Temperature-dependent crystal structure refinement and ⁵⁷Fe Mössbauer spectroscopy of Cu₂Fe₂Ge₄O₁₃

The germanate compound Cu₂Fe₂Ge₄O₁₃, dicopper diiron germanate, was synthesized by solid-state reaction at 1403 K and ambient pressure. There is no change of space-group symmetry between 10 and 900 K. Between 40 K and room temperature the a lattice parameter shows a negative thermal expansion which can be connected to a decreasing Cu-Cu interatomic distance. Above room temperature all the lattice parameters are positively correlated with temperature. Among the structural parameters several alterations with temperature occur, which are most prominent for the distorted Fe³⁺ octahedral site. Besides an increase of the average bond length and of the interatomic Fe-Fe distances, distortional parameters also increase with temperature, while the average Cu-O bond length remains almost constant between 100 and 900 K, as do the average Ge-O distances. ⁵⁷Fe Mössbauer spectroscopy was used to detect long-range magnetic ordering in Cu₂Fe₂Ge₄O₁₃. While around 100 K, which is the temperature at which a broad maximum is observed in the magnetic susceptibility, no magnetic ordering was detected in the Mössbauer spectrum, below 40 K a narrow split sextet is developed which is indicative of a three-dimensional magnetic ordering of the sample.

S1. Comment

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Computing details

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.

Figures

Figure 1. View of (I) (50% probability displacement ellipsoids)

(cf5_090)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	3 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0238P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.032	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0024 (3)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.747 (4)	Fe1—O8^v	2.0467 (10)
Ge1—O4	1.748 (3)	Fe1—O1	2.050 (3)
Ge1—O4^i	1.748 (3)	Fe1—O6	2.0831 (15)
Ge1—O3	1.769 (5)	Cu1—O9^vi	1.929 (3)
Ge2—O2	1.702 (5)	Cu1—O4^v	1.931 (3)
Ge2—O7	1.746 (3)	Cu1—O9^v	1.951 (3)
Ge2—O7^i	1.746 (3)	Cu1—O7^iv	1.998 (3)
Ge2—O5	1.777 (4)	Cu1—Cu1^vii	3.0331 (12)
Ge3—O9	1.737 (3)	O1—Fe1^i	2.050 (3)
Ge3—O9^i	1.737 (3)	O4—Cu1^viii	1.931 (3)
Ge3—O3	1.750 (4)	O4—Fe1^viii	2.038 (3)
Ge3—O5^ii	1.758 (5)	O5—Ge3^ix	1.758 (5)
Ge4—O2	1.733 (4)	O6—Fe1^iii	1.953 (3)
Ge4—O8	1.747 (3)	O7—Cu1^iv	1.998 (3)
Ge4—O6^i	1.756 (3)	O7—Fe1^iv	2.007 (3)
Ge4—O6	1.756 (3)	O8—Fe1^viii	2.0467 (10)
Fe1—O6^iii	1.953 (3)	O8—Fe1^x	2.0467 (10)
Fe1—O7^iv	2.007 (3)	O9—Cu1^vi	1.929 (3)
Fe1—O4^v	2.038 (3)	O9—Cu1^viii	1.951 (3)
O1—Ge1—O4	114.70 (12)	O7^iv—Fe1—O6	107.70 (13)
O1—Ge1—O4^i	114.70 (12)	O4^v—Fe1—O6	171.55 (12)
O4—Ge1—O4^i	107.8 (2)	O8^v—Fe1—O6	92.84 (15)
O1—Ge1—O3	98.5 (2)	O1—Fe1—O6	76.44 (15)
O4—Ge1—O3	110.40 (13)	O9^vi—Cu1—O4^v	177.87 (15)
O4^i—Ge1—O3	110.40 (13)	O9^vi—Cu1—O9^v	77.17 (16)
O2—Ge2—O7	113.56 (13)	O4^v—Cu1—O9^v	101.79 (13)
O2—Ge2—O7^i	113.56 (13)	O9^vi—Cu1—O7^iv	102.44 (13)
O7—Ge2—O7^i	111.1 (2)	O4^v—Cu1—O7^iv	78.49 (13)
O2—Ge2—O5	98.8 (2)	O9^v—Cu1—O7^iv	176.51 (15)
O7—Ge2—O5	109.50 (12)	O9^vi—Cu1—Cu1^vii	38.84 (10)
O7^i—Ge2—O5	109.50 (12)	O4^v—Cu1—Cu1^vii	140.09 (10)
O9—Ge3—O9^i	109.9 (2)	O9^v—Cu1—Cu1^vii	38.33 (9)
O9—Ge3—O3	108.69 (13)	O7^iv—Cu1—Cu1^vii	141.17 (10)
O9^i—Ge3—O3	108.69 (13)	Ge1—O1—Fe1^i	127.13 (10)
O9—Ge3—O5^ii	108.94 (13)	Ge1—O1—Fe1	127.13 (10)
O9^i—Ge3—O5^ii	108.94 (13)	Fe1^i—O1—Fe1	102.7 (2)
O3—Ge3—O5^ii	111.7 (2)	Ge2—O2—Ge4	142.6 (3)
O2—Ge4—O8	110.6 (2)	Ge3—O3—Ge1	113.6 (3)
O2—Ge4—O6^i	99.17 (11)	Ge1—O4—Cu1^viii	125.21 (17)
O8—Ge4—O6^i	114.25 (11)	Ge1—O4—Fe1^viii	119.79 (17)
O2—Ge4—O6	99.17 (11)	Cu1^viii—O4—Fe1^viii	101.28 (15)
O8—Ge4—O6	114.25 (11)	Ge3^ix—O5—Ge2	114.5 (3)
O6^i—Ge4—O6	116.86 (17)	Ge4—O6—Fe1^iii	128.43 (12)
O6^iii—Fe1—O7^iv	107.02 (12)	Ge4—O6—Fe1	116.10 (13)
O6^iii—Fe1—O4^v	114.14 (11)	Fe1^iii—O6—Fe1	107.43 (12)
O7^iv—Fe1—O4^v	75.84 (13)	Ge2—O7—Cu1^iv	122.38 (16)
O6^iii—Fe1—O8^v	91.93 (11)	Ge2—O7—Fe1^iv	136.57 (18)
O7^iv—Fe1—O8^v	155.28 (15)	Cu1^iv—O7—Fe1^iv	100.09 (15)
O4^v—Fe1—O8^v	82.05 (15)	Ge4—O8—Fe1^viii	128.48 (4)
O6^iii—Fe1—O1	146.41 (14)	Ge4—O8—Fe1^x	128.48 (4)
O7^iv—Fe1—O1	94.37 (14)	Fe1^viii—O8—Fe1^x	102.92 (7)
O4^v—Fe1—O1	95.78 (16)	Ge3—O9—Cu1^vi	125.45 (17)
O8^v—Fe1—O1	76.85 (10)	Ge3—O9—Cu1^viii	126.53 (16)
O6^iii—Fe1—O6	72.57 (12)	Cu1^vi—O9—Cu1^viii	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.

