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CaCuGe2O6 shows a strongly distorted clinopyroxene-type structure with P21/c symmetry at 298 K. The Cu2+ ion at the M1 site is coordinated by six O atoms forming an octahedron, which deviates significantly from ideal geometry. Individual M1 sites are connected via common edges to form an infinite zigzag chain parallel to the crystallographic c axis. The Ca2+ ion at M2 shows a sevenfold coordination. M2 sites are connected to the M1 chain via three common edges, thereby forming a metal layer within the bc plane. Besides the strong Jahn-Teller distortion of the Cu site, the structure of the title compound differs from `normal' clinopyroxenes by a distortion of alternate layers of Ge sites. While the Ge(A) site is fourfold coordinated by O atoms, forming infinite chains of corner-sharing chains parallel to the c axis, the Ge(B) site exhibits a fivefold coordination, thereby forming a true two-dimensional layer of edge-sharing GeO5 bipyramids. Decreasing the temperature causes a magnetic phase transition at 40 K, as monitored by a broad maximum in the magnetic susceptibility and by discontinuities in the lattice parameters. Increasing the temperature causes variations in bond lengths, edge lengths and bond angles. Most prominent is the increase of one bond length of the Ge(B) site and the increase of the tetrahedral bridging angle of the Ge(A) site. At 660 K a crystallographic phase transition is observed where the symmetry changes from P21/c to C2/c. The transition is accompanied by large changes in the lattice parameters which are indicative of distinct topological changes of several structural building units. The high-temperature C2/c structure is similar to that of the germanate clinopyroxene CaMgGe2O6.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105013455/ws5021sup1.cif Contains datablocks global, cacu_100K, cacu_150K, cacu_200K, cacu_250, cacu_298K, cacu_328K, cacu_361K, cacu_470K, cacu_570K, cacu_612K, cacu_629K, cacu_646K, cacu_654K, cacu_717K, cacu_729K, cacu_763K, cacu_796K |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021100Ksup2.fcf Contains datablock cacu_100 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021150Ksup3.fcf Contains datablock cacu_150 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021200Ksup4.fcf Contains datablock cacu_200 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021250Ksup5.fcf Contains datablock cacu_250 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021298Ksup6.fcf Contains datablock cacu_rt |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021328Ksup7.fcf Contains datablock cacu3_060 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021361Ksup8.fcf Contains datablock cacu3_100 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021470Ksup9.fcf Contains datablock cacu3_230 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021570Ksup10.fcf Contains datablock cacu3_350 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021612Ksup11.fcf Contains datablock cacu3_400 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021629Ksup12.fcf Contains datablock cacu3_420 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021646Ksup13.fcf Contains datablock cacu3_440 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021654Ksup14.fcf Contains datablock cacu3_450 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021717Ksup15.fcf Contains datablock cacu3_525 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021729Ksup16.fcf Contains datablock cacu3_540 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021763Ksup17.fcf Contains datablock cacu3_580 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768105013455/ws5021796Ksup18.fcf Contains datablock cacu3_630 |
For all compounds, data collection: Stoe X-AREA (Stoe & Cie, 1998); cell refinement: Stoe X-AREA (Stoe & Cie, 1998); data reduction: Stoe X-AREA (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Diamond 2.0e (Berndt & Brandenburg, 1996); software used to prepare material for publication: WinGX 1.64.05 (Farrugia, 1999).
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.892 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6685 reflections |
a = 10.1798 (12) Å | θ = 2.2–32.1° |
b = 9.1869 (7) Å | µ = 18.22 mm−1 |
c = 5.1978 (6) Å | T = 100 K |
β = 105.614 (12)° | Cuboid, pale green |
V = 468.16 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 2 diffractometer | 1616 independent reflections |
Plane graphite monochromator | 1415 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.039 |
rotation method scans | θmax = 32.2°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) ? | h = −15→15 |
Tmin = 0.097, Tmax = 0.150 | k = −13→13 |
5815 measured reflections | l = −7→7 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0229P)2 + 1.6631P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max < 0.001 |
wR(F2) = 0.056 | Δρmax = 0.80 e Å−3 |
S = 1.06 | Δρmin = −0.91 e Å−3 |
1616 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0091 (6) |
Crystal data top
CaCuGe2O6 | V = 468.16 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1798 (12) Å | µ = 18.22 mm−1 |
b = 9.1869 (7) Å | T = 100 K |
c = 5.1978 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.614 (12)° | |
Data collection top
STOE IPDS 2 diffractometer | 1616 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 1415 reflections with I > 2σ(I) |
Tmin = 0.097, Tmax = 0.150 | Rint = 0.039 |
5815 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.025 | 92 parameters |
wR(F2) = 0.056 | 0 restraints |
S = 1.06 | Δρmax = 0.80 e Å−3 |
1616 reflections | Δρmin = −0.91 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28387 (6) | 0.45280 (7) | 0.81060 (13) | 0.00915 (12) | |
Cu | 0.22729 (4) | 0.66186 (4) | 0.25667 (8) | 0.00821 (9) | |
GeA | 0.04922 (3) | 0.34927 (3) | 0.20904 (7) | 0.00753 (9) | |
GeB | 0.49134 (3) | 0.35095 (3) | 0.40437 (7) | 0.00778 (9) | |
O1A | −0.1274 (2) | 0.3619 (3) | 0.1155 (5) | 0.0100 (4) | |
O1B | 0.6584 (2) | 0.3197 (2) | 0.3777 (5) | 0.0095 (4) | |
O2A | 0.1465 (2) | 0.4888 (3) | 0.3774 (5) | 0.0111 (4) | |
O2B | 0.4326 (2) | 0.5225 (2) | 0.2629 (5) | 0.0098 (4) | |
O3A | 0.1028 (2) | 0.1936 (2) | 0.4183 (5) | 0.0102 (4) | |
O3B | 0.3994 (2) | 0.2514 (2) | 0.5919 (5) | 0.0094 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0082 (2) | 0.0091 (2) | 0.0098 (3) | 0.00001 (19) | 0.00183 (18) | 0.00048 (19) |
Cu | 0.00767 (16) | 0.00815 (16) | 0.00798 (17) | −0.00054 (12) | 0.00067 (12) | −0.00010 (13) |
GeA | 0.00645 (14) | 0.00756 (14) | 0.00815 (15) | −0.00009 (10) | 0.00121 (10) | −0.00019 (10) |
GeB | 0.00704 (14) | 0.00741 (14) | 0.00886 (15) | −0.00010 (10) | 0.00207 (10) | 0.00037 (10) |
O1A | 0.0071 (9) | 0.0116 (10) | 0.0106 (10) | −0.0003 (7) | 0.0011 (7) | −0.0008 (8) |
O1B | 0.0072 (9) | 0.0097 (9) | 0.0110 (10) | 0.0006 (7) | 0.0016 (7) | −0.0005 (8) |
O2A | 0.0123 (10) | 0.0086 (9) | 0.0108 (10) | −0.0024 (7) | 0.0004 (8) | −0.0002 (8) |
O2B | 0.0112 (9) | 0.0075 (9) | 0.0104 (10) | 0.0005 (7) | 0.0022 (8) | 0.0003 (8) |
O3A | 0.0115 (9) | 0.0105 (9) | 0.0094 (10) | 0.0017 (8) | 0.0041 (8) | 0.0019 (8) |
O3B | 0.0083 (9) | 0.0114 (10) | 0.0092 (10) | −0.0008 (7) | 0.0031 (7) | 0.0005 (8) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (3) | GeA—Caviii | 3.6828 (8) |
Ca—O1Ai | 2.432 (2) | GeB—O1B | 1.767 (2) |
Ca—O1Bii | 2.445 (2) | GeB—O2B | 1.774 (2) |
Ca—O3Aiii | 2.465 (2) | GeB—O3B | 1.776 (2) |
Ca—O3Biii | 2.473 (2) | GeB—O3Bx | 1.892 (2) |
Ca—O2Biv | 2.512 (2) | GeB—O2Bii | 2.055 (2) |
Ca—O3B | 2.612 (2) | GeB—GeBii | 2.9026 (7) |
Ca—O2Bii | 3.021 (2) | GeB—Cuii | 2.9335 (7) |
Ca—Cuiv | 3.1804 (8) | GeB—Caii | 3.3334 (7) |
Ca—GeBii | 3.3334 (7) | GeB—Caviii | 3.3694 (9) |
Ca—GeBiv | 3.3694 (9) | GeB—Cax | 3.4542 (7) |
Ca—Cu | 3.3790 (8) | O1A—Cuv | 1.940 (2) |
Cu—O1Av | 1.940 (2) | O1A—Cuxi | 2.284 (2) |
Cu—O1Bii | 1.950 (2) | O1A—Cai | 2.432 (2) |
Cu—O2A | 1.969 (2) | O1B—Cuii | 1.950 (2) |
Cu—O1Bvi | 2.093 (2) | O1B—Cuxii | 2.093 (2) |
Cu—O1Avii | 2.284 (2) | O1B—Caii | 2.445 (2) |
Cu—GeBii | 2.9335 (7) | O2B—GeBii | 2.055 (2) |
Cu—Caviii | 3.1804 (8) | O2B—Caviii | 2.512 (2) |
Cu—Caix | 3.5855 (8) | O2B—Caii | 3.021 (2) |
GeA—O2A | 1.710 (2) | O3A—GeAiii | 1.783 (2) |
GeA—O1A | 1.735 (2) | O3A—Cax | 2.465 (2) |
GeA—O3Ax | 1.783 (2) | O3B—GeBiii | 1.892 (2) |
GeA—O3A | 1.790 (2) | O3B—Cax | 2.473 (2) |
GeA—Cax | 3.6065 (7) | | |
| | | |
O2A—Ca—O1Ai | 78.77 (8) | O1A—GeA—O3Ax | 107.89 (11) |
O2A—Ca—O1Bii | 68.82 (8) | O2A—GeA—O3A | 104.37 (11) |
O1Ai—Ca—O1Bii | 72.73 (8) | O1A—GeA—O3A | 110.29 (11) |
O2A—Ca—O3Aiii | 90.34 (8) | O3Ax—GeA—O3A | 103.05 (8) |
O1Ai—Ca—O3Aiii | 77.54 (8) | O2A—GeA—Ca | 35.00 (8) |
O1Bii—Ca—O3Aiii | 146.31 (8) | O1A—GeA—Ca | 129.47 (8) |
O2A—Ca—O3Biii | 138.12 (8) | O3Ax—GeA—Ca | 121.60 (8) |
O1Ai—Ca—O3Biii | 131.70 (8) | O3A—GeA—Ca | 69.69 (8) |
O1Bii—Ca—O3Biii | 139.26 (8) | O2A—GeA—Cax | 103.44 (8) |
O3Aiii—Ca—O3Biii | 73.60 (8) | O1A—GeA—Cax | 133.47 (8) |
O2A—Ca—O2Biv | 157.05 (8) | O3Ax—GeA—Cax | 67.20 (8) |
O1Ai—Ca—O2Biv | 85.93 (8) | O3A—GeA—Cax | 38.30 (7) |
O1Bii—Ca—O2Biv | 90.43 (8) | Ca—GeA—Cax | 79.24 (2) |
O3Aiii—Ca—O2Biv | 103.04 (8) | O2A—GeA—Caviii | 73.75 (9) |
O3Biii—Ca—O2Biv | 64.48 (8) | O1A—GeA—Caviii | 127.22 (8) |
O2A—Ca—O3B | 84.46 (8) | O3Ax—GeA—Caviii | 35.71 (7) |
O1Ai—Ca—O3B | 162.91 (8) | O3A—GeA—Caviii | 114.23 (7) |
O1Bii—Ca—O3B | 104.27 (8) | Ca—GeA—Caviii | 92.406 (18) |
O3Aiii—Ca—O3B | 99.45 (8) | Cax—GeA—Caviii | 77.100 (19) |
O3Biii—Ca—O3B | 61.41 (3) | O1B—GeB—O2B | 109.65 (11) |
O2Biv—Ca—O3B | 111.06 (8) | O1B—GeB—O3B | 128.31 (11) |
O2A—Ca—O2Bii | 102.26 (8) | O2B—GeB—O3B | 121.10 (11) |
O1Ai—Ca—O2Bii | 131.03 (7) | O1B—GeB—O3Bx | 96.66 (10) |
O1Bii—Ca—O2Bii | 62.91 (7) | O2B—GeB—O3Bx | 92.97 (10) |
O3Aiii—Ca—O2Bii | 150.26 (7) | O3B—GeB—O3Bx | 90.19 (7) |
O3Biii—Ca—O2Bii | 79.22 (7) | O1B—GeB—O2Bii | 90.30 (10) |
O2Biv—Ca—O2Bii | 75.14 (8) | O2B—GeB—O2Bii | 81.66 (11) |
O3B—Ca—O2Bii | 55.97 (7) | O3B—GeB—O2Bii | 87.96 (10) |
O2A—Ca—Cuiv | 116.04 (6) | O3Bx—GeB—O2Bii | 172.36 (9) |
O1Ai—Ca—Cuiv | 37.55 (6) | O1B—GeB—GeBii | 102.08 (8) |
O1Bii—Ca—Cuiv | 83.44 (6) | O2B—GeB—GeBii | 44.46 (8) |
O3Aiii—Ca—Cuiv | 82.57 (6) | O3B—GeB—GeBii | 106.88 (8) |
O3Biii—Ca—Cuiv | 100.24 (6) | O3Bx—GeB—GeBii | 137.16 (7) |
O2Biv—Ca—Cuiv | 49.13 (5) | O2Bii—GeB—GeBii | 37.20 (6) |
O3B—Ca—Cuiv | 159.45 (6) | O1B—GeB—Cuii | 40.15 (8) |
O2Bii—Ca—Cuiv | 114.43 (5) | O2B—GeB—Cuii | 116.78 (8) |
O2A—Ca—GeBii | 83.51 (6) | O3B—GeB—Cuii | 102.90 (7) |
O1Ai—Ca—GeBii | 102.27 (6) | O3Bx—GeB—Cuii | 132.30 (7) |
O1Bii—Ca—GeBii | 31.03 (5) | O2Bii—GeB—Cuii | 55.33 (6) |
O3Aiii—Ca—GeBii | 173.74 (6) | GeBii—GeB—Cuii | 82.684 (16) |
O3Biii—Ca—GeBii | 110.38 (6) | O1B—GeB—Caii | 45.52 (8) |
O2Biv—Ca—GeBii | 83.15 (6) | O2B—GeB—Caii | 64.27 (7) |
O3B—Ca—GeBii | 78.87 (5) | O3B—GeB—Caii | 166.72 (8) |
O2Bii—Ca—GeBii | 31.94 (4) | O3Bx—GeB—Caii | 101.92 (7) |
Cuiv—Ca—GeBii | 101.13 (2) | O2Bii—GeB—Caii | 80.72 (7) |
O2A—Ca—GeBiv | 171.42 (6) | GeBii—GeB—Caii | 67.705 (16) |
O1Ai—Ca—GeBiv | 108.99 (6) | Cuii—GeB—Caii | 64.889 (16) |
O1Bii—Ca—GeBiv | 116.43 (6) | O1B—GeB—Caviii | 110.64 (8) |
O3Aiii—Ca—GeBiv | 87.89 (6) | O2B—GeB—Caviii | 46.77 (8) |
O3Biii—Ca—GeBiv | 33.54 (6) | O3B—GeB—Caviii | 110.66 (8) |
O2Biv—Ca—GeBiv | 30.96 (5) | O3Bx—GeB—Caviii | 46.24 (7) |
O3B—Ca—GeBiv | 87.55 (5) | O2Bii—GeB—Caviii | 127.97 (7) |
O2Bii—Ca—GeBiv | 75.64 (5) | GeBii—GeB—Caviii | 90.975 (18) |
Cuiv—Ca—GeBiv | 72.048 (17) | Cuii—GeB—Caviii | 146.230 (18) |
GeBii—Ca—GeBiv | 98.026 (19) | Caii—GeB—Caviii | 81.974 (19) |
O2A—Ca—Cu | 34.55 (6) | O1B—GeB—Cax | 115.00 (8) |
O1Ai—Ca—Cu | 76.59 (6) | O2B—GeB—Cax | 122.28 (8) |
O1Bii—Ca—Cu | 34.66 (6) | O3B—GeB—Cax | 43.01 (8) |
O3Aiii—Ca—Cu | 122.50 (6) | O3Bx—GeB—Cax | 48.33 (7) |
O3Biii—Ca—Cu | 151.62 (6) | O2Bii—GeB—Cax | 130.81 (7) |
O2Biv—Ca—Cu | 125.03 (6) | GeBii—GeB—Cax | 142.09 (2) |
O3B—Ca—Cu | 91.45 (6) | Cuii—GeB—Cax | 120.893 (17) |
O2Bii—Ca—Cu | 78.41 (5) | Caii—GeB—Cax | 146.981 (15) |
Cuiv—Ca—Cu | 104.78 (2) | Caviii—GeB—Cax | 83.48 (2) |
GeBii—Ca—Cu | 51.823 (15) | O1B—GeB—Ca | 147.42 (8) |
GeBiv—Ca—Cu | 149.25 (2) | O2B—GeB—Ca | 79.70 (8) |
O1Av—Cu—O1Bii | 175.12 (9) | O3B—GeB—Ca | 46.56 (8) |
