1.751 (3) | Fe1—O4v | 2.035 (3) |
Ge2—O7i | 1.751 (3) | Fe1—O8v | 2.055 (3) |
Ge2—O5 | 1.773 (5) | Fe1—O1 | 2.058 (3) |
Ge3—O9 | 1.734 (3) | Fe1—O6 | 2.090 (3) |
Ge3—O9i | 1.734 (3) | Cu1—O9vi | 1.923 (3) |
Ge3—O3 | 1.745 (5) | Cu1—O4v | 1.937 (3) |
Ge3—O5ii | 1.759 (5) | Cu1—O9v | 1.951 (3) |
Ge4—O2 | 1.729 (4) | Cu1—O7iv | 1.999 (3) |
O1—Ge1—O4 | 114.59 (12) | O6i—Ge4—O6 | 116.7 (2) |
O1—Ge1—O4i | 114.59 (12) | O6iii—Fe1—O7iv | 106.86 (13) |
O4—Ge1—O4i | 108.0 (2) | O6iii—Fe1—O4v | 114.07 (14) |
O1—Ge1—O3 | 98.6 (2) | O7iv—Fe1—O4v | 75.84 (13) |
O4—Ge1—O3 | 110.35 (12) | O6iii—Fe1—O8v | 92.10 (13) |
O4i—Ge1—O3 | 110.35 (12) | O7iv—Fe1—O8v | 155.07 (14) |
O2—Ge2—O7 | 113.52 (13) | O4v—Fe1—O8v | 81.76 (15) |
O2—Ge2—O7i | 113.52 (13) | O6iii—Fe1—O1 | 146.30 (14) |
O7—Ge2—O7i | 111.3 (2) | O7iv—Fe1—O1 | 94.38 (14) |
O2—Ge2—O5 | 99.2 (2) | O4v—Fe1—O1 | 96.09 (15) |
O7—Ge2—O5 | 109.26 (13) | O8v—Fe1—O1 | 77.11 (14) |
O7i—Ge2—O5 | 109.26 (13) | O6iii—Fe1—O6 | 72.81 (15) |
O9—Ge3—O9i | 109.9 (3) | O7iv—Fe1—O6 | 107.83 (13) |
O9—Ge3—O3 | 108.85 (13) | O4v—Fe1—O6 | 171.33 (12) |
O9i—Ge3—O3 | 108.85 (13) | O8v—Fe1—O6 | 92.97 (15) |
O9—Ge3—O5ii | 108.75 (13) | O1—Fe1—O6 | 75.95 (14) |
O9i—Ge3—O5ii | 108.75 (13) | O9vi—Cu1—O4v | 178.16 (16) |
O3—Ge3—O5ii | 111.7 (2) | O9vi—Cu1—O9v | 77.58 (16) |
O2—Ge4—O8 | 110.1 (2) | O4v—Cu1—O9v | 101.85 (13) |
O2—Ge4—O6i | 99.51 (13) | O9vi—Cu1—O7iv | 102.25 (14) |
O8—Ge4—O6i | 114.25 (12) | O4v—Cu1—O7iv | 78.21 (13) |
O2—Ge4—O6 | 99.51 (13) | O9v—Cu1—O7iv | 176.42 (16) |
O8—Ge4—O6 | 114.25 (12) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.915 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.0883 (8) Å | Cell parameters from 4906 reflections |
b = 8.5076 (7) Å | θ = 2.9–28.0° |
c = 4.8727 (5) Å | µ = 18.98 mm−1 |
β = 96.18 (2)° | T = 362 K |
V = 498.21 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 956 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.049 |
rotation method, ϕ scans | θmax = 28.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4515 measured reflections | l = −5→5 |
1164 independent reflections |
Refinement on F2 | 4 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0286P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max < 0.001 |
wR(F2) = 0.053 | Δρmax = 1.16 e Å−3 |
S = 0.97 | Δρmin = −0.85 e Å−3 |
1164 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0242 (8) |
Cu2Fe2Ge4O13 | V = 498.21 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0883 (8) Å | µ = 18.98 mm−1 |
b = 8.5076 (7) Å | T = 362 K |
c = 4.8727 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.18 (2)° |
STOE IPDS-I diffractometer | 1164 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 956 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.049 |
4515 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 110 parameters |
wR(F2) = 0.053 | 4 restraints |
S = 0.97 | Δρmax = 1.16 e Å−3 |
1164 reflections | Δρmin = −0.85 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.23996 (4) | 0.25 | 0.49306 (14) | 0.00631 (16) | |
Ge2 | 0.74735 (4) | 0.25 | 0.33719 (14) | 0.00635 (16) | |
Ge3 | −0.00508 (4) | 0.25 | 0.40499 (14) | 0.00770 (16) | |
Ge4 | 0.51235 (5) | 0.25 | 0.60638 (14) | 0.00577 (16) | |
Fe1 | 0.37590 (4) | 0.06137 (7) | 1.04840 (14) | 0.00651 (16) | |
Cu1 | 0.12549 (4) | −0.00345 (7) | 1.04351 (13) | 0.01229 (15) | |
O1 | 0.3322 (3) | 0.25 | 0.7944 (10) | 0.0085 (9) | |
O2 | 0.6532 (3) | 0.25 | 0.5707 (11) | 0.0151 (10) | |
O3 | 0.1133 (3) | 0.25 | 0.6449 (11) | 0.0105 (9) | |
O4 | 0.2480 (2) | 0.0839 (4) | 0.2852 (7) | 0.0100 (6) | |
O5 | 0.8719 (3) | 0.25 | 0.5667 (11) | 0.0116 (9) | |
O6 | 0.5036 (2) | 0.0750 (3) | 0.7913 (6) | 0.0095 (6) | |
O7 | 0.74264 (10) | 0.0804 (3) | 0.1343 (5) | 0.0107 (7) | |
O8 | 0.4360 (3) | 0.25 | 0.2819 (10) | 0.0082 (9) | |
O9 | −0.0029 (2) | 0.0831 (4) | 0.2011 (8) | 0.0176 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0026 (3) | 0.0064 (3) | 0.0098 (4) | 0 | 0.0003 (2) | 0 |
Ge2 | 0.0020 (3) | 0.0057 (3) | 0.0115 (4) | 0 | 0.0010 (2) | 0 |
Ge3 | 0.0016 (3) | 0.0104 (3) | 0.0111 (4) | 0 | 0.0008 (2) | 0 |
Ge4 | 0.0036 (2) | 0.0051 (3) | 0.0085 (4) | 0 | 0.0001 (2) | 0 |
Fe1 | 0.0027 (2) | 0.0059 (3) | 0.0111 (4) | 0.00030 (19) | 0.0013 (2) | −0.0001 (2) |
Cu1 | 0.0029 (2) | 0.0156 (3) | 0.0185 (4) | −0.00133 (18) | 0.00161 (17) | −0.0074 (2) |
O1 | 0.0031 (16) | 0.0057 (19) | 0.017 (3) | 0 | 0.0008 (15) | 0 |
O2 | 0.0066 (19) | 0.026 (3) | 0.013 (3) | 0 | 0.0034 (16) | 0 |
O3 | 0.0023 (16) | 0.018 (2) | 0.011 (3) | 0 | 0.0014 (15) | 0 |
O4 | 0.0055 (12) | 0.0103 (15) | 0.014 (2) | −0.0013 (10) | 0.0013 (10) | −0.0030 (12) |
O5 | 0.0036 (16) | 0.018 (2) | 0.013 (3) | 0 | 0.0026 (16) | 0 |
O6 | 0.0048 (12) | 0.0075 (14) | 0.017 (2) | 0.0049 (10) | 0.0030 (11) | 0.0048 (13) |
O7 | 0.0070 (13) | 0.0077 (14) | 0.017 (2) | 0.0000 (10) | 0.0016 (11) | −0.0054 (12) |
O8 | 0.0067 (18) | 0.0081 (19) | 0.010 (3) | 0 | 0.0001 (15) | 0 |
O9 | 0.0049 (13) | 0.0228 (18) | 0.025 (2) | 0.0021 (12) | 0.0012 (12) | −0.0134 (16) |
Ge1—O1 | 1.746 (5) | Ge4—O8 | 1.743 (5) |
Ge1—O4 | 1.748 (3) | Ge4—O6i | 1.750 (4) |
Ge1—O4i | 1.748 (3) | Ge4—O6 | 1.750 (4) |
Ge1—O3 | 1.771 (4) | Fe1—O6iii | 1.958 (2) |
Ge2—O2 | 1.694 (5) | Fe1—O7iv | 2.007 (3) |
Ge2—O7 | 1.747 (4) | Fe1—O4v | 2.035 (3) |
Ge2—O7i | 1.747 (4) | Fe1—O8v | 2.054 (3) |
Ge2—O5 | 1.776 (4) | Fe1—O1 | 2.060 (3) |
Ge3—O9 | 1.735 (3) | Fe1—O6 | 2.093 (3) |
Ge3—O9i | 1.735 (3) | Cu1—O9vi | 1.922 (3) |
Ge3—O3 | 1.747 (4) | Cu1—O4v | 1.939 (3) |
Ge3—O5ii | 1.756 (5) | Cu1—O9v | 1.949 (3) |
Ge4—O2 | 1.729 (4) | Cu1—O7iv | 2.004 (3) |
O1—Ge1—O4 | 114.65 (12) | O6i—Ge4—O6 | 116.7 (2) |
O1—Ge1—O4i | 114.65 (12) | O6iii—Fe1—O7iv | 106.62 (11) |
O4—Ge1—O4i | 107.9 (2) | O6iii—Fe1—O4v | 114.04 (13) |
O1—Ge1—O3 | 98.7 (2) | O7iv—Fe1—O4v | 76.02 (10) |
O4—Ge1—O3 | 110.29 (12) | O6iii—Fe1—O8v | 92.19 (13) |
O4i—Ge1—O3 | 110.29 (12) | O7iv—Fe1—O8v | 155.30 (12) |
O2—Ge2—O7 | 113.38 (10) | O4v—Fe1—O8v | 81.80 (15) |
O2—Ge2—O7i | 113.38 (9) | O6iii—Fe1—O1 | 146.38 (13) |
O7—Ge2—O7i | 111.4 (2) | O7iv—Fe1—O1 | 94.43 (13) |
O2—Ge2—O5 | 99.4 (2) | O4v—Fe1—O1 | 96.09 (15) |
O7—Ge2—O5 | 109.29 (11) | O8v—Fe1—O1 | 77.10 (14) |
O7i—Ge2—O5 | 109.29 (11) | O6iii—Fe1—O6 | 72.94 (10) |
O9—Ge3—O9i | 109.9 (3) | O7iv—Fe1—O6 | 107.76 (10) |
O9—Ge3—O3 | 108.76 (13) | O4v—Fe1—O6 | 171.19 (11) |
O9i—Ge3—O3 | 108.76 (13) | O8v—Fe1—O6 | 92.79 (15) |
O9—Ge3—O5ii | 108.82 (13) | O1—Fe1—O6 | 75.83 (13) |
O9i—Ge3—O5ii | 108.82 (13) | O9vi—Cu1—O4v | 178.09 (16) |
O3—Ge3—O5ii | 111.8 (2) | O9vi—Cu1—O9v | 77.53 (16) |
O2—Ge4—O8 | 109.8 (2) | O4v—Cu1—O9v | 101.82 (13) |
O2—Ge4—O6i | 99.58 (13) | O9vi—Cu1—O7iv | 102.27 (11) |
O8—Ge4—O6i | 114.31 (12) | O4v—Cu1—O7iv | 78.26 (10) |
O2—Ge4—O6 | 99.58 (13) | O9v—Cu1—O7iv | 176.34 (16) |
O8—Ge4—O6 | 114.31 (12) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.904 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.0943 (8) Å | Cell parameters from 4453 reflections |
b = 8.5142 (7) Å | θ = 2.9–28.0° |
c = 4.8763 (5) Å | µ = 18.94 mm−1 |