(cf5_130)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	1 restraint
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0229P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.031	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0032 (3)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4	1.745 (3)	Ge4—O6^i	1.754 (3)
Ge1—O4^i	1.745 (3)	Ge4—O6	1.754 (3)
Ge1—O1	1.747 (4)	Fe1—O6^iii	1.954 (3)
Ge1—O3	1.775 (4)	Fe1—O7^iv	2.003 (3)
Ge2—O2	1.695 (5)	Fe1—O4^v	2.041 (3)
Ge2—O7	1.748 (3)	Fe1—O8^v	2.049 (3)
Ge2—O7^i	1.748 (3)	Fe1—O1	2.053 (3)
Ge2—O5	1.773 (4)	Fe1—O6	2.085 (3)
Ge3—O9	1.734 (3)	Cu1—O9^vi	1.928 (3)
Ge3—O9^i	1.734 (3)	Cu1—O4^v	1.935 (3)
Ge3—O3	1.747 (4)	Cu1—O9^v	1.951 (3)
Ge3—O5^ii	1.7559 (19)	Cu1—O7^iv	2.001 (3)
Ge4—O2	1.735 (4)	Cu1—Cu1^vii	3.0292 (10)
Ge4—O8	1.741 (4)
O4—Ge1—O4^i	108.1 (2)	O6^i—Ge4—O6	116.7 (2)
O4—Ge1—O1	114.48 (12)	O6^iii—Fe1—O7^iv	106.84 (12)
O4^i—Ge1—O1	114.48 (12)	O6^iii—Fe1—O4^v	114.03 (13)
O4—Ge1—O3	110.33 (12)	O7^iv—Fe1—O4^v	75.95 (13)
O4^i—Ge1—O3	110.33 (12)	O6^iii—Fe1—O8^v	91.95 (13)
O1—Ge1—O3	98.8 (2)	O7^iv—Fe1—O8^v	155.36 (15)
O2—Ge2—O7	113.46 (13)	O4^v—Fe1—O8^v	81.94 (15)
O2—Ge2—O7^i	113.46 (13)	O6^iii—Fe1—O1	146.26 (15)
O7—Ge2—O7^i	110.9 (2)	O7^iv—Fe1—O1	94.49 (13)
O2—Ge2—O5	99.11 (19)	O4^v—Fe1—O1	96.11 (15)
O7—Ge2—O5	109.63 (11)	O8^v—Fe1—O1	77.01 (13)
O7^i—Ge2—O5	109.63 (11)	O6^iii—Fe1—O6	72.70 (15)
O9—Ge3—O9^i	109.7 (2)	O7^iv—Fe1—O6	107.68 (13)
O9—Ge3—O3	108.83 (13)	O4^v—Fe1—O6	171.50 (12)
O9^i—Ge3—O3	108.83 (13)	O8^v—Fe1—O6	92.86 (15)
O9—Ge3—O5^ii	108.92 (13)	O1—Fe1—O6	76.09 (15)
O9^i—Ge3—O5^ii	108.92 (13)	O9^vi—Cu1—O4^v	178.09 (14)
O3—Ge3—O5^ii	111.6 (2)	O9^vi—Cu1—O9^v	77.31 (16)
O2—Ge4—O8	110.4 (2)	O4^v—Cu1—O9^v	101.65 (13)
O2—Ge4—O6^i	99.31 (13)	O9^vi—Cu1—O7^iv	102.52 (13)
O8—Ge4—O6^i	114.28 (11)	O4^v—Cu1—O7^iv	78.42 (13)
O2—Ge4—O6	99.31 (13)	O9^v—Cu1—O7^iv	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.

(cf5_170)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	3 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0301P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.031	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0058 (4)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4	1.744 (3)	Ge4—O8	1.7451 (19)
Ge1—O4^i	1.744 (3)	Ge4—O6^i	1.749 (3)
Ge1—O1	1.744 (5)	Ge4—O6	1.749 (3)
Ge1—O3	1.761 (5)	Fe1—O6^iii	1.948 (3)
Ge2—O2	1.683 (4)	Fe1—O7^iv	1.998 (3)
Ge2—O7	1.747 (3)	Fe1—O4^v	2.030 (3)
Ge2—O7^i	1.747 (3)	Fe1—O8^v	2.0472 (14)
Ge2—O5	1.768 (5)	Fe1—O1	2.052 (3)
Ge3—O9^i	1.731 (3)	Fe1—O6	2.078 (3)
Ge3—O9	1.731 (3)	Cu1—O9^vi	1.925 (3)
Ge3—O3	1.737 (5)	Cu1—O4^v	1.930 (3)
Ge3—O5^ii	1.755 (4)	Cu1—O9^v	1.944 (4)
Ge4—O2	1.7325 (19)	Cu1—O7^iv	1.992 (3)
O4—Ge1—O4^i	107.9 (2)	O6^i—Ge4—O6	116.2 (2)
O4—Ge1—O1	114.76 (13)	O6^iii—Fe1—O7^iv	106.30 (13)
O4^i—Ge1—O1	114.76 (13)	O6^iii—Fe1—O4^v	113.85 (14)
O4—Ge1—O3	110.35 (13)	O7^iv—Fe1—O4^v	76.36 (14)
O4^i—Ge1—O3	110.35 (13)	O6^iii—Fe1—O8^v	92.54 (12)
O1—Ge1—O3	98.4 (2)	O7^iv—Fe1—O8^v	155.29 (16)
O2—Ge2—O7	113.74 (13)	O4^v—Fe1—O8^v	81.51 (16)
O2—Ge2—O7^i	113.74 (13)	O6^iii—Fe1—O1	146.58 (17)
O7—Ge2—O7^i	111.0 (2)	O7^iv—Fe1—O1	94.61 (14)
O2—Ge2—O5	98.18 (18)	O4^v—Fe1—O1	96.04 (17)
O7—Ge2—O5	109.71 (12)	O8^v—Fe1—O1	76.80 (12)
O7^i—Ge2—O5	109.71 (12)	O6^iii—Fe1—O6	72.96 (15)
O9^i—Ge3—O9	110.1 (3)	O7^iv—Fe1—O6	107.75 (14)
O9^i—Ge3—O3	108.64 (14)	O4^v—Fe1—O6	171.15 (12)
O9—Ge3—O3	108.64 (14)	O8^v—Fe1—O6	92.79 (16)
O9^i—Ge3—O5^ii	109.03 (14)	O1—Fe1—O6	75.99 (16)
O9—Ge3—O5^ii	109.03 (14)	O9^vi—Cu1—O4^v	177.99 (16)
O3—Ge3—O5^ii	111.4 (2)	O9^vi—Cu1—O9^v	77.98 (17)
O2—Ge4—O8	110.3 (2)	O4^v—Cu1—O9^v	101.20 (14)
O2—Ge4—O6^i	99.21 (14)	O9^vi—Cu1—O7^iv	101.90 (14)
O8—Ge4—O6^i	114.62 (12)	O4^v—Cu1—O7^iv	78.81 (14)
O2—Ge4—O6	99.21 (14)	O9^v—Cu1—O7^iv	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.

(cf5_200)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0234P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.031	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0063 (4)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4	1.747 (3)	Ge4—O8	1.7455 (19)
Ge1—O4^i	1.747 (3)	Ge4—O6^i	1.7505 (17)
Ge1—O1	1.751 (4)	Ge4—O6	1.7505 (17)
Ge1—O3	1.770 (5)	Fe1—O6^iii	1.955 (2)
Ge2—O2	1.698 (5)	Fe1—O7^iv	2.008 (3)
Ge2—O7	1.746 (3)	Fe1—O4^v	2.039 (3)
Ge2—O7^i	1.746 (3)	Fe1—O8^v	2.0491 (13)
Ge2—O5	1.783 (4)	Fe1—O1	2.054 (3)
Ge3—O9	1.7332 (17)	Fe1—O6	2.084 (3)
Ge3—O9^i	1.7332 (17)	Cu1—O9^vi	1.930 (3)
Ge3—O3	1.744 (4)	Cu1—O4^v	1.932 (3)
Ge3—O5^ii	1.754 (5)	Cu1—O9^v	1.951 (3)
Ge4—O2	1.732 (4)	Cu1—O7^iv	2.000 (3)
O4—Ge1—O4^i	107.9 (2)	O6^i—Ge4—O6	116.4 (2)
O4—Ge1—O1	114.61 (12)	O6^iii—Fe1—O7^iv	106.76 (11)
O4^i—Ge1—O1	114.61 (12)	O6^iii—Fe1—O4^v	114.24 (12)
O4—Ge1—O3	110.23 (12)	O7^iv—Fe1—O4^v	75.86 (13)
O4^i—Ge1—O3	110.23 (12)	O6^iii—Fe1—O8^v	92.28 (11)
O1—Ge1—O3	99.0 (2)	O7^iv—Fe1—O8^v	155.15 (15)
O2—Ge2—O7	113.60 (13)	O4^v—Fe1—O8^v	81.87 (15)
O2—Ge2—O7^i	113.60 (13)	O6^iii—Fe1—O1	146.17 (14)
O7—Ge2—O7^i	111.1 (2)	O7^iv—Fe1—O1	94.49 (13)
O2—Ge2—O5	98.9 (2)	O4^v—Fe1—O1	96.09 (16)
O7—Ge2—O5	109.40 (13)	O8^v—Fe1—O1	76.88 (11)
O7^i—Ge2—O5	109.40 (13)	O6^iii—Fe1—O6	72.74 (10)
O9—Ge3—O9^i	110.1 (2)	O7^iv—Fe1—O6	107.88 (13)
O9—Ge3—O3	108.56 (10)	O4^v—Fe1—O6	171.21 (10)
O9^i—Ge3—O3	108.56 (10)	O8^v—Fe1—O6	92.75 (15)
O9—Ge3—O5^ii	108.98 (12)	O1—Fe1—O6	75.85 (14)
O9^i—Ge3—O5^ii	108.98 (12)	O9^vi—Cu1—O4^v	177.99 (14)
O3—Ge3—O5^ii	111.6 (2)	O9^vi—Cu1—O9^v	77.61 (9)
O2—Ge4—O8	110.5 (2)	O4^v—Cu1—O9^v	101.59 (11)
O2—Ge4—O6^i	99.32 (13)	O9^vi—Cu1—O7^iv	102.20 (12)
O8—Ge4—O6^i	114.41 (11)	O4^v—Cu1—O7^iv	78.48 (13)
O2—Ge4—O6	99.32 (13)	O9^v—Cu1—O7^iv	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.