O1Av—Cu—O2A | 94.30 (10) | O3Bx—GeB—Ca | 114.36 (7) |
O1Bii—Cu—O2A | 87.15 (10) | O2Bii—GeB—Ca | 59.46 (6) |
O1Av—Cu—O1Bvi | 86.26 (10) | GeBii—GeB—Ca | 62.028 (15) |
O1Bii—Cu—O1Bvi | 91.47 (9) | Cuii—GeB—Ca | 107.412 (18) |
O2A—Cu—O1Bvi | 169.49 (9) | Caii—GeB—Ca | 129.733 (14) |
O1Av—Cu—O1Avii | 103.03 (9) | Caviii—GeB—Ca | 98.477 (19) |
O1Bii—Cu—O1Avii | 80.92 (9) | Cax—GeB—Ca | 81.688 (19) |
O2A—Cu—O1Avii | 107.46 (9) | GeA—O1A—Cuv | 119.84 (13) |
O1Bvi—Cu—O1Avii | 82.57 (9) | GeA—O1A—Cuxi | 111.93 (11) |
O1Av—Cu—GeBii | 139.41 (7) | Cuv—O1A—Cuxi | 92.55 (9) |
O1Bii—Cu—GeBii | 35.74 (7) | GeA—O1A—Cai | 132.53 (12) |
O2A—Cu—GeBii | 101.56 (7) | Cuv—O1A—Cai | 92.65 (9) |
O1Bvi—Cu—GeBii | 71.80 (6) | Cuxi—O1A—Cai | 98.93 (8) |
O1Avii—Cu—GeBii | 107.27 (6) | GeB—O1B—Cuii | 104.10 (12) |
O1Av—Cu—Caviii | 49.80 (7) | GeB—O1B—Cuxii | 140.53 (13) |
O1Bii—Cu—Caviii | 125.83 (7) | Cuii—O1B—Cuxii | 98.40 (10) |
O2A—Cu—Caviii | 85.29 (7) | GeB—O1B—Caii | 103.45 (10) |
O1Bvi—Cu—Caviii | 87.09 (7) | Cuii—O1B—Caii | 99.86 (9) |
O1Avii—Cu—Caviii | 151.66 (6) | Cuxii—O1B—Caii | 104.10 (9) |
GeBii—Cu—Caviii | 94.274 (19) | GeA—O2A—Cu | 132.57 (14) |
O1Av—Cu—Ca | 135.14 (7) | GeA—O2A—Ca | 120.13 (12) |
O1Bii—Cu—Ca | 45.48 (7) | Cu—O2A—Ca | 103.23 (10) |
O2A—Cu—Ca | 42.22 (7) | GeB—O2B—GeBii | 98.34 (11) |
O1Bvi—Cu—Ca | 134.07 (7) | GeB—O2B—Caviii | 102.27 (10) |
O1Avii—Cu—Ca | 101.33 (6) | GeBii—O2B—Caviii | 158.05 (11) |
GeBii—Cu—Ca | 63.289 (16) | GeB—O2B—Caii | 83.79 (8) |
Caviii—Cu—Ca | 104.78 (2) | GeBii—O2B—Caii | 84.68 (8) |
O1Av—Cu—Caix | 102.66 (7) | Caviii—O2B—Caii | 104.86 (8) |
O1Bii—Cu—Caix | 78.28 (7) | GeAiii—O3A—GeA | 125.37 (13) |
O2A—Cu—Caix | 147.62 (7) | GeAiii—O3A—Cax | 119.32 (11) |
O1Bvi—Cu—Caix | 41.41 (6) | GeA—O3A—Cax | 114.95 (11) |
O1Avii—Cu—Caix | 42.07 (6) | GeB—O3B—GeBiii | 121.02 (12) |
GeBii—Cu—Caix | 83.242 (15) | GeB—O3B—Cax | 107.66 (11) |
Caviii—Cu—Caix | 126.61 (2) | GeBiii—O3B—Cax | 100.21 (10) |
Ca—Cu—Caix | 120.51 (2) | GeB—O3B—Ca | 103.86 (10) |
O2A—GeA—O1A | 120.46 (11) | GeBiii—O3B—Ca | 98.92 (10) |
O2A—GeA—O3Ax | 109.41 (11) | Cax—O3B—Ca | 126.62 (9) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.887 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6671 reflections |
a = 10.1822 (12) Å | θ = 2.2–32.1° |
b = 9.1912 (7) Å | µ = 18.29 mm−1 |
c = 5.1995 (6) Å | T = 150 K |
β = 105.636 (12)° | Cuboid, pale green |
V = 468.60 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 2 diffractometer | 1626 independent reflections |
Plane graphite monochromator | 1416 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.040 |
rotation method scans | θmax = 32.2°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −15→15 |
Tmin = 0.097, Tmax = 0.150 | k = −13→13 |
5820 measured reflections | l = −7→7 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0237P)2 + 1.8196P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max = 0.001 |
wR(F2) = 0.061 | Δρmax = 0.88 e Å−3 |
S = 1.08 | Δρmin = −0.90 e Å−3 |
1626 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0094 (6) |
Crystal data top
CaCuGe2O6 | V = 468.60 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1822 (12) Å | µ = 18.29 mm−1 |
b = 9.1912 (7) Å | T = 150 K |
c = 5.1995 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.636 (12)° | |
Data collection top
STOE IPDS 2 diffractometer | 1626 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 1416 reflections with I > 2σ(I) |
Tmin = 0.097, Tmax = 0.150 | Rint = 0.040 |
5820 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.027 | 92 parameters |
wR(F2) = 0.061 | 0 restraints |
S = 1.08 | Δρmax = 0.88 e Å−3 |
1626 reflections | Δρmin = −0.90 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28369 (6) | 0.45272 (7) | 0.81034 (14) | 0.00973 (13) | |
Cu | 0.22723 (4) | 0.66177 (4) | 0.25661 (8) | 0.00880 (10) | |
GeA | 0.04923 (3) | 0.34921 (4) | 0.20908 (7) | 0.00786 (9) | |
GeB | 0.49129 (3) | 0.35094 (4) | 0.40383 (7) | 0.00822 (9) | |
O1A | −0.1271 (2) | 0.3617 (3) | 0.1151 (5) | 0.0099 (4) | |
O1B | 0.6586 (2) | 0.3198 (3) | 0.3780 (5) | 0.0089 (4) | |
O2A | 0.1462 (3) | 0.4887 (3) | 0.3772 (5) | 0.0121 (4) | |
O2B | 0.4325 (3) | 0.5225 (3) | 0.2624 (5) | 0.0112 (4) | |
O3A | 0.1030 (2) | 0.1940 (3) | 0.4185 (5) | 0.0102 (4) | |
O3B | 0.3992 (2) | 0.2511 (3) | 0.5906 (5) | 0.0101 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0090 (3) | 0.0100 (3) | 0.0095 (3) | −0.0001 (2) | 0.0013 (2) | 0.0005 (2) |
Cu | 0.00836 (17) | 0.00903 (17) | 0.00795 (18) | −0.00077 (13) | 0.00040 (13) | −0.00003 (14) |
GeA | 0.00674 (15) | 0.00861 (15) | 0.00763 (16) | −0.00042 (10) | 0.00091 (11) | −0.00036 (11) |
GeB | 0.00737 (15) | 0.00818 (15) | 0.00895 (16) | 0.00010 (10) | 0.00192 (11) | 0.00042 (11) |
O1A | 0.0074 (9) | 0.0117 (10) | 0.0098 (11) | 0.0000 (8) | 0.0010 (8) | −0.0006 (8) |
O1B | 0.0062 (9) | 0.0107 (10) | 0.0095 (10) | 0.0011 (7) | 0.0017 (7) | 0.0002 (8) |
O2A | 0.0122 (10) | 0.0102 (10) | 0.0119 (11) | −0.0024 (8) | −0.0001 (8) | −0.0010 (9) |
O2B | 0.0139 (10) | 0.0089 (10) | 0.0100 (11) | 0.0006 (8) | 0.0017 (8) | 0.0000 (8) |
O3A | 0.0108 (10) | 0.0106 (10) | 0.0100 (11) | 0.0024 (8) | 0.0042 (8) | 0.0020 (8) |
O3B | 0.0094 (10) | 0.0112 (10) | 0.0096 (11) | −0.0018 (8) | 0.0026 (8) | 0.0017 (8) |
Geometric parameters (Å, º) top
Ca—O2A | 2.333 (3) | GeA—Caviii | 3.6838 (8) |
Ca—O1Ai | 2.436 (2) | GeB—O1B | 1.768 (2) |
Ca—O1Bii | 2.447 (3) | GeB—O2B | 1.774 (2) |
Ca—O3Aiii | 2.465 (2) | GeB—O3B | 1.776 (2) |
Ca—O3Biii | 2.468 (3) | GeB—O3Bx | 1.894 (2) |
Ca—O2Biv | 2.512 (3) | GeB—O2Bii | 2.060 (3) |
Ca—O3B | 2.617 (3) | GeB—GeBii | 2.9059 (7) |
Ca—O2Bii | 3.022 (3) | GeB—Cuii | 2.9356 (7) |
Ca—Cuiv | 3.1820 (8) | GeB—Caii | 3.3350 (8) |
Ca—GeBii | 3.3350 (8) | GeB—Caviii | 3.3690 (9) |
Ca—GeBiv | 3.3690 (9) | GeB—Cax | 3.4555 (8) |
Ca—Cu | 3.3792 (8) | O1A—Cuv | 1.939 (3) |
Cu—O1Av | 1.939 (3) | O1A—Cuxi | 2.286 (2) |
Cu—O1Bii | 1.949 (2) | O1A—Cai | 2.436 (2) |
Cu—O2A | 1.970 (3) | O1B—Cuii | 1.949 (2) |
Cu—O1Bvi | 2.095 (2) | O1B—Cuxii | 2.095 (2) |
Cu—O1Avii | 2.286 (2) | O1B—Caii | 2.447 (3) |
Cu—GeBii | 2.9356 (7) | O2B—GeBii | 2.060 (3) |
Cu—Caviii | 3.1820 (8) | O2B—Caviii | 2.512 (3) |
Cu—Caix | 3.5885 (8) | O2B—Caii | 3.022 (3) |
GeA—O2A | 1.708 (2) | O3A—GeAiii | 1.785 (3) |
GeA—O1A | 1.733 (2) | O3A—Cax | 2.465 (2) |
GeA—O3Ax | 1.785 (3) | O3B—GeBiii | 1.894 (2) |
GeA—O3A | 1.789 (2) | O3B—Cax | 2.468 (3) |
GeA—Cax | 3.6056 (8) | | |
| | | |
O2A—Ca—O1Ai | 78.83 (9) | O1A—GeA—O3Ax | 107.87 (12) |
O2A—Ca—O1Bii | 68.84 (8) | O2A—GeA—O3A | 104.33 (12) |
O1Ai—Ca—O1Bii | 72.75 (8) | O1A—GeA—O3A | 110.37 (11) |
O2A—Ca—O3Aiii | 90.41 (9) | O3Ax—GeA—O3A | 102.98 (8) |
O1Ai—Ca—O3Aiii | 77.64 (8) | O2A—GeA—Ca | 35.05 (9) |
O1Bii—Ca—O3Aiii | 146.43 (8) | O1A—GeA—Ca | 129.53 (9) |
O2A—Ca—O3Biii | 138.08 (9) | O3Ax—GeA—Ca | 121.57 (8) |
O1Ai—Ca—O3Biii | 131.73 (9) | O3A—GeA—Ca | 69.61 (8) |
O1Bii—Ca—O3Biii | 139.22 (8) | O2A—GeA—Cax | 103.55 (9) |
O3Aiii—Ca—O3Biii | 73.53 (8) | O1A—GeA—Cax | 133.41 (8) |
O2A—Ca—O2Biv | 157.04 (9) | O3Ax—GeA—Cax | 67.08 (8) |
O1Ai—Ca—O2Biv | 85.88 (8) | O3A—GeA—Cax | 38.31 (8) |
O1Bii—Ca—O2Biv | 90.40 (8) | Ca—GeA—Cax | 79.29 (2) |
O3Aiii—Ca—O2Biv | 103.02 (9) | O2A—GeA—Caviii | 73.81 (9) |
O3Biii—Ca—O2Biv | 64.53 (8) | O1A—GeA—Caviii | 127.13 (9) |
O2A—Ca—O3B | 84.39 (9) | O3Ax—GeA—Caviii | 35.71 (8) |
O1Ai—Ca—O3B | 162.90 (9) | O3A—GeA—Caviii | 114.22 (8) |
O1Bii—Ca—O3B | 104.23 (8) | Ca—GeA—Caviii | 92.455 (19) |
O3Aiii—Ca—O3B | 99.39 (8) | Cax—GeA—Caviii | 77.11 (2) |
O3Biii—Ca—O3B | 61.42 (3) | O1B—GeB—O2B | 109.68 (12) |
O2Biv—Ca—O3B | 111.12 (8) | O1B—GeB—O3B | 128.26 (11) |
O2A—Ca—O2Bii | 102.33 (8) | O2B—GeB—O3B | 121.13 (12) |
O1Ai—Ca—O2Bii | 130.98 (8) | O1B—GeB—O3Bx | 96.79 (11) |
O1Bii—Ca—O2Bii | 62.90 (7) | O2B—GeB—O3Bx | 92.87 (11) |
O3Aiii—Ca—O2Bii | 150.16 (8) | O3B—GeB—O3Bx | 90.14 (7) |
O3Biii—Ca—O2Bii | 79.15 (8) | O1B—GeB—O2Bii | 90.22 (11) |
O2Biv—Ca—O2Bii | 75.04 (9) | O2B—GeB—O2Bii | 81.69 (12) |
O3B—Ca—O2Bii | 56.04 (7) | O3B—GeB—O2Bii | 88.04 (11) |
O2A—Ca—Cuiv | 116.05 (7) | O3Bx—GeB—O2Bii | 172.29 (10) |
O1Ai—Ca—Cuiv | 37.49 (6) | O1B—GeB—GeBii | 102.02 (8) |
O1Bii—Ca—Cuiv | 83.45 (6) | O2B—GeB—GeBii | 44.53 (8) |
O3Aiii—Ca—Cuiv | 82.60 (6) | O3B—GeB—GeBii | 106.94 (8) |
O3Biii—Ca—Cuiv | 100.29 (6) | O3Bx—GeB—GeBii | 137.13 (8) |
O2Biv—Ca—Cuiv | 49.13 (6) | O2Bii—GeB—GeBii | 37.16 (7) |
O3B—Ca—Cuiv | 159.52 (6) | O1B—GeB—Cuii | 40.07 (8) |
O2Bii—Ca—Cuiv | 114.36 (5) | O2B—GeB—Cuii | 116.76 (8) |
O2A—Ca—GeBii | 83.59 (7) | O3B—GeB—Cuii | 102.96 (8) |
O1Ai—Ca—GeBii | 102.25 (6) | O3Bx—GeB—Cuii | 132.40 (7) |
O1Bii—Ca—GeBii | 31.03 (5) | O2Bii—GeB—Cuii | 55.30 (7) |
O3Aiii—Ca—GeBii | 173.88 (6) | GeBii—GeB—Cuii | 82.609 (17) |
O3Biii—Ca—GeBii | 110.30 (6) | O1B—GeB—Caii | 45.53 (8) |
O2Biv—Ca—GeBii | 83.05 (6) | O2B—GeB—Caii | 64.28 (8) |
O3B—Ca—GeBii | 78.89 (6) | O3B—GeB—Caii | 166.78 (8) |
O2Bii—Ca—GeBii | 31.92 (5) | O3Bx—GeB—Caii | 101.90 (8) |
Cuiv—Ca—GeBii | 101.08 (2) | O2Bii—GeB—Caii | 80.73 (7) |
O2A—Ca—GeBiv | 171.41 (7) | GeBii—GeB—Caii | 67.724 (18) |
O1Ai—Ca—GeBiv | 108.95 (6) | Cuii—GeB—Caii | 64.853 (17) |
O1Bii—Ca—GeBiv | 116.40 (6) | O1B—GeB—Caviii | 110.79 (8) |
O3Aiii—Ca—GeBiv | 87.82 (6) | O2B—GeB—Caviii | 46.79 (8) |
O3Biii—Ca—GeBiv | 33.58 (6) | O3B—GeB—Caviii | 110.54 (8) |
O2Biv—Ca—GeBiv | 30.97 (6) | O3Bx—GeB—Caviii | 46.12 (7) |
O3B—Ca—GeBiv | 87.61 (6) | O2Bii—GeB—Caviii | 128.01 (7) |
O2Bii—Ca—GeBiv | 75.56 (5) | GeBii—GeB—Caviii | 91.055 (19) |
Cuiv—Ca—GeBiv | 72.049 (18) | Cuii—GeB—Caviii | 146.282 (19) |
GeBii—Ca—GeBiv | 97.94 (2) | Caii—GeB—Caviii | 82.06 (2) |
O2A—Ca—Cu | 34.60 (6) | O1B—GeB—Cax | 115.08 (8) |
O1Ai—Ca—Cu | 76.65 (6) | O2B—GeB—Cax | 122.29 (8) |
O1Bii—Ca—Cu | 34.64 (6) | O3B—GeB—Cax | 42.83 (8) |
O3Aiii—Ca—Cu | 122.63 (6) | O3Bx—GeB—Cax | 48.46 (8) |
O3Biii—Ca—Cu | 151.54 (6) | O2Bii—GeB—Cax | 130.70 (7) |
O2Biv—Ca—Cu | 124.98 (6) | GeBii—GeB—Cax | 142.03 (2) |
O3B—Ca—Cu | 91.38 (6) | Cuii—GeB—Cax | 120.902 (18) |
O2Bii—Ca—Cu | 78.42 (5) | Caii—GeB—Cax | 147.074 (16) |
Cuiv—Ca—Cu | 104.79 (2) | Caviii—GeB—Cax | 83.48 (2) |
GeBii—Ca—Cu | 51.848 (15) | O1B—GeB—Ca | 147.30 (8) |
GeBiv—Ca—Cu | 149.20 (2) | O2B—GeB—Ca | 79.71 (8) |
O1Av—Cu—O1Bii | 175.22 (10) | O3B—GeB—Ca | 46.64 (8) |
O1Av—Cu—O2A | 94.28 (10) | O3Bx—GeB—Ca | 114.36 (7) |
O1Bii—Cu—O2A | 87.20 (10) | O2Bii—GeB—Ca | 59.42 (7) |
O1Av—Cu—O1Bvi | 86.23 (10) | GeBii—GeB—Ca | 61.988 (16) |
O1Bii—Cu—O1Bvi | 91.50 (9) | Cuii—GeB—Ca | 107.37 (2) |
O2A—Cu—O1Bvi | 169.57 (10) | Caii—GeB—Ca | 129.712 (15) |
O1Av—Cu—O1Avii | 102.96 (10) | Caviii—GeB—Ca | 98.46 (2) |
O1Bii—Cu—O1Avii | 80.88 (9) | Cax—GeB—Ca | 81.64 (2) |
O2A—Cu—O1Avii | 107.36 (10) | GeA—O1A—Cuv | 120.00 (13) |
O1Bvi—Cu—O1Avii | 82.62 (9) | GeA—O1A—Cuxi | 111.96 (12) |
O1Av—Cu—GeBii | 139.54 (7) | Cuv—O1A—Cuxi | 92.60 (9) |
O1Bii—Cu—GeBii | 35.71 (7) | GeA—O1A—Cai | 132.41 (13) |
O2A—Cu—GeBii | 101.61 (8) | Cuv—O1A—Cai | 92.63 (9) |
O1Bvi—Cu—GeBii | 71.86 (7) | Cuxi—O1A—Cai | 98.86 (9) |
O1Avii—Cu—GeBii | 107.24 (6) | GeB—O1B—Cuii | 104.22 (12) |
O1Av—Cu—Caviii | 49.88 (7) | GeB—O1B—Cuxii | 140.42 (14) |
O1Bii—Cu—Caviii | 125.86 (7) | Cuii—O1B—Cuxii | 98.45 (10) |
O2A—Cu—Caviii | 85.29 (8) | GeB—O1B—Caii | 103.43 (11) |
O1Bvi—Cu—Caviii | 87.10 (7) | Cuii—O1B—Caii | 99.85 (10) |
O1Avii—Cu—Caviii | 151.69 (7) | Cuxii—O1B—Caii | 104.11 (10) |
GeBii—Cu—Caviii | 94.33 (2) | GeA—O2A—Cu | 132.62 (16) |
O1Av—Cu—Ca | 135.16 (7) | GeA—O2A—Ca | 120.09 (13) |
O1Bii—Cu—Ca | 45.52 (7) | Cu—O2A—Ca | 103.17 (10) |
O2A—Cu—Ca | 42.24 (8) | GeB—O2B—GeBii | 98.31 (12) |
O1Bvi—Cu—Ca | 134.14 (7) | GeB—O2B—Caviii | 102.25 (11) |
O1Avii—Cu—Ca | 101.27 (7) | GeBii—O2B—Caviii | 158.08 (12) |
GeBii—Cu—Ca | 63.299 (17) | GeB—O2B—Caii | 83.79 (9) |
Caviii—Cu—Ca | 104.79 (2) | GeBii—O2B—Caii | 84.67 (8) |
O1Av—Cu—Caix | 102.57 (7) | Caviii—O2B—Caii | 104.96 (9) |
O1Bii—Cu—Caix | 78.30 (7) | GeAiii—O3A—GeA | 125.41 (14) |
O2A—Cu—Caix | 147.61 (8) | GeAiii—O3A—Cax | 119.30 (12) |
O1Bvi—Cu—Caix | 41.40 (7) | GeA—O3A—Cax | 114.97 (12) |
O1Avii—Cu—Caix | 42.12 (6) | GeB—O3B—GeBiii | 120.92 (13) |
GeBii—Cu—Caix | 83.252 (16) | GeB—O3B—Cax | 107.88 (12) |
Caviii—Cu—Caix | 126.61 (2) | GeBiii—O3B—Cax | 100.29 (10) |
Ca—Cu—Caix | 120.54 (2) | GeB—O3B—Ca | 103.79 (10) |