β = 96.21 (2)° | T = 445 K |
V = 499.19 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 962 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.045 |
rotation method, ϕ scans | θmax = 28.0°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4494 measured reflections | l = −5→5 |
1164 independent reflections |
Refinement on F2 | 6 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0372P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.028 | (Δ/σ)max < 0.001 |
wR(F2) = 0.062 | Δρmax = 0.92 e Å−3 |
S = 0.97 | Δρmin = −0.77 e Å−3 |
1164 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0257 (10) |
Cu2Fe2Ge4O13 | V = 499.19 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0943 (8) Å | µ = 18.94 mm−1 |
b = 8.5142 (7) Å | T = 445 K |
c = 4.8763 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.21 (2)° |
STOE IPDS-I diffractometer | 1164 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 962 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.045 |
4494 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 110 parameters |
wR(F2) = 0.062 | 6 restraints |
S = 0.97 | Δρmax = 0.92 e Å−3 |
1164 reflections | Δρmin = −0.77 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24005 (5) | 0.25 | 0.49269 (16) | 0.00776 (18) | |
Ge2 | 0.74729 (5) | 0.25 | 0.33662 (16) | 0.00788 (18) | |
Ge3 | −0.00512 (5) | 0.25 | 0.40452 (16) | 0.00941 (18) | |
Ge4 | 0.51243 (5) | 0.25 | 0.60659 (15) | 0.00709 (17) | |
Fe1 | 0.37578 (5) | 0.06149 (8) | 1.04840 (15) | 0.00783 (17) | |
Cu1 | 0.12545 (4) | −0.00338 (8) | 1.04345 (15) | 0.01485 (18) | |
O1 | 0.3318 (4) | 0.25 | 0.7953 (12) | 0.0118 (10) | |
O2 | 0.65277 (19) | 0.25 | 0.5682 (7) | 0.0185 (12) | |
O3 | 0.1129 (4) | 0.25 | 0.6445 (12) | 0.0124 (10) | |
O4 | 0.24817 (19) | 0.0842 (4) | 0.2837 (6) | 0.0118 (7) | |
O5 | 0.8722 (4) | 0.25 | 0.5657 (12) | 0.0127 (10) | |
O6 | 0.5038 (2) | 0.0753 (3) | 0.7916 (7) | 0.0112 (7) | |
O7 | 0.7425 (3) | 0.0806 (4) | 0.1340 (8) | 0.0131 (7) | |
O8 | 0.4360 (3) | 0.25 | 0.2822 (6) | 0.0102 (10) | |
O9 | −0.00284 (19) | 0.0831 (5) | 0.2014 (8) | 0.0212 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0044 (3) | 0.0072 (3) | 0.0114 (5) | 0 | −0.0006 (2) | 0 |
Ge2 | 0.0044 (3) | 0.0057 (3) | 0.0135 (4) | 0 | 0.0007 (2) | 0 |
Ge3 | 0.0038 (3) | 0.0119 (4) | 0.0125 (5) | 0 | 0.0006 (3) | 0 |
Ge4 | 0.0058 (3) | 0.0055 (3) | 0.0097 (4) | 0 | −0.0001 (2) | 0 |
Fe1 | 0.0051 (3) | 0.0057 (3) | 0.0126 (4) | 0.0002 (2) | 0.0009 (2) | 0.0000 (3) |
Cu1 | 0.0052 (3) | 0.0177 (3) | 0.0216 (4) | −0.0016 (2) | 0.00132 (19) | −0.0089 (3) |
O1 | 0.0075 (19) | 0.008 (2) | 0.019 (3) | 0 | −0.0012 (17) | 0 |
O2 | 0.009 (2) | 0.031 (3) | 0.016 (3) | 0 | 0.0063 (19) | 0 |
O3 | 0.0033 (18) | 0.018 (2) | 0.016 (3) | 0 | 0.0017 (17) | 0 |
O4 | 0.0073 (14) | 0.0133 (18) | 0.015 (2) | −0.0027 (12) | 0.0023 (12) | −0.0036 (14) |
O5 | 0.0032 (18) | 0.019 (3) | 0.016 (3) | 0 | 0.0018 (17) | 0 |
O6 | 0.0068 (13) | 0.0083 (16) | 0.019 (2) | 0.0030 (12) | 0.0025 (12) | 0.0049 (14) |
O7 | 0.0114 (15) | 0.0113 (17) | 0.016 (2) | −0.0030 (12) | −0.0002 (12) | −0.0052 (14) |
O8 | 0.011 (2) | 0.009 (2) | 0.010 (3) | 0 | −0.0014 (17) | 0 |
O9 | 0.0074 (15) | 0.026 (2) | 0.031 (3) | 0.0011 (14) | 0.0015 (14) | −0.0165 (19) |
Ge1—O1 | 1.748 (5) | Ge4—O8 | 1.744 (2) |
Ge1—O4 | 1.750 (3) | Ge4—O6i | 1.749 (3) |
Ge1—O4i | 1.750 (3) | Ge4—O6 | 1.749 (3) |
Ge1—O3 | 1.777 (5) | Fe1—O6iii | 1.960 (3) |
Ge2—O2 | 1.692 (4) | Fe1—O7iv | 2.007 (3) |
Ge2—O7 | 1.746 (4) | Fe1—O4v | 2.029 (3) |
Ge2—O7i | 1.746 (4) | Fe1—O8v | 2.056 (3) |
Ge2—O5 | 1.779 (5) | Fe1—O1 | 2.059 (3) |
Ge3—O9 | 1.734 (3) | Fe1—O6 | 2.097 (3) |
Ge3—O9i | 1.734 (3) | Cu1—O9vi | 1.924 (4) |
Ge3—O3 | 1.746 (5) | Cu1—O4v | 1.938 (4) |
Ge3—O5ii | 1.752 (5) | Cu1—O9v | 1.950 (4) |
Ge4—O2 | 1.728 (3) | Cu1—O7iv | 2.007 (4) |
O1—Ge1—O4 | 114.92 (12) | O6i—Ge4—O6 | 116.6 (2) |
O1—Ge1—O4i | 114.92 (12) | O6iii—Fe1—O7iv | 106.38 (14) |
O4—Ge1—O4i | 107.5 (2) | O6iii—Fe1—O4v | 114.18 (13) |
O1—Ge1—O3 | 98.4 (2) | O7iv—Fe1—O4v | 76.02 (12) |
O4—Ge1—O3 | 110.37 (13) | O6iii—Fe1—O8v | 92.27 (13) |
O4i—Ge1—O3 | 110.37 (13) | O7iv—Fe1—O8v | 155.40 (16) |
O2—Ge2—O7 | 113.25 (13) | O4v—Fe1—O8v | 81.81 (15) |
O2—Ge2—O7i | 113.25 (13) | O6iii—Fe1—O1 | 146.56 (14) |
O7—Ge2—O7i | 111.4 (3) | O7iv—Fe1—O1 | 94.51 (16) |
O2—Ge2—O5 | 99.8 (2) | O4v—Fe1—O1 | 95.83 (17) |
O7—Ge2—O5 | 109.21 (14) | O8v—Fe1—O1 | 77.12 (13) |
O7i—Ge2—O5 | 109.21 (14) | O6iii—Fe1—O6 | 72.90 (11) |
O9—Ge3—O9i | 110.1 (3) | O7iv—Fe1—O6 | 107.84 (15) |
O9—Ge3—O3 | 108.70 (15) | O4v—Fe1—O6 | 171.08 (12) |
O9i—Ge3—O3 | 108.70 (15) | O8v—Fe1—O6 | 92.72 (16) |
O9—Ge3—O5ii | 108.83 (12) | O1—Fe1—O6 | 76.01 (15) |
O9i—Ge3—O5ii | 108.83 (12) | O9vi—Cu1—O4v | 177.95 (18) |
O3—Ge3—O5ii | 111.7 (2) | O9vi—Cu1—O9v | 77.62 (14) |
O2—Ge4—O8 | 109.4 (2) | O4v—Cu1—O9v | 101.89 (14) |
O2—Ge4—O6i | 99.80 (12) | O9vi—Cu1—O7iv | 102.27 (12) |
O8—Ge4—O6i | 114.37 (13) | O4v—Cu1—O7iv | 78.09 (14) |
O2—Ge4—O6 | 99.80 (12) | O9v—Cu1—O7iv | 176.46 (19) |
O8—Ge4—O6 | 114.37 (13) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.896 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.0971 (8) Å | Cell parameters from 4318 reflections |
b = 8.5205 (7) Å | θ = 2.9–27.9° |
c = 4.8803 (5) Å | µ = 18.91 mm−1 |
β = 96.22 (2)° | T = 528 K |
V = 500.07 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 949 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.038 |
rotation method, ϕ scans | θmax = 27.9°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4513 measured reflections | l = −5→5 |
1167 independent reflections |
Refinement on F2 | 1 restraint |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0309P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.026 | (Δ/σ)max = 0.001 |
wR(F2) = 0.054 | Δρmax = 1.00 e Å−3 |
S = 0.98 | Δρmin = −0.70 e Å−3 |
1167 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0212 (8) |
Cu2Fe2Ge4O13 | V = 500.07 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.0971 (8) Å | µ = 18.91 mm−1 |
b = 8.5205 (7) Å | T = 528 K |
c = 4.8803 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.22 (2)° |
STOE IPDS-I diffractometer | 1167 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 949 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.038 |
4513 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 110 parameters |
wR(F2) = 0.054 | 1 restraint |
S = 0.98 | Δρmax = 1.00 e Å−3 |
1167 reflections | Δρmin = −0.70 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24013 (5) | 0.25 | 0.49253 (15) | 0.00790 (17) | |
Ge2 | 0.74727 (5) | 0.25 | 0.33601 (15) | 0.00811 (17) | |
Ge3 | −0.00513 (5) | 0.25 | 0.40419 (15) | 0.00966 (17) | |
Ge4 | 0.51257 (5) | 0.25 | 0.60660 (15) | 0.00699 (16) | |
Fe1 | 0.37571 (5) | 0.06146 (7) | 1.04840 (15) | 0.00805 (16) | |
Cu1 | 0.12532 (4) | −0.00333 (8) | 1.04367 (14) | 0.01626 (17) | |
O1 | 0.3322 (3) | 0.25 | 0.7947 (11) | 0.0106 (9) | |
O2 | 0.6524 (4) | 0.25 | 0.5669 (12) | 0.0213 (12) | |
O3 | 0.1131 (4) | 0.25 | 0.6433 (12) | 0.0141 (10) | |
O4 | 0.2480 (2) | 0.0836 (4) | 0.2843 (8) | 0.0133 (7) | |