(cf5_250)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	8 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0231P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.033	(Δ/σ)max = 0.002
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0057 (4)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.748 (5)	Ge4—O8	1.745 (5)
Ge1—O4	1.749 (3)	Ge4—O6^i	1.751 (4)
Ge1—O4^i	1.749 (3)	Ge4—O6	1.751 (4)
Ge1—O3	1.774 (5)	Fe1—O6^iii	1.956 (3)
Ge2—O2	1.698 (4)	Fe1—O7^iv	2.004 (4)
Ge2—O7	1.748 (3)	Fe1—O4^v	2.039 (4)
Ge2—O7^i	1.748 (3)	Fe1—O8^v	2.050 (3)
Ge2—O5	1.777 (4)	Fe1—O1	2.055 (3)
Ge3—O9	1.733 (4)	Fe1—O6	2.086 (3)
Ge3—O9^i	1.733 (4)	Cu1—O9^vi	1.928 (3)
Ge3—O3	1.744 (5)	Cu1—O4^v	1.932 (3)
Ge3—O5^ii	1.756 (4)	Cu1—O9^v	1.948 (3)
Ge4—O2	1.733 (3)	Cu1—O7^iv	2.001 (3)
O1—Ge1—O4	114.76 (13)	O6^iii—Fe1—O4^v	114.15 (13)
O1—Ge1—O4^i	114.76 (13)	O7^iv—Fe1—O4^v	75.76 (10)
O4—Ge1—O4^i	107.9 (2)	O6^iii—Fe1—O8^v	92.26 (14)
O1—Ge1—O3	98.8 (2)	O7^iv—Fe1—O8^v	155.00 (13)
O4—Ge1—O3	110.15 (11)	O4^v—Fe1—O8^v	81.73 (16)
O4^i—Ge1—O3	110.15 (11)	O6^iii—Fe1—O1	146.31 (15)
O2—Ge2—O7	113.58 (11)	O7^iv—Fe1—O1	94.57 (14)
O2—Ge2—O7^i	113.58 (10)	O4^v—Fe1—O1	96.02 (16)
O7—Ge2—O7^i	111.0 (2)	O8^v—Fe1—O1	76.97 (14)
O2—Ge2—O5	98.98 (19)	O6^iii—Fe1—O6	72.79 (11)
O7—Ge2—O5	109.52 (10)	O7^iv—Fe1—O6	107.91 (11)
O7^i—Ge2—O5	109.52 (10)	O4^v—Fe1—O6	171.30 (11)
O9—Ge3—O9^i	109.9 (3)	O8^v—Fe1—O6	92.99 (16)
O9—Ge3—O3	108.61 (14)	O1—Fe1—O6	75.97 (15)
O9^i—Ge3—O3	108.61 (14)	O9^vi—Cu1—O4^v	178.07 (15)
O9—Ge3—O5^ii	109.03 (14)	O9^vi—Cu1—O9^v	77.65 (11)
O9^i—Ge3—O5^ii	109.03 (14)	O4^v—Cu1—O9^v	101.56 (10)
O3—Ge3—O5^ii	111.7 (2)	O9^vi—Cu1—O7^iv	102.41 (10)
O2—Ge4—O8	110.5 (2)	O4^v—Cu1—O7^iv	78.27 (8)
O2—Ge4—O6^i	99.38 (12)	O9^v—Cu1—O7^iv	176.58 (17)
O8—Ge4—O6^i	114.29 (12)	O9^vi—Cu1—Cu1^vii	39.07 (8)
O2—Ge4—O6	99.38 (12)	O4^v—Cu1—Cu1^vii	140.12 (8)
O8—Ge4—O6	114.29 (12)	O9^v—Cu1—Cu1^vii	38.59 (8)
O6^i—Ge4—O6	116.5 (2)	O7^iv—Cu1—Cu1^vii	141.37 (7)
O6^iii—Fe1—O7^iv	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.

(cf5_290)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0282P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.026	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0179 (7)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.746 (3)	Ge4—O8	1.744 (3)
Ge1—O4	1.750 (2)	Ge4—O6^i	1.749 (3)
Ge1—O4^i	1.750 (2)	Ge4—O6	1.749 (3)
Ge1—O3	1.772 (4)	Fe1—O6^iii	1.957 (2)
Ge2—O2	1.694 (4)	Fe1—O7^iv	2.004 (3)
Ge2—O7	1.751 (3)	Fe1—O4^v	2.038 (3)
Ge2—O7^i	1.751 (3)	Fe1—O8^v	2.052 (2)
Ge2—O5	1.771 (3)	Fe1—O1	2.059 (3)
Ge3—O9	1.733 (3)	Fe1—O6	2.088 (3)
Ge3—O9^i	1.733 (3)	Cu1—O9^vi	1.925 (3)
Ge3—O3	1.747 (4)	Cu1—O4^v	1.932 (3)
Ge3—O5^ii	1.7541 (19)	Cu1—O9^v	1.951 (3)
Ge4—O2	1.730 (4)	Cu1—O7^iv	1.999 (3)
O1—Ge1—O4	114.75 (9)	O6^i—Ge4—O6	116.51 (18)
O1—Ge1—O4^i	114.75 (9)	O6^iii—Fe1—O7^iv	106.69 (10)
O4—Ge1—O4^i	107.94 (18)	O6^iii—Fe1—O4^v	114.17 (10)
O1—Ge1—O3	98.67 (18)	O7^iv—Fe1—O4^v	75.74 (10)
O4—Ge1—O3	110.21 (10)	O6^iii—Fe1—O8^v	92.21 (10)
O4^i—Ge1—O3	110.21 (10)	O7^iv—Fe1—O8^v	155.17 (13)
O2—Ge2—O7	113.46 (11)	O4^v—Fe1—O8^v	81.95 (12)
O2—Ge2—O7^i	113.46 (11)	O6^iii—Fe1—O1	146.34 (12)
O7—Ge2—O7^i	111.03 (18)	O7^iv—Fe1—O1	94.44 (10)
O2—Ge2—O5	99.50 (16)	O4^v—Fe1—O1	96.04 (13)
O7—Ge2—O5	109.35 (9)	O8^v—Fe1—O1	77.06 (9)
O7^i—Ge2—O5	109.35 (9)	O6^iii—Fe1—O6	72.85 (9)
O9—Ge3—O9^i	109.8 (2)	O7^iv—Fe1—O6	107.93 (11)
O9—Ge3—O3	108.75 (11)	O4^v—Fe1—O6	171.22 (9)
O9^i—Ge3—O3	108.75 (11)	O8^v—Fe1—O6	92.75 (13)
O9—Ge3—O5^ii	108.77 (11)	O1—Fe1—O6	75.88 (12)
O9^i—Ge3—O5^ii	108.77 (11)	O9^vi—Cu1—O4^v	178.10 (13)
O3—Ge3—O5^ii	111.97 (18)	O9^vi—Cu1—O9^v	77.56 (13)
O2—Ge4—O8	109.90 (19)	O4^v—Cu1—O9^v	101.72 (11)
O2—Ge4—O6^i	99.58 (11)	O9^vi—Cu1—O7^iv	102.37 (11)
O8—Ge4—O6^i	114.37 (9)	O4^v—Cu1—O7^iv	78.24 (11)
O2—Ge4—O6	99.58 (11)	O9^v—Cu1—O7^iv	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.