O2A—GeA—O1A | 120.44 (12) | GeBiii—O3B—Ca | 98.74 (11) |
O2A—GeA—O3Ax | 109.47 (12) | Cax—O3B—Ca | 126.63 (10) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.882 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6540 reflections |
a = 10.1853 (12) Å | θ = 2.1–32.1° |
b = 9.1959 (7) Å | µ = 18.22 mm−1 |
c = 5.2013 (6) Å | T = 200 K |
β = 105.649 (12)° | Cuboid, pale green |
V = 469.11 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 2 diffractometer | 1626 independent reflections |
Plane graphite monochromator | 1415 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.037 |
rotation method scans | θmax = 32.2°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −15→15 |
Tmin = 0.084, Tmax = 0.162 | k = −13→13 |
5828 measured reflections | l = −7→7 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0163P)2 + 1.812P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max = 0.001 |
wR(F2) = 0.052 | Δρmax = 0.75 e Å−3 |
S = 1.07 | Δρmin = −0.81 e Å−3 |
1626 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0097 (5) |
Crystal data top
CaCuGe2O6 | V = 469.11 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1853 (12) Å | µ = 18.22 mm−1 |
b = 9.1959 (7) Å | T = 200 K |
c = 5.2013 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.649 (12)° | |
Data collection top
STOE IPDS 2 diffractometer | 1626 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 1415 reflections with I > 2σ(I) |
Tmin = 0.084, Tmax = 0.162 | Rint = 0.037 |
5828 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.025 | 92 parameters |
wR(F2) = 0.052 | 0 restraints |
S = 1.07 | Δρmax = 0.75 e Å−3 |
1626 reflections | Δρmin = −0.81 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28359 (6) | 0.45288 (7) | 0.80976 (13) | 0.01053 (12) | |
Cu | 0.22728 (4) | 0.66164 (4) | 0.25643 (8) | 0.00936 (9) | |
GeA | 0.04919 (3) | 0.34920 (4) | 0.20921 (6) | 0.00811 (8) | |
GeB | 0.49121 (3) | 0.35092 (4) | 0.40301 (7) | 0.00852 (8) | |
O1A | −0.1269 (2) | 0.3615 (2) | 0.1155 (5) | 0.0102 (4) | |
O1B | 0.6588 (2) | 0.3198 (2) | 0.3779 (5) | 0.0092 (4) | |
O2A | 0.1460 (2) | 0.4887 (3) | 0.3771 (5) | 0.0131 (4) | |
O2B | 0.4323 (2) | 0.5224 (2) | 0.2612 (5) | 0.0112 (4) | |
O3A | 0.1032 (2) | 0.1941 (2) | 0.4183 (5) | 0.0108 (4) | |
O3B | 0.3995 (2) | 0.2511 (2) | 0.5901 (5) | 0.0100 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0102 (2) | 0.0101 (2) | 0.0107 (3) | −0.00004 (19) | 0.00186 (19) | 0.0005 (2) |
Cu | 0.00908 (16) | 0.00932 (16) | 0.00860 (17) | −0.00096 (12) | 0.00050 (12) | −0.00023 (13) |
GeA | 0.00707 (13) | 0.00836 (14) | 0.00846 (15) | −0.00045 (10) | 0.00133 (10) | −0.00050 (11) |
GeB | 0.00789 (14) | 0.00788 (14) | 0.00999 (15) | 0.00018 (10) | 0.00277 (10) | 0.00073 (11) |
O1A | 0.0086 (9) | 0.0117 (10) | 0.0098 (10) | 0.0005 (7) | 0.0017 (7) | −0.0013 (8) |
O1B | 0.0070 (9) | 0.0116 (9) | 0.0090 (10) | 0.0011 (7) | 0.0023 (7) | 0.0003 (8) |
O2A | 0.0138 (10) | 0.0115 (10) | 0.0116 (11) | −0.0030 (8) | −0.0006 (8) | −0.0010 (8) |
O2B | 0.0144 (10) | 0.0084 (9) | 0.0100 (10) | 0.0002 (8) | 0.0016 (8) | −0.0002 (8) |
O3A | 0.0114 (9) | 0.0117 (9) | 0.0106 (10) | 0.0029 (8) | 0.0049 (8) | 0.0024 (8) |
O3B | 0.0098 (9) | 0.0109 (9) | 0.0091 (10) | −0.0013 (7) | 0.0023 (7) | 0.0019 (8) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (3) | GeA—Caviii | 3.6881 (8) |
Ca—O1Ai | 2.438 (2) | GeB—O1B | 1.770 (2) |
Ca—O1Bii | 2.444 (2) | GeB—O2B | 1.775 (2) |
Ca—O3Aiii | 2.466 (2) | GeB—O3B | 1.776 (2) |
Ca—O3Biii | 2.472 (2) | GeB—O3Bx | 1.892 (2) |
Ca—O2Biv | 2.510 (2) | GeB—O2Bii | 2.069 (2) |
Ca—O3B | 2.621 (2) | GeB—GeBii | 2.9104 (7) |
Ca—O2Bii | 3.023 (2) | GeB—Cuii | 2.9381 (7) |
Ca—Cuiv | 3.1828 (8) | GeB—Caii | 3.3332 (8) |
Ca—GeBii | 3.3332 (7) | GeB—Caviii | 3.3692 (9) |
Ca—GeBiv | 3.3692 (9) | GeB—Cax | 3.4581 (7) |
Ca—Cu | 3.3774 (8) | O1A—Cuv | 1.941 (2) |
Cu—O1Av | 1.941 (2) | O1A—Cuxi | 2.288 (2) |
Cu—O1Bii | 1.950 (2) | O1A—Cai | 2.438 (2) |
Cu—O2A | 1.972 (2) | O1B—Cuii | 1.950 (2) |
Cu—O1Bvi | 2.095 (2) | O1B—Cuxii | 2.095 (2) |
Cu—O1Avii | 2.288 (2) | O1B—Caii | 2.444 (2) |
Cu—GeBii | 2.9381 (7) | O2B—GeBii | 2.069 (2) |
Cu—Caviii | 3.1828 (8) | O2B—Caviii | 2.510 (2) |
Cu—Caix | 3.5897 (8) | O2B—Caii | 3.023 (2) |
GeA—O2A | 1.708 (2) | O3A—GeAiii | 1.789 (2) |
GeA—O1A | 1.731 (2) | O3A—Cax | 2.466 (2) |
GeA—O3A | 1.788 (2) | O3B—GeBiii | 1.892 (2) |
GeA—O3Ax | 1.789 (2) | O3B—Cax | 2.472 (2) |
GeA—Cax | 3.6078 (7) | | |
| | | |
O2A—Ca—O1Ai | 78.80 (8) | O1A—GeA—O3A | 110.41 (11) |
O2A—Ca—O1Bii | 68.91 (8) | O2A—GeA—O3Ax | 109.45 (11) |
O1Ai—Ca—O1Bii | 72.72 (8) | O1A—GeA—O3Ax | 107.95 (11) |
O2A—Ca—O3Aiii | 90.42 (8) | O3A—GeA—O3Ax | 102.87 (8) |
O1Ai—Ca—O3Aiii | 77.70 (8) | O2A—GeA—Ca | 35.06 (8) |
O1Bii—Ca—O3Aiii | 146.51 (8) | O1A—GeA—Ca | 129.54 (8) |
O2A—Ca—O3Biii | 138.06 (8) | O3A—GeA—Ca | 69.64 (8) |
O1Ai—Ca—O3Biii | 131.76 (8) | O3Ax—GeA—Ca | 121.49 (7) |
O1Bii—Ca—O3Biii | 139.17 (8) | O2A—GeA—Cax | 103.67 (8) |
O3Aiii—Ca—O3Biii | 73.49 (8) | O1A—GeA—Cax | 133.33 (8) |
O2A—Ca—O2Biv | 157.09 (8) | O3A—GeA—Cax | 38.25 (7) |
O1Ai—Ca—O2Biv | 85.89 (8) | O3Ax—GeA—Cax | 66.98 (8) |
O1Bii—Ca—O2Biv | 90.38 (8) | Ca—GeA—Cax | 79.38 (2) |
O3Aiii—Ca—O2Biv | 102.96 (8) | O2A—GeA—Caviii | 73.84 (9) |
O3Biii—Ca—O2Biv | 64.51 (8) | O1A—GeA—Caviii | 127.13 (8) |
O2A—Ca—O3B | 84.47 (8) | O3A—GeA—Caviii | 114.16 (7) |
O1Ai—Ca—O3B | 162.96 (8) | O3Ax—GeA—Caviii | 35.66 (7) |
O1Bii—Ca—O3B | 104.28 (7) | Ca—GeA—Caviii | 92.452 (18) |
O3Aiii—Ca—O3B | 99.37 (8) | Cax—GeA—Caviii | 77.121 (19) |
O3Biii—Ca—O3B | 61.34 (3) | O1B—GeB—O2B | 109.73 (11) |
O2Biv—Ca—O3B | 111.05 (8) | O1B—GeB—O3B | 128.13 (10) |
O2A—Ca—O2Bii | 102.56 (8) | O2B—GeB—O3B | 121.19 (11) |
O1Ai—Ca—O2Bii | 131.00 (7) | O1B—GeB—O3Bx | 96.82 (10) |
O1Bii—Ca—O2Bii | 63.01 (7) | O2B—GeB—O3Bx | 92.86 (10) |
O3Aiii—Ca—O2Bii | 150.02 (7) | O3B—GeB—O3Bx | 90.24 (7) |
O3Biii—Ca—O2Bii | 78.97 (7) | O1B—GeB—O2Bii | 90.12 (10) |
O2Biv—Ca—O2Bii | 74.88 (8) | O2B—GeB—O2Bii | 81.87 (11) |
O3B—Ca—O2Bii | 56.05 (7) | O3B—GeB—O2Bii | 87.86 (10) |
O2A—Ca—Cuiv | 116.07 (7) | O3Bx—GeB—O2Bii | 172.41 (9) |
O1Ai—Ca—Cuiv | 37.53 (6) | O1B—GeB—GeBii | 101.97 (8) |
O1Bii—Ca—Cuiv | 83.43 (6) | O2B—GeB—GeBii | 44.73 (8) |
O3Aiii—Ca—Cuiv | 82.61 (6) | O3B—GeB—GeBii | 106.81 (8) |
O3Biii—Ca—Cuiv | 100.28 (6) | O3Bx—GeB—GeBii | 137.31 (7) |
O2Biv—Ca—Cuiv | 49.11 (5) | O2Bii—GeB—GeBii | 37.15 (6) |
O3B—Ca—Cuiv | 159.43 (6) | O1B—GeB—Cuii | 40.04 (7) |
O2Bii—Ca—Cuiv | 114.25 (5) | O2B—GeB—Cuii | 116.81 (8) |
O2A—Ca—GeBii | 83.76 (6) | O3B—GeB—Cuii | 102.80 (7) |
O1Ai—Ca—GeBii | 102.28 (6) | O3Bx—GeB—Cuii | 132.39 (7) |
O1Bii—Ca—GeBii | 31.11 (5) | O2Bii—GeB—Cuii | 55.18 (6) |
O3Aiii—Ca—GeBii | 174.05 (6) | GeBii—GeB—Cuii | 82.486 (16) |
O3Biii—Ca—GeBii | 110.17 (6) | O1B—GeB—Caii | 45.51 (7) |
O2Biv—Ca—GeBii | 82.95 (6) | O2B—GeB—Caii | 64.35 (8) |
O3B—Ca—GeBii | 78.90 (5) | O3B—GeB—Caii | 166.58 (8) |
O2Bii—Ca—GeBii | 31.96 (4) | O3Bx—GeB—Caii | 101.96 (7) |
Cuiv—Ca—GeBii | 101.04 (2) | O2Bii—GeB—Caii | 80.75 (7) |
O2A—Ca—GeBiv | 171.38 (6) | GeBii—GeB—Caii | 67.770 (17) |
O1Ai—Ca—GeBiv | 108.96 (6) | Cuii—GeB—Caii | 64.812 (16) |
O1Bii—Ca—GeBiv | 116.40 (6) | O1B—GeB—Caviii | 110.91 (8) |
O3Aiii—Ca—GeBiv | 87.72 (6) | O2B—GeB—Caviii | 46.69 (8) |
O3Biii—Ca—GeBiv | 33.56 (5) | O3B—GeB—Caviii | 110.65 (7) |
O2Biv—Ca—GeBiv | 30.98 (5) | O3Bx—GeB—Caviii | 46.21 (7) |
O3B—Ca—GeBiv | 87.54 (5) | O2Bii—GeB—Caviii | 128.08 (7) |
O2Bii—Ca—GeBiv | 75.39 (5) | GeBii—GeB—Caviii | 91.149 (18) |
Cuiv—Ca—GeBiv | 72.033 (18) | Cuii—GeB—Caviii | 146.351 (18) |
GeBii—Ca—GeBiv | 97.85 (2) | Caii—GeB—Caviii | 82.15 (2) |
O2A—Ca—Cu | 34.66 (6) | O1B—GeB—Cax | 115.12 (8) |
O1Ai—Ca—Cu | 76.70 (6) | O2B—GeB—Cax | 122.27 (8) |
O1Bii—Ca—Cu | 34.67 (5) | O3B—GeB—Cax | 42.86 (8) |
O3Aiii—Ca—Cu | 122.74 (6) | O3Bx—GeB—Cax | 48.51 (7) |
O3Biii—Ca—Cu | 151.45 (6) | O2Bii—GeB—Cax | 130.56 (7) |
O2Biv—Ca—Cu | 125.00 (6) | GeBii—GeB—Cax | 141.98 (2) |
O3B—Ca—Cu | 91.37 (5) | Cuii—GeB—Cax | 120.877 (17) |
O2Bii—Ca—Cu | 78.54 (5) | Caii—GeB—Cax | 147.166 (15) |
Cuiv—Ca—Cu | 104.87 (2) | Caviii—GeB—Cax | 83.53 (2) |
GeBii—Ca—Cu | 51.925 (15) | O1B—GeB—Ca | 147.16 (8) |
GeBiv—Ca—Cu | 149.20 (2) | O2B—GeB—Ca | 79.71 (8) |
O1Av—Cu—O1Bii | 175.42 (9) | O3B—GeB—Ca | 46.68 (8) |
O1Av—Cu—O2A | 94.31 (10) | O3Bx—GeB—Ca | 114.46 (7) |
O1Bii—Cu—O2A | 87.16 (10) | O2Bii—GeB—Ca | 59.35 (7) |
O1Av—Cu—O1Bvi | 86.22 (9) | GeBii—GeB—Ca | 61.874 (15) |
O1Bii—Cu—O1Bvi | 91.56 (8) | Cuii—GeB—Ca | 107.258 (19) |
O2A—Cu—O1Bvi | 169.78 (10) | Caii—GeB—Ca | 129.643 (14) |
O1Av—Cu—O1Avii | 102.81 (9) | Caviii—GeB—Ca | 98.442 (19) |
O1Bii—Cu—O1Avii | 80.85 (9) | Cax—GeB—Ca | 81.65 (2) |
O2A—Cu—O1Avii | 107.22 (9) | GeA—O1A—Cuv | 120.05 (12) |
O1Bvi—Cu—O1Avii | 82.55 (9) | GeA—O1A—Cuxi | 112.08 (11) |
O1Av—Cu—GeBii | 139.71 (7) | Cuv—O1A—Cuxi | 92.60 (9) |
O1Bii—Cu—GeBii | 35.73 (6) | GeA—O1A—Cai | 132.39 (12) |
O2A—Cu—GeBii | 101.65 (7) | Cuv—O1A—Cai | 92.53 (9) |
O1Bvi—Cu—GeBii | 71.95 (6) | Cuxi—O1A—Cai | 98.79 (8) |
O1Avii—Cu—GeBii | 107.23 (6) | GeB—O1B—Cuii | 104.22 (11) |
O1Av—Cu—Caviii | 49.94 (7) | GeB—O1B—Cuxii | 140.24 (13) |
O1Bii—Cu—Caviii | 126.00 (7) | Cuii—O1B—Cuxii | 98.55 (9) |
O2A—Cu—Caviii | 85.40 (8) | GeB—O1B—Caii | 103.39 (10) |
O1Bvi—Cu—Caviii | 87.16 (6) | Cuii—O1B—Caii | 99.85 (9) |
O1Avii—Cu—Caviii | 151.60 (6) | Cuxii—O1B—Caii | 104.27 (9) |
GeBii—Cu—Caviii | 94.455 (19) | GeA—O2A—Cu | 132.63 (15) |
O1Av—Cu—Ca | 135.22 (7) | GeA—O2A—Ca | 120.06 (12) |
O1Bii—Cu—Ca | 45.48 (7) | Cu—O2A—Ca | 103.09 (10) |
O2A—Cu—Ca | 42.26 (7) | GeB—O2B—GeBii | 98.13 (11) |
O1Bvi—Cu—Ca | 134.18 (6) | GeB—O2B—Caviii | 102.33 (10) |
O1Avii—Cu—Ca | 101.25 (6) | GeBii—O2B—Caviii | 158.14 (11) |
GeBii—Cu—Ca | 63.263 (17) | GeB—O2B—Caii | 83.69 (8) |
Caviii—Cu—Ca | 104.87 (2) | GeBii—O2B—Caii | 84.59 (8) |
O1Av—Cu—Caix | 102.45 (7) | Caviii—O2B—Caii | 105.12 (8) |
O1Bii—Cu—Caix | 78.33 (7) | GeA—O3A—GeAiii | 125.28 (13) |
O2A—Cu—Caix | 147.53 (8) | GeA—O3A—Cax | 115.08 (11) |
O1Bvi—Cu—Caix | 41.29 (6) | GeAiii—O3A—Cax | 119.33 (11) |
O1Avii—Cu—Caix | 42.17 (6) | GeB—O3B—GeBiii | 121.11 (12) |
GeBii—Cu—Caix | 83.259 (15) | GeB—O3B—Cax | 107.88 (11) |
Caviii—Cu—Caix | 126.55 (2) | GeBiii—O3B—Cax | 100.23 (10) |
Ca—Cu—Caix | 120.57 (2) | GeB—O3B—Ca | 103.78 (10) |
O2A—GeA—O1A | 120.40 (11) | GeBiii—O3B—Ca | 98.75 (10) |
O2A—GeA—O3A | 104.37 (11) | Cax—O3B—Ca | 126.51 (9) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.876 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6528 reflections |
a = 10.1893 (12) Å | θ = 2.2–32.1° |
b = 9.1996 (7) Å | µ = 18.25 mm−1 |
c = 5.2043 (6) Å | T = 250 K |
β = 105.669 (12)° | Cuboid, pale green |
V = 469.71 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 2 diffractometer | 1631 independent reflections |
Plane graphite monochromator | 1404 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.040 |
rotation method scans | θmax = 32.2°, θmin = 2.1° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −15→15 |
Tmin = 0.097, Tmax = 0.150 | k = −13→13 |
5849 measured reflections | l = −7→7 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0243P)2 + 1.1408P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max < 0.001 |
wR(F2) = 0.055 | Δρmax = 0.74 e Å−3 |
S = 1.03 | Δρmin = −0.70 e Å−3 |
1631 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0109 (6) |
Crystal data top
CaCuGe2O6 | V = 469.71 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1893 (12) Å | µ = 18.25 mm−1 |
b = 9.1996 (7) Å | T = 250 K |
c = 5.2043 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.669 (12)° | |
Data collection top
STOE IPDS 2 diffractometer | 1631 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 1404 reflections with I > 2σ(I) |
Tmin = 0.097, Tmax = 0.150 | Rint = 0.040 |
5849 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.025 | 92 parameters |
wR(F2) = 0.055 | 0 restraints |
S = 1.03 | Δρmax = 0.74 e Å−3 |
1631 reflections | Δρmin = −0.70 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28332 (6) | 0.45266 (7) | 0.80927 (13) | 0.01214 (12) | |
Cu | 0.22741 (4) | 0.66155 (4) | 0.25644 (8) | 0.01089 (9) | |
GeA | 0.04914 (3) | 0.34920 (3) | 0.20930 (6) | 0.00942 (8) | |
GeB | 0.49119 (3) | 0.35087 (3) | 0.40209 (7) | 0.00990 (8) | |
O1A | −0.1271 (2) | 0.3615 (2) | 0.1151 (5) | 0.0115 (4) | |