O5 | 0.8719 (3) | 0.25 | 0.5646 (12) | 0.0132 (10) | |
O6 | 0.5042 (2) | 0.0755 (4) | 0.7922 (8) | 0.0121 (7) | |
O7 | 0.7427 (3) | 0.0813 (4) | 0.1327 (8) | 0.0133 (7) | |
O8 | 0.4361 (4) | 0.25 | 0.2831 (11) | 0.0114 (9) | |
O9 | −0.0030 (3) | 0.0833 (3) | 0.2002 (8) | 0.0239 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0050 (3) | 0.0079 (3) | 0.0104 (4) | 0 | −0.0009 (2) | 0 |
Ge2 | 0.0051 (3) | 0.0072 (3) | 0.0120 (4) | 0 | 0.0008 (2) | 0 |
Ge3 | 0.0045 (3) | 0.0127 (3) | 0.0117 (4) | 0 | 0.0007 (2) | 0 |
Ge4 | 0.0064 (3) | 0.0061 (3) | 0.0083 (4) | 0 | −0.0001 (2) | 0 |
Fe1 | 0.0060 (3) | 0.0064 (3) | 0.0118 (4) | 0.0007 (2) | 0.0010 (2) | −0.0001 (3) |
Cu1 | 0.0058 (2) | 0.0202 (3) | 0.0228 (4) | −0.0019 (2) | 0.00150 (19) | −0.0102 (3) |
O1 | 0.0078 (18) | 0.006 (2) | 0.017 (3) | 0 | −0.0027 (16) | 0 |
O2 | 0.012 (2) | 0.034 (3) | 0.019 (4) | 0 | 0.0057 (19) | 0 |
O3 | 0.0057 (18) | 0.022 (2) | 0.014 (3) | 0 | 0.0021 (16) | 0 |
O4 | 0.0063 (13) | 0.0151 (17) | 0.018 (2) | −0.0038 (11) | 0.0018 (11) | −0.0057 (14) |
O5 | 0.0030 (17) | 0.020 (2) | 0.017 (3) | 0 | 0.0038 (16) | 0 |
O6 | 0.0086 (13) | 0.0098 (15) | 0.018 (2) | 0.0037 (11) | 0.0030 (12) | 0.0068 (14) |
O7 | 0.0112 (14) | 0.0085 (15) | 0.020 (2) | −0.0010 (11) | 0.0010 (12) | −0.0070 (14) |
O8 | 0.012 (2) | 0.009 (2) | 0.012 (3) | 0 | −0.0021 (17) | 0 |
O9 | 0.0118 (15) | 0.031 (2) | 0.028 (3) | 0.0007 (14) | 0.0003 (14) | −0.0176 (19) |
Ge1—O1 | 1.749 (5) | Ge4—O8 | 1.741 (5) |
Ge1—O4 | 1.753 (3) | Ge4—O6i | 1.749 (3) |
Ge1—O4i | 1.753 (3) | Ge4—O6 | 1.749 (3) |
Ge1—O3 | 1.775 (5) | Fe1—O6iii | 1.958 (3) |
Ge2—O2 | 1.693 (5) | Fe1—O7iv | 2.009 (3) |
Ge2—O7 | 1.744 (3) | Fe1—O4v | 2.033 (3) |
Ge2—O7i | 1.744 (3) | Fe1—O8v | 2.061 (3) |
Ge2—O5 | 1.776 (5) | Fe1—O1 | 2.061 (3) |
Ge3—O9 | 1.736 (3) | Fe1—O6 | 2.101 (3) |
Ge3—O9i | 1.736 (3) | Cu1—O9vi | 1.921 (3) |
Ge3—O3 | 1.745 (5) | Cu1—O4v | 1.937 (3) |
Ge3—O5ii | 1.754 (5) | Cu1—O9v | 1.949 (3) |
Ge4—O2 | 1.723 (5) | Cu1—O7iv | 2.008 (3) |
O1—Ge1—O4 | 114.77 (13) | O6i—Ge4—O6 | 116.4 (2) |
O1—Ge1—O4i | 114.77 (13) | O6iii—Fe1—O7iv | 106.06 (14) |
O4—Ge1—O4i | 108.0 (3) | O6iii—Fe1—O4v | 114.02 (15) |
O1—Ge1—O3 | 98.7 (2) | O7iv—Fe1—O4v | 75.90 (14) |
O4—Ge1—O3 | 110.14 (13) | O6iii—Fe1—O8v | 92.33 (14) |
O4i—Ge1—O3 | 110.14 (13) | O7iv—Fe1—O8v | 155.44 (16) |
O2—Ge2—O7 | 113.35 (14) | O4v—Fe1—O8v | 81.85 (16) |
O2—Ge2—O7i | 113.35 (14) | O6iii—Fe1—O1 | 146.44 (15) |
O7—Ge2—O7i | 111.0 (3) | O7iv—Fe1—O1 | 94.84 (14) |
O2—Ge2—O5 | 99.9 (3) | O4v—Fe1—O1 | 96.18 (17) |
O7—Ge2—O5 | 109.27 (13) | O8v—Fe1—O1 | 77.19 (15) |
O7i—Ge2—O5 | 109.27 (13) | O6iii—Fe1—O6 | 72.88 (16) |
O9—Ge3—O9i | 109.8 (3) | O7iv—Fe1—O6 | 108.10 (14) |
O9—Ge3—O3 | 108.76 (15) | O4v—Fe1—O6 | 171.19 (13) |
O9i—Ge3—O3 | 108.76 (15) | O8v—Fe1—O6 | 92.62 (17) |
O9—Ge3—O5ii | 108.77 (15) | O1—Fe1—O6 | 75.82 (15) |
O9i—Ge3—O5ii | 108.77 (15) | O9vi—Cu1—O4v | 178.23 (17) |
O3—Ge3—O5ii | 112.0 (2) | O9vi—Cu1—O9v | 77.55 (9) |
O2—Ge4—O8 | 109.2 (3) | O4v—Cu1—O9v | 102.00 (12) |
O2—Ge4—O6i | 99.84 (14) | O9vi—Cu1—O7iv | 102.23 (13) |
O8—Ge4—O6i | 114.49 (13) | O4v—Cu1—O7iv | 78.11 (14) |
O2—Ge4—O6 | 99.84 (14) | O9v—Cu1—O7iv | 176.55 (18) |
O8—Ge4—O6 | 114.49 (13) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.885 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.1011 (8) Å | Cell parameters from 4497 reflections |
b = 8.5290 (7) Å | θ = 2.9–28.1° |
c = 4.8841 (5) Å | µ = 18.87 mm−1 |
β = 96.24 (2)° | T = 611 K |
V = 501.10 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 914 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.046 |
rotation method, ϕ scans | θmax = 27.9°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4515 measured reflections | l = −5→5 |
1165 independent reflections |
Refinement on F2 | 3 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0335P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.028 | (Δ/σ)max = 0.001 |
wR(F2) = 0.062 | Δρmax = 0.83 e Å−3 |
S = 0.99 | Δρmin = −0.90 e Å−3 |
1165 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0211 (9) |
Cu2Fe2Ge4O13 | V = 501.10 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.1011 (8) Å | µ = 18.87 mm−1 |
b = 8.5290 (7) Å | T = 611 K |
c = 4.8841 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.24 (2)° |
STOE IPDS-I diffractometer | 1165 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 914 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.046 |
4515 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 110 parameters |
wR(F2) = 0.062 | 3 restraints |
S = 0.99 | Δρmax = 0.83 e Å−3 |
1165 reflections | Δρmin = −0.90 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24021 (5) | 0.25 | 0.49216 (17) | 0.00973 (19) | |
Ge2 | 0.74727 (5) | 0.25 | 0.33568 (18) | 0.01009 (19) | |
Ge3 | −0.00516 (5) | 0.25 | 0.40374 (17) | 0.0119 (2) | |
Ge4 | 0.51268 (6) | 0.25 | 0.60690 (17) | 0.00892 (18) | |
Fe1 | 0.37569 (5) | 0.06147 (8) | 1.04850 (17) | 0.01032 (18) | |
Cu1 | 0.12516 (5) | −0.00330 (9) | 1.04360 (16) | 0.0195 (2) | |
O1 | 0.3319 (4) | 0.25 | 0.7946 (12) | 0.0136 (11) | |
O2 | 0.6524 (4) | 0.25 | 0.5652 (10) | 0.0236 (14) | |
O3 | 0.1135 (4) | 0.25 | 0.6420 (13) | 0.0145 (11) | |
O4 | 0.2478 (2) | 0.0839 (4) | 0.2845 (7) | 0.0150 (8) | |
O5 | 0.8720 (3) | 0.25 | 0.5646 (11) | 0.0161 (12) | |
O6 | 0.5046 (3) | 0.0755 (4) | 0.7924 (9) | 0.0138 (8) | |
O7 | 0.7428 (3) | 0.0808 (4) | 0.1329 (9) | 0.0161 (8) | |
O8 | 0.4357 (4) | 0.25 | 0.2834 (12) | 0.0130 (11) | |
O9 | −0.0030 (3) | 0.0836 (6) | 0.1995 (11) | 0.0288 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0068 (3) | 0.0104 (4) | 0.0115 (5) | 0 | −0.0010 (3) | 0 |
Ge2 | 0.0060 (3) | 0.0093 (4) | 0.0149 (5) | 0 | 0.0010 (3) | 0 |
Ge3 | 0.0056 (3) | 0.0161 (4) | 0.0140 (5) | 0 | 0.0005 (3) | 0 |
Ge4 | 0.0080 (3) | 0.0081 (3) | 0.0104 (5) | 0 | −0.0005 (3) | 0 |
Fe1 | 0.0070 (3) | 0.0094 (3) | 0.0146 (5) | 0.0003 (2) | 0.0011 (2) | −0.0005 (3) |
Cu1 | 0.0069 (3) | 0.0253 (4) | 0.0264 (5) | −0.0025 (2) | 0.0016 (2) | −0.0118 (3) |
O1 | 0.012 (2) | 0.009 (2) | 0.018 (3) | 0 | −0.0024 (19) | 0 |
O2 | 0.008 (2) | 0.041 (4) | 0.022 (4) | 0 | 0.007 (2) | 0 |
O3 | 0.006 (2) | 0.027 (3) | 0.010 (3) | 0 | 0.0009 (18) | 0 |
O4 | 0.0078 (15) | 0.017 (2) | 0.021 (3) | −0.0044 (13) | 0.0027 (13) | −0.0068 (16) |
O5 | 0.008 (2) | 0.025 (3) | 0.016 (4) | 0 | 0.0021 (19) | 0 |
O6 | 0.0110 (15) | 0.0128 (18) | 0.018 (2) | 0.0067 (13) | 0.0019 (13) | 0.0079 (16) |
O7 | 0.0109 (16) | 0.0124 (18) | 0.025 (3) | −0.0011 (13) | 0.0023 (14) | −0.0090 (16) |
O8 | 0.013 (2) | 0.012 (2) | 0.013 (3) | 0 | −0.0016 (19) | 0 |
O9 | 0.0098 (17) | 0.039 (3) | 0.037 (3) | −0.0006 (16) | −0.0004 (16) | −0.023 (2) |
Ge1—O1 | 1.749 (5) | Ge4—O8 | 1.745 (6) |
Ge1—O4 | 1.751 (3) | Ge4—O6i | 1.751 (4) |
Ge1—O4i | 1.751 (3) | Ge4—O6 | 1.751 (4) |
Ge1—O3 | 1.770 (5) | Fe1—O6iii | 1.955 (3) |
Ge2—O2 | 1.690 (5) | Fe1—O7iv | 2.009 (4) |
Ge2—O7 | 1.748 (4) | Fe1—O4v | 2.037 (4) |
Ge2—O7i | 1.748 (4) | Fe1—O8v | 2.061 (4) |
Ge2—O5 | 1.778 (5) | Fe1—O1 | 2.064 (4) |