(cufege)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0291P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.021	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
107 parameters	Extinction coefficient: 0.0332 (9)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.740 (3)	Ge4—O8	1.744 (3)
Ge1—O4	1.748 (2)	Ge4—O6^i	1.753 (2)
Ge1—O4^i	1.748 (2)	Ge4—O6	1.753 (2)
Ge1—O3	1.772 (3)	Fe1—O6^iii	1.955 (2)
Ge2—O2	1.699 (3)	Fe1—O7^iv	2.004 (2)
Ge2—O7	1.746 (2)	Fe1—O4^v	2.037 (2)
Ge2—O7^i	1.746 (2)	Fe1—O8^v	2.0529 (19)
Ge2—O5	1.781 (3)	Fe1—O1	2.0592 (19)
Ge3—O9	1.734 (2)	Fe1—O6	2.089 (2)
Ge3—O9^i	1.734 (2)	Cu1—O9^vi	1.925 (2)
Ge3—O3	1.747 (3)	Cu1—O4^v	1.933 (2)
Ge3—O5^ii	1.748 (3)	Cu1—O9^v	1.952 (2)
Ge4—O2	1.727 (3)	Cu1—O7^iv	2.005 (2)
O1—Ge1—O4	115.02 (8)	O6^i—Ge4—O6	116.67 (15)
O1—Ge1—O4^i	115.02 (8)	O6^iii—Fe1—O7^iv	106.77 (9)
O4—Ge1—O4^i	107.82 (15)	O6^iii—Fe1—O4^v	114.24 (9)
O1—Ge1—O3	98.19 (15)	O7^iv—Fe1—O4^v	75.97 (9)
O4—Ge1—O3	110.22 (9)	O6^iii—Fe1—O8^v	92.17 (9)
O4^i—Ge1—O3	110.22 (9)	O7^iv—Fe1—O8^v	155.18 (11)
O2—Ge2—O7	113.36 (9)	O4^v—Fe1—O8^v	81.73 (11)
O2—Ge2—O7^i	113.36 (9)	O6^iii—Fe1—O1	146.68 (11)
O7—Ge2—O7^i	111.44 (15)	O7^iv—Fe1—O1	94.17 (9)
O2—Ge2—O5	99.47 (16)	O4^v—Fe1—O1	95.59 (11)
O7—Ge2—O5	109.23 (9)	O8^v—Fe1—O1	77.13 (9)
O7^i—Ge2—O5	109.23 (9)	O6^iii—Fe1—O6	72.70 (10)
O9—Ge3—O9^i	110.02 (17)	O7^iv—Fe1—O6	107.72 (9)
O9—Ge3—O3	108.74 (10)	O4^v—Fe1—O6	171.27 (9)
O9^i—Ge3—O3	108.74 (10)	O8^v—Fe1—O6	92.95 (11)
O9—Ge3—O5^ii	108.75 (9)	O1—Fe1—O6	76.40 (10)
O9^i—Ge3—O5^ii	108.75 (9)	O9^vi—Cu1—O4^v	178.02 (11)
O3—Ge3—O5^ii	111.83 (15)	O9^vi—Cu1—O9^v	77.61 (11)
O2—Ge4—O8	110.22 (16)	O4^v—Cu1—O9^v	101.72 (9)
O2—Ge4—O6^i	99.46 (9)	O9^vi—Cu1—O7^iv	102.25 (10)
O8—Ge4—O6^i	114.27 (8)	O4^v—Cu1—O7^iv	78.31 (9)
O2—Ge4—O6	99.46 (9)	O9^v—Cu1—O7^iv	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.

(cf9_050)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0272P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.025	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0268 (8)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.748 (5)	Ge4—O8	1.740 (5)
Ge1—O4	1.749 (3)	Ge4—O6^i	1.753 (3)
Ge1—O4^i	1.749 (3)	Ge4—O6	1.753 (3)
Ge1—O3	1.776 (4)	Fe1—O6^iii	1.956 (3)
Ge2—O2	1.698 (5)	Fe1—O7^iv	2.005 (3)
Ge2—O7	1.751 (3)	Fe1—O4^v	2.035 (3)
Ge2—O7^i	1.751 (3)	Fe1—O8^v	2.055 (3)
Ge2—O5	1.773 (5)	Fe1—O1	2.058 (3)
Ge3—O9	1.734 (3)	Fe1—O6	2.090 (3)
Ge3—O9^i	1.734 (3)	Cu1—O9^vi	1.923 (3)
Ge3—O3	1.745 (5)	Cu1—O4^v	1.937 (3)
Ge3—O5^ii	1.759 (5)	Cu1—O9^v	1.951 (3)
Ge4—O2	1.729 (4)	Cu1—O7^iv	1.999 (3)
O1—Ge1—O4	114.59 (12)	O6^i—Ge4—O6	116.7 (2)
O1—Ge1—O4^i	114.59 (12)	O6^iii—Fe1—O7^iv	106.86 (13)
O4—Ge1—O4^i	108.0 (2)	O6^iii—Fe1—O4^v	114.07 (14)
O1—Ge1—O3	98.6 (2)	O7^iv—Fe1—O4^v	75.84 (13)
O4—Ge1—O3	110.35 (12)	O6^iii—Fe1—O8^v	92.10 (13)
O4^i—Ge1—O3	110.35 (12)	O7^iv—Fe1—O8^v	155.07 (14)
O2—Ge2—O7	113.52 (13)	O4^v—Fe1—O8^v	81.76 (15)
O2—Ge2—O7^i	113.52 (13)	O6^iii—Fe1—O1	146.30 (14)
O7—Ge2—O7^i	111.3 (2)	O7^iv—Fe1—O1	94.38 (14)
O2—Ge2—O5	99.2 (2)	O4^v—Fe1—O1	96.09 (15)
O7—Ge2—O5	109.26 (13)	O8^v—Fe1—O1	77.11 (14)
O7^i—Ge2—O5	109.26 (13)	O6^iii—Fe1—O6	72.81 (15)
O9—Ge3—O9^i	109.9 (3)	O7^iv—Fe1—O6	107.83 (13)
O9—Ge3—O3	108.85 (13)	O4^v—Fe1—O6	171.33 (12)
O9^i—Ge3—O3	108.85 (13)	O8^v—Fe1—O6	92.97 (15)
O9—Ge3—O5^ii	108.75 (13)	O1—Fe1—O6	75.95 (14)
O9^i—Ge3—O5^ii	108.75 (13)	O9^vi—Cu1—O4^v	178.16 (16)
O3—Ge3—O5^ii	111.7 (2)	O9^vi—Cu1—O9^v	77.58 (16)
O2—Ge4—O8	110.1 (2)	O4^v—Cu1—O9^v	101.85 (13)
O2—Ge4—O6^i	99.51 (13)	O9^vi—Cu1—O7^iv	102.25 (14)
O8—Ge4—O6^i	114.25 (12)	O4^v—Cu1—O7^iv	78.21 (13)
O2—Ge4—O6	99.51 (13)	O9^v—Cu1—O7^iv	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.