O1B | 0.6585 (2) | 0.3200 (2) | 0.3784 (5) | 0.0107 (4) | |
O2A | 0.1458 (2) | 0.4889 (3) | 0.3767 (5) | 0.0148 (4) | |
O2B | 0.4321 (2) | 0.5219 (2) | 0.2614 (5) | 0.0134 (4) | |
O3A | 0.1031 (2) | 0.1940 (2) | 0.4197 (5) | 0.0126 (4) | |
O3B | 0.3997 (2) | 0.2512 (2) | 0.5899 (5) | 0.0118 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0118 (2) | 0.0119 (2) | 0.0121 (3) | 0.00016 (19) | 0.00206 (18) | 0.0008 (2) |
Cu | 0.01064 (16) | 0.01099 (16) | 0.00968 (16) | −0.00111 (12) | 0.00041 (12) | 0.00016 (13) |
GeA | 0.00807 (13) | 0.00995 (14) | 0.00957 (15) | −0.00047 (10) | 0.00123 (10) | −0.00044 (10) |
GeB | 0.00895 (13) | 0.00955 (14) | 0.01139 (15) | 0.00016 (10) | 0.00309 (10) | 0.00079 (10) |
O1A | 0.0092 (8) | 0.0131 (10) | 0.0110 (10) | 0.0000 (7) | 0.0008 (7) | −0.0009 (7) |
O1B | 0.0082 (8) | 0.0120 (9) | 0.0114 (9) | 0.0007 (7) | 0.0017 (7) | 0.0004 (8) |
O2A | 0.0151 (10) | 0.0134 (10) | 0.0132 (10) | −0.0045 (8) | −0.0011 (8) | −0.0007 (8) |
O2B | 0.0177 (10) | 0.0103 (9) | 0.0116 (10) | 0.0013 (8) | 0.0029 (8) | 0.0001 (8) |
O3A | 0.0126 (9) | 0.0130 (9) | 0.0126 (10) | 0.0032 (7) | 0.0042 (7) | 0.0027 (8) |
O3B | 0.0104 (9) | 0.0137 (9) | 0.0113 (10) | −0.0021 (7) | 0.0028 (7) | 0.0016 (8) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (2) | GeA—Cax | 3.6063 (7) |
Ca—O1Ai | 2.439 (2) | GeB—O1B | 1.765 (2) |
Ca—O1Bii | 2.448 (2) | GeB—O2B | 1.771 (2) |
Ca—O3Aiii | 2.468 (2) | GeB—O3B | 1.777 (2) |
Ca—O3Biii | 2.474 (2) | GeB—O3Bx | 1.890 (2) |
Ca—O2Biv | 2.513 (2) | GeB—O2Bii | 2.075 (2) |
Ca—O3B | 2.623 (2) | GeB—GeBii | 2.9156 (7) |
Ca—O2Bii | 3.029 (2) | GeB—Cuii | 2.9394 (7) |
Ca—Cuiv | 3.1858 (8) | GeB—Caii | 3.3347 (7) |
Ca—GeBii | 3.3347 (7) | GeB—Caviii | 3.3693 (8) |
Ca—GeBiv | 3.3693 (8) | GeB—Cax | 3.4590 (7) |
Ca—Cu | 3.3778 (8) | O1A—Cuv | 1.939 (2) |
Cu—O1Av | 1.939 (2) | O1A—Cuxi | 2.290 (2) |
Cu—O1Bii | 1.949 (2) | O1A—Cai | 2.439 (2) |
Cu—O2A | 1.971 (2) | O1B—Cuii | 1.949 (2) |
Cu—O1Bvi | 2.100 (2) | O1B—Cuxii | 2.100 (2) |
Cu—O1Avii | 2.290 (2) | O1B—Caii | 2.448 (2) |
Cu—GeBii | 2.9394 (6) | O2B—GeBii | 2.075 (2) |
Cu—Caviii | 3.1858 (8) | O2B—Caviii | 2.513 (2) |
Cu—Caix | 3.5933 (8) | O2B—Caii | 3.029 (2) |
GeA—O2A | 1.708 (2) | O3A—GeAiii | 1.783 (2) |
GeA—O1A | 1.733 (2) | O3A—Cax | 2.468 (2) |
GeA—O3Ax | 1.783 (2) | O3B—GeBiii | 1.890 (2) |
GeA—O3A | 1.793 (2) | O3B—Cax | 2.474 (2) |
| | | |
O2A—Ca—O1Ai | 78.90 (8) | Ca—Cu—Caix | 120.66 (2) |
O2A—Ca—O1Bii | 68.88 (8) | O2A—GeA—O1A | 120.40 (11) |
O1Ai—Ca—O1Bii | 72.80 (7) | O2A—GeA—O3Ax | 109.37 (11) |
O2A—Ca—O3Aiii | 90.71 (8) | O1A—GeA—O3Ax | 107.95 (11) |
O1Ai—Ca—O3Aiii | 77.69 (8) | O2A—GeA—O3A | 104.38 (11) |
O1Bii—Ca—O3Aiii | 146.67 (8) | O1A—GeA—O3A | 110.37 (10) |
O2A—Ca—O3Biii | 138.21 (8) | O3Ax—GeA—O3A | 103.00 (7) |
O1Ai—Ca—O3Biii | 131.75 (8) | O2A—GeA—Ca | 35.18 (8) |
O1Bii—Ca—O3Biii | 138.93 (8) | O1A—GeA—Ca | 129.60 (8) |
O3Aiii—Ca—O3Biii | 73.53 (8) | O3Ax—GeA—Ca | 121.43 (7) |
O2A—Ca—O2Biv | 157.05 (8) | O3A—GeA—Ca | 69.51 (8) |
O1Ai—Ca—O2Biv | 85.76 (8) | O2A—GeA—Cax | 103.76 (8) |
O1Bii—Ca—O2Biv | 90.41 (8) | O1A—GeA—Cax | 133.30 (7) |
O3Aiii—Ca—O2Biv | 102.66 (8) | O3Ax—GeA—Cax | 66.87 (8) |
O3Biii—Ca—O2Biv | 64.38 (8) | O3A—GeA—Cax | 38.45 (7) |
O2A—Ca—O3B | 84.57 (8) | Ca—GeA—Cax | 79.41 (2) |
O1Ai—Ca—O3B | 163.18 (8) | O1B—GeB—O2B | 109.94 (11) |
O1Bii—Ca—O3B | 104.09 (7) | O1B—GeB—O3B | 127.96 (10) |
O3Aiii—Ca—O3B | 99.63 (7) | O2B—GeB—O3B | 121.06 (11) |
O3Biii—Ca—O3B | 61.32 (3) | O1B—GeB—O3Bx | 96.96 (10) |
O2Biv—Ca—O3B | 110.94 (8) | O2B—GeB—O3Bx | 93.00 (10) |
O2A—Ca—O2Bii | 102.52 (8) | O3B—GeB—O3Bx | 90.37 (7) |
O1Ai—Ca—O2Bii | 130.78 (7) | O1B—GeB—O2Bii | 89.94 (10) |
O1Bii—Ca—O2Bii | 62.78 (7) | O2B—GeB—O2Bii | 81.73 (11) |
O3Aiii—Ca—O2Bii | 150.14 (7) | O3B—GeB—O2Bii | 87.76 (10) |
O3Biii—Ca—O2Bii | 78.93 (7) | O3Bx—GeB—O2Bii | 172.45 (9) |
O2Biv—Ca—O2Bii | 74.87 (8) | O1B—GeB—GeBii | 101.92 (7) |
O3B—Ca—O2Bii | 56.03 (7) | O2B—GeB—GeBii | 44.78 (8) |
O2A—Ca—Cuiv | 116.08 (7) | O3B—GeB—GeBii | 106.59 (8) |
O1Ai—Ca—Cuiv | 37.45 (5) | O3Bx—GeB—GeBii | 137.52 (7) |
O1Bii—Ca—Cuiv | 83.48 (6) | O2Bii—GeB—GeBii | 36.95 (6) |
O3Aiii—Ca—Cuiv | 82.45 (6) | O1B—GeB—Cuii | 39.93 (7) |
O3Biii—Ca—Cuiv | 100.24 (6) | O2B—GeB—Cuii | 116.84 (8) |
O2Biv—Ca—Cuiv | 49.06 (5) | O3B—GeB—Cuii | 102.61 (7) |
O3B—Ca—Cuiv | 159.31 (6) | O3Bx—GeB—Cuii | 132.41 (7) |
O2Bii—Ca—Cuiv | 114.09 (5) | O2Bii—GeB—Cuii | 55.13 (6) |
O2A—Ca—GeBii | 83.79 (6) | GeBii—GeB—Cuii | 82.377 (15) |
O1Ai—Ca—GeBii | 102.18 (6) | O1B—GeB—Caii | 45.56 (7) |
O1Bii—Ca—GeBii | 30.98 (5) | O2B—GeB—Caii | 64.51 (8) |
O3Aiii—Ca—GeBii | 174.39 (6) | O3B—GeB—Caii | 166.33 (8) |
O3Biii—Ca—GeBii | 110.01 (6) | O3Bx—GeB—Caii | 102.08 (7) |
O2Biv—Ca—GeBii | 82.89 (6) | O2Bii—GeB—Caii | 80.61 (7) |
O3B—Ca—GeBii | 78.84 (5) | GeBii—GeB—Caii | 67.813 (16) |
O2Bii—Ca—GeBii | 31.86 (4) | Cuii—GeB—Caii | 64.787 (16) |
Cuiv—Ca—GeBii | 100.90 (2) | O1B—GeB—Caviii | 111.16 (8) |
O2A—Ca—GeBiv | 171.46 (6) | O2B—GeB—Caviii | 46.77 (8) |
O1Ai—Ca—GeBiv | 108.86 (6) | O3B—GeB—Caviii | 110.72 (7) |
O1Bii—Ca—GeBiv | 116.28 (6) | O3Bx—GeB—Caviii | 46.27 (7) |
O3Aiii—Ca—GeBiv | 87.60 (6) | O2Bii—GeB—Caviii | 128.04 (7) |
O3Biii—Ca—GeBiv | 33.51 (5) | GeBii—GeB—Caviii | 91.297 (18) |
O2Biv—Ca—GeBiv | 30.90 (5) | Cuii—GeB—Caviii | 146.485 (18) |
O3B—Ca—GeBiv | 87.47 (5) | Caii—GeB—Caviii | 82.302 (19) |
O2Bii—Ca—GeBiv | 75.35 (5) | O1B—GeB—Cax | 115.26 (7) |
Cuiv—Ca—GeBiv | 71.998 (17) | O2B—GeB—Cax | 122.19 (8) |
GeBii—Ca—GeBiv | 97.698 (19) | O3B—GeB—Cax | 42.92 (8) |
O2A—Ca—Cu | 34.63 (6) | O3Bx—GeB—Cax | 48.53 (7) |
O1Ai—Ca—Cu | 76.78 (6) | O2Bii—GeB—Cax | 130.53 (7) |
O1Bii—Ca—Cu | 34.65 (5) | GeBii—GeB—Cax | 141.825 (19) |
O3Aiii—Ca—Cu | 122.98 (6) | Cuii—GeB—Cax | 120.903 (16) |
O3Biii—Ca—Cu | 151.36 (6) | Caii—GeB—Cax | 147.344 (15) |
O2Biv—Ca—Cu | 125.01 (6) | Caviii—GeB—Cax | 83.49 (2) |
O3B—Ca—Cu | 91.34 (5) | O1B—GeB—Ca | 146.95 (8) |
O2Bii—Ca—Cu | 78.43 (5) | O2B—GeB—Ca | 79.57 (8) |
Cuiv—Ca—Cu | 104.88 (2) | O3B—GeB—Ca | 46.60 (8) |
GeBii—Ca—Cu | 51.935 (15) | O3Bx—GeB—Ca | 114.49 (7) |
GeBiv—Ca—Cu | 149.07 (2) | O2Bii—GeB—Ca | 59.36 (7) |
O1Av—Cu—O1Bii | 175.32 (9) | GeBii—GeB—Ca | 61.791 (15) |
O1Av—Cu—O2A | 94.29 (10) | Cuii—GeB—Ca | 107.159 (18) |
O1Bii—Cu—O2A | 87.27 (9) | Caii—GeB—Ca | 129.605 (14) |
O1Av—Cu—O1Bvi | 86.14 (9) | Caviii—GeB—Ca | 98.413 (19) |
O1Bii—Cu—O1Bvi | 91.55 (8) | Cax—GeB—Ca | 81.538 (19) |
O2A—Cu—O1Bvi | 169.85 (9) | GeA—O1A—Cuv | 120.10 (12) |
O1Av—Cu—O1Avii | 102.85 (9) | GeA—O1A—Cuxi | 112.03 (11) |
O1Bii—Cu—O1Avii | 80.85 (9) | Cuv—O1A—Cuxi | 92.69 (9) |
O2A—Cu—O1Avii | 107.15 (9) | GeA—O1A—Cai | 132.19 (12) |
O1Bvi—Cu—O1Avii | 82.58 (8) | Cuv—O1A—Cai | 92.67 (9) |
O1Av—Cu—GeBii | 139.80 (6) | Cuxi—O1A—Cai | 98.86 (8) |
O1Bii—Cu—GeBii | 35.54 (6) | GeB—O1B—Cuii | 104.53 (11) |
O2A—Cu—GeBii | 101.71 (7) | GeB—O1B—Cuxii | 140.12 (12) |
O1Bvi—Cu—GeBii | 72.02 (6) | Cuii—O1B—Cuxii | 98.52 (9) |
O1Avii—Cu—GeBii | 107.10 (6) | GeB—O1B—Caii | 103.46 (10) |
O1Av—Cu—Caviii | 49.88 (7) | Cuii—O1B—Caii | 99.76 (9) |
O1Bii—Cu—Caviii | 125.99 (7) | Cuxii—O1B—Caii | 104.13 (9) |
O2A—Cu—Caviii | 85.41 (8) | GeA—O2A—Cu | 132.76 (14) |
O1Bvi—Cu—Caviii | 87.14 (6) | GeA—O2A—Ca | 119.86 (12) |
O1Avii—Cu—Caviii | 151.61 (6) | Cu—O2A—Ca | 103.12 (10) |
GeBii—Cu—Caviii | 94.618 (19) | GeB—O2B—GeBii | 98.27 (11) |
O1Av—Cu—Ca | 135.19 (7) | GeB—O2B—Caviii | 102.33 (10) |
O1Bii—Cu—Ca | 45.58 (7) | GeBii—O2B—Caviii | 158.05 (11) |
O2A—Cu—Ca | 42.25 (7) | GeB—O2B—Caii | 83.63 (8) |
O1Bvi—Cu—Ca | 134.29 (6) | GeBii—O2B—Caii | 84.51 (8) |
O1Avii—Cu—Ca | 101.20 (6) | Caviii—O2B—Caii | 105.13 (8) |
GeBii—Cu—Ca | 63.278 (16) | GeAiii—O3A—GeA | 125.45 (13) |
Caviii—Cu—Ca | 104.88 (2) | GeAiii—O3A—Cax | 119.57 (11) |
O1Av—Cu—Caix | 102.36 (7) | GeA—O3A—Cax | 114.70 (11) |
O1Bii—Cu—Caix | 78.39 (7) | GeB—O3B—GeBiii | 121.29 (12) |
O2A—Cu—Caix | 147.48 (8) | GeB—O3B—Cax | 107.80 (11) |
O1Bvi—Cu—Caix | 41.35 (6) | GeBiii—O3B—Cax | 100.22 (9) |
O1Avii—Cu—Caix | 42.12 (6) | GeB—O3B—Ca | 103.92 (10) |
GeBii—Cu—Caix | 83.311 (15) | GeBiii—O3B—Ca | 98.78 (10) |
Caviii—Cu—Caix | 126.56 (2) | Cax—O3B—Ca | 126.27 (9) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.869 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6631 reflections |
a = 10.1930 (12) Å | θ = 2.2–32.1° |
b = 9.2039 (7) Å | µ = 18.22 mm−1 |
c = 5.2078 (6) Å | T = 298 K |
β = 105.688 (12)° | Cuboid, pale green |
V = 470.37 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 2 diffractometer | 1622 independent reflections |
Plane graphite monochromator | 1438 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.038 |
rotation method scans | θmax = 32.2°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −15→15 |
Tmin = 0.093, Tmax = 0.158 | k = −13→13 |
5565 measured reflections | l = −7→7 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0237P)2 + 1.7862P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.030 | (Δ/σ)max < 0.001 |
wR(F2) = 0.063 | Δρmax = 0.85 e Å−3 |
S = 1.1 | Δρmin = −0.85 e Å−3 |
1622 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0108 (6) |
Crystal data top
CaCuGe2O6 | V = 470.37 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1930 (12) Å | µ = 18.22 mm−1 |
b = 9.2039 (7) Å | T = 298 K |
c = 5.2078 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.688 (12)° | |
Data collection top
STOE IPDS 2 diffractometer | 1622 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 1438 reflections with I > 2σ(I) |
Tmin = 0.093, Tmax = 0.158 | Rint = 0.038 |
5565 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.030 | 92 parameters |
wR(F2) = 0.063 | 0 restraints |
S = 1.1 | Δρmax = 0.85 e Å−3 |
1622 reflections | Δρmin = −0.85 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28320 (7) | 0.45269 (8) | 0.80882 (15) | 0.01293 (14) | |
Cu | 0.22733 (4) | 0.66143 (5) | 0.25622 (9) | 0.01126 (11) | |
GeA | 0.04917 (3) | 0.34917 (4) | 0.20951 (7) | 0.00973 (10) | |
GeB | 0.49106 (4) | 0.35081 (4) | 0.40114 (8) | 0.01033 (10) | |
O1A | −0.1270 (3) | 0.3615 (3) | 0.1151 (5) | 0.0125 (5) | |
O1B | 0.6584 (2) | 0.3200 (3) | 0.3790 (5) | 0.0116 (4) | |
O2A | 0.1460 (3) | 0.4890 (3) | 0.3758 (6) | 0.0152 (5) | |
O2B | 0.4321 (3) | 0.5221 (3) | 0.2614 (6) | 0.0141 (5) | |
O3A | 0.1030 (3) | 0.1946 (3) | 0.4203 (5) | 0.0125 (5) | |
O3B | 0.3998 (3) | 0.2513 (3) | 0.5885 (5) | 0.0123 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0125 (3) | 0.0131 (3) | 0.0125 (3) | 0.0001 (2) | 0.0020 (2) | 0.0008 (2) |
Cu | 0.01125 (18) | 0.01171 (19) | 0.00932 (19) | −0.00110 (14) | 0.00019 (14) | −0.00010 (15) |
GeA | 0.00842 (16) | 0.01059 (16) | 0.00942 (17) | −0.00051 (11) | 0.00113 (12) | −0.00034 (12) |
GeB | 0.00952 (16) | 0.01012 (16) | 0.01160 (18) | 0.00040 (12) | 0.00328 (12) | 0.00108 (12) |
O1A | 0.0103 (10) | 0.0151 (12) | 0.0106 (11) | 0.0005 (9) | 0.0004 (8) | −0.0015 (9) |
O1B | 0.0090 (10) | 0.0131 (11) | 0.0121 (11) | 0.0005 (8) | 0.0017 (8) | −0.0009 (9) |
O2A | 0.0161 (12) | 0.0126 (11) | 0.0139 (12) | −0.0053 (9) | −0.0012 (9) | −0.0017 (10) |
O2B | 0.0189 (12) | 0.0108 (11) | 0.0120 (12) | 0.0007 (9) | 0.0031 (9) | 0.0002 (9) |
O3A | 0.0131 (11) | 0.0139 (11) | 0.0114 (11) | 0.0035 (9) | 0.0052 (9) | 0.0038 (9) |
O3B | 0.0117 (11) | 0.0147 (11) | 0.0102 (12) | −0.0025 (9) | 0.0024 (9) | 0.0012 (9) |
Geometric parameters (Å, º) top
Ca—O2A | 2.334 (3) | GeA—Cax | 3.6069 (8) |
Ca—O1Ai | 2.441 (3) | GeB—O1B | 1.764 (2) |
Ca—O1Bii | 2.450 (3) | GeB—O2B | 1.772 (3) |
Ca—O3Biii | 2.474 (3) | GeB—O3B | 1.774 (3) |
Ca—O3Aiii | 2.475 (3) | GeB—O3Bx | 1.892 (3) |
Ca—O2Biv | 2.517 (3) | GeB—O2Bii | 2.080 (3) |
Ca—O3B | 2.627 (3) | GeB—GeBii | 2.9212 (8) |
Ca—O2Bii | 3.031 (3) | GeB—Cuii | 2.9439 (7) |
Ca—Cuiv | 3.1877 (9) | GeB—Caii | 3.3349 (8) |
Ca—GeBii | 3.3349 (8) | GeB—Caviii | 3.3688 (10) |
Ca—GeBiv | 3.3688 (10) | GeB—Cax | 3.4602 (8) |
Ca—Cu | 3.3780 (9) | O1A—Cuv | 1.939 (3) |
Cu—O1Av | 1.939 (3) | O1A—Cuxi | 2.293 (3) |
Cu—O1Bii | 1.949 (3) | O1A—Cai | 2.441 (3) |
Cu—O2A | 1.968 (3) | O1B—Cuii | 1.949 (3) |
Cu—O1Bvi | 2.104 (3) | O1B—Cuxii | 2.104 (3) |
Cu—O1Avii | 2.293 (3) | O1B—Caii | 2.450 (3) |
Cu—GeBii | 2.9439 (7) | O2B—GeBii | 2.080 (3) |
Cu—Caviii | 3.1877 (9) | O2B—Caviii | 2.517 (3) |
Cu—Caix | 3.5956 (9) | O2B—Caii | 3.031 (3) |