Ge3—O9 | 1.737 (4) | Fe1—O6 | 2.106 (4) |
Ge3—O9i | 1.737 (4) | Cu1—O9vi | 1.919 (4) |
Ge3—O3 | 1.747 (5) | Cu1—O4v | 1.939 (4) |
Ge3—O5ii | 1.755 (4) | Cu1—O9v | 1.947 (4) |
Ge4—O2 | 1.725 (4) | Cu1—O7iv | 2.009 (4) |
O1—Ge1—O4 | 114.90 (13) | O6i—Ge4—O6 | 116.5 (3) |
O1—Ge1—O4i | 114.90 (13) | O6iii—Fe1—O7iv | 106.08 (16) |
O4—Ge1—O4i | 108.1 (3) | O6iii—Fe1—O4v | 114.02 (16) |
O1—Ge1—O3 | 98.6 (3) | O7iv—Fe1—O4v | 75.90 (13) |
O4—Ge1—O3 | 109.99 (14) | O6iii—Fe1—O8v | 92.51 (16) |
O4i—Ge1—O3 | 109.99 (14) | O7iv—Fe1—O8v | 155.23 (18) |
O2—Ge2—O7 | 113.24 (16) | O4v—Fe1—O8v | 81.68 (16) |
O2—Ge2—O7i | 113.24 (15) | O6iii—Fe1—O1 | 146.59 (18) |
O7—Ge2—O7i | 111.3 (3) | O7iv—Fe1—O1 | 94.68 (17) |
O2—Ge2—O5 | 100.0 (2) | O4v—Fe1—O1 | 96.07 (19) |
O7—Ge2—O5 | 109.17 (13) | O8v—Fe1—O1 | 77.20 (17) |
O7i—Ge2—O5 | 109.17 (13) | O6iii—Fe1—O6 | 72.86 (18) |
O9—Ge3—O9i | 109.6 (4) | O7iv—Fe1—O6 | 108.13 (16) |
O9—Ge3—O3 | 108.67 (17) | O4v—Fe1—O6 | 171.18 (14) |
O9i—Ge3—O3 | 108.67 (17) | O8v—Fe1—O6 | 92.73 (19) |
O9—Ge3—O5ii | 108.88 (17) | O1—Fe1—O6 | 75.95 (18) |
O9i—Ge3—O5ii | 108.88 (17) | O9vi—Cu1—O4v | 178.3 (2) |
O3—Ge3—O5ii | 112.1 (3) | O9vi—Cu1—O9v | 77.6 (2) |
O2—Ge4—O8 | 109.1 (2) | O4v—Cu1—O9v | 101.90 (16) |
O2—Ge4—O6i | 99.90 (14) | O9vi—Cu1—O7iv | 102.27 (17) |
O8—Ge4—O6i | 114.46 (14) | O4v—Cu1—O7iv | 78.14 (15) |
O2—Ge4—O6 | 99.90 (14) | O9v—Cu1—O7iv | 176.3 (2) |
O8—Ge4—O6 | 114.46 (14) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.877 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.1039 (8) Å | Cell parameters from 4536 reflections |
b = 8.5353 (7) Å | θ = 2.9–28.1° |
c = 4.8886 (5) Å | µ = 18.84 mm−1 |
β = 96.28 (2)° | T = 695 K |
V = 502.01 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 891 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.047 |
rotation method, ϕ scans | θmax = 28.1°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4549 measured reflections | l = −5→5 |
1169 independent reflections |
Refinement on F2 | 5 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0295P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.029 | (Δ/σ)max < 0.001 |
wR(F2) = 0.061 | Δρmax = 0.85 e Å−3 |
S = 1.01 | Δρmin = −0.81 e Å−3 |
1169 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0232 (8) |
Cu2Fe2Ge4O13 | V = 502.01 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.1039 (8) Å | µ = 18.84 mm−1 |
b = 8.5353 (7) Å | T = 695 K |
c = 4.8886 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.28 (2)° |
STOE IPDS-I diffractometer | 1169 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 891 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.047 |
4549 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 110 parameters |
wR(F2) = 0.061 | 5 restraints |
S = 1.01 | Δρmax = 0.85 e Å−3 |
1169 reflections | Δρmin = −0.81 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24022 (6) | 0.25 | 0.49198 (18) | 0.0107 (2) | |
Ge2 | 0.74723 (6) | 0.25 | 0.33510 (19) | 0.0107 (2) | |
Ge3 | −0.00515 (6) | 0.25 | 0.40311 (18) | 0.0131 (2) | |
Ge4 | 0.51278 (6) | 0.25 | 0.60688 (18) | 0.0097 (2) | |
Fe1 | 0.37556 (6) | 0.06141 (8) | 1.04865 (18) | 0.01115 (19) | |
Cu1 | 0.12522 (5) | −0.00337 (10) | 1.04390 (18) | 0.0216 (2) | |
O1 | 0.3317 (4) | 0.25 | 0.7948 (13) | 0.0140 (12) | |
O2 | 0.6523 (4) | 0.25 | 0.5638 (15) | 0.0263 (15) | |
O3 | 0.1130 (3) | 0.25 | 0.6419 (10) | 0.0177 (12) | |
O4 | 0.2475 (3) | 0.0839 (5) | 0.2849 (10) | 0.0177 (9) | |
O5 | 0.8720 (3) | 0.25 | 0.5637 (11) | 0.0171 (12) | |
O6 | 0.5049 (3) | 0.0760 (4) | 0.7928 (9) | 0.0146 (8) | |
O7 | 0.74281 (11) | 0.0806 (4) | 0.1335 (7) | 0.0179 (9) | |
O8 | 0.4359 (4) | 0.25 | 0.2841 (13) | 0.0132 (11) | |
O9 | −0.0031 (2) | 0.0838 (6) | 0.1983 (9) | 0.0305 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0073 (3) | 0.0118 (4) | 0.0125 (5) | 0 | −0.0011 (3) | 0 |
Ge2 | 0.0066 (3) | 0.0099 (4) | 0.0154 (5) | 0 | 0.0009 (3) | 0 |
Ge3 | 0.0063 (3) | 0.0183 (4) | 0.0146 (5) | 0 | 0.0005 (3) | 0 |
Ge4 | 0.0096 (3) | 0.0087 (4) | 0.0104 (5) | 0 | −0.0009 (3) | 0 |
Fe1 | 0.0076 (3) | 0.0098 (3) | 0.0159 (5) | 0.0007 (3) | 0.0007 (3) | −0.0003 (3) |
Cu1 | 0.0082 (3) | 0.0282 (4) | 0.0282 (5) | −0.0022 (3) | 0.0013 (2) | −0.0131 (3) |
O1 | 0.010 (2) | 0.010 (2) | 0.021 (4) | 0 | −0.003 (2) | 0 |
O2 | 0.010 (3) | 0.044 (4) | 0.025 (4) | 0 | 0.008 (2) | 0 |
O3 | 0.008 (2) | 0.029 (3) | 0.016 (4) | 0 | 0.002 (2) | 0 |
O4 | 0.0098 (16) | 0.018 (2) | 0.025 (3) | −0.0053 (14) | 0.0039 (14) | −0.0102 (18) |
O5 | 0.008 (2) | 0.028 (3) | 0.015 (4) | 0 | 0.002 (2) | 0 |
O6 | 0.0103 (16) | 0.0151 (19) | 0.019 (3) | 0.0076 (14) | 0.0028 (14) | 0.0089 (17) |
O7 | 0.0132 (17) | 0.016 (2) | 0.024 (3) | −0.0015 (15) | 0.0000 (14) | −0.0069 (18) |
O8 | 0.017 (2) | 0.010 (2) | 0.013 (3) | 0 | 0.000 (2) | 0 |
O9 | 0.0118 (18) | 0.041 (3) | 0.038 (3) | 0.0032 (18) | −0.0004 (17) | −0.024 (2) |
Ge1—O1 | 1.749 (6) | Ge4—O8 | 1.742 (6) |
Ge1—O4 | 1.750 (4) | Ge4—O6i | 1.750 (4) |
Ge1—O4i | 1.750 (4) | Ge4—O6 | 1.750 (4) |
Ge1—O3 | 1.776 (6) | Fe1—O6iii | 1.955 (3) |
Ge2—O2 | 1.689 (6) | Fe1—O7iv | 2.009 (3) |
Ge2—O7 | 1.748 (6) | Fe1—O4v | 2.041 (4) |
Ge2—O7i | 1.748 (6) | Fe1—O8v | 2.065 (4) |
Ge2—O5 | 1.778 (6) | Fe1—O1 | 2.066 (4) |
Ge3—O9 | 1.738 (4) | Fe1—O6 | 2.111 (4) |
Ge3—O9i | 1.738 (4) | Cu1—O9vi | 1.917 (4) |
Ge3—O3 | 1.744 (2) | Cu1—O4v | 1.937 (4) |
Ge3—O5ii | 1.755 (2) | Cu1—O9v | 1.947 (4) |
Ge4—O2 | 1.724 (5) | Cu1—O7iv | 2.010 (4) |
O1—Ge1—O4 | 115.00 (16) | O6i—Ge4—O6 | 116.2 (3) |
O1—Ge1—O4i | 115.00 (16) | O6iii—Fe1—O7iv | 105.97 (16) |
O4—Ge1—O4i | 108.2 (3) | O6iii—Fe1—O4v | 114.02 (18) |
O1—Ge1—O3 | 98.5 (2) | O7iv—Fe1—O4v | 76.03 (12) |
O4—Ge1—O3 | 109.85 (13) | O6iii—Fe1—O8v | 92.59 (17) |
O4i—Ge1—O3 | 109.85 (13) | O7iv—Fe1—O8v | 155.34 (15) |
O2—Ge2—O7 | 113.10 (13) | O4v—Fe1—O8v | 81.68 (19) |
O2—Ge2—O7i | 113.10 (13) | O6iii—Fe1—O1 | 146.69 (19) |
O7—Ge2—O7i | 111.7 (3) | O7iv—Fe1—O1 | 94.57 (17) |
O2—Ge2—O5 | 100.2 (3) | O4v—Fe1—O1 | 96.0 (2) |
O7—Ge2—O5 | 109.02 (11) | O8v—Fe1—O1 | 77.27 (18) |
O7i—Ge2—O5 | 109.02 (11) | O6iii—Fe1—O6 | 72.88 (18) |
O9—Ge3—O9i | 109.4 (4) | O7iv—Fe1—O6 | 108.18 (13) |
O9—Ge3—O3 | 108.86 (15) | O4v—Fe1—O6 | 171.05 (15) |
O9i—Ge3—O3 | 108.86 (15) | O8v—Fe1—O6 | 92.5 (2) |
O9—Ge3—O5ii | 108.89 (17) | O1—Fe1—O6 | 75.94 (18) |
O9i—Ge3—O5ii | 108.89 (17) | O9vi—Cu1—O4v | 178.4 (2) |
O3—Ge3—O5ii | 111.9 (3) | O9vi—Cu1—O9v | 77.44 (16) |
O2—Ge4—O8 | 108.8 (3) | O4v—Cu1—O9v | 101.89 (13) |
O2—Ge4—O6i | 99.98 (17) | O9vi—Cu1—O7iv | 102.21 (14) |
O8—Ge4—O6i | 114.61 (15) | O4v—Cu1—O7iv | 78.35 (13) |
O2—Ge4—O6 | 99.98 (17) | O9v—Cu1—O7iv | 176.0 (2) |
O8—Ge4—O6 | 114.61 (15) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.872 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.1073 (8) Å | Cell parameters from 4541 reflections |
b = 8.5380 (7) Å | θ = 2.9–28.1° |
c = 4.8899 (5) Å | µ = 18.82 mm−1 |
β = 96.28 (2)° | T = 736 K |
V = 502.45 (8) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 877 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.047 |