(cf9_100)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0286P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.027	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0242 (8)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.746 (5)	Ge4—O8	1.743 (5)
Ge1—O4	1.748 (3)	Ge4—O6^i	1.750 (4)
Ge1—O4^i	1.748 (3)	Ge4—O6	1.750 (4)
Ge1—O3	1.771 (4)	Fe1—O6^iii	1.958 (2)
Ge2—O2	1.694 (5)	Fe1—O7^iv	2.007 (3)
Ge2—O7	1.747 (4)	Fe1—O4^v	2.035 (3)
Ge2—O7^i	1.747 (4)	Fe1—O8^v	2.054 (3)
Ge2—O5	1.776 (4)	Fe1—O1	2.060 (3)
Ge3—O9	1.735 (3)	Fe1—O6	2.093 (3)
Ge3—O9^i	1.735 (3)	Cu1—O9^vi	1.922 (3)
Ge3—O3	1.747 (4)	Cu1—O4^v	1.939 (3)
Ge3—O5^ii	1.756 (5)	Cu1—O9^v	1.949 (3)
Ge4—O2	1.729 (4)	Cu1—O7^iv	2.004 (3)
O1—Ge1—O4	114.65 (12)	O6^i—Ge4—O6	116.7 (2)
O1—Ge1—O4^i	114.65 (12)	O6^iii—Fe1—O7^iv	106.62 (11)
O4—Ge1—O4^i	107.9 (2)	O6^iii—Fe1—O4^v	114.04 (13)
O1—Ge1—O3	98.7 (2)	O7^iv—Fe1—O4^v	76.02 (10)
O4—Ge1—O3	110.29 (12)	O6^iii—Fe1—O8^v	92.19 (13)
O4^i—Ge1—O3	110.29 (12)	O7^iv—Fe1—O8^v	155.30 (12)
O2—Ge2—O7	113.38 (10)	O4^v—Fe1—O8^v	81.80 (15)
O2—Ge2—O7^i	113.38 (9)	O6^iii—Fe1—O1	146.38 (13)
O7—Ge2—O7^i	111.4 (2)	O7^iv—Fe1—O1	94.43 (13)
O2—Ge2—O5	99.4 (2)	O4^v—Fe1—O1	96.09 (15)
O7—Ge2—O5	109.29 (11)	O8^v—Fe1—O1	77.10 (14)
O7^i—Ge2—O5	109.29 (11)	O6^iii—Fe1—O6	72.94 (10)
O9—Ge3—O9^i	109.9 (3)	O7^iv—Fe1—O6	107.76 (10)
O9—Ge3—O3	108.76 (13)	O4^v—Fe1—O6	171.19 (11)
O9^i—Ge3—O3	108.76 (13)	O8^v—Fe1—O6	92.79 (15)
O9—Ge3—O5^ii	108.82 (13)	O1—Fe1—O6	75.83 (13)
O9^i—Ge3—O5^ii	108.82 (13)	O9^vi—Cu1—O4^v	178.09 (16)
O3—Ge3—O5^ii	111.8 (2)	O9^vi—Cu1—O9^v	77.53 (16)
O2—Ge4—O8	109.8 (2)	O4^v—Cu1—O9^v	101.82 (13)
O2—Ge4—O6^i	99.58 (13)	O9^vi—Cu1—O7^iv	102.27 (11)
O8—Ge4—O6^i	114.31 (12)	O4^v—Cu1—O7^iv	78.26 (10)
O2—Ge4—O6	99.58 (13)	O9^v—Cu1—O7^iv	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.

(cf9_200)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	6 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0372P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.028	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0257 (10)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.748 (5)	Ge4—O8	1.744 (2)
Ge1—O4	1.750 (3)	Ge4—O6^i	1.749 (3)
Ge1—O4^i	1.750 (3)	Ge4—O6	1.749 (3)
Ge1—O3	1.777 (5)	Fe1—O6^iii	1.960 (3)
Ge2—O2	1.692 (4)	Fe1—O7^iv	2.007 (3)
Ge2—O7	1.746 (4)	Fe1—O4^v	2.029 (3)
Ge2—O7^i	1.746 (4)	Fe1—O8^v	2.056 (3)
Ge2—O5	1.779 (5)	Fe1—O1	2.059 (3)
Ge3—O9	1.734 (3)	Fe1—O6	2.097 (3)
Ge3—O9^i	1.734 (3)	Cu1—O9^vi	1.924 (4)
Ge3—O3	1.746 (5)	Cu1—O4^v	1.938 (4)
Ge3—O5^ii	1.752 (5)	Cu1—O9^v	1.950 (4)
Ge4—O2	1.728 (3)	Cu1—O7^iv	2.007 (4)
O1—Ge1—O4	114.92 (12)	O6^i—Ge4—O6	116.6 (2)
O1—Ge1—O4^i	114.92 (12)	O6^iii—Fe1—O7^iv	106.38 (14)
O4—Ge1—O4^i	107.5 (2)	O6^iii—Fe1—O4^v	114.18 (13)
O1—Ge1—O3	98.4 (2)	O7^iv—Fe1—O4^v	76.02 (12)
O4—Ge1—O3	110.37 (13)	O6^iii—Fe1—O8^v	92.27 (13)
O4^i—Ge1—O3	110.37 (13)	O7^iv—Fe1—O8^v	155.40 (16)
O2—Ge2—O7	113.25 (13)	O4^v—Fe1—O8^v	81.81 (15)
O2—Ge2—O7^i	113.25 (13)	O6^iii—Fe1—O1	146.56 (14)
O7—Ge2—O7^i	111.4 (3)	O7^iv—Fe1—O1	94.51 (16)
O2—Ge2—O5	99.8 (2)	O4^v—Fe1—O1	95.83 (17)
O7—Ge2—O5	109.21 (14)	O8^v—Fe1—O1	77.12 (13)
O7^i—Ge2—O5	109.21 (14)	O6^iii—Fe1—O6	72.90 (11)
O9—Ge3—O9^i	110.1 (3)	O7^iv—Fe1—O6	107.84 (15)
O9—Ge3—O3	108.70 (15)	O4^v—Fe1—O6	171.08 (12)
O9^i—Ge3—O3	108.70 (15)	O8^v—Fe1—O6	92.72 (16)
O9—Ge3—O5^ii	108.83 (12)	O1—Fe1—O6	76.01 (15)
O9^i—Ge3—O5^ii	108.83 (12)	O9^vi—Cu1—O4^v	177.95 (18)
O3—Ge3—O5^ii	111.7 (2)	O9^vi—Cu1—O9^v	77.62 (14)
O2—Ge4—O8	109.4 (2)	O4^v—Cu1—O9^v	101.89 (14)
O2—Ge4—O6^i	99.80 (12)	O9^vi—Cu1—O7^iv	102.27 (12)
O8—Ge4—O6^i	114.37 (13)	O4^v—Cu1—O7^iv	78.09 (14)
O2—Ge4—O6	99.80 (12)	O9^v—Cu1—O7^iv	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.