GeA—O2A | 1.708 (3) | O3A—GeAiii | 1.783 (3) |
GeA—O1A | 1.733 (3) | O3A—Cax | 2.475 (3) |
GeA—O3Ax | 1.783 (3) | O3B—GeBiii | 1.892 (3) |
GeA—O3A | 1.790 (3) | O3B—Cax | 2.474 (3) |
| | | |
O2A—Ca—O1Ai | 79.04 (10) | Ca—Cu—Caix | 120.67 (3) |
O2A—Ca—O1Bii | 68.82 (9) | O2A—GeA—O1A | 120.45 (13) |
O1Ai—Ca—O1Bii | 72.91 (9) | O2A—GeA—O3Ax | 109.31 (13) |
O2A—Ca—O3Biii | 138.09 (10) | O1A—GeA—O3Ax | 107.89 (13) |
O1Ai—Ca—O3Biii | 131.80 (10) | O2A—GeA—O3A | 104.40 (13) |
O1Bii—Ca—O3Biii | 138.87 (9) | O1A—GeA—O3A | 110.40 (12) |
O2A—Ca—O3Aiii | 90.93 (10) | O3Ax—GeA—O3A | 103.02 (9) |
O1Ai—Ca—O3Aiii | 77.73 (9) | O2A—GeA—Ca | 35.30 (10) |
O1Bii—Ca—O3Aiii | 146.84 (9) | O1A—GeA—Ca | 129.62 (9) |
O3Biii—Ca—O3Aiii | 73.44 (9) | O3Ax—GeA—Ca | 121.48 (9) |
O2A—Ca—O2Biv | 157.03 (10) | O3A—GeA—Ca | 69.42 (9) |
O1Ai—Ca—O2Biv | 85.68 (9) | O2A—GeA—Cax | 103.80 (10) |
O1Bii—Ca—O2Biv | 90.40 (9) | O1A—GeA—Cax | 133.30 (9) |
O3Biii—Ca—O2Biv | 64.50 (9) | O3Ax—GeA—Cax | 66.70 (9) |
O3Aiii—Ca—O2Biv | 102.54 (9) | O3A—GeA—Cax | 38.62 (8) |
O2A—Ca—O3B | 84.41 (9) | Ca—GeA—Cax | 79.48 (2) |
O1Ai—Ca—O3B | 163.17 (9) | O1B—GeB—O2B | 110.06 (13) |
O1Bii—Ca—O3B | 103.93 (9) | O1B—GeB—O3B | 127.84 (12) |
O3Biii—Ca—O3B | 61.30 (4) | O2B—GeB—O3B | 120.99 (13) |
O3Aiii—Ca—O3B | 99.68 (9) | O1B—GeB—O3Bx | 97.07 (12) |
O2Biv—Ca—O3B | 111.03 (9) | O2B—GeB—O3Bx | 93.18 (12) |
O2A—Ca—O2Bii | 102.45 (9) | O3B—GeB—O3Bx | 90.45 (8) |
O1Ai—Ca—O2Bii | 130.85 (8) | O1B—GeB—O2Bii | 89.75 (12) |
O1Bii—Ca—O2Bii | 62.78 (8) | O2B—GeB—O2Bii | 81.66 (13) |
O3Biii—Ca—O2Bii | 78.81 (8) | O3B—GeB—O2Bii | 87.67 (12) |
O3Aiii—Ca—O2Bii | 149.98 (8) | O3Bx—GeB—O2Bii | 172.57 (11) |
O2Biv—Ca—O2Bii | 74.88 (9) | O1B—GeB—GeBii | 101.82 (9) |
O3B—Ca—O2Bii | 55.96 (8) | O2B—GeB—GeBii | 44.78 (9) |
O2A—Ca—Cuiv | 116.18 (8) | O3B—GeB—GeBii | 106.46 (9) |
O1Ai—Ca—Cuiv | 37.42 (6) | O3Bx—GeB—GeBii | 137.69 (8) |
O1Bii—Ca—Cuiv | 83.56 (7) | O2Bii—GeB—GeBii | 36.89 (7) |
O3Biii—Ca—Cuiv | 100.34 (7) | O1B—GeB—Cuii | 39.79 (9) |
O3Aiii—Ca—Cuiv | 82.42 (6) | O2B—GeB—Cuii | 116.74 (9) |
O2Biv—Ca—Cuiv | 49.00 (6) | O3B—GeB—Cuii | 102.55 (9) |
O3B—Ca—Cuiv | 159.35 (7) | O3Bx—GeB—Cuii | 132.42 (8) |
O2Bii—Ca—Cuiv | 114.10 (6) | O2Bii—GeB—Cuii | 55.01 (8) |
O2A—Ca—GeBii | 83.79 (7) | GeBii—GeB—Cuii | 82.222 (18) |
O1Ai—Ca—GeBii | 102.21 (7) | O1B—GeB—Caii | 45.60 (9) |
O1Bii—Ca—GeBii | 30.96 (6) | O2B—GeB—Caii | 64.56 (9) |
O3Biii—Ca—GeBii | 109.90 (7) | O3B—GeB—Caii | 166.23 (9) |
O3Aiii—Ca—GeBii | 174.62 (7) | O3Bx—GeB—Caii | 102.10 (8) |
O2Biv—Ca—GeBii | 82.80 (7) | O2Bii—GeB—Caii | 80.58 (8) |
O3B—Ca—GeBii | 78.80 (6) | GeBii—GeB—Caii | 67.850 (19) |
O2Bii—Ca—GeBii | 31.87 (5) | Cuii—GeB—Caii | 64.747 (18) |
Cuiv—Ca—GeBii | 100.85 (2) | O1B—GeB—Caviii | 111.39 (9) |
O2A—Ca—GeBiv | 171.39 (8) | O2B—GeB—Caviii | 46.91 (9) |
O1Ai—Ca—GeBiv | 108.83 (7) | O3B—GeB—Caviii | 110.71 (9) |
O1Bii—Ca—GeBiv | 116.28 (7) | O3Bx—GeB—Caviii | 46.31 (8) |
O3Biii—Ca—GeBiv | 33.57 (6) | O2Bii—GeB—Caviii | 128.11 (8) |
O3Aiii—Ca—GeBiv | 87.46 (7) | GeBii—GeB—Caviii | 91.43 (2) |
O2Biv—Ca—GeBiv | 30.95 (6) | Cuii—GeB—Caviii | 146.56 (2) |
O3B—Ca—GeBiv | 87.52 (6) | Caii—GeB—Caviii | 82.40 (2) |
O2Bii—Ca—GeBiv | 75.29 (6) | O1B—GeB—Cax | 115.34 (9) |
Cuiv—Ca—GeBiv | 72.00 (2) | O2B—GeB—Cax | 122.29 (9) |
GeBii—Ca—GeBiv | 97.60 (2) | O3B—GeB—Cax | 42.88 (9) |
O2A—Ca—Cu | 34.56 (7) | O3Bx—GeB—Cax | 48.65 (8) |
O1Ai—Ca—Cu | 76.87 (7) | O2Bii—GeB—Cax | 130.39 (8) |
O1Bii—Ca—Cu | 34.66 (6) | GeBii—GeB—Cax | 141.76 (2) |
O3Biii—Ca—Cu | 151.22 (7) | Cuii—GeB—Cax | 120.889 (19) |
O3Aiii—Ca—Cu | 123.13 (7) | Caii—GeB—Cax | 147.470 (17) |
O2Biv—Ca—Cu | 125.00 (7) | Caviii—GeB—Cax | 83.55 (2) |
O3B—Ca—Cu | 91.21 (6) | O1B—GeB—Ca | 146.69 (9) |
O2Bii—Ca—Cu | 78.46 (6) | O2B—GeB—Ca | 79.47 (9) |
Cuiv—Ca—Cu | 104.93 (2) | O3B—GeB—Ca | 46.59 (9) |
GeBii—Ca—Cu | 52.017 (17) | O3Bx—GeB—Ca | 114.62 (8) |
GeBiv—Ca—Cu | 149.07 (3) | O2Bii—GeB—Ca | 59.31 (8) |
O1Av—Cu—O1Bii | 175.31 (11) | GeBii—GeB—Ca | 61.689 (18) |
O1Av—Cu—O2A | 94.24 (11) | Cuii—GeB—Ca | 107.03 (2) |
O1Bii—Cu—O2A | 87.36 (11) | Caii—GeB—Ca | 129.539 (16) |
O1Av—Cu—O1Bvi | 86.12 (11) | Caviii—GeB—Ca | 98.42 (2) |
O1Bii—Cu—O1Bvi | 91.52 (10) | Cax—GeB—Ca | 81.52 (2) |
O2A—Cu—O1Bvi | 169.76 (11) | GeA—O1A—Cuv | 120.17 (15) |
O1Av—Cu—O1Avii | 102.85 (11) | GeA—O1A—Cuxi | 111.98 (13) |
O1Bii—Cu—O1Avii | 80.84 (10) | Cuv—O1A—Cuxi | 92.71 (10) |
O2A—Cu—O1Avii | 107.22 (11) | GeA—O1A—Cai | 132.18 (14) |
O1Bvi—Cu—O1Avii | 82.62 (10) | Cuv—O1A—Cai | 92.69 (10) |
O1Av—Cu—GeBii | 139.92 (8) | Cuxi—O1A—Cai | 98.81 (10) |
O1Bii—Cu—GeBii | 35.40 (7) | GeB—O1B—Cuii | 104.81 (13) |
O2A—Cu—GeBii | 101.68 (8) | GeB—O1B—Cuxii | 140.01 (15) |
O1Bvi—Cu—GeBii | 72.07 (7) | Cuii—O1B—Cuxii | 98.52 (11) |
O1Avii—Cu—GeBii | 107.00 (7) | GeB—O1B—Caii | 103.45 (12) |
O1Av—Cu—Caviii | 49.89 (8) | Cuii—O1B—Caii | 99.72 (11) |
O1Bii—Cu—Caviii | 125.99 (8) | Cuxii—O1B—Caii | 104.05 (11) |
O2A—Cu—Caviii | 85.35 (9) | GeA—O2A—Cu | 133.02 (17) |
O1Bvi—Cu—Caviii | 87.08 (8) | GeA—O2A—Ca | 119.68 (14) |
O1Avii—Cu—Caviii | 151.60 (7) | Cu—O2A—Ca | 103.15 (11) |
GeBii—Cu—Caviii | 94.72 (2) | GeB—O2B—GeBii | 98.34 (13) |
O1Av—Cu—Ca | 135.19 (8) | GeB—O2B—Caviii | 102.14 (12) |
O1Bii—Cu—Ca | 45.63 (8) | GeBii—O2B—Caviii | 158.17 (13) |
O2A—Cu—Ca | 42.28 (8) | GeB—O2B—Caii | 83.56 (10) |
O1Bvi—Cu—Ca | 134.32 (8) | GeBii—O2B—Caii | 84.53 (9) |
O1Avii—Cu—Ca | 101.16 (7) | Caviii—O2B—Caii | 105.12 (9) |
GeBii—Cu—Ca | 63.237 (18) | GeAiii—O3A—GeA | 125.75 (15) |
Caviii—Cu—Ca | 104.93 (2) | GeAiii—O3A—Cax | 119.47 (12) |
O1Av—Cu—Caix | 102.33 (8) | GeA—O3A—Cax | 114.54 (12) |
O1Bii—Cu—Caix | 78.38 (8) | GeB—O3B—GeBiii | 121.37 (14) |
O2A—Cu—Caix | 147.57 (9) | GeB—O3B—Cax | 107.93 (13) |
O1Bvi—Cu—Caix | 41.37 (7) | GeBiii—O3B—Cax | 100.12 (11) |
O1Avii—Cu—Caix | 42.13 (7) | GeB—O3B—Ca | 104.03 (12) |
GeBii—Cu—Caix | 83.295 (17) | GeBiii—O3B—Ca | 98.62 (11) |
Caviii—Cu—Caix | 126.52 (3) | Cax—O3B—Ca | 126.19 (11) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.864 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2724 reflections |
a = 10.1944 (12) Å | θ = 2.1–27.7° |
b = 9.2078 (7) Å | µ = 18.20 mm−1 |
c = 5.2103 (6) Å | T = 328 K |
β = 105.699 (12)° | Cuboid, pale green |
V = 470.84 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1018 independent reflections |
Plane graphite monochromator | 827 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.038 |
rotation method scans | θmax = 27.8°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.091, Tmax = 0.161 | k = −11→12 |
3509 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 5 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0261P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.035 | (Δ/σ)max < 0.001 |
wR(F2) = 0.064 | Δρmax = 0.88 e Å−3 |
S = 1.16 | Δρmin = −0.90 e Å−3 |
1018 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0079 (6) |
Crystal data top
CaCuGe2O6 | V = 470.84 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1944 (12) Å | µ = 18.20 mm−1 |
b = 9.2078 (7) Å | T = 328 K |
c = 5.2103 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.699 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1018 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 827 reflections with I > 2σ(I) |
Tmin = 0.091, Tmax = 0.161 | Rint = 0.038 |
3509 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.035 | 92 parameters |
wR(F2) = 0.064 | 5 restraints |
S = 1.16 | Δρmax = 0.88 e Å−3 |
1018 reflections | Δρmin = −0.90 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28283 (13) | 0.45246 (14) | 0.8085 (3) | 0.0082 (3) | |
Cu | 0.22765 (8) | 0.66139 (8) | 0.25626 (15) | 0.0067 (2) | |
GeA | 0.04901 (6) | 0.34920 (7) | 0.20955 (13) | 0.00466 (18) | |
GeB | 0.49099 (6) | 0.35070 (7) | 0.40044 (14) | 0.00576 (18) | |
O1A | −0.1266 (4) | 0.3613 (3) | 0.1153 (9) | 0.0097 (10) | |
O1B | 0.6584 (4) | 0.3200 (5) | 0.3790 (4) | 0.0061 (9) | |
O2A | 0.1456 (5) | 0.4892 (5) | 0.3766 (11) | 0.0115 (11) | |
O2B | 0.4321 (3) | 0.5219 (4) | 0.2611 (10) | 0.0093 (10) | |
O3A | 0.1034 (4) | 0.1948 (3) | 0.4211 (6) | 0.0081 (10) | |
O3B | 0.4003 (5) | 0.2521 (5) | 0.5894 (10) | 0.0087 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0095 (6) | 0.0080 (5) | 0.0071 (7) | 0.0007 (5) | 0.0019 (5) | 0.0014 (5) |
Cu | 0.0078 (3) | 0.0066 (3) | 0.0045 (4) | −0.0017 (3) | −0.0002 (3) | −0.0002 (3) |
GeA | 0.0041 (3) | 0.0053 (3) | 0.0038 (3) | −0.0004 (2) | 0.0000 (2) | −0.0002 (2) |
GeB | 0.0057 (3) | 0.0047 (3) | 0.0075 (3) | 0.0006 (2) | 0.0028 (2) | 0.0013 (3) |
O1A | 0.007 (2) | 0.013 (2) | 0.008 (2) | 0.0010 (18) | 0.0009 (18) | −0.0035 (19) |
O1B | 0.007 (2) | 0.006 (2) | 0.005 (2) | 0.0009 (15) | 0.0021 (18) | 0.0006 (16) |
O2A | 0.018 (2) | 0.007 (2) | 0.008 (3) | −0.0070 (17) | 0.000 (2) | −0.0010 (18) |
O2B | 0.017 (2) | 0.004 (2) | 0.006 (2) | 0.0013 (17) | 0.002 (2) | −0.0006 (17) |
O3A | 0.009 (2) | 0.011 (2) | 0.005 (2) | 0.0022 (16) | 0.004 (2) | 0.0017 (17) |
O3B | 0.010 (2) | 0.011 (2) | 0.007 (2) | −0.0032 (17) | 0.0043 (19) | 0.0007 (18) |
Geometric parameters (Å, º) top
Ca—O2A | 2.331 (5) | GeA—Cax | 3.6052 (15) |
Ca—O1Ai | 2.445 (5) | GeB—O1B | 1.763 (5) |
Ca—O1Bii | 2.453 (5) | GeB—O2B | 1.771 (4) |
Ca—O3Aiii | 2.472 (3) | GeB—O3B | 1.773 (5) |
Ca—O3Biii | 2.485 (5) | GeB—O3Bx | 1.888 (5) |
Ca—O2Biv | 2.519 (5) | GeB—O2Bii | 2.086 (5) |
Ca—O3B | 2.623 (5) | GeB—GeBii | 2.9269 (14) |
Ca—O2Bii | 3.034 (3) | GeB—Cuii | 2.9432 (10) |
Ca—Cuiv | 3.1892 (17) | GeB—Caii | 3.3384 (16) |
Ca—GeBii | 3.3384 (16) | GeB—Caviii | 3.3693 (16) |
Ca—GeBiv | 3.3693 (16) | GeB—Cax | 3.4605 (15) |
Ca—Cu | 3.3794 (16) | O1A—Cuv | 1.943 (5) |
Cu—O1Av | 1.943 (5) | O1A—Cuxi | 2.2958 (10) |
Cu—O1Bii | 1.9481 (11) | O1A—Cai | 2.445 (5) |
Cu—O2A | 1.973 (5) | O1B—Cuii | 1.9481 (11) |
Cu—O1Bvi | 2.103 (5) | O1B—Cuxii | 2.103 (5) |
Cu—O1Avii | 2.2958 (10) | O1B—Caii | 2.453 (5) |
Cu—GeBii | 2.9432 (10) | O2B—GeBii | 2.086 (5) |
Cu—Caviii | 3.1892 (17) | O2B—Caviii | 2.519 (5) |
Cu—Caix | 3.5986 (15) | O2B—Caii | 3.034 (3) |
GeA—O2A | 1.710 (5) | O3A—GeAiii | 1.7838 (19) |
GeA—O1A | 1.727 (4) | O3A—Cax | 2.472 (3) |
GeA—O3Ax | 1.7838 (19) | O3B—GeBiii | 1.888 (5) |
GeA—O3A | 1.7920 (18) | O3B—Cax | 2.485 (5) |
| | | |
O2A—Ca—O1Ai | 78.93 (17) | Ca—Cu—Caix | 120.76 (5) |
O2A—Ca—O1Bii | 68.84 (12) | O2A—GeA—O1A | 120.4 (2) |
O1Ai—Ca—O1Bii | 72.88 (12) | O2A—GeA—O3Ax | 109.4 (2) |
O2A—Ca—O3Aiii | 91.11 (16) | O1A—GeA—O3Ax | 108.0 (2) |
O1Ai—Ca—O3Aiii | 77.87 (10) | O2A—GeA—O3A | 104.2 (2) |
O1Bii—Ca—O3Aiii | 147.05 (15) | O1A—GeA—O3A | 110.52 (14) |
O2A—Ca—O3Biii | 138.27 (17) | O3Ax—GeA—O3A | 102.88 (11) |
O1Ai—Ca—O3Biii | 131.84 (16) | O2A—GeA—Ca | 35.28 (17) |
O1Bii—Ca—O3Biii | 138.70 (15) | O1A—GeA—Ca | 129.66 (17) |
O3Aiii—Ca—O3Biii | 73.37 (16) | O3Ax—GeA—Ca | 121.33 (12) |
O2A—Ca—O2Biv | 156.93 (16) | O3A—GeA—Ca | 69.21 (14) |
O1Ai—Ca—O2Biv | 85.70 (12) | O2A—GeA—Cax | 103.91 (17) |
O1Bii—Ca—O2Biv | 90.31 (12) | O1A—GeA—Cax | 133.22 (11) |
O3Aiii—Ca—O2Biv | 102.44 (14) | O3Ax—GeA—Cax | 66.49 (15) |
O3Biii—Ca—O2Biv | 64.41 (15) | O3A—GeA—Cax | 38.60 (9) |
O2A—Ca—O3B | 84.67 (17) | Ca—GeA—Cax | 79.50 (4) |
O1Ai—Ca—O3B | 163.37 (16) | O1B—GeB—O2B | 110.08 (18) |
O1Bii—Ca—O3B | 103.77 (16) | O1B—GeB—O3B | 127.8 (2) |
O3Aiii—Ca—O3B | 99.88 (13) | O2B—GeB—O3B | 120.90 (19) |
O3Biii—Ca—O3B | 61.27 (7) | O1B—GeB—O3Bx | 97.07 (17) |
O2Biv—Ca—O3B | 110.77 (12) | O2B—GeB—O3Bx | 93.5 (2) |
O2A—Ca—O2Bii | 102.55 (18) | O3B—GeB—O3Bx | 90.68 (14) |
O1Ai—Ca—O2Bii | 130.70 (10) | O1B—GeB—O2Bii | 89.70 (10) |
O1Bii—Ca—O2Bii | 62.68 (13) | O2B—GeB—O2Bii | 81.6 (2) |
O3Aiii—Ca—O2Bii | 149.93 (13) | O3B—GeB—O2Bii | 87.2 (2) |
O3Biii—Ca—O2Bii | 78.76 (15) | O3Bx—GeB—O2Bii | 172.72 (15) |
O2Biv—Ca—O2Bii | 74.73 (15) | O1B—GeB—GeBii | 101.77 (13) |
O3B—Ca—O2Bii | 55.80 (13) | O2B—GeB—GeBii | 44.84 (16) |
O2A—Ca—Cuiv | 116.13 (14) | O3B—GeB—GeBii | 106.04 (17) |
O1Ai—Ca—Cuiv | 37.48 (11) | O3Bx—GeB—GeBii | 138.09 (15) |
O1Bii—Ca—Cuiv | 83.49 (10) | O2Bii—GeB—GeBii | 36.77 (11) |
O3Aiii—Ca—Cuiv | 82.48 (6) | O1B—GeB—Cuii | 39.78 (6) |
O3Biii—Ca—Cuiv | 100.28 (13) | O2B—GeB—Cuii | 116.70 (13) |
O2Biv—Ca—Cuiv | 48.96 (4) | O3B—GeB—Cuii | 102.25 (15) |
O3B—Ca—Cuiv | 159.11 (12) | O3Bx—GeB—Cuii | 132.30 (15) |
O2Bii—Ca—Cuiv | 113.88 (9) | O2Bii—GeB—Cuii | 54.97 (4) |