rotation method, ϕ scans | θmax = 28.1°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4541 measured reflections | l = −5→5 |
1171 independent reflections |
Refinement on F2 | 3 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0246P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max = 0.001 |
wR(F2) = 0.054 | Δρmax = 0.73 e Å−3 |
S = 0.97 | Δρmin = −0.67 e Å−3 |
1171 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0323 (9) |
Cu2Fe2Ge4O13 | V = 502.45 (8) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.1073 (8) Å | µ = 18.82 mm−1 |
b = 8.5380 (7) Å | T = 736 K |
c = 4.8899 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.28 (2)° |
STOE IPDS-I diffractometer | 1171 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 877 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.047 |
4541 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 110 parameters |
wR(F2) = 0.054 | 3 restraints |
S = 0.97 | Δρmax = 0.73 e Å−3 |
1171 reflections | Δρmin = −0.67 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24026 (6) | 0.25 | 0.49185 (18) | 0.0125 (2) | |
Ge2 | 0.74725 (6) | 0.25 | 0.33482 (18) | 0.0127 (2) | |
Ge3 | −0.00509 (5) | 0.25 | 0.40275 (18) | 0.0150 (2) | |
Ge4 | 0.51282 (6) | 0.25 | 0.60671 (18) | 0.01136 (19) | |
Fe1 | 0.37561 (6) | 0.06141 (8) | 1.04885 (19) | 0.01295 (18) | |
Cu1 | 0.12524 (5) | −0.00328 (10) | 1.04395 (18) | 0.0241 (2) | |
O1 | 0.3322 (4) | 0.25 | 0.7949 (12) | 0.0164 (11) | |
O2 | 0.6519 (4) | 0.25 | 0.5624 (15) | 0.0303 (15) | |
O3 | 0.1133 (3) | 0.25 | 0.6407 (9) | 0.0188 (12) | |
O4 | 0.2476 (3) | 0.0840 (5) | 0.2848 (9) | 0.0185 (9) | |
O5 | 0.8721 (3) | 0.25 | 0.5633 (11) | 0.0195 (12) | |
O6 | 0.5048 (3) | 0.0762 (4) | 0.7927 (9) | 0.0171 (8) | |
O7 | 0.7426 (3) | 0.0810 (4) | 0.1318 (10) | 0.0205 (9) | |
O8 | 0.4360 (4) | 0.25 | 0.2846 (13) | 0.0164 (11) | |
O9 | −0.0034 (3) | 0.0842 (4) | 0.1974 (10) | 0.0342 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0087 (3) | 0.0127 (4) | 0.0156 (5) | 0 | −0.0014 (3) | 0 |
Ge2 | 0.0077 (3) | 0.0114 (4) | 0.0188 (5) | 0 | 0.0006 (3) | 0 |
Ge3 | 0.0065 (3) | 0.0191 (4) | 0.0192 (5) | 0 | 0.0002 (3) | 0 |
Ge4 | 0.0096 (3) | 0.0093 (3) | 0.0148 (5) | 0 | −0.0008 (3) | 0 |
Fe1 | 0.0084 (3) | 0.0108 (3) | 0.0195 (5) | 0.0005 (3) | 0.0005 (2) | −0.0003 (3) |
Cu1 | 0.0088 (3) | 0.0295 (4) | 0.0337 (5) | −0.0025 (2) | 0.0012 (2) | −0.0144 (3) |
O1 | 0.016 (2) | 0.015 (3) | 0.018 (3) | 0 | −0.002 (2) | 0 |
O2 | 0.012 (3) | 0.048 (4) | 0.032 (4) | 0 | 0.008 (2) | 0 |
O3 | 0.009 (2) | 0.033 (3) | 0.013 (3) | 0 | −0.0012 (18) | 0 |
O4 | 0.0075 (15) | 0.019 (2) | 0.029 (3) | −0.0044 (13) | 0.0020 (13) | −0.0094 (17) |
O5 | 0.009 (2) | 0.032 (3) | 0.017 (3) | 0 | 0.0010 (19) | 0 |
O6 | 0.0123 (16) | 0.0141 (18) | 0.025 (3) | 0.0056 (14) | 0.0046 (14) | 0.0062 (16) |
O7 | 0.0149 (17) | 0.0140 (19) | 0.032 (3) | −0.0019 (14) | 0.0014 (14) | −0.0104 (18) |
O8 | 0.018 (2) | 0.012 (2) | 0.019 (3) | 0 | −0.004 (2) | 0 |
O9 | 0.0108 (17) | 0.046 (3) | 0.044 (4) | 0.0017 (17) | −0.0020 (16) | −0.028 (3) |
Ge1—O4 | 1.750 (4) | Ge4—O8 | 1.740 (6) |
Ge1—O4i | 1.750 (4) | Ge4—O6i | 1.749 (4) |
Ge1—O1 | 1.753 (6) | Ge4—O6 | 1.749 (4) |
Ge1—O3 | 1.771 (5) | Fe1—O6iii | 1.958 (3) |
Ge2—O2 | 1.689 (6) | Fe1—O7iv | 2.008 (4) |
Ge2—O7 | 1.748 (4) | Fe1—O4v | 2.040 (4) |
Ge2—O7i | 1.748 (4) | Fe1—O1 | 2.066 (4) |
Ge2—O5 | 1.778 (5) | Fe1—O8v | 2.067 (4) |
Ge3—O9 | 1.737 (4) | Fe1—O6 | 2.112 (4) |
Ge3—O9i | 1.737 (4) | Cu1—O9vi | 1.915 (3) |
Ge3—O3 | 1.745 (4) | Cu1—O4v | 1.938 (4) |
Ge3—O5ii | 1.756 (4) | Cu1—O9v | 1.950 (3) |
Ge4—O2 | 1.721 (5) | Cu1—O7iv | 2.010 (4) |
O4—Ge1—O4i | 108.2 (3) | O6i—Ge4—O6 | 116.1 (3) |
O4—Ge1—O1 | 114.91 (15) | O6iii—Fe1—O7iv | 105.75 (15) |
O4i—Ge1—O1 | 114.91 (15) | O6iii—Fe1—O4v | 114.05 (17) |
O4—Ge1—O3 | 109.84 (13) | O7iv—Fe1—O4v | 75.93 (16) |
O4i—Ge1—O3 | 109.84 (13) | O6iii—Fe1—O1 | 146.55 (18) |
O1—Ge1—O3 | 98.7 (2) | O7iv—Fe1—O1 | 94.89 (17) |
O2—Ge2—O7 | 113.10 (17) | O4v—Fe1—O1 | 96.16 (19) |
O2—Ge2—O7i | 113.10 (17) | O6iii—Fe1—O8v | 92.63 (16) |
O7—Ge2—O7i | 111.2 (3) | O7iv—Fe1—O8v | 155.34 (19) |
O2—Ge2—O5 | 100.4 (2) | O4v—Fe1—O8v | 81.66 (19) |
O7—Ge2—O5 | 109.20 (14) | O1—Fe1—O8v | 77.24 (17) |
O7i—Ge2—O5 | 109.20 (14) | O6iii—Fe1—O6 | 72.96 (18) |
O9—Ge3—O9i | 109.2 (4) | O7iv—Fe1—O6 | 108.29 (17) |
O9—Ge3—O3 | 108.95 (17) | O4v—Fe1—O6 | 170.97 (14) |
O9i—Ge3—O3 | 108.95 (17) | O1—Fe1—O6 | 75.71 (18) |
O9—Ge3—O5ii | 108.83 (17) | O8v—Fe1—O6 | 92.6 (2) |
O9i—Ge3—O5ii | 108.83 (17) | O9vi—Cu1—O4v | 178.5 (2) |
O3—Ge3—O5ii | 112.1 (3) | O9vi—Cu1—O9v | 77.39 (10) |
O2—Ge4—O8 | 108.7 (3) | O4v—Cu1—O9v | 102.04 (14) |
O2—Ge4—O6i | 100.15 (17) | O9vi—Cu1—O7iv | 102.28 (15) |
O8—Ge4—O6i | 114.60 (15) | O4v—Cu1—O7iv | 78.20 (16) |
O2—Ge4—O6 | 100.15 (17) | O9v—Cu1—O7iv | 176.1 (2) |
O8—Ge4—O6 | 114.60 (15) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684 |
Mr = 737.14 | Dx = 4.868 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.1083 (8) Å | Cell parameters from 4473 reflections |
b = 8.5422 (7) Å | θ = 2.9–28.1° |
c = 4.8916 (5) Å | µ = 18.80 mm−1 |
β = 96.295 (11)° | T = 778 K |
V = 502.90 (7) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 856 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.055 |
rotation method, ϕ scans | θmax = 28.1°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4541 measured reflections | l = −5→5 |
1170 independent reflections |
Refinement on F2 | 2 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0259P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.032 | (Δ/σ)max < 0.001 |
wR(F2) = 0.060 | Δρmax = 0.64 e Å−3 |
S = 0.98 | Δρmin = −0.78 e Å−3 |
1170 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0324 (10) |
Cu2Fe2Ge4O13 | V = 502.90 (7) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.1083 (8) Å | µ = 18.80 mm−1 |
b = 8.5422 (7) Å | T = 778 K |
c = 4.8916 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.295 (11)° |
STOE IPDS-I diffractometer | 1170 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 856 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.055 |
4541 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 110 parameters |
wR(F2) = 0.060 | 2 restraints |
S = 0.98 | Δρmax = 0.64 e Å−3 |
1170 reflections | Δρmin = −0.78 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24028 (6) | 0.25 | 0.4917 (2) | 0.0119 (2) | |
Ge2 | 0.74720 (6) | 0.25 | 0.3345 (2) | 0.0120 (2) | |
Ge3 | −0.00518 (6) | 0.25 | 0.4026 (2) | 0.0146 (2) | |
Ge4 | 0.51302 (7) | 0.25 | 0.6071 (2) | 0.0108 (2) | |
Fe1 | 0.37551 (7) | 0.06148 (9) | 1.0490 (2) | 0.0124 (2) | |
Cu1 | 0.12510 (6) | −0.00317 (11) | 1.0438 (2) | 0.0241 (2) | |
O1 | 0.3321 (4) | 0.25 | 0.7948 (14) | 0.0148 (13) | |
O2 | 0.6519 (5) | 0.25 | 0.5628 (18) | 0.0313 (18) | |
O3 | 0.1133 (5) | 0.25 | 0.6404 (15) | 0.0175 (13) | |
O4 | 0.2475 (3) | 0.0839 (5) | 0.2855 (11) | 0.0189 (10) | |
O5 | 0.8720 (3) | 0.25 | 0.5624 (13) | 0.0190 (14) | |
O6 | 0.5051 (3) | 0.0763 (5) | 0.7933 (10) | 0.0171 (10) | |
O7 | 0.7429 (3) | 0.0806 (5) | 0.1334 (11) | 0.0197 (10) | |