(cf9_300)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	1 restraint
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0309P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.026	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0212 (8)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.749 (5)	Ge4—O8	1.741 (5)
Ge1—O4	1.753 (3)	Ge4—O6^i	1.749 (3)
Ge1—O4^i	1.753 (3)	Ge4—O6	1.749 (3)
Ge1—O3	1.775 (5)	Fe1—O6^iii	1.958 (3)
Ge2—O2	1.693 (5)	Fe1—O7^iv	2.009 (3)
Ge2—O7	1.744 (3)	Fe1—O4^v	2.033 (3)
Ge2—O7^i	1.744 (3)	Fe1—O8^v	2.061 (3)
Ge2—O5	1.776 (5)	Fe1—O1	2.061 (3)
Ge3—O9	1.736 (3)	Fe1—O6	2.101 (3)
Ge3—O9^i	1.736 (3)	Cu1—O9^vi	1.921 (3)
Ge3—O3	1.745 (5)	Cu1—O4^v	1.937 (3)
Ge3—O5^ii	1.754 (5)	Cu1—O9^v	1.949 (3)
Ge4—O2	1.723 (5)	Cu1—O7^iv	2.008 (3)
O1—Ge1—O4	114.77 (13)	O6^i—Ge4—O6	116.4 (2)
O1—Ge1—O4^i	114.77 (13)	O6^iii—Fe1—O7^iv	106.06 (14)
O4—Ge1—O4^i	108.0 (3)	O6^iii—Fe1—O4^v	114.02 (15)
O1—Ge1—O3	98.7 (2)	O7^iv—Fe1—O4^v	75.90 (14)
O4—Ge1—O3	110.14 (13)	O6^iii—Fe1—O8^v	92.33 (14)
O4^i—Ge1—O3	110.14 (13)	O7^iv—Fe1—O8^v	155.44 (16)
O2—Ge2—O7	113.35 (14)	O4^v—Fe1—O8^v	81.85 (16)
O2—Ge2—O7^i	113.35 (14)	O6^iii—Fe1—O1	146.44 (15)
O7—Ge2—O7^i	111.0 (3)	O7^iv—Fe1—O1	94.84 (14)
O2—Ge2—O5	99.9 (3)	O4^v—Fe1—O1	96.18 (17)
O7—Ge2—O5	109.27 (13)	O8^v—Fe1—O1	77.19 (15)
O7^i—Ge2—O5	109.27 (13)	O6^iii—Fe1—O6	72.88 (16)
O9—Ge3—O9^i	109.8 (3)	O7^iv—Fe1—O6	108.10 (14)
O9—Ge3—O3	108.76 (15)	O4^v—Fe1—O6	171.19 (13)
O9^i—Ge3—O3	108.76 (15)	O8^v—Fe1—O6	92.62 (17)
O9—Ge3—O5^ii	108.77 (15)	O1—Fe1—O6	75.82 (15)
O9^i—Ge3—O5^ii	108.77 (15)	O9^vi—Cu1—O4^v	178.23 (17)
O3—Ge3—O5^ii	112.0 (2)	O9^vi—Cu1—O9^v	77.55 (9)
O2—Ge4—O8	109.2 (3)	O4^v—Cu1—O9^v	102.00 (12)
O2—Ge4—O6^i	99.84 (14)	O9^vi—Cu1—O7^iv	102.23 (13)
O8—Ge4—O6^i	114.49 (13)	O4^v—Cu1—O7^iv	78.11 (14)
O2—Ge4—O6	99.84 (14)	O9^v—Cu1—O7^iv	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.

(cf9_400)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	3 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0335P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.028	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0211 (9)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.749 (5)	Ge4—O8	1.745 (6)
Ge1—O4	1.751 (3)	Ge4—O6^i	1.751 (4)
Ge1—O4^i	1.751 (3)	Ge4—O6	1.751 (4)
Ge1—O3	1.770 (5)	Fe1—O6^iii	1.955 (3)
Ge2—O2	1.690 (5)	Fe1—O7^iv	2.009 (4)
Ge2—O7	1.748 (4)	Fe1—O4^v	2.037 (4)
Ge2—O7^i	1.748 (4)	Fe1—O8^v	2.061 (4)
Ge2—O5	1.778 (5)	Fe1—O1	2.064 (4)
Ge3—O9	1.737 (4)	Fe1—O6	2.106 (4)
Ge3—O9^i	1.737 (4)	Cu1—O9^vi	1.919 (4)
Ge3—O3	1.747 (5)	Cu1—O4^v	1.939 (4)
Ge3—O5^ii	1.755 (4)	Cu1—O9^v	1.947 (4)
Ge4—O2	1.725 (4)	Cu1—O7^iv	2.009 (4)
O1—Ge1—O4	114.90 (13)	O6^i—Ge4—O6	116.5 (3)
O1—Ge1—O4^i	114.90 (13)	O6^iii—Fe1—O7^iv	106.08 (16)
O4—Ge1—O4^i	108.1 (3)	O6^iii—Fe1—O4^v	114.02 (16)
O1—Ge1—O3	98.6 (3)	O7^iv—Fe1—O4^v	75.90 (13)
O4—Ge1—O3	109.99 (14)	O6^iii—Fe1—O8^v	92.51 (16)
O4^i—Ge1—O3	109.99 (14)	O7^iv—Fe1—O8^v	155.23 (18)
O2—Ge2—O7	113.24 (16)	O4^v—Fe1—O8^v	81.68 (16)
O2—Ge2—O7^i	113.24 (15)	O6^iii—Fe1—O1	146.59 (18)
O7—Ge2—O7^i	111.3 (3)	O7^iv—Fe1—O1	94.68 (17)
O2—Ge2—O5	100.0 (2)	O4^v—Fe1—O1	96.07 (19)
O7—Ge2—O5	109.17 (13)	O8^v—Fe1—O1	77.20 (17)
O7^i—Ge2—O5	109.17 (13)	O6^iii—Fe1—O6	72.86 (18)
O9—Ge3—O9^i	109.6 (4)	O7^iv—Fe1—O6	108.13 (16)
O9—Ge3—O3	108.67 (17)	O4^v—Fe1—O6	171.18 (14)
O9^i—Ge3—O3	108.67 (17)	O8^v—Fe1—O6	92.73 (19)
O9—Ge3—O5^ii	108.88 (17)	O1—Fe1—O6	75.95 (18)
O9^i—Ge3—O5^ii	108.88 (17)	O9^vi—Cu1—O4^v	178.3 (2)
O3—Ge3—O5^ii	112.1 (3)	O9^vi—Cu1—O9^v	77.6 (2)
O2—Ge4—O8	109.1 (2)	O4^v—Cu1—O9^v	101.90 (16)
O2—Ge4—O6^i	99.90 (14)	O9^vi—Cu1—O7^iv	102.27 (17)
O8—Ge4—O6^i	114.46 (14)	O4^v—Cu1—O7^iv	78.14 (15)
O2—Ge4—O6	99.90 (14)	O9^v—Cu1—O7^iv	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.

(cf9_500)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	5 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0295P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.029	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0232 (8)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.749 (6)	Ge4—O8	1.742 (6)
Ge1—O4	1.750 (4)	Ge4—O6^i	1.750 (4)
Ge1—O4^i	1.750 (4)	Ge4—O6	1.750 (4)
Ge1—O3	1.776 (6)	Fe1—O6^iii	1.955 (3)
Ge2—O2	1.689 (6)	Fe1—O7^iv	2.009 (3)
Ge2—O7	1.748 (6)	Fe1—O4^v	2.041 (4)
Ge2—O7^i	1.748 (6)	Fe1—O8^v	2.065 (4)
Ge2—O5	1.778 (6)	Fe1—O1	2.066 (4)
Ge3—O9	1.738 (4)	Fe1—O6	2.111 (4)
Ge3—O9^i	1.738 (4)	Cu1—O9^vi	1.917 (4)
Ge3—O3	1.744 (2)	Cu1—O4^v	1.937 (4)
Ge3—O5^ii	1.755 (2)	Cu1—O9^v	1.947 (4)
Ge4—O2	1.724 (5)	Cu1—O7^iv	2.010 (4)
O1—Ge1—O4	115.00 (16)	O6^i—Ge4—O6	116.2 (3)
O1—Ge1—O4^i	115.00 (16)	O6^iii—Fe1—O7^iv	105.97 (16)
O4—Ge1—O4^i	108.2 (3)	O6^iii—Fe1—O4^v	114.02 (18)
O1—Ge1—O3	98.5 (2)	O7^iv—Fe1—O4^v	76.03 (12)
O4—Ge1—O3	109.85 (13)	O6^iii—Fe1—O8^v	92.59 (17)
O4^i—Ge1—O3	109.85 (13)	O7^iv—Fe1—O8^v	155.34 (15)
O2—Ge2—O7	113.10 (13)	O4^v—Fe1—O8^v	81.68 (19)
O2—Ge2—O7^i	113.10 (13)	O6^iii—Fe1—O1	146.69 (19)
O7—Ge2—O7^i	111.7 (3)	O7^iv—Fe1—O1	94.57 (17)
O2—Ge2—O5	100.2 (3)	O4^v—Fe1—O1	96.0 (2)
O7—Ge2—O5	109.02 (11)	O8^v—Fe1—O1	77.27 (18)
O7^i—Ge2—O5	109.02 (11)	O6^iii—Fe1—O6	72.88 (18)
O9—Ge3—O9^i	109.4 (4)	O7^iv—Fe1—O6	108.18 (13)
O9—Ge3—O3	108.86 (15)	O4^v—Fe1—O6	171.05 (15)
O9^i—Ge3—O3	108.86 (15)	O8^v—Fe1—O6	92.5 (2)
O9—Ge3—O5^ii	108.89 (17)	O1—Fe1—O6	75.94 (18)
O9^i—Ge3—O5^ii	108.89 (17)	O9^vi—Cu1—O4^v	178.4 (2)
O3—Ge3—O5^ii	111.9 (3)	O9^vi—Cu1—O9^v	77.44 (16)
O2—Ge4—O8	108.8 (3)	O4^v—Cu1—O9^v	101.89 (13)
O2—Ge4—O6^i	99.98 (17)	O9^vi—Cu1—O7^iv	102.21 (14)
O8—Ge4—O6^i	114.61 (15)	O4^v—Cu1—O7^iv	78.35 (13)
O2—Ge4—O6	99.98 (17)	O9^v—Cu1—O7^iv	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.