O2A—Ca—GeBii | 83.88 (13) | GeBii—GeB—Cuii | 82.11 (3) |
O1Ai—Ca—GeBii | 102.12 (6) | O1B—GeB—Caii | 45.61 (14) |
O1Bii—Ca—GeBii | 30.90 (11) | O2B—GeB—Caii | 64.57 (11) |
O3Aiii—Ca—GeBii | 174.88 (10) | O3B—GeB—Caii | 165.80 (16) |
O3Biii—Ca—GeBii | 109.78 (13) | O3Bx—GeB—Caii | 102.33 (17) |
O2Biv—Ca—GeBii | 82.64 (11) | O2Bii—GeB—Caii | 80.54 (13) |
O3B—Ca—GeBii | 78.65 (11) | GeBii—GeB—Caii | 67.85 (4) |
O2Bii—Ca—GeBii | 31.82 (8) | Cuii—GeB—Caii | 64.74 (3) |
Cuiv—Ca—GeBii | 100.67 (4) | O1B—GeB—Caviii | 111.55 (9) |
O2A—Ca—GeBiv | 171.51 (13) | O2B—GeB—Caviii | 46.96 (15) |
O1Ai—Ca—GeBiv | 108.85 (12) | O3B—GeB—Caviii | 110.91 (15) |
O1Bii—Ca—GeBiv | 116.16 (6) | O3Bx—GeB—Caviii | 46.61 (15) |
O3Aiii—Ca—GeBiv | 87.33 (10) | O2Bii—GeB—Caviii | 128.09 (10) |
O3Biii—Ca—GeBiv | 33.52 (11) | GeBii—GeB—Caviii | 91.53 (4) |
O2Biv—Ca—GeBiv | 30.93 (9) | Cuii—GeB—Caviii | 146.69 (4) |
O3B—Ca—GeBiv | 87.37 (11) | Caii—GeB—Caviii | 82.53 (4) |
O2Bii—Ca—GeBiv | 75.20 (10) | O1B—GeB—Cax | 115.46 (14) |
Cuiv—Ca—GeBiv | 71.95 (4) | O2B—GeB—Cax | 122.28 (13) |
GeBii—Ca—GeBiv | 97.47 (4) | O3B—GeB—Cax | 43.21 (16) |
O2A—Ca—Cu | 34.63 (12) | O3Bx—GeB—Cax | 48.49 (16) |
O1Ai—Ca—Cu | 76.90 (9) | O2Bii—GeB—Cax | 130.30 (14) |
O1Bii—Ca—Cu | 34.63 (4) | GeBii—GeB—Cax | 141.64 (4) |
O3Aiii—Ca—Cu | 123.44 (11) | Cuii—GeB—Cax | 120.93 (3) |
O3Biii—Ca—Cu | 151.13 (14) | Caii—GeB—Cax | 147.63 (3) |
O2Biv—Ca—Cu | 124.88 (12) | Caviii—GeB—Cax | 83.50 (4) |
O3B—Ca—Cu | 91.17 (12) | O1B—GeB—Ca | 146.58 (7) |
O2Bii—Ca—Cu | 78.35 (10) | O2B—GeB—Ca | 79.48 (13) |
Cuiv—Ca—Cu | 104.94 (4) | O3B—GeB—Ca | 46.29 (16) |
GeBii—Ca—Cu | 51.96 (3) | O3Bx—GeB—Ca | 114.65 (16) |
GeBiv—Ca—Cu | 148.90 (5) | O2Bii—GeB—Ca | 59.26 (9) |
O1Av—Cu—O1Bii | 175.59 (19) | GeBii—GeB—Ca | 61.65 (3) |
O1Av—Cu—O2A | 94.25 (15) | Cuii—GeB—Ca | 106.93 (4) |
O1Bii—Cu—O2A | 87.3 (2) | Caii—GeB—Ca | 129.50 (3) |
O1Av—Cu—O1Bvi | 86.15 (6) | Caviii—GeB—Ca | 98.38 (4) |
O1Bii—Cu—O1Bvi | 91.62 (13) | Cax—GeB—Ca | 81.42 (4) |
O2A—Cu—O1Bvi | 170.1 (2) | GeA—O1A—Cuv | 120.4 (2) |
O1Av—Cu—O1Avii | 102.59 (18) | GeA—O1A—Cuxi | 112.19 (17) |
O1Bii—Cu—O1Avii | 80.87 (18) | Cuv—O1A—Cuxi | 92.60 (13) |
O2A—Cu—O1Avii | 106.8 (2) | GeA—O1A—Cai | 132.1 (2) |
O1Bvi—Cu—O1Avii | 82.70 (18) | Cuv—O1A—Cai | 92.54 (17) |
O1Av—Cu—GeBii | 140.21 (13) | Cuxi—O1A—Cai | 98.72 (14) |
O1Bii—Cu—GeBii | 35.39 (14) | GeB—O1B—Cuii | 104.83 (19) |
O2A—Cu—GeBii | 101.75 (14) | GeB—O1B—Cuxii | 139.9 (2) |
O1Bvi—Cu—GeBii | 72.19 (6) | Cuii—O1B—Cuxii | 98.65 (16) |
O1Avii—Cu—GeBii | 107.07 (11) | GeB—O1B—Caii | 103.48 (18) |
O1Av—Cu—Caviii | 49.98 (14) | Cuii—O1B—Caii | 99.67 (16) |
O1Bii—Cu—Caviii | 126.16 (14) | Cuxii—O1B—Caii | 104.07 (19) |
O2A—Cu—Caviii | 85.49 (16) | GeA—O2A—Cu | 132.8 (3) |
O1Bvi—Cu—Caviii | 87.19 (12) | GeA—O2A—Ca | 119.6 (2) |
O1Avii—Cu—Caviii | 151.50 (13) | Cu—O2A—Ca | 103.2 (2) |
GeBii—Cu—Caviii | 94.93 (4) | GeB—O2B—GeBii | 98.4 (2) |
O1Av—Cu—Ca | 135.11 (7) | GeB—O2B—Caviii | 102.11 (19) |
O1Bii—Cu—Ca | 45.70 (13) | GeBii—O2B—Caviii | 158.10 (13) |
O2A—Cu—Ca | 42.18 (14) | GeB—O2B—Caii | 83.62 (7) |
O1Bvi—Cu—Ca | 134.51 (5) | GeBii—O2B—Caii | 84.50 (12) |
O1Avii—Cu—Ca | 101.11 (13) | Caviii—O2B—Caii | 105.27 (15) |
GeBii—Cu—Ca | 63.30 (3) | GeAiii—O3A—GeA | 125.70 (16) |
Caviii—Cu—Ca | 104.94 (4) | GeAiii—O3A—Cax | 119.60 (11) |
O1Av—Cu—Caix | 102.22 (9) | GeA—O3A—Cax | 114.51 (10) |
O1Bii—Cu—Caix | 78.44 (13) | GeB—O3B—GeBiii | 121.7 (3) |
O2A—Cu—Caix | 147.29 (17) | GeB—O3B—Cax | 107.5 (2) |
O1Bvi—Cu—Caix | 41.40 (13) | GeBiii—O3B—Cax | 99.9 (2) |
O1Avii—Cu—Caix | 42.18 (12) | GeB—O3B—Ca | 104.5 (2) |
GeBii—Cu—Caix | 83.38 (3) | GeBiii—O3B—Ca | 98.9 (2) |
Caviii—Cu—Caix | 126.61 (5) | Cax—O3B—Ca | 125.8 (2) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.858 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2661 reflections |
a = 10.1957 (12) Å | θ = 2.1–27.7° |
b = 9.2123 (7) Å | µ = 18.18 mm−1 |
c = 5.2142 (6) Å | T = 361 K |
β = 105.702 (12)° | Cuboid, pale green |
V = 471.47 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1040 independent reflections |
Plane graphite monochromator | 820 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.049 |
rotation method scans | θmax = 27.9°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.089, Tmax = 0.152 | k = −11→12 |
3763 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 3 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0263P)2 + 2.7574P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.038 | (Δ/σ)max < 0.001 |
wR(F2) = 0.073 | Δρmax = 0.93 e Å−3 |
S = 1.11 | Δρmin = −1.09 e Å−3 |
1040 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0081 (7) |
Crystal data top
CaCuGe2O6 | V = 471.47 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.1957 (12) Å | µ = 18.18 mm−1 |
b = 9.2123 (7) Å | T = 361 K |
c = 5.2142 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.702 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1040 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 820 reflections with I > 2σ(I) |
Tmin = 0.089, Tmax = 0.152 | Rint = 0.049 |
3763 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.038 | 92 parameters |
wR(F2) = 0.073 | 3 restraints |
S = 1.11 | Δρmax = 0.93 e Å−3 |
1040 reflections | Δρmin = −1.09 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28273 (15) | 0.45246 (16) | 0.8078 (3) | 0.0090 (3) | |
Cu | 0.22776 (9) | 0.66124 (10) | 0.25611 (17) | 0.0077 (2) | |
GeA | 0.04904 (7) | 0.34912 (8) | 0.20980 (15) | 0.0054 (2) | |
GeB | 0.49081 (7) | 0.35070 (8) | 0.39921 (16) | 0.0066 (2) | |
O1A | −0.1265 (5) | 0.3612 (6) | 0.1156 (11) | 0.0095 (10) | |
O1B | 0.6585 (4) | 0.3202 (5) | 0.3794 (4) | 0.0072 (10) | |
O2A | 0.1454 (5) | 0.4892 (4) | 0.3758 (10) | 0.0117 (12) | |
O2B | 0.4321 (3) | 0.5218 (5) | 0.2606 (11) | 0.0110 (11) | |
O3A | 0.1038 (5) | 0.1951 (5) | 0.4218 (11) | 0.0090 (11) | |
O3B | 0.4004 (5) | 0.2521 (6) | 0.5889 (11) | 0.0093 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0106 (7) | 0.0083 (6) | 0.0076 (7) | −0.0001 (6) | 0.0019 (6) | 0.0011 (6) |
Cu | 0.0090 (4) | 0.0075 (4) | 0.0055 (5) | −0.0016 (3) | −0.0003 (3) | 0.0002 (3) |
GeA | 0.0049 (3) | 0.0059 (3) | 0.0046 (4) | −0.0009 (3) | 0.0001 (3) | −0.0002 (3) |
GeB | 0.0065 (4) | 0.0052 (4) | 0.0086 (4) | 0.0007 (3) | 0.0030 (3) | 0.0014 (3) |
O1A | 0.005 (2) | 0.014 (3) | 0.009 (3) | 0.003 (2) | 0.001 (2) | −0.002 (2) |
O1B | 0.006 (2) | 0.008 (2) | 0.007 (3) | 0.0006 (17) | 0.001 (2) | −0.0026 (18) |
O2A | 0.015 (3) | 0.010 (3) | 0.008 (3) | −0.0069 (19) | −0.001 (2) | −0.002 (2) |
O2B | 0.019 (3) | 0.006 (2) | 0.007 (3) | 0.001 (2) | 0.002 (2) | 0.0016 (19) |
O3A | 0.011 (3) | 0.010 (3) | 0.006 (3) | 0.0042 (18) | 0.004 (2) | 0.0030 (19) |
O3B | 0.008 (2) | 0.012 (3) | 0.008 (3) | −0.0016 (19) | 0.002 (2) | 0.002 (2) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (5) | GeA—Cax | 3.6052 (17) |
Ca—O1Ai | 2.448 (5) | GeB—O1B | 1.763 (5) |
Ca—O1Bii | 2.452 (5) | GeB—O2B | 1.770 (4) |
Ca—O3Aiii | 2.473 (6) | GeB—O3B | 1.774 (6) |
Ca—O3Biii | 2.487 (6) | GeB—O3Bx | 1.886 (5) |
Ca—O2Biv | 2.521 (6) | GeB—O2Bii | 2.095 (5) |
Ca—O3B | 2.625 (6) | GeB—GeBii | 2.9325 (16) |
Ca—O2Bii | 3.033 (4) | GeB—Cuii | 2.9469 (12) |
Ca—Cuiv | 3.1917 (19) | GeB—Caii | 3.3366 (18) |
Ca—GeBii | 3.3366 (18) | GeB—Caviii | 3.3687 (18) |
Ca—GeBiv | 3.3687 (18) | GeB—Cax | 3.4614 (17) |
Ca—Cu | 3.3786 (18) | O1A—Cuv | 1.945 (5) |
Cu—O1Av | 1.945 (5) | O1A—Cuxi | 2.298 (6) |
Cu—O1Bii | 1.9475 (11) | O1A—Cai | 2.448 (5) |
Cu—O2A | 1.9726 (10) | O1B—Cuii | 1.9475 (11) |
Cu—O1Bvi | 2.105 (5) | O1B—Cuxii | 2.105 (5) |
Cu—O1Avii | 2.298 (6) | O1B—Caii | 2.452 (5) |
Cu—GeBii | 2.9469 (12) | O2B—GeBii | 2.095 (5) |
Cu—Caviii | 3.1917 (19) | O2B—Caviii | 2.521 (6) |
Cu—Caix | 3.6012 (17) | O2B—Caii | 3.033 (4) |
GeA—O2A | 1.709 (4) | O3A—GeAiii | 1.785 (6) |
GeA—O1A | 1.726 (5) | O3A—Cax | 2.473 (6) |
GeA—O3Ax | 1.785 (6) | O3B—GeBiii | 1.886 (5) |
GeA—O3A | 1.792 (5) | O3B—Cax | 2.487 (6) |
| | | |
O2A—Ca—O1Ai | 78.97 (19) | Ca—Cu—Caix | 120.81 (5) |
O2A—Ca—O1Bii | 68.86 (7) | O2A—GeA—O1A | 120.4 (3) |
O1Ai—Ca—O1Bii | 72.90 (19) | O2A—GeA—O3Ax | 109.3 (2) |
O2A—Ca—O3Aiii | 91.29 (14) | O1A—GeA—O3Ax | 108.1 (2) |
O1Ai—Ca—O3Aiii | 77.94 (19) | O2A—GeA—O3A | 104.2 (2) |
O1Bii—Ca—O3Aiii | 147.20 (18) | O1A—GeA—O3A | 110.6 (3) |
O2A—Ca—O3Biii | 138.30 (18) | O3Ax—GeA—O3A | 102.84 (19) |
O1Ai—Ca—O3Biii | 131.8 (2) | O2A—GeA—Ca | 35.40 (14) |
O1Bii—Ca—O3Biii | 138.64 (17) | O1A—GeA—Ca | 129.68 (19) |
O3Aiii—Ca—O3Biii | 73.25 (18) | O3Ax—GeA—Ca | 121.23 (17) |
O2A—Ca—O2Biv | 156.95 (16) | O3A—GeA—Ca | 69.10 (17) |
O1Ai—Ca—O2Biv | 85.65 (13) | O2A—GeA—Cax | 104.05 (19) |
O1Bii—Ca—O2Biv | 90.32 (14) | O1A—GeA—Cax | 133.18 (19) |
O3Aiii—Ca—O2Biv | 102.26 (18) | O3Ax—GeA—Cax | 66.32 (17) |
O3Biii—Ca—O2Biv | 64.36 (16) | O3A—GeA—Cax | 38.65 (19) |
O2A—Ca—O3B | 84.71 (19) | Ca—GeA—Cax | 79.58 (4) |
O1Ai—Ca—O3B | 163.45 (18) | O1B—GeB—O2B | 110.1 (2) |
O1Bii—Ca—O3B | 103.76 (18) | O1B—GeB—O3B | 127.6 (2) |
O3Aiii—Ca—O3B | 99.89 (18) | O2B—GeB—O3B | 121.0 (2) |
O3Biii—Ca—O3B | 61.26 (7) | O1B—GeB—O3Bx | 97.26 (19) |
O2Biv—Ca—O3B | 110.74 (13) | O2B—GeB—O3Bx | 93.7 (2) |
O2A—Ca—O2Bii | 102.66 (16) | O3B—GeB—O3Bx | 90.81 (16) |
O1Ai—Ca—O2Bii | 130.66 (16) | O1B—GeB—O2Bii | 89.50 (12) |
O1Bii—Ca—O2Bii | 62.70 (15) | O2B—GeB—O2Bii | 81.6 (2) |
O3Aiii—Ca—O2Bii | 149.80 (16) | O3B—GeB—O2Bii | 87.0 (2) |
O3Biii—Ca—O2Bii | 78.67 (17) | O3Bx—GeB—O2Bii | 172.80 (17) |
O2Biv—Ca—O2Bii | 74.63 (17) | O1B—GeB—GeBii | 101.62 (15) |
O3B—Ca—O2Bii | 55.83 (15) | O2B—GeB—GeBii | 44.97 (18) |
O2A—Ca—Cuiv | 116.19 (15) | O3B—GeB—GeBii | 105.85 (19) |
O1Ai—Ca—Cuiv | 37.50 (12) | O3Bx—GeB—GeBii | 138.36 (17) |
O1Bii—Ca—Cuiv | 83.52 (11) | O2Bii—GeB—GeBii | 36.66 (12) |
O3Aiii—Ca—Cuiv | 82.41 (14) | O1B—GeB—Cuii | 39.66 (6) |
O3Biii—Ca—Cuiv | 100.20 (14) | O2B—GeB—Cuii | 116.63 (16) |
O2Biv—Ca—Cuiv | 48.90 (5) | O3B—GeB—Cuii | 102.00 (17) |
O3B—Ca—Cuiv | 159.02 (13) | O3Bx—GeB—Cuii | 132.35 (17) |
O2Bii—Ca—Cuiv | 113.77 (11) | O2Bii—GeB—Cuii | 54.85 (4) |
O2A—Ca—GeBii | 84.03 (8) | GeBii—GeB—Cuii | 81.91 (3) |
O1Ai—Ca—GeBii | 102.10 (14) | O1B—GeB—Caii | 45.62 (16) |
O1Bii—Ca—GeBii | 30.92 (12) | O2B—GeB—Caii | 64.59 (13) |
O3Aiii—Ca—GeBii | 175.21 (14) | O3B—GeB—Caii | 165.51 (17) |
O3Biii—Ca—GeBii | 109.67 (14) | O3Bx—GeB—Caii | 102.45 (19) |
O2Biv—Ca—GeBii | 82.51 (13) | O2Bii—GeB—Caii | 80.53 (14) |
O3B—Ca—GeBii | 78.69 (13) | GeBii—GeB—Caii | 67.88 (4) |
O2Bii—Ca—GeBii | 31.81 (9) | Cuii—GeB—Caii | 64.71 (3) |
Cuiv—Ca—GeBii | 100.57 (5) | O1B—GeB—Caviii | 111.78 (10) |
O2A—Ca—GeBiv | 171.50 (14) | O2B—GeB—Caviii | 47.05 (18) |
O1Ai—Ca—GeBiv | 108.80 (13) | O3B—GeB—Caviii | 111.06 (17) |
O1Bii—Ca—GeBiv | 116.16 (7) | O3Bx—GeB—Caviii | 46.67 (17) |
O3Aiii—Ca—GeBiv | 87.13 (13) | O2Bii—GeB—Caviii | 128.18 (11) |
O3Biii—Ca—GeBiv | 33.47 (13) | GeBii—GeB—Caviii | 91.74 (4) |
O2Biv—Ca—GeBiv | 30.92 (10) | Cuii—GeB—Caviii | 146.79 (4) |
O3B—Ca—GeBiv | 87.34 (12) | Caii—GeB—Caviii | 82.65 (4) |
O2Bii—Ca—GeBiv | 75.11 (11) | O1B—GeB—Cax | 115.56 (16) |
Cuiv—Ca—GeBiv | 71.89 (4) | O2B—GeB—Cax | 122.38 (15) |
GeBii—Ca—GeBiv | 97.35 (4) | O3B—GeB—Cax | 43.27 (18) |
O2A—Ca—Cu | 34.66 (5) | O3Bx—GeB—Cax | 48.53 (18) |
O1Ai—Ca—Cu | 76.96 (14) | O2Bii—GeB—Cax | 130.12 (15) |
O1Bii—Ca—Cu | 34.62 (4) | GeBii—GeB—Cax | 141.59 (5) |
O3Aiii—Ca—Cu | 123.66 (13) | Cuii—GeB—Cax | 120.88 (4) |
O3Biii—Ca—Cu | 151.09 (15) | Caii—GeB—Cax | 147.77 (4) |
O2Biv—Ca—Cu | 124.89 (14) | Caviii—GeB—Cax | 83.56 (5) |
O3B—Ca—Cu | 91.16 (13) | O1B—GeB—Ca | 146.27 (8) |
O2Bii—Ca—Cu | 78.40 (11) | O2B—GeB—Ca | 79.46 (14) |
Cuiv—Ca—Cu | 105.01 (5) | O3B—GeB—Ca | 46.30 (18) |
GeBii—Ca—Cu | 52.05 (3) | O3Bx—GeB—Ca | 114.75 (18) |
GeBiv—Ca—Cu | 148.88 (5) | O2Bii—GeB—Ca | 59.15 (10) |
O1Av—Cu—O1Bii | 175.7 (2) | GeBii—GeB—Ca | 61.53 (4) |
O1Av—Cu—O2A | 94.2 (2) | Cuii—GeB—Ca | 106.74 (4) |
O1Bii—Cu—O2A | 87.3 (2) | Caii—GeB—Ca | 129.41 (3) |
O1Av—Cu—O1Bvi | 86.07 (17) | Caviii—GeB—Ca | 98.43 (4) |
O1Bii—Cu—O1Bvi | 91.72 (15) | Cax—GeB—Ca | 81.42 (5) |
O2A—Cu—O1Bvi | 170.2 (2) | GeA—O1A—Cuv | 120.5 (3) |
O1Av—Cu—O1Avii | 102.5 (2) | GeA—O1A—Cuxi | 112.2 (3) |
O1Bii—Cu—O1Avii | 80.88 (19) | Cuv—O1A—Cuxi | 92.6 (2) |
O2A—Cu—O1Avii | 106.8 (2) | GeA—O1A—Cai | 132.0 (3) |