O8 | 0.4358 (5) | 0.25 | 0.2848 (14) | 0.0163 (13) | |
O9 | −0.0032 (2) | 0.0837 (6) | 0.1975 (12) | 0.0344 (15) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0087 (4) | 0.0133 (5) | 0.0130 (6) | 0 | −0.0020 (3) | 0 |
Ge2 | 0.0078 (4) | 0.0117 (4) | 0.0163 (6) | 0 | 0.0001 (3) | 0 |
Ge3 | 0.0069 (4) | 0.0203 (5) | 0.0164 (6) | 0 | 0.0002 (3) | 0 |
Ge4 | 0.0102 (4) | 0.0102 (4) | 0.0116 (6) | 0 | −0.0010 (3) | 0 |
Fe1 | 0.0089 (3) | 0.0112 (4) | 0.0170 (5) | 0.0007 (3) | 0.0005 (3) | 0.0001 (4) |
Cu1 | 0.0090 (3) | 0.0315 (4) | 0.0314 (6) | −0.0030 (3) | 0.0009 (3) | −0.0146 (4) |
O1 | 0.013 (3) | 0.011 (3) | 0.019 (4) | 0 | −0.002 (2) | 0 |
O2 | 0.014 (3) | 0.053 (5) | 0.029 (5) | 0 | 0.011 (3) | 0 |
O3 | 0.011 (3) | 0.030 (3) | 0.011 (4) | 0 | 0.001 (2) | 0 |
O4 | 0.0103 (18) | 0.021 (2) | 0.026 (3) | −0.0051 (15) | 0.0038 (16) | −0.007 (2) |
O5 | 0.011 (2) | 0.028 (3) | 0.018 (4) | 0 | 0.000 (2) | 0 |
O6 | 0.0137 (19) | 0.015 (2) | 0.023 (3) | 0.0070 (16) | 0.0031 (16) | 0.0074 (19) |
O7 | 0.0155 (19) | 0.014 (2) | 0.030 (3) | −0.0019 (16) | 0.0032 (17) | −0.009 (2) |
O8 | 0.016 (3) | 0.016 (3) | 0.015 (4) | 0 | −0.003 (2) | 0 |
O9 | 0.012 (2) | 0.046 (3) | 0.045 (4) | 0.001 (2) | −0.0004 (19) | −0.028 (3) |
Ge1—O4i | 1.749 (5) | Ge4—O8 | 1.742 (7) |
Ge1—O4 | 1.749 (5) | Ge4—O6i | 1.749 (4) |
Ge1—O1 | 1.753 (6) | Ge4—O6 | 1.749 (4) |
Ge1—O3 | 1.771 (6) | Fe1—O6iii | 1.956 (4) |
Ge2—O2 | 1.691 (7) | Fe1—O7iv | 2.011 (4) |
Ge2—O7 | 1.748 (5) | Fe1—O4v | 2.042 (5) |
Ge2—O7i | 1.748 (5) | Fe1—O8v | 2.067 (4) |
Ge2—O5 | 1.777 (6) | Fe1—O1 | 2.067 (4) |
Ge3—O9 | 1.741 (4) | Fe1—O6 | 2.115 (5) |
Ge3—O9i | 1.741 (4) | Cu1—O9vi | 1.914 (5) |
Ge3—O3 | 1.745 (6) | Cu1—O4v | 1.940 (4) |
Ge3—O5ii | 1.755 (4) | Cu1—O9v | 1.946 (4) |
Ge4—O2 | 1.719 (6) | Cu1—O7iv | 2.012 (5) |
O4i—Ge1—O4 | 108.5 (3) | O6i—Ge4—O6 | 116.0 (3) |
O4i—Ge1—O1 | 114.87 (18) | O6iii—Fe1—O7iv | 105.79 (18) |
O4—Ge1—O1 | 114.87 (18) | O6iii—Fe1—O4v | 114.0 (2) |
O4i—Ge1—O3 | 109.71 (17) | O7iv—Fe1—O4v | 76.08 (19) |
O4—Ge1—O3 | 109.71 (17) | O6iii—Fe1—O8v | 92.76 (19) |
O1—Ge1—O3 | 98.7 (3) | O7iv—Fe1—O8v | 155.3 (2) |
O2—Ge2—O7 | 113.04 (19) | O4v—Fe1—O8v | 81.6 (2) |
O2—Ge2—O7i | 113.04 (19) | O6iii—Fe1—O1 | 146.5 (2) |
O7—Ge2—O7i | 111.8 (4) | O7iv—Fe1—O1 | 94.7 (2) |
O2—Ge2—O5 | 100.4 (3) | O4v—Fe1—O1 | 96.3 (2) |
O7—Ge2—O5 | 108.91 (16) | O8v—Fe1—O1 | 77.27 (19) |
O7i—Ge2—O5 | 108.91 (16) | O6iii—Fe1—O6 | 72.8 (2) |
O9—Ge3—O9i | 109.4 (4) | O7iv—Fe1—O6 | 108.2 (2) |
O9—Ge3—O3 | 108.76 (19) | O4v—Fe1—O6 | 171.05 (16) |
O9i—Ge3—O3 | 108.76 (19) | O8v—Fe1—O6 | 92.5 (2) |
O9—Ge3—O5ii | 108.84 (16) | O1—Fe1—O6 | 75.8 (2) |
O9i—Ge3—O5ii | 108.84 (16) | O9vi—Cu1—O4v | 178.5 (2) |
O3—Ge3—O5ii | 112.2 (3) | O9vi—Cu1—O9v | 77.36 (18) |
O2—Ge4—O8 | 108.7 (4) | O4v—Cu1—O9v | 101.94 (19) |
O2—Ge4—O6i | 100.1 (2) | O9vi—Cu1—O7iv | 102.22 (15) |
O8—Ge4—O6i | 114.62 (17) | O4v—Cu1—O7iv | 78.39 (19) |
O2—Ge4—O6 | 100.1 (2) | O9v—Cu1—O7iv | 176.1 (3) |
O8—Ge4—O6 | 114.62 (17) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | F(000) = 684.0 |
Mr = 737.14 | Dx = 4.819 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
a = 12.149 (5) Å | Cell parameters from 4513 reflections |
b = 8.577 (3) Å | θ = 2.9–28.1° |
c = 4.9048 (19) Å | µ = 18.61 mm−1 |
β = 96.25 (3)° | T = 819 K |
V = 508.1 (3) Å3 | Prismatic, pale green |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 802 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.076 |
rotation method, ϕ scans | θmax = 27.9°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→16 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4527 measured reflections | l = −5→5 |
1164 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0302P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.039 | (Δ/σ)max < 0.001 |
wR(F2) = 0.072 | Δρmax = 1.09 e Å−3 |
S = 0.97 | Δρmin = −1.10 e Å−3 |
1164 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.0417 (14) |
Cu2Fe2Ge4O13 | V = 508.1 (3) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.149 (5) Å | µ = 18.61 mm−1 |
b = 8.577 (3) Å | T = 819 K |
c = 4.9048 (19) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.25 (3)° |
STOE IPDS-I diffractometer | 1164 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 802 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.076 |
4527 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 110 parameters |
wR(F2) = 0.072 | 0 restraints |
S = 0.97 | Δρmax = 1.09 e Å−3 |
1164 reflections | Δρmin = −1.10 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24042 (8) | 0.25 | 0.4912 (3) | 0.0126 (3) | |
Ge2 | 0.74706 (8) | 0.25 | 0.3345 (3) | 0.0127 (3) | |
Ge3 | −0.00517 (8) | 0.25 | 0.4023 (3) | 0.0148 (3) | |
Ge4 | 0.51296 (9) | 0.25 | 0.6067 (3) | 0.0111 (3) | |
Fe1 | 0.37562 (9) | 0.06129 (12) | 1.0489 (3) | 0.0128 (3) | |
Cu1 | 0.12521 (8) | −0.00315 (15) | 1.0440 (3) | 0.0250 (3) | |
O1 | 0.3322 (6) | 0.25 | 0.7945 (19) | 0.0160 (17) | |
O2 | 0.6525 (6) | 0.25 | 0.562 (2) | 0.029 (2) | |
O3 | 0.1129 (6) | 0.25 | 0.639 (2) | 0.0184 (18) | |
O4 | 0.2475 (4) | 0.0840 (7) | 0.2847 (14) | 0.0182 (13) | |
O5 | 0.8721 (7) | 0.25 | 0.561 (2) | 0.0206 (18) | |
O6 | 0.5052 (4) | 0.0771 (6) | 0.7939 (14) | 0.0191 (13) | |
O7 | 0.7432 (4) | 0.0806 (7) | 0.1298 (15) | 0.0221 (14) | |
O8 | 0.4358 (6) | 0.25 | 0.2855 (19) | 0.0164 (18) | |
O9 | −0.0021 (5) | 0.0831 (9) | 0.1983 (18) | 0.0373 (19) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0088 (5) | 0.0141 (6) | 0.0142 (9) | 0 | −0.0023 (4) | 0 |
Ge2 | 0.0076 (5) | 0.0118 (6) | 0.0187 (8) | 0 | 0.0005 (4) | 0 |
Ge3 | 0.0070 (5) | 0.0216 (6) | 0.0155 (9) | 0 | 0.0002 (4) | 0 |
Ge4 | 0.0110 (5) | 0.0110 (5) | 0.0107 (8) | 0 | −0.0011 (4) | 0 |
Fe1 | 0.0090 (4) | 0.0121 (5) | 0.0172 (7) | 0.0008 (4) | 0.0008 (4) | 0.0002 (5) |
Cu1 | 0.0098 (4) | 0.0328 (5) | 0.0321 (8) | −0.0035 (4) | 0.0014 (4) | −0.0157 (5) |
O1 | 0.013 (3) | 0.017 (4) | 0.017 (5) | 0 | −0.001 (3) | 0 |
O2 | 0.015 (4) | 0.048 (6) | 0.026 (7) | 0 | 0.012 (3) | 0 |
O3 | 0.008 (3) | 0.033 (4) | 0.014 (6) | 0 | 0.003 (3) | 0 |
O4 | 0.011 (2) | 0.021 (3) | 0.023 (4) | −0.005 (2) | 0.005 (2) | −0.010 (3) |
O5 | 0.011 (3) | 0.031 (4) | 0.020 (6) | 0 | −0.001 (3) | 0 |
O6 | 0.014 (3) | 0.018 (3) | 0.026 (4) | 0.006 (2) | 0.005 (2) | 0.009 (3) |
O7 | 0.016 (3) | 0.016 (3) | 0.034 (5) | −0.006 (2) | 0.002 (2) | −0.009 (3) |
O8 | 0.017 (4) | 0.015 (4) | 0.016 (5) | 0 | −0.006 (3) | 0 |
O9 | 0.018 (3) | 0.049 (4) | 0.044 (6) | 0.000 (3) | −0.003 (3) | −0.021 (4) |
Ge1—O4 | 1.754 (6) | Ge4—O8 | 1.743 (8) |
Ge1—O4i | 1.754 (6) | Ge4—O6i | 1.752 (6) |
Ge1—O1 | 1.759 (8) | Ge4—O6 | 1.752 (6) |
Ge1—O3 | 1.780 (8) | Fe1—O6iii | 1.964 (5) |
Ge2—O2 | 1.688 (9) | Fe1—O7iv | 2.014 (6) |
Ge2—O7 | 1.764 (6) | Fe1—O4v | 2.047 (6) |
Ge2—O7i | 1.764 (6) | Fe1—O1 | 2.076 (6) |
Ge2—O5 | 1.783 (9) | Fe1—O8v | 2.078 (5) |
Ge3—O3 | 1.745 (8) | Fe1—O6 | 2.119 (6) |
Ge3—O9 | 1.749 (7) | Cu1—O9vi | 1.932 (7) |
Ge3—O9i | 1.749 (7) | Cu1—O9v | 1.941 (7) |
Ge3—O5ii | 1.756 (9) | Cu1—O4v | 1.944 (6) |
Ge4—O2 | 1.732 (8) | Cu1—O7iv | 2.005 (6) |