(cf9_550)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	3 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0246P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.027	(Δ/σ)max = 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0323 (9)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4	1.750 (4)	Ge4—O8	1.740 (6)
Ge1—O4^i	1.750 (4)	Ge4—O6^i	1.749 (4)
Ge1—O1	1.753 (6)	Ge4—O6	1.749 (4)
Ge1—O3	1.771 (5)	Fe1—O6^iii	1.958 (3)
Ge2—O2	1.689 (6)	Fe1—O7^iv	2.008 (4)
Ge2—O7	1.748 (4)	Fe1—O4^v	2.040 (4)
Ge2—O7^i	1.748 (4)	Fe1—O1	2.066 (4)
Ge2—O5	1.778 (5)	Fe1—O8^v	2.067 (4)
Ge3—O9	1.737 (4)	Fe1—O6	2.112 (4)
Ge3—O9^i	1.737 (4)	Cu1—O9^vi	1.915 (3)
Ge3—O3	1.745 (4)	Cu1—O4^v	1.938 (4)
Ge3—O5^ii	1.756 (4)	Cu1—O9^v	1.950 (3)
Ge4—O2	1.721 (5)	Cu1—O7^iv	2.010 (4)
O4—Ge1—O4^i	108.2 (3)	O6^i—Ge4—O6	116.1 (3)
O4—Ge1—O1	114.91 (15)	O6^iii—Fe1—O7^iv	105.75 (15)
O4^i—Ge1—O1	114.91 (15)	O6^iii—Fe1—O4^v	114.05 (17)
O4—Ge1—O3	109.84 (13)	O7^iv—Fe1—O4^v	75.93 (16)
O4^i—Ge1—O3	109.84 (13)	O6^iii—Fe1—O1	146.55 (18)
O1—Ge1—O3	98.7 (2)	O7^iv—Fe1—O1	94.89 (17)
O2—Ge2—O7	113.10 (17)	O4^v—Fe1—O1	96.16 (19)
O2—Ge2—O7^i	113.10 (17)	O6^iii—Fe1—O8^v	92.63 (16)
O7—Ge2—O7^i	111.2 (3)	O7^iv—Fe1—O8^v	155.34 (19)
O2—Ge2—O5	100.4 (2)	O4^v—Fe1—O8^v	81.66 (19)
O7—Ge2—O5	109.20 (14)	O1—Fe1—O8^v	77.24 (17)
O7^i—Ge2—O5	109.20 (14)	O6^iii—Fe1—O6	72.96 (18)
O9—Ge3—O9^i	109.2 (4)	O7^iv—Fe1—O6	108.29 (17)
O9—Ge3—O3	108.95 (17)	O4^v—Fe1—O6	170.97 (14)
O9^i—Ge3—O3	108.95 (17)	O1—Fe1—O6	75.71 (18)
O9—Ge3—O5^ii	108.83 (17)	O8^v—Fe1—O6	92.6 (2)
O9^i—Ge3—O5^ii	108.83 (17)	O9^vi—Cu1—O4^v	178.5 (2)
O3—Ge3—O5^ii	112.1 (3)	O9^vi—Cu1—O9^v	77.39 (10)
O2—Ge4—O8	108.7 (3)	O4^v—Cu1—O9^v	102.04 (14)
O2—Ge4—O6^i	100.15 (17)	O9^vi—Cu1—O7^iv	102.28 (15)
O8—Ge4—O6^i	114.60 (15)	O4^v—Cu1—O7^iv	78.20 (16)
O2—Ge4—O6	100.15 (17)	O9^v—Cu1—O7^iv	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.

(cf9_600)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	2 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0259P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.032	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0324 (10)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4^i	1.749 (5)	Ge4—O8	1.742 (7)
Ge1—O4	1.749 (5)	Ge4—O6^i	1.749 (4)
Ge1—O1	1.753 (6)	Ge4—O6	1.749 (4)
Ge1—O3	1.771 (6)	Fe1—O6^iii	1.956 (4)
Ge2—O2	1.691 (7)	Fe1—O7^iv	2.011 (4)
Ge2—O7	1.748 (5)	Fe1—O4^v	2.042 (5)
Ge2—O7^i	1.748 (5)	Fe1—O8^v	2.067 (4)
Ge2—O5	1.777 (6)	Fe1—O1	2.067 (4)
Ge3—O9	1.741 (4)	Fe1—O6	2.115 (5)
Ge3—O9^i	1.741 (4)	Cu1—O9^vi	1.914 (5)
Ge3—O3	1.745 (6)	Cu1—O4^v	1.940 (4)
Ge3—O5^ii	1.755 (4)	Cu1—O9^v	1.946 (4)
Ge4—O2	1.719 (6)	Cu1—O7^iv	2.012 (5)
O4^i—Ge1—O4	108.5 (3)	O6^i—Ge4—O6	116.0 (3)
O4^i—Ge1—O1	114.87 (18)	O6^iii—Fe1—O7^iv	105.79 (18)
O4—Ge1—O1	114.87 (18)	O6^iii—Fe1—O4^v	114.0 (2)
O4^i—Ge1—O3	109.71 (17)	O7^iv—Fe1—O4^v	76.08 (19)
O4—Ge1—O3	109.71 (17)	O6^iii—Fe1—O8^v	92.76 (19)
O1—Ge1—O3	98.7 (3)	O7^iv—Fe1—O8^v	155.3 (2)
O2—Ge2—O7	113.04 (19)	O4^v—Fe1—O8^v	81.6 (2)
O2—Ge2—O7^i	113.04 (19)	O6^iii—Fe1—O1	146.5 (2)
O7—Ge2—O7^i	111.8 (4)	O7^iv—Fe1—O1	94.7 (2)
O2—Ge2—O5	100.4 (3)	O4^v—Fe1—O1	96.3 (2)
O7—Ge2—O5	108.91 (16)	O8^v—Fe1—O1	77.27 (19)
O7^i—Ge2—O5	108.91 (16)	O6^iii—Fe1—O6	72.8 (2)
O9—Ge3—O9^i	109.4 (4)	O7^iv—Fe1—O6	108.2 (2)
O9—Ge3—O3	108.76 (19)	O4^v—Fe1—O6	171.05 (16)
O9^i—Ge3—O3	108.76 (19)	O8^v—Fe1—O6	92.5 (2)
O9—Ge3—O5^ii	108.84 (16)	O1—Fe1—O6	75.8 (2)
O9^i—Ge3—O5^ii	108.84 (16)	O9^vi—Cu1—O4^v	178.5 (2)
O3—Ge3—O5^ii	112.2 (3)	O9^vi—Cu1—O9^v	77.36 (18)
O2—Ge4—O8	108.7 (4)	O4^v—Cu1—O9^v	101.94 (19)
O2—Ge4—O6^i	100.1 (2)	O9^vi—Cu1—O7^iv	102.22 (15)
O8—Ge4—O6^i	114.62 (17)	O4^v—Cu1—O7^iv	78.39 (19)
O2—Ge4—O6	100.1 (2)	O9^v—Cu1—O7^iv	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.