O1Bvi—Cu—O1Avii | 82.6 (2) | Cuv—O1A—Cai | 92.50 (19) |
O1Av—Cu—GeBii | 140.41 (16) | Cuxi—O1A—Cai | 98.7 (2) |
O1Bii—Cu—GeBii | 35.30 (16) | GeB—O1B—Cuii | 105.0 (2) |
O2A—Cu—GeBii | 101.81 (16) | GeB—O1B—Cuxii | 139.6 (2) |
O1Bvi—Cu—GeBii | 72.35 (7) | Cuii—O1B—Cuxii | 98.74 (17) |
O1Avii—Cu—GeBii | 107.01 (13) | GeB—O1B—Caii | 103.5 (2) |
O1Av—Cu—Caviii | 50.01 (16) | Cuii—O1B—Caii | 99.71 (18) |
O1Bii—Cu—Caviii | 126.25 (16) | Cuxii—O1B—Caii | 104.1 (2) |
O2A—Cu—Caviii | 85.51 (18) | GeA—O2A—Cu | 133.0 (3) |
O1Bvi—Cu—Caviii | 87.23 (13) | GeA—O2A—Ca | 119.50 (15) |
O1Avii—Cu—Caviii | 151.41 (14) | Cu—O2A—Ca | 103.09 (19) |
GeBii—Cu—Caviii | 95.12 (4) | GeB—O2B—GeBii | 98.4 (2) |
O1Av—Cu—Ca | 135.16 (17) | GeB—O2B—Caviii | 102.0 (2) |
O1Bii—Cu—Ca | 45.67 (15) | GeBii—O2B—Caviii | 158.16 (14) |
O2A—Cu—Ca | 42.26 (16) | GeB—O2B—Caii | 83.60 (8) |
O1Bvi—Cu—Ca | 134.61 (5) | GeBii—O2B—Caii | 84.48 (14) |
O1Avii—Cu—Ca | 101.10 (14) | Caviii—O2B—Caii | 105.37 (16) |
GeBii—Cu—Ca | 63.24 (3) | GeAiii—O3A—GeA | 125.7 (3) |
Caviii—Cu—Ca | 105.01 (5) | GeAiii—O3A—Cax | 119.7 (2) |
O1Av—Cu—Caix | 102.08 (17) | GeA—O3A—Cax | 114.4 (3) |
O1Bii—Cu—Caix | 78.52 (15) | GeB—O3B—GeBiii | 121.9 (3) |
O2A—Cu—Caix | 147.28 (18) | GeB—O3B—Cax | 107.5 (3) |
O1Bvi—Cu—Caix | 41.32 (14) | GeBiii—O3B—Cax | 99.9 (2) |
O1Avii—Cu—Caix | 42.21 (13) | GeB—O3B—Ca | 104.5 (2) |
GeBii—Cu—Caix | 83.40 (3) | GeBiii—O3B—Ca | 98.9 (2) |
Caviii—Cu—Caix | 126.56 (6) | Cax—O3B—Ca | 125.8 (2) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.838 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2594 reflections |
a = 10.2047 (12) Å | θ = 2.1–27.7° |
b = 9.2255 (7) Å | µ = 18.11 mm−1 |
c = 5.2249 (6) Å | T = 470 K |
β = 105.785 (12)° | Cuboid, pale green |
V = 473.34 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1041 independent reflections |
Plane graphite monochromator | 814 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.047 |
rotation method scans | θmax = 27.9°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −11→12 |
3745 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 4 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0313P)2 + 1.3224P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.040 | (Δ/σ)max < 0.001 |
wR(F2) = 0.078 | Δρmax = 0.97 e Å−3 |
S = 1.14 | Δρmin = −0.89 e Å−3 |
1041 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0071 (7) |
Crystal data top
CaCuGe2O6 | V = 473.34 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2047 (12) Å | µ = 18.11 mm−1 |
b = 9.2255 (7) Å | T = 470 K |
c = 5.2249 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.785 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1041 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 814 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0.047 |
3745 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 92 parameters |
wR(F2) = 0.078 | 4 restraints |
S = 1.14 | Δρmax = 0.97 e Å−3 |
1041 reflections | Δρmin = −0.89 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28207 (16) | 0.45236 (17) | 0.8061 (3) | 0.0125 (3) | |
Cu | 0.22814 (9) | 0.66100 (10) | 0.25558 (18) | 0.0102 (3) | |
GeA | 0.04877 (8) | 0.34914 (9) | 0.21022 (16) | 0.0075 (2) | |
GeB | 0.49029 (8) | 0.35038 (9) | 0.39552 (17) | 0.0091 (2) | |
O1A | −0.1266 (2) | 0.36097 (19) | 0.1159 (3) | 0.0111 (11) | |
O1B | 0.6583 (5) | 0.3203 (6) | 0.3804 (11) | 0.0079 (11) | |
O2A | 0.1447 (6) | 0.4899 (6) | 0.3751 (13) | 0.0155 (13) | |
O2B | 0.4315 (6) | 0.5209 (6) | 0.2594 (7) | 0.0144 (12) | |
O3A | 0.1038 (6) | 0.1953 (6) | 0.4239 (12) | 0.0114 (12) | |
O3B | 0.4003 (6) | 0.2524 (6) | 0.5852 (12) | 0.0128 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0141 (7) | 0.0114 (7) | 0.0114 (8) | 0.0005 (6) | 0.0024 (6) | 0.0009 (6) |
Cu | 0.0114 (4) | 0.0095 (4) | 0.0079 (5) | −0.0025 (4) | −0.0006 (4) | −0.0005 (4) |
GeA | 0.0069 (4) | 0.0076 (4) | 0.0071 (4) | −0.0010 (3) | 0.0004 (3) | −0.0002 (3) |
GeB | 0.0081 (4) | 0.0070 (4) | 0.0129 (4) | 0.0014 (3) | 0.0039 (3) | 0.0018 (3) |
O1A | 0.006 (2) | 0.018 (3) | 0.008 (3) | 0.004 (2) | 0.001 (2) | −0.001 (2) |
O1B | 0.007 (2) | 0.007 (2) | 0.009 (3) | 0.0009 (18) | 0.001 (2) | 0.0002 (19) |
O2A | 0.021 (3) | 0.011 (3) | 0.012 (3) | −0.008 (2) | 0.000 (3) | −0.001 (2) |
O2B | 0.023 (3) | 0.005 (2) | 0.014 (3) | 0.002 (2) | 0.003 (2) | 0.003 (2) |
O3A | 0.015 (3) | 0.010 (3) | 0.010 (3) | 0.0035 (19) | 0.005 (2) | 0.005 (2) |
O3B | 0.012 (3) | 0.018 (3) | 0.009 (3) | −0.004 (2) | 0.004 (2) | 0.001 (2) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (6) | GeA—Cax | 3.6064 (18) |
Ca—O1Ai | 2.450 (2) | GeB—O1B | 1.759 (5) |
Ca—O1Bii | 2.458 (6) | GeB—O2B | 1.763 (5) |
Ca—O3Aiii | 2.481 (6) | GeB—O3B | 1.771 (6) |
Ca—O3Biii | 2.489 (6) | GeB—O3Bx | 1.887 (6) |
Ca—O2Biv | 2.524 (2) | GeB—O2Bii | 2.125 (3) |
Ca—O3B | 2.636 (7) | GeB—Cuii | 2.9564 (12) |
Ca—O2Bii | 3.044 (7) | GeB—Caii | 3.3390 (19) |
Ca—Cuiv | 3.198 (2) | GeB—Caviii | 3.3651 (19) |
Ca—GeBii | 3.3390 (19) | GeB—Cax | 3.4632 (18) |
Ca—GeBiv | 3.3651 (19) | O1A—Cuv | 1.9461 (11) |
Ca—Cu | 3.379 (2) | O1A—Cuxi | 2.3036 (10) |
Cu—O1Av | 1.9461 (11) | O1A—Cai | 2.450 (2) |
Cu—O1Bii | 1.947 (5) | O1B—Cuii | 1.947 (5) |
Cu—O2A | 1.973 (6) | O1B—Cuxii | 2.111 (6) |
Cu—O1Bvi | 2.111 (6) | O1B—Caii | 2.458 (6) |
Cu—O1Avii | 2.3036 (10) | O2B—GeBii | 2.125 (3) |
Cu—GeBii | 2.9564 (12) | O2B—Caviii | 2.524 (2) |
Cu—Caviii | 3.198 (2) | O2B—Caii | 3.044 (7) |
Cu—Caix | 3.6078 (18) | O3A—GeAiii | 1.783 (6) |
GeA—O2A | 1.711 (6) | O3A—Cax | 2.481 (6) |
GeA—O1A | 1.726 (2) | O3B—GeBiii | 1.887 (6) |
GeA—O3Ax | 1.783 (6) | O3B—Cax | 2.489 (6) |
GeA—O3A | 1.798 (5) | | |
| | | |
O2A—Ca—O1Ai | 79.03 (17) | O2A—Cu—Caix | 146.9 (2) |
O2A—Ca—O1Bii | 68.84 (19) | O1Bvi—Cu—Caix | 41.37 (15) |
O1Ai—Ca—O1Bii | 73.00 (14) | O1Avii—Cu—Caix | 42.16 (6) |
O2A—Ca—O3Aiii | 91.9 (2) | GeBii—Cu—Caix | 83.49 (4) |
O1Ai—Ca—O3Aiii | 78.04 (14) | Caviii—Cu—Caix | 126.55 (6) |
O1Bii—Ca—O3Aiii | 147.61 (19) | Ca—Cu—Caix | 120.97 (6) |
O2A—Ca—O3Biii | 138.3 (2) | O2A—GeA—O1A | 120.2 (2) |
O1Ai—Ca—O3Biii | 131.98 (17) | O2A—GeA—O3Ax | 109.2 (3) |
O1Bii—Ca—O3Biii | 138.33 (19) | O1A—GeA—O3Ax | 108.28 (19) |
O3Aiii—Ca—O3Biii | 73.11 (19) | O2A—GeA—O3A | 104.3 (3) |
O2A—Ca—O2Biv | 156.9 (2) | O1A—GeA—O3A | 110.6 (2) |
O1Ai—Ca—O2Biv | 85.47 (15) | O3Ax—GeA—O3A | 102.9 (2) |
O1Bii—Ca—O2Biv | 90.39 (19) | O2A—GeA—Ca | 35.7 (2) |
O3Aiii—Ca—O2Biv | 101.6 (2) | O1A—GeA—Ca | 129.71 (7) |
O3Biii—Ca—O2Biv | 64.35 (19) | O3Ax—GeA—Ca | 121.07 (18) |
O2A—Ca—O3B | 84.7 (2) | O3A—GeA—Ca | 68.93 (18) |
O1Ai—Ca—O3B | 163.57 (15) | O2A—GeA—Cax | 104.5 (2) |
O1Bii—Ca—O3B | 103.4 (2) | O1A—GeA—Cax | 133.05 (8) |
O3Aiii—Ca—O3B | 100.27 (19) | O3Ax—GeA—Cax | 65.96 (18) |
O3Biii—Ca—O3B | 61.22 (8) | O3A—GeA—Cax | 39.0 (2) |
O2Biv—Ca—O3B | 110.76 (19) | Ca—GeA—Cax | 79.78 (5) |
O2A—Ca—O2Bii | 102.86 (19) | O1B—GeB—O2B | 110.6 (3) |
O1Ai—Ca—O2Bii | 130.30 (12) | O1B—GeB—O3B | 127.2 (3) |
O1Bii—Ca—O2Bii | 62.43 (16) | O2B—GeB—O3B | 120.6 (3) |
O3Aiii—Ca—O2Bii | 149.77 (17) | O1B—GeB—O3Bx | 97.7 (3) |
O3Biii—Ca—O2Bii | 78.47 (18) | O2B—GeB—O3Bx | 94.0 (2) |
O2Biv—Ca—O2Bii | 74.4 (2) | O3B—GeB—O3Bx | 91.11 (17) |
O3B—Ca—O2Bii | 55.92 (15) | O1B—GeB—O2Bii | 88.9 (2) |
O2A—Ca—Cuiv | 116.19 (17) | O2B—GeB—O2Bii | 81.46 (15) |
O1Ai—Ca—Cuiv | 37.44 (4) | O3B—GeB—O2Bii | 86.7 (3) |
O1Bii—Ca—Cuiv | 83.58 (14) | O3Bx—GeB—O2Bii | 173.0 (2) |
O3Aiii—Ca—Cuiv | 82.19 (14) | O1B—GeB—Cuii | 39.35 (18) |
O3Biii—Ca—Cuiv | 100.34 (16) | O2B—GeB—Cuii | 116.59 (15) |
O2Biv—Ca—Cuiv | 48.76 (14) | O3B—GeB—Cuii | 101.62 (18) |
O3B—Ca—Cuiv | 158.98 (14) | O3Bx—GeB—Cuii | 132.53 (18) |
O2Bii—Ca—Cuiv | 113.33 (10) | O2Bii—GeB—Cuii | 54.48 (16) |
O2A—Ca—GeBii | 84.34 (16) | O1B—GeB—Caii | 45.72 (17) |
O1Ai—Ca—GeBii | 101.95 (6) | O2B—GeB—Caii | 64.9 (2) |
O1Bii—Ca—GeBii | 30.82 (12) | O3B—GeB—Caii | 164.94 (19) |
O3Aiii—Ca—GeBii | 176.11 (15) | O3Bx—GeB—Caii | 102.7 (2) |
O3Biii—Ca—GeBii | 109.29 (15) | O2Bii—GeB—Caii | 80.21 (18) |
O2Biv—Ca—GeBii | 82.25 (16) | Cuii—GeB—Caii | 64.60 (4) |
O3B—Ca—GeBii | 78.62 (14) | O1B—GeB—Caviii | 112.54 (19) |
O2Bii—Ca—GeBii | 31.63 (10) | O2B—GeB—Caviii | 47.19 (8) |
Cuiv—Ca—GeBii | 100.20 (5) | O3B—GeB—Caviii | 111.13 (18) |
O2A—Ca—GeBiv | 171.60 (16) | O3Bx—GeB—Caviii | 46.81 (18) |
O1Ai—Ca—GeBiv | 108.70 (7) | O2Bii—GeB—Caviii | 128.17 (14) |
O1Bii—Ca—GeBiv | 116.01 (13) | Cuii—GeB—Caviii | 147.15 (5) |
O3Aiii—Ca—GeBiv | 86.71 (14) | Caii—GeB—Caviii | 83.06 (5) |
O3Biii—Ca—GeBiv | 33.56 (14) | O1B—GeB—Cax | 115.87 (17) |
O2Biv—Ca—GeBiv | 30.82 (12) | O2B—GeB—Cax | 122.42 (16) |
O3B—Ca—GeBiv | 87.40 (13) | O3B—GeB—Cax | 43.2 (2) |
O2Bii—Ca—GeBiv | 74.87 (9) | O3Bx—GeB—Cax | 48.8 (2) |
Cuiv—Ca—GeBiv | 71.83 (4) | O2Bii—GeB—Cax | 129.82 (18) |
GeBii—Ca—GeBiv | 96.94 (5) | Cuii—GeB—Cax | 120.81 (4) |
O2A—Ca—Cu | 34.67 (14) | Caii—GeB—Cax | 148.32 (4) |
O1Ai—Ca—Cu | 77.19 (5) | Caviii—GeB—Cax | 83.71 (5) |
O1Bii—Ca—Cu | 34.62 (12) | O1B—GeB—Ca | 145.44 (18) |
O3Aiii—Ca—Cu | 124.28 (14) | O2B—GeB—Ca | 79.2 (2) |
O3Biii—Ca—Cu | 150.67 (17) | O3B—GeB—Ca | 46.2 (2) |
O2Biv—Ca—Cu | 124.97 (14) | O3Bx—GeB—Ca | 115.04 (19) |
O3B—Ca—Cu | 90.80 (14) | O2Bii—GeB—Ca | 59.01 (18) |
O2Bii—Ca—Cu | 78.29 (10) | Cuii—GeB—Ca | 106.21 (4) |
Cuiv—Ca—Cu | 105.16 (5) | Caii—GeB—Ca | 129.15 (4) |
GeBii—Ca—Cu | 52.21 (3) | Caviii—GeB—Ca | 98.45 (4) |
GeBiv—Ca—Cu | 148.68 (6) | Cax—GeB—Ca | 81.28 (5) |
O1Av—Cu—O1Bii | 175.82 (19) | GeA—O1A—Cuv | 120.51 (11) |
O1Av—Cu—O2A | 94.22 (18) | GeA—O1A—Cuxi | 112.32 (9) |
O1Bii—Cu—O2A | 87.4 (2) | Cuv—O1A—Cuxi | 92.73 (6) |
O1Av—Cu—O1Bvi | 85.93 (15) | GeA—O1A—Cai | 131.70 (9) |
O1Bii—Cu—O1Bvi | 91.81 (19) | Cuv—O1A—Cai | 92.64 (10) |
O2A—Cu—O1Bvi | 170.7 (2) | Cuxi—O1A—Cai | 98.71 (9) |
O1Av—Cu—O1Avii | 102.39 (9) | GeB—O1B—Cuii | 105.7 (3) |
O1Bii—Cu—O1Avii | 80.78 (16) | GeB—O1B—Cuxii | 139.1 (3) |
O2A—Cu—O1Avii | 106.3 (2) | Cuii—O1B—Cuxii | 98.9 (2) |
O1Bvi—Cu—O1Avii | 82.66 (17) | GeB—O1B—Caii | 103.5 (2) |
O1Av—Cu—GeBii | 140.87 (8) | Cuii—O1B—Caii | 99.5 (2) |
O1Bii—Cu—GeBii | 34.95 (17) | Cuxii—O1B—Caii | 104.0 (2) |
O2A—Cu—GeBii | 101.96 (17) | GeA—O2A—Cu | 133.2 (4) |
O1Bvi—Cu—GeBii | 72.65 (14) | GeA—O2A—Ca | 119.0 (3) |
O1Avii—Cu—GeBii | 106.71 (5) | Cu—O2A—Ca | 103.1 (2) |
O1Av—Cu—Caviii | 49.93 (7) | GeB—O2B—GeBii | 98.54 (15) |
O1Bii—Cu—Caviii | 126.51 (17) | GeB—O2B—Caviii | 101.98 (18) |
O2A—Cu—Caviii | 85.8 (2) | GeBii—O2B—Caviii | 158.1 (3) |
O1Bvi—Cu—Caviii | 87.25 (16) | GeB—O2B—Caii | 83.4 (2) |
O1Avii—Cu—Caviii | 151.29 (4) | GeBii—O2B—Caii | 84.23 (17) |
GeBii—Cu—Caviii | 95.68 (4) | Caviii—O2B—Caii | 105.6 (2) |
O1Av—Cu—Ca | 135.13 (8) | GeAiii—O3A—GeA | 125.9 (3) |
O1Bii—Cu—Ca | 45.83 (16) | GeAiii—O3A—Cax | 120.1 (3) |
O2A—Cu—Ca | 42.24 (17) | GeA—O3A—Cax | 113.9 (3) |
O1Bvi—Cu—Ca | 134.89 (15) | GeB—O3B—GeBiii | 122.2 (3) |
O1Avii—Cu—Ca | 100.95 (6) | GeB—O3B—Cax | 107.6 (3) |
GeBii—Cu—Ca | 63.19 (4) | GeBiii—O3B—Cax | 99.6 (2) |
Caviii—Cu—Ca | 105.16 (5) | GeB—O3B—Ca | 104.9 (3) |
O1Av—Cu—Caix | 101.84 (7) | GeBiii—O3B—Ca | 98.6 (3) |
O1Bii—Cu—Caix | 78.61 (16) | Cax—O3B—Ca | 125.5 (2) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.82 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2501 reflections |
a = 10.2130 (12) Å | θ = 2.1–27.7° |
b = 9.2385 (7) Å | µ = 18.04 mm−1 |
c = 5.2359 (6) Å | T = 570 K |
β = 105.870 (12)° | Cuboid, pale green |
V = 475.19 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1032 independent reflections |
Plane graphite monochromator | 795 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.048 |
rotation method scans | θmax = 28.0°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −12→12 |
3696 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 5 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0395P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.043 | (Δ/σ)max < 0.001 |
wR(F2) = 0.085 | Δρmax = 1.15 e Å−3 |
S = 1.11 | Δρmin = −0.85 e Å−3 |
1032 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0068 (8) |
Crystal data top
CaCuGe2O6 | V = 475.19 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2130 (12) Å | µ = 18.04 mm−1 |
b = 9.2385 (7) Å | T = 570 K |
c = 5.2359 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.870 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1032 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 795 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0.048 |
3696 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.043 | 92 parameters |
wR(F2) = 0.085 | 5 restraints |
S = 1.11 | Δρmax = 1.15 e Å−3 |
1032 reflections | Δρmin = −0.85 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28122 (16) | 0.45209 (17) | 0.8037 (3) | 0.0155 (4) | |
Cu | 0.22867 (10) | 0.66057 (10) | 0.25525 (19) | 0.0127 (3) | |
GeA | 0.04836 (8) | 0.34917 (9) | 0.21064 (16) | 0.0089 (2) | |
GeB | 0.48966 (8) | 0.35011 (9) | 0.39090 (18) | 0.0120 (2) | |
O1A | −0.1271 (2) | 0.3601 (5) | 0.1164 (11) | 0.0141 (12) | |
O1B | 0.6581 (4) | 0.3205 (2) | 0.3818 (9) | 0.0112 (12) | |
O2A | 0.1434 (4) | 0.4909 (3) | 0.3742 (5) | 0.0185 (14) | |
O2B | 0.4310 (4) | 0.5198 (6) | 0.2578 (14) | 0.0194 (14) | |
O3A | 0.1033 (5) | 0.1963 (4) | 0.4258 (8) | 0.0146 (13) | |
O3B | 0.4003 (5) | 0.2532 (6) | 0.5817 (10) | 0.0138 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0164 (8) | 0.0148 (7) | 0.0144 (9) | 0.0018 (7) | 0.0031 (7) | 0.0022 (7) |
Cu | 0.0139 (5) | 0.0120 (4) | 0.0096 (5) | −0.0026 (4) | −0.0010 (4) | 0.0003 (4) |
GeA | 0.0079 (4) | 0.0090 (4) | 0.0089 (4) | −0.0010 (3) | 0.0006 (3) | −0.0006 (3) |
GeB | 0.0102 (4) | 0.0096 (4) | 0.0171 (5) | 0.0013 (3) | 0.0051 (3) | 0.0031 (3) |
O1A | 0.010 (2) | 0.019 (3) | 0.012 (3) | 0.001 (2) | 0.001 (2) | −0.002 (2) |
O1B | 0.011 (3) | 0.010 (3) | 0.012 (3) | −0.0002 (19) | 0.001 (2) | −0.002 (2) |
O2A | 0.024 (3) | 0.012 (3) | 0.015 (3) | −0.007 (2) | −0.004 (3) | 0.001 (2) |
O2B | 0.028 (3) | 0.010 (3) | 0.020 (4) | 0.004 (2) | 0.005 (3) | 0.004 (2) |
O3A | 0.017 (3) | 0.018 (3) | 0.011 (3) | 0.005 (2) | 0.009 (3) | 0.004 (2) |
O3B | 0.011 (3) | 0.018 (3) | 0.012 (3) | −0.006 (2) | 0.004 (2) | 0.002 (2) |
Geometric parameters (Å, º) top
Ca—O2A | 2.3315 (19) | GeA—O3A | 1.7981 (17) |
Ca—O1Ai | 2.4539 (19) | GeA—Cax | 3.6063 (17) |
Ca—O1Bii | 2.464 (2) | GeB—O2B | 1.754 (5) |
Ca—O3Aiii | 2.4946 (18) | GeB—O1B | 1.755 (3) |
Ca—O3Biii | 2.495 (6) | GeB—O3B | 1.769 (2) |
Ca—O2Biv | 2.529 (7) | GeB—O3Bx | 1.886 (5) |
Ca—O3B | 2.642 (6) | GeB—O2Bii | 2.161 (7) |
Ca—O2Bii | 3.054 (4) | GeB—Cuii | 2.9670 (13) |
Ca—Cuiv | 3.206 (2) | GeB—Caii | 3.3402 (18) |
Ca—GeBii | 3.3402 (18) | GeB—Caviii | 3.3604 (19) |
Ca—GeBiv | 3.3604 (19) | GeB—Cax | 3.4646 (18) |
Ca—Cu | 3.3765 (19) | O1A—Cuv | 1.948 (5) |
Cu—O1Bii | 1.944 (5) | O1A—Cuxi | 2.304 (5) |
Cu—O1Av | 1.948 (5) | O1A—Cai | 2.4539 (19) |
Cu—O2A | 1.9749 (10) | O1B—Cuii | 1.944 (5) |
Cu—O1Bvi | 2.1189 (10) | O1B—Cuxii | 2.1189 (10) |
Cu—O1Avii | 2.304 (5) | O1B—Caii | 2.464 (2) |
Cu—O2B | 2.4382 (11) | O2B—GeBii | 2.161 (7) |
Cu—GeBii | 2.9670 (13) | O2B—Caviii | 2.529 (7) |
Cu—Caviii | 3.206 (2) | O2B—Caii | 3.054 (4) |
Cu—Caix | 3.6171 (18) | O3A—GeAiii | 1.7817 (17) |
GeA—O2A | 1.7132 (17) | O3A—Cax | 2.4946 (18) |
GeA—O1A | 1.7269 (19) | O3B—GeBiii | 1.886 (5) |
GeA—O3Ax | 1.7817 (17) | O3B—Cax | 2.495 (6) |
| | | |
O2A—Ca—O1Ai | 79.02 (18) | O1Av—Cu—Caix | 101.27 (14) |
O2A—Ca—O1Bii | 68.86 (13) | O2A—Cu—Caix | 146.40 (15) |
O1Ai—Ca—O1Bii | 72.94 (14) | O1Bvi—Cu—Caix | 41.37 (7) |
O2A—Ca—O3Aiii | 92.39 (14) | O1Avii—Cu—Caix | 42.08 (6) |
O1Ai—Ca—O3Aiii | 78.40 (17) | O2B—Cu—Caix | 114.70 (15) |
O1Bii—Ca—O3Aiii | 148.09 (17) | GeBii—Cu—Caix | 83.64 (4) |
O2A—Ca—O3Biii | 138.49 (17) | Caviii—Cu—Caix | 126.47 (6) |
O1Ai—Ca—O3Biii | 132.13 (18) | Ca—Cu—Caix | 121.24 (6) |
O1Bii—Ca—O3Biii | 137.99 (18) | O2A—GeA—O1A | 120.0 (2) |
O3Aiii—Ca—O3Biii | 72.89 (19) | O2A—GeA—O3Ax | 109.48 (17) |
O2A—Ca—O2Biv | 156.81 (16) | O1A—GeA—O3Ax | 108.3 (2) |
O1Ai—Ca—O2Biv | 85.18 (12) | O2A—GeA—O3A | 104.5 (2) |
O1Bii—Ca—O2Biv | 90.4 (2) | O1A—GeA—O3A | 110.3 (3) |
O3Aiii—Ca—O2Biv | 100.99 (18) | O3Ax—GeA—O3A | 102.91 (13) |
O3Biii—Ca—O2Biv | 64.32 (16) | O2A—GeA—Ca | 36.04 (8) |
O2A—Ca—O3B | 84.93 (19) | O1A—GeA—Ca | 129.81 (16) |
O1Ai—Ca—O3B | 163.86 (18) | O3Ax—GeA—Ca | 121.02 (15) |
O1Bii—Ca—O3B | 102.94 (9) | O3A—GeA—Ca | 68.67 (19) |
O3Aiii—Ca—O3B | 100.70 (12) | O2A—GeA—Cax | 105.06 (18) |
O3Biii—Ca—O3B | 61.22 (7) | O1A—GeA—Cax | 132.71 (15) |
O2Biv—Ca—O3B | 110.67 (14) | O3Ax—GeA—Cax | 65.42 (19) |
O2A—Ca—O2Bii | 103.29 (18) | O3A—GeA—Cax | 39.44 (6) |
O1Ai—Ca—O2Bii | 129.68 (15) | Ca—GeA—Cax | 79.99 (5) |
O1Bii—Ca—O2Bii | 62.15 (12) | O2B—GeB—O1B | 111.06 (18) |
O3Aiii—Ca—O2Bii | 149.65 (17) | O2B—GeB—O3B | 120.3 (3) |
O3Biii—Ca—O2Bii | 78.26 (16) | O1B—GeB—O3B | 126.7 (2) |
O2Biv—Ca—O2Bii | 74.1 (2) | O2B—GeB—O3Bx | 94.5 (3) |
O3B—Ca—O2Bii | 55.99 (14) | O1B—GeB—O3Bx | 98.37 (19) |
O2A—Ca—Cuiv | 116.12 (14) | O3B—GeB—O3Bx | 91.45 (16) |
O1Ai—Ca—Cuiv | 37.36 (12) | O2B—GeB—O2Bii | 81.3 (3) |
O1Bii—Ca—Cuiv | 83.65 (8) | O1B—GeB—O2Bii | 88.14 (16) |
O3Aiii—Ca—Cuiv | 81.99 (7) | O3B—GeB—O2Bii | 86.1 (3) |
O3Biii—Ca—Cuiv | 100.35 (9) | O3Bx—GeB—O2Bii | 173.22 (13) |
O2Biv—Ca—Cuiv | 48.57 (5) | O2B—GeB—Cuii | 116.46 (19) |
O3B—Ca—Cuiv | 158.78 (13) | O1B—GeB—Cuii | 38.90 (15) |
O2Bii—Ca—Cuiv | 112.75 (13) | O3B—GeB—Cuii | 101.09 (19) |
O2A—Ca—GeBii | 84.85 (9) | O3Bx—GeB—Cuii | 132.70 (12) |
O1Ai—Ca—GeBii | 101.58 (13) | O2Bii—GeB—Cuii | 54.05 (5) |
O1Bii—Ca—GeBii | 30.74 (7) | O2B—GeB—Caii | 65.25 (15) |
O3Aiii—Ca—GeBii | 177.19 (12) | O1B—GeB—Caii | 45.85 (8) |
O3Biii—Ca—GeBii | 108.87 (13) | O3B—GeB—Caii | 164.06 (19) |
O2Biv—Ca—GeBii | 81.80 (15) | O3Bx—GeB—Caii | 103.30 (17) |
O3B—Ca—GeBii | 78.53 (8) | O2Bii—GeB—Caii | 79.89 (16) |
O2Bii—Ca—GeBii | 31.43 (10) | Cuii—GeB—Caii | 64.42 (4) |
Cuiv—Ca—GeBii | 99.72 (5) | O2B—GeB—Caviii | 47.4 (2) |
O2A—Ca—GeBiv | 171.85 (14) | O1B—GeB—Caviii | 113.52 (15) |
O1Ai—Ca—GeBiv | 108.51 (14) | O3B—GeB—Caviii | 111.27 (19) |
O1Bii—Ca—GeBiv | 115.78 (13) | O3Bx—GeB—Caviii | 47.13 (18) |
O3Aiii—Ca—GeBiv | 86.27 (14) | O2Bii—GeB—Caviii | 128.26 (13) |
O3Biii—Ca—GeBiv | 33.64 (12) | Cuii—GeB—Caviii | 147.58 (5) |
O2Biv—Ca—GeBiv | 30.71 (11) | Caii—GeB—Caviii | 83.62 (5) |
O3B—Ca—GeBiv | 87.42 (12) | O2B—GeB—Cax | 122.50 (18) |
O2Bii—Ca—GeBiv | 74.52 (13) | O1B—GeB—Cax | 116.25 (10) |
Cuiv—Ca—GeBiv | 71.68 (4) | O3B—GeB—Cax | 43.4 (2) |
GeBii—Ca—GeBiv | 96.38 (5) | O3Bx—GeB—Cax | 48.96 (19) |
O2A—Ca—Cu | 34.75 (4) | O2Bii—GeB—Cax | 129.36 (17) |
O1Ai—Ca—Cu | 77.38 (15) | Cuii—GeB—Cax | 120.76 (4) |
O1Bii—Ca—Cu | 34.61 (12) | Caii—GeB—Cax | 148.99 (4) |
O3Aiii—Ca—Cu | 125.02 (14) | Caviii—GeB—Cax | 83.84 (5) |
O3Biii—Ca—Cu | 150.27 (10) | O2B—GeB—Ca | 78.93 (17) |
O2Biv—Ca—Cu | 124.96 (15) | O1B—GeB—Ca | 144.39 (16) |
O3B—Ca—Cu | 90.44 (10) | O3B—GeB—Ca | 45.8 (2) |
O2Bii—Ca—Cu | 78.21 (12) | O3Bx—GeB—Ca | 115.27 (12) |
Cuiv—Ca—Cu | 105.35 (5) | O2Bii—GeB—Ca | 58.80 (11) |
GeBii—Ca—Cu | 52.43 (3) | Cuii—GeB—Ca | 105.61 (4) |
GeBiv—Ca—Cu | 148.39 (6) | Caii—GeB—Ca | 128.84 (4) |
O1Bii—Cu—O1Av | 175.88 (12) | Caviii—GeB—Ca | 98.47 (4) |
O1Bii—Cu—O2A | 87.64 (11) | Cax—GeB—Ca | 81.08 (5) |
O1Av—Cu—O2A | 94.41 (17) | GeA—O1A—Cuv | 120.5 (3) |
O1Bii—Cu—O1Bvi | 91.97 (18) | GeA—O1A—Cuxi | 112.6 (2) |
O1Av—Cu—O1Bvi | 85.5 (2) | Cuv—O1A—Cuxi | 93.08 (14) |
O2A—Cu—O1Bvi | 171.47 (19) | GeA—O1A—Cai | 131.04 (18) |
O1Bii—Cu—O1Avii | 80.66 (13) | Cuv—O1A—Cai | 92.79 (14) |
O1Av—Cu—O1Avii | 102.17 (15) | Cuxi—O1A—Cai | 98.93 (15) |
O2A—Cu—O1Avii | 105.70 (17) | GeB—O1B—Cuii | 106.55 (14) |
O1Bvi—Cu—O1Avii | 82.63 (11) | GeB—O1B—Cuxii | 138.4 (2) |
O1Bii—Cu—O2B | 76.46 (17) | Cuii—O1B—Cuxii | 99.20 (17) |
O1Av—Cu—O2B | 99.91 (18) | GeB—O1B—Caii | 103.41 (12) |
O2A—Cu—O2B | 91.2 (2) | Cuii—O1B—Caii | 99.33 (17) |
O1Bvi—Cu—O2B | 80.42 (18) | Cuxii—O1B—Caii | 103.99 (10) |
O1Avii—Cu—O2B | 150.87 (18) | GeA—O2A—Cu | 133.42 (15) |
O1Bii—Cu—GeBii | 34.55 (7) | GeA—O2A—Ca | 118.34 (13) |
O1Av—Cu—GeBii | 141.35 (10) | Cu—O2A—Ca | 102.96 (10) |
O2A—Cu—GeBii | 102.27 (11) | GeB—O2B—GeBii | 98.7 (3) |
O1Bvi—Cu—GeBii | 73.07 (15) | GeB—O2B—Cu | 132.5 (3) |
O1Avii—Cu—GeBii | 106.34 (10) | GeBii—O2B—Cu | 80.11 (13) |
O2B—Cu—GeBii | 45.84 (16) | GeB—O2B—Caviii | 101.9 (3) |
O1Bii—Cu—Caviii | 126.88 (7) | GeBii—O2B—Caviii | 158.07 (16) |
O1Av—Cu—Caviii | 49.85 (7) | Cu—O2B—Caviii | 80.39 (14) |
O2A—Cu—Caviii | 86.16 (14) | GeB—O2B—Caii | 83.32 (9) |
O1Bvi—Cu—Caviii | 87.27 (10) | GeBii—O2B—Caii | 83.96 (17) |
O1Avii—Cu—Caviii | 151.08 (13) | Cu—O2B—Caii | 142.4 (2) |
O2B—Cu—Caviii | 51.04 (16) | Caviii—O2B—Caii | 105.9 (2) |
GeBii—Cu—Caviii | 96.39 (5) | GeAiii—O3A—GeA | 126.42 (12) |
O1Bii—Cu—Ca | 46.05 (7) | GeAiii—O3A—Cax | 120.22 (11) |
O1Av—Cu—Ca | 135.31 (16) | GeA—O3A—Cax | 113.31 (9) |
O2A—Cu—Ca | 42.29 (7) | GeB—O3B—GeBiii | 122.5 (3) |
O1Bvi—Cu—Ca | 135.34 (15) | GeB—O3B—Cax | 107.4 (2) |
O1Avii—Cu—Ca | 100.83 (13) | GeBiii—O3B—Cax | 99.2 (2) |
O2B—Cu—Ca | 75.75 (16) | GeB—O3B—Ca | 105.5 (3) |
GeBii—Cu—Ca | 63.16 (4) | GeBiii—O3B—Ca | 98.5 (2) |
Caviii—Cu—Ca | 105.35 (5) | Cax—O3B—Ca | 125.2 (2) |
O1Bii—Cu—Caix | 78.77 (7) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.812 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3171 reflections |
a = 10.2150 (12) Å | θ = 2.1–27.7° |
b = 9.2455 (7) Å | µ = 18.01 mm−1 |
c = 5.2407 (6) Å | T = 612 K |
β = 105.928 (12)° | Cuboid, pale green |
V = 475.94 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1037 independent reflections |
Plane graphite monochromator | 777 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.057 |
rotation method scans | θmax = 27.8°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −12→12 |
4729 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 2 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.031P)2 + 2.5799P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.047 | (Δ/σ)max < 0.001 |
wR(F2) = 0.084 | Δρmax = 0.96 e Å−3 |
S = 1.11 | Δρmin = −0.85 e Å−3 |
1037 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0060 (7) |
Crystal data top
CaCuGe2O6 | V = 475.94 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2150 (12) Å | µ = 18.01 mm−1 |
b = 9.2455 (7) Å | T = 612 K |
c = 5.2407 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.928 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1037 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 777 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0.057 |
4729 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.047 | 92 parameters |
wR(F2) = 0.084 | 2 restraints |
S = 1.11 | Δρmax = 0.96 e Å−3 |
1037 reflections | Δρmin = −0.85 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.28070 (19) | 0.4520 (2) | 0.8025 (4) | 0.0170 (4) | |
Cu | 0.22927 (11) | 0.66038 (12) | 0.2552 (2) | 0.0132 (3) | |
GeA | 0.04820 (8) | 0.34931 (10) | 0.21095 (18) | 0.0096 (2) | |
GeB | 0.48906 (9) | 0.34984 (11) | 0.3875 (2) | 0.0129 (3) | |
O1A | −0.1271 (5) | 0.3601 (4) | 0.1163 (3) | 0.0151 (13) | |
O1B | 0.6579 (5) | 0.3204 (6) | 0.3817 (5) | 0.0105 (13) | |
O2A | 0.1428 (6) | 0.4915 (5) | 0.3741 (13) | 0.0182 (16) | |
O2B | 0.4308 (7) | 0.5190 (7) | 0.2569 (9) | 0.0241 (17) | |
O3A | 0.1038 (5) | 0.1969 (4) | 0.4275 (9) | 0.0148 (14) | |
O3B | 0.4003 (6) | 0.2531 (7) | 0.5801 (14) | 0.0150 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0204 (9) | 0.0144 (8) | 0.0162 (10) | 0.0015 (8) | 0.0048 (8) | 0.0037 (8) |
Cu | 0.0153 (5) | 0.0124 (5) | 0.0101 (6) | −0.0024 (4) | 0.0004 (4) | −0.0001 (4) |
GeA | 0.0094 (4) | 0.0093 (4) | 0.0096 (5) | −0.0006 (3) | 0.0018 (3) | −0.0004 (4) |
GeB | 0.0112 (4) | 0.0103 (4) | 0.0189 (5) | 0.0014 (4) | 0.0070 (4) | 0.0034 (4) |
O1A | 0.015 (3) | 0.018 (3) | 0.011 (3) | 0.005 (3) | 0.002 (3) | 0.001 (3) |
O1B | 0.013 (3) | 0.007 (3) | 0.012 (3) | 0.002 (2) | 0.004 (2) | 0.001 (2) |
O2A | 0.025 (4) | 0.009 (3) | 0.017 (4) | −0.012 (2) | −0.001 (3) | −0.005 (2) |
O2B | 0.039 (4) | 0.016 (3) | 0.016 (4) | 0.004 (3) | 0.005 (3) | 0.002 (3) |
O3A | 0.017 (3) | 0.017 (3) | 0.012 (4) | 0.001 (2) | 0.007 (3) | 0.003 (3) |
O3B | 0.013 (3) | 0.016 (3) | 0.018 (4) | −0.003 (2) | 0.009 (3) | 0.001 (3) |
Geometric parameters (Å, º) top
Ca—O2A | 2.329 (7) | GeA—O3A | 1.800 (2) |
Ca—O1Ai | 2.455 (7) | GeA—Cax | 3.607 (2) |
Ca—O1Bii | 2.466 (6) | GeB—O2B | 1.745 (7) |
Ca—O3Biii | 2.496 (7) | GeB—O1B | 1.755 (6) |
Ca—O3Aiii | 2.498 (2) | GeB—O3B | 1.773 (7) |
Ca—O2Biv | 2.530 (2) | GeB—O3Bx | 1.877 (7) |
Ca—O3B | 2.648 (7) | GeB—O2Bii | 2.185 (4) |
Ca—O2Bii | 3.059 (9) | GeB—Cuii | 2.9727 (14) |
Ca—Cuiv | 3