O4—Ge1—O4i | 108.4 (4) | O6i—Ge4—O6 | 115.7 (4) |
O4—Ge1—O1 | 114.9 (2) | O6iii—Fe1—O7iv | 105.6 (2) |
O4i—Ge1—O1 | 114.9 (2) | O6iii—Fe1—O4v | 114.1 (3) |
O4—Ge1—O3 | 109.6 (2) | O7iv—Fe1—O4v | 75.6 (2) |
O4i—Ge1—O3 | 109.6 (2) | O6iii—Fe1—O1 | 146.7 (3) |
O1—Ge1—O3 | 98.9 (4) | O7iv—Fe1—O1 | 94.9 (3) |
O2—Ge2—O7 | 113.5 (2) | O4v—Fe1—O1 | 96.1 (3) |
O2—Ge2—O7i | 113.5 (2) | O6iii—Fe1—O8v | 93.0 (2) |
O7—Ge2—O7i | 110.9 (5) | O7iv—Fe1—O8v | 154.9 (3) |
O2—Ge2—O5 | 100.5 (5) | O4v—Fe1—O8v | 81.6 (3) |
O7—Ge2—O5 | 108.9 (3) | O1—Fe1—O8v | 77.3 (2) |
O7i—Ge2—O5 | 108.9 (3) | O6iii—Fe1—O6 | 73.0 (3) |
O3—Ge3—O9 | 108.3 (3) | O7iv—Fe1—O6 | 109.0 (3) |
O3—Ge3—O9i | 108.3 (3) | O4v—Fe1—O6 | 170.7 (2) |
O9—Ge3—O9i | 109.8 (6) | O1—Fe1—O6 | 75.7 (3) |
O3—Ge3—O5ii | 112.4 (4) | O8v—Fe1—O6 | 92.3 (3) |
O9—Ge3—O5ii | 109.0 (3) | O9vi—Cu1—O9v | 77.2 (4) |
O9i—Ge3—O5ii | 109.0 (3) | O9vi—Cu1—O4v | 178.2 (3) |
O2—Ge4—O8 | 108.9 (5) | O9v—Cu1—O4v | 101.9 (3) |
O2—Ge4—O6i | 100.1 (3) | O9vi—Cu1—O7iv | 102.7 (3) |
O8—Ge4—O6i | 114.8 (2) | O9v—Cu1—O7iv | 176.5 (4) |
O2—Ge4—O6 | 100.1 (3) | O4v—Cu1—O7iv | 78.1 (2) |
O8—Ge4—O6 | 114.8 (2) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Cu2Fe2Ge4O13 | Z = 2 |
Mr = 737.14 | F(000) = 684 |
Monoclinic, P21/m | Dx = 4.853 Mg m−3 |
a = 12.1165 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.5535 (7) Å | µ = 18.75 mm−1 |
c = 4.8974 (5) Å | T = 903 K |
β = 96.326 (11)° | Prismatic, pale green |
V = 504.47 (7) Å3 | 0.12 × 0.11 × 0.08 mm |
STOE IPDS-I diffractometer | 699 reflections with I > 2σ(I) |
Radiation source: sealed x-ray tupe | Rint = 0.127 |
rotation method, ϕ scans | θmax = 27.9°, θmin = 2.9° |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | h = −15→15 |
Tmin = 0.12, Tmax = 0.25 | k = −11→11 |
4491 measured reflections | l = −5→5 |
1155 independent reflections |
Refinement on F2 | 4 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0648P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.058 | (Δ/σ)max < 0.001 |
wR(F2) = 0.136 | Δρmax = 1.74 e Å−3 |
S = 0.97 | Δρmin = −1.93 e Å−3 |
1155 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
110 parameters | Extinction coefficient: 0.055 (3) |
Cu2Fe2Ge4O13 | V = 504.47 (7) Å3 |
Mr = 737.14 | Z = 2 |
Monoclinic, P21/m | Mo Kα radiation |
a = 12.1165 (8) Å | µ = 18.75 mm−1 |
b = 8.5535 (7) Å | T = 903 K |
c = 4.8974 (5) Å | 0.12 × 0.11 × 0.08 mm |
β = 96.326 (11)° |
STOE IPDS-I diffractometer | 1155 independent reflections |
Absorption correction: numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | 699 reflections with I > 2σ(I) |
Tmin = 0.12, Tmax = 0.25 | Rint = 0.127 |
4491 measured reflections |
R[F2 > 2σ(F2)] = 0.058 | 110 parameters |
wR(F2) = 0.136 | 4 restraints |
S = 0.97 | Δρmax = 1.74 e Å−3 |
1155 reflections | Δρmin = −1.93 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ge1 | 0.24039 (14) | 0.25 | 0.4914 (5) | 0.0115 (6) | |
Ge2 | 0.74722 (14) | 0.25 | 0.3337 (5) | 0.0113 (5) | |
Ge3 | −0.00519 (14) | 0.25 | 0.4015 (5) | 0.0139 (6) | |
Ge4 | 0.51322 (15) | 0.25 | 0.6066 (4) | 0.0092 (5) | |
Fe1 | 0.37523 (13) | 0.06107 (18) | 1.0491 (4) | 0.0118 (5) | |
Cu1 | 0.12515 (12) | −0.0033 (3) | 1.0449 (5) | 0.0251 (6) | |
O1 | 0.3311 (9) | 0.25 | 0.795 (3) | 0.013 (3) | |
O2 | 0.6518 (3) | 0.25 | 0.5591 (13) | 0.033 (4) | |
O3 | 0.1130 (7) | 0.25 | 0.639 (2) | 0.020 (3) | |
O4 | 0.2475 (2) | 0.0828 (11) | 0.2873 (9) | 0.017 (2) | |
O5 | 0.87212 (17) | 0.25 | 0.5609 (7) | 0.019 (3) | |
O6 | 0.5056 (3) | 0.0768 (7) | 0.7934 (19) | 0.017 (2) | |
O7 | 0.7430 (8) | 0.0806 (11) | 0.134 (3) | 0.020 (2) | |
O8 | 0.4365 (9) | 0.25 | 0.2842 (13) | 0.014 (3) | |
O9 | −0.00317 (15) | 0.0842 (7) | 0.1958 (13) | 0.032 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0047 (8) | 0.0162 (11) | 0.0126 (15) | 0.000 | −0.0034 (7) | 0.000 |
Ge2 | 0.0022 (8) | 0.0132 (10) | 0.0183 (15) | 0.000 | −0.0007 (7) | 0.000 |
Ge3 | 0.0016 (8) | 0.0221 (11) | 0.0173 (15) | 0.000 | −0.0015 (8) | 0.000 |
Ge4 | 0.0072 (8) | 0.0111 (9) | 0.0088 (14) | 0.000 | −0.0016 (7) | 0.000 |
Fe1 | 0.0048 (8) | 0.0152 (9) | 0.0149 (13) | 0.0024 (7) | −0.0005 (6) | 0.0009 (9) |
Cu1 | 0.0049 (7) | 0.0369 (10) | 0.0331 (14) | −0.0045 (7) | 0.0006 (6) | −0.0183 (10) |
O1 | 0.005 (5) | 0.018 (7) | 0.015 (9) | 0.000 | −0.001 (5) | 0.000 |
O2 | 0.024 (8) | 0.053 (11) | 0.026 (13) | 0.000 | 0.017 (7) | 0.000 |
O3 | 0.014 (6) | 0.041 (9) | 0.007 (10) | 0.000 | −0.001 (5) | 0.000 |
O4 | 0.003 (4) | 0.026 (6) | 0.023 (7) | −0.005 (3) | 0.003 (4) | −0.012 (5) |
O5 | 0.012 (6) | 0.036 (8) | 0.009 (9) | 0.000 | −0.001 (5) | 0.000 |
O6 | 0.011 (4) | 0.011 (5) | 0.031 (8) | 0.002 (4) | 0.003 (4) | 0.011 (5) |
O7 | 0.011 (4) | 0.014 (5) | 0.036 (8) | −0.005 (4) | 0.002 (4) | −0.010 (5) |
O8 | 0.013 (6) | 0.015 (6) | 0.012 (9) | 0.000 | −0.006 (5) | 0.000 |
O9 | 0.012 (5) | 0.045 (7) | 0.039 (10) | 0.004 (5) | −0.001 (5) | −0.020 (7) |
Ge1—O1 | 1.750 (14) | Ge4—O8 | 1.742 (8) |
Ge1—O4 | 1.752 (6) | Ge4—O6i | 1.749 (8) |
Ge1—O4i | 1.752 (6) | Ge4—O6 | 1.749 (8) |
Ge1—O3 | 1.776 (14) | Fe1—O6iii | 1.956 (6) |
Ge2—O2 | 1.684 (8) | Fe1—O7iv | 2.010 (9) |
Ge2—O7 | 1.747 (10) | Fe1—O4v | 2.047 (6) |
Ge2—O7i | 1.747 (10) | Fe1—O1 | 2.073 (9) |
Ge2—O5 | 1.777 (3) | Fe1—O8v | 2.074 (6) |
Ge3—O9 | 1.741 (9) | Fe1—O6 | 2.125 (6) |
Ge3—O9i | 1.741 (9) | Cu1—O9vi | 1.915 (4) |
Ge3—O3 | 1.743 (9) | Cu1—O4v | 1.940 (9) |
Ge3—O5ii | 1.754 (3) | Cu1—O9v | 1.944 (9) |
Ge4—O2 | 1.720 (8) | Cu1—O7iv | 2.015 (10) |
O1—Ge1—O4 | 114.8 (3) | O6i—Ge4—O6 | 115.8 (7) |
O1—Ge1—O4i | 114.8 (3) | O6iii—Fe1—O7iv | 105.7 (4) |
O4—Ge1—O4i | 109.4 (6) | O6iii—Fe1—O4v | 113.7 (3) |
O1—Ge1—O3 | 98.4 (5) | O7iv—Fe1—O4v | 76.2 (3) |
O4—Ge1—O3 | 109.39 (16) | O6iii—Fe1—O1 | 146.8 (4) |
O4i—Ge1—O3 | 109.39 (15) | O7iv—Fe1—O1 | 94.5 (4) |
O2—Ge2—O7 | 112.8 (4) | O4v—Fe1—O1 | 96.3 (5) |
O2—Ge2—O7i | 112.8 (4) | O6iii—Fe1—O8v | 92.7 (3) |
O7—Ge2—O7i | 112.1 (8) | O7iv—Fe1—O8v | 155.7 (5) |
O2—Ge2—O5 | 100.9 (2) | O4v—Fe1—O8v | 81.9 (4) |
O7—Ge2—O5 | 108.8 (3) | O1—Fe1—O8v | 77.2 (3) |
O7i—Ge2—O5 | 108.8 (3) | O6iii—Fe1—O6 | 72.9 (2) |
O9—Ge3—O9i | 109.0 (6) | O7iv—Fe1—O6 | 108.4 (4) |
O9—Ge3—O3 | 108.9 (3) | O4v—Fe1—O6 | 171.1 (3) |
O9i—Ge3—O3 | 108.9 (3) | O1—Fe1—O6 | 75.9 (4) |
O9—Ge3—O5ii | 108.92 (18) | O8v—Fe1—O6 | 91.9 (5) |
O9i—Ge3—O5ii | 108.92 (18) | O9vi—Cu1—O4v | 178.8 (4) |
O3—Ge3—O5ii | 112.1 (5) | O9vi—Cu1—O9v | 77.17 (15) |
O2—Ge4—O8 | 108.0 (5) | O4v—Cu1—O9v | 102.12 (17) |
O2—Ge4—O6i | 100.35 (16) | O9vi—Cu1—O7iv | 102.1 (3) |
O8—Ge4—O6i | 114.9 (3) | O4v—Cu1—O7iv | 78.5 (3) |
O2—Ge4—O6 | 100.35 (16) | O9v—Cu1—O7iv | 175.5 (5) |
O8—Ge4—O6 | 114.9 (4) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1, y, z; (iii) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) −x, −y, −z+1. |
Experimental details
(cf5_090) | (cf5_130) | (cf5_170) | (cf5_200) | |
Crystal data | ||||
Chemical formula | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 |
Mr | 737.14 | 737.14 | 737.14 | 737.14 |
Crystal system, space group | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m |