(cf9_650)

Crystal data

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) Å^3	Prismatic, pale green
Z = 2	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0302P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.039	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.0417 (14)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O4	1.754 (6)	Ge4—O8	1.743 (8)
Ge1—O4^i	1.754 (6)	Ge4—O6^i	1.752 (6)
Ge1—O1	1.759 (8)	Ge4—O6	1.752 (6)
Ge1—O3	1.780 (8)	Fe1—O6^iii	1.964 (5)
Ge2—O2	1.688 (9)	Fe1—O7^iv	2.014 (6)
Ge2—O7	1.764 (6)	Fe1—O4^v	2.047 (6)
Ge2—O7^i	1.764 (6)	Fe1—O1	2.076 (6)
Ge2—O5	1.783 (9)	Fe1—O8^v	2.078 (5)
Ge3—O3	1.745 (8)	Fe1—O6	2.119 (6)
Ge3—O9	1.749 (7)	Cu1—O9^vi	1.932 (7)
Ge3—O9^i	1.749 (7)	Cu1—O9^v	1.941 (7)
Ge3—O5^ii	1.756 (9)	Cu1—O4^v	1.944 (6)
Ge4—O2	1.732 (8)	Cu1—O7^iv	2.005 (6)
O4—Ge1—O4^i	108.4 (4)	O6^i—Ge4—O6	115.7 (4)
O4—Ge1—O1	114.9 (2)	O6^iii—Fe1—O7^iv	105.6 (2)
O4^i—Ge1—O1	114.9 (2)	O6^iii—Fe1—O4^v	114.1 (3)
O4—Ge1—O3	109.6 (2)	O7^iv—Fe1—O4^v	75.6 (2)
O4^i—Ge1—O3	109.6 (2)	O6^iii—Fe1—O1	146.7 (3)
O1—Ge1—O3	98.9 (4)	O7^iv—Fe1—O1	94.9 (3)
O2—Ge2—O7	113.5 (2)	O4^v—Fe1—O1	96.1 (3)
O2—Ge2—O7^i	113.5 (2)	O6^iii—Fe1—O8^v	93.0 (2)
O7—Ge2—O7^i	110.9 (5)	O7^iv—Fe1—O8^v	154.9 (3)
O2—Ge2—O5	100.5 (5)	O4^v—Fe1—O8^v	81.6 (3)
O7—Ge2—O5	108.9 (3)	O1—Fe1—O8^v	77.3 (2)
O7^i—Ge2—O5	108.9 (3)	O6^iii—Fe1—O6	73.0 (3)
O3—Ge3—O9	108.3 (3)	O7^iv—Fe1—O6	109.0 (3)
O3—Ge3—O9^i	108.3 (3)	O4^v—Fe1—O6	170.7 (2)
O9—Ge3—O9^i	109.8 (6)	O1—Fe1—O6	75.7 (3)
O3—Ge3—O5^ii	112.4 (4)	O8^v—Fe1—O6	92.3 (3)
O9—Ge3—O5^ii	109.0 (3)	O9^vi—Cu1—O9^v	77.2 (4)
O9^i—Ge3—O5^ii	109.0 (3)	O9^vi—Cu1—O4^v	178.2 (3)
O2—Ge4—O8	108.9 (5)	O9^v—Cu1—O4^v	101.9 (3)
O2—Ge4—O6^i	100.1 (3)	O9^vi—Cu1—O7^iv	102.7 (3)
O8—Ge4—O6^i	114.8 (2)	O9^v—Cu1—O7^iv	176.5 (4)
O2—Ge4—O6	100.1 (3)	O4^v—Cu1—O7^iv	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.

(cf9_750)

Crystal data

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) Å^3	0.12 × 0.11 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0648P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.058	(Δ/σ)max < 0.001
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
110 parameters	Extinction coefficient: 0.055 (3)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ge1—O1	1.750 (14)	Ge4—O8	1.742 (8)
Ge1—O4	1.752 (6)	Ge4—O6^i	1.749 (8)
Ge1—O4^i	1.752 (6)	Ge4—O6	1.749 (8)
Ge1—O3	1.776 (14)	Fe1—O6^iii	1.956 (6)
Ge2—O2	1.684 (8)	Fe1—O7^iv	2.010 (9)
Ge2—O7	1.747 (10)	Fe1—O4^v	2.047 (6)
Ge2—O7^i	1.747 (10)	Fe1—O1	2.073 (9)
Ge2—O5	1.777 (3)	Fe1—O8^v	2.074 (6)
Ge3—O9	1.741 (9)	Fe1—O6	2.125 (6)
Ge3—O9^i	1.741 (9)	Cu1—O9^vi	1.915 (4)
Ge3—O3	1.743 (9)	Cu1—O4^v	1.940 (9)
Ge3—O5^ii	1.754 (3)	Cu1—O9^v	1.944 (9)
Ge4—O2	1.720 (8)	Cu1—O7^iv	2.015 (10)
O1—Ge1—O4	114.8 (3)	O6^i—Ge4—O6	115.8 (7)
O1—Ge1—O4^i	114.8 (3)	O6^iii—Fe1—O7^iv	105.7 (4)
O4—Ge1—O4^i	109.4 (6)	O6^iii—Fe1—O4^v	113.7 (3)
O1—Ge1—O3	98.4 (5)	O7^iv—Fe1—O4^v	76.2 (3)
O4—Ge1—O3	109.39 (16)	O6^iii—Fe1—O1	146.8 (4)
O4^i—Ge1—O3	109.39 (15)	O7^iv—Fe1—O1	94.5 (4)
O2—Ge2—O7	112.8 (4)	O4^v—Fe1—O1	96.3 (5)
O2—Ge2—O7^i	112.8 (4)	O6^iii—Fe1—O8^v	92.7 (3)
O7—Ge2—O7^i	112.1 (8)	O7^iv—Fe1—O8^v	155.7 (5)
O2—Ge2—O5	100.9 (2)	O4^v—Fe1—O8^v	81.9 (4)
O7—Ge2—O5	108.8 (3)	O1—Fe1—O8^v	77.2 (3)
O7^i—Ge2—O5	108.8 (3)	O6^iii—Fe1—O6	72.9 (2)
O9—Ge3—O9^i	109.0 (6)	O7^iv—Fe1—O6	108.4 (4)
O9—Ge3—O3	108.9 (3)	O4^v—Fe1—O6	171.1 (3)
O9^i—Ge3—O3	108.9 (3)	O1—Fe1—O6	75.9 (4)
O9—Ge3—O5^ii	108.92 (18)	O8^v—Fe1—O6	91.9 (5)
O9^i—Ge3—O5^ii	108.92 (18)	O9^vi—Cu1—O4^v	178.8 (4)
O3—Ge3—O5^ii	112.1 (5)	O9^vi—Cu1—O9^v	77.17 (15)
O2—Ge4—O8	108.0 (5)	O4^v—Cu1—O9^v	102.12 (17)
O2—Ge4—O6^i	100.35 (16)	O9^vi—Cu1—O7^iv	102.1 (3)
O8—Ge4—O6^i	114.9 (3)	O4^v—Cu1—O7^iv	78.5 (3)
O2—Ge4—O6	100.35 (16)	O9^v—Cu1—O7^iv	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.