Temperature (K) | 90 | 130 | 170 | 200 |
a, b, c (Å) | 12.090 (2), 8.4901 (9), 4.8626 (8) | 12.0881 (9), 8.4914 (5), 4.8644 (4) | 12.0087 (9), 8.4931 (5), 4.8657 (4) | 12.0859 (9), 8.4947 (5), 4.8667 (4) |
β (°) | 96.13 (2) | 96.137 (9) | 96.139 (9) | 96.143 (9) |
V (Å3) | 496.27 (13) | 496.44 (6) | 493.41 (6) | 496.78 (6) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 19.06 | 19.05 | 19.17 | 19.04 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 |
Data collection | ||||
Diffractometer | STOE IPDS-II diffractometer | STOE IPDS-II diffractometer | STOE IPDS-II diffractometer | STOE IPDS-II diffractometer |
Absorption correction | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) |
Tmin, Tmax | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.22 | 0.12, 0.25 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5776, 1527, 1202 | 5770, 1530, 1198 | 5729, 1518, 1171 | 5779, 1530, 1196 |
Rint | 0.060 | 0.056 | 0.057 | 0.059 |
(sin θ/λ)max (Å−1) | 0.704 | 0.704 | 0.704 | 0.704 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.058, 1.02 | 0.031, 0.055, 1.00 | 0.031, 0.062, 0.98 | 0.031, 0.055, 0.97 |
No. of reflections | 1527 | 1530 | 1518 | 1530 |
No. of parameters | 110 | 110 | 110 | 110 |
No. of restraints | 3 | 1 | 3 | 4 |
Δρmax, Δρmin (e Å−3) | 1.51, −1.16 | 1.31, −1.17 | 1.03, −1.15 | 0.92, −1.09 |
(cf5_250) | (cf5_290) | (cufege) | (cf9_050) | |
Crystal data | ||||
Chemical formula | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 |
Mr | 737.14 | 737.14 | 737.14 | 737.14 |
Crystal system, space group | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m |
Temperature (K) | 250 | 290 | 298 | 320 |
a, b, c (Å) | 12.0858 (9), 8.4979 (5), 4.8691 (4) | 12.0861 (12), 8.5008 (8), 4.8704 (5) | 12.088 (2), 8.5019 (9), 4.8703 (8) | 12.0876 (8), 8.5043 (7), 4.8715 (5) |
β (°) | 96.161 (9) | 96.167 (9) | 96.17 (2) | 96.19 (2) |
V (Å3) | 497.19 (6) | 497.50 (9) | 497.61 (13) | 497.86 (7) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 19.02 | 19.00 | 18.99 | 18.99 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 |
Data collection | ||||
Diffractometer | STOE IPDS-II diffractometer | STOE IPDS-II diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer |
Absorption correction | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) |
Tmin, Tmax | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5751, 1523, 1172 | 7188, 1524, 1256 | 4906, 1267, 1087 | 4481, 1162, 955 |
Rint | 0.065 | 0.055 | 0.039 | 0.038 |
(sin θ/λ)max (Å−1) | 0.704 | 0.704 | 0.662 | 0.662 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.059, 1.00 | 0.026, 0.054, 1.02 | 0.021, 0.048, 1.02 | 0.025, 0.051, 1.01 |
No. of reflections | 1523 | 1524 | 1267 | 1162 |
No. of parameters | 110 | 110 | 107 | 110 |
No. of restraints | 8 | 4 | 0 | 0 |
Δρmax, Δρmin (e Å−3) | 1.38, −1.09 | 0.91, −1.04 | 1.45, −1.59 | 0.75, −0.81 |
(cf9_100) | (cf9_200) | (cf9_300) | (cf9_400) | |
Crystal data | ||||
Chemical formula | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 |
Mr | 737.14 | 737.14 | 737.14 | 737.14 |
Crystal system, space group | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m |
Temperature (K) | 362 | 445 | 528 | 611 |
a, b, c (Å) | 12.0883 (8), 8.5076 (7), 4.8727 (5) | 12.0943 (8), 8.5142 (7), 4.8763 (5) | 12.0971 (8), 8.5205 (7), 4.8803 (5) | 12.1011 (8), 8.5290 (7), 4.8841 (5) |
β (°) | 96.18 (2) | 96.21 (2) | 96.22 (2) | 96.24 (2) |
V (Å3) | 498.21 (8) | 499.19 (8) | 500.07 (8) | 501.10 (8) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.98 | 18.94 | 18.91 | 18.87 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 |
Data collection | ||||
Diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer |
Absorption correction | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) |
Tmin, Tmax | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4515, 1164, 956 | 4494, 1164, 962 | 4513, 1167, 949 | 4515, 1165, 914 |
Rint | 0.049 | 0.045 | 0.038 | 0.046 |
(sin θ/λ)max (Å−1) | 0.660 | 0.659 | 0.659 | 0.659 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.053, 0.97 | 0.028, 0.062, 0.97 | 0.026, 0.054, 0.98 | 0.028, 0.062, 0.99 |
No. of reflections | 1164 | 1164 | 1167 | 1165 |
No. of parameters | 110 | 110 | 110 | 110 |
No. of restraints | 4 | 6 | 1 | 3 |
Δρmax, Δρmin (e Å−3) | 1.16, −0.85 | 0.92, −0.77 | 1.00, −0.70 | 0.83, −0.90 |
(cf9_500) | (cf9_550) | (cf9_600) | (cf9_650) | |
Crystal data | ||||
Chemical formula | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 | Cu2Fe2Ge4O13 |
Mr | 737.14 | 737.14 | 737.14 | 737.14 |
Crystal system, space group | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m | Monoclinic, P21/m |
Temperature (K) | 695 | 736 | 778 | 819 |
a, b, c (Å) | 12.1039 (8), 8.5353 (7), 4.8886 (5) | 12.1073 (8), 8.5380 (7), 4.8899 (5) | 12.1083 (8), 8.5422 (7), 4.8916 (5) | 12.149 (5), 8.577 (3), 4.9048 (19) |
β (°) | 96.28 (2) | 96.28 (2) | 96.295 (11) | 96.25 (3) |
V (Å3) | 502.01 (8) | 502.45 (8) | 502.90 (7) | 508.1 (3) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.84 | 18.82 | 18.80 | 18.61 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 | 0.12 × 0.11 × 0.08 |
Data collection | ||||
Diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer | STOE IPDS-I diffractometer |
Absorption correction | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) |
Tmin, Tmax | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 | 0.12, 0.25 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4549, 1169, 891 | 4541, 1171, 877 | 4541, 1170, 856 | 4527, 1164, 802 |
Rint | 0.047 | 0.047 | 0.055 | 0.076 |
(sin θ/λ)max (Å−1) | 0.662 | 0.662 | 0.662 | 0.659 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.061, 1.01 | 0.027, 0.054, 0.97 | 0.032, 0.060, 0.98 | 0.039, 0.072, 0.97 |
No. of reflections | 1169 | 1171 | 1170 | 1164 |
No. of parameters | 110 | 110 | 110 | 110 |
No. of restraints | 5 | 3 | 2 | 0 |
Δρmax, Δρmin (e Å−3) | 0.85, −0.81 | 0.73, −0.67 | 0.64, −0.78 | 1.09, −1.10 |
(cf9_750) | |
Crystal data | |
Chemical formula | Cu2Fe2Ge4O13 |
Mr | 737.14 |
Crystal system, space group | Monoclinic, P21/m |
Temperature (K) | 903 |
a, b, c (Å) | 12.1165 (8), 8.5535 (7), 4.8974 (5) |
β (°) | 96.326 (11) |
V (Å3) | 504.47 (7) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 18.75 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 |
Data collection | |
Diffractometer | STOE IPDS-I diffractometer |
Absorption correction | Numerical via equivalents using Stoe X-SHAPE and X-RED (Stoe & Cie 1996) |
Tmin, Tmax | 0.12, 0.25 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4491, 1155, 699 |
Rint | 0.127 |
(sin θ/λ)max (Å−1) | 0.658 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.136, 0.97 |
No. of reflections | 1155 |
No. of parameters | 110 |
No. of restraints | 4 |
Δρmax, Δρmin (e Å−3) | 1.74, −1.93 |
Computer programs: STOE X-AREA (Stoe & Cie, 2002), Stoe X-AREA (Stoe & Cie, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), Diamond 3.0 Bradenburg & Berndt 1999), WinGX 1.70.00 (Farrugia, 1999)'.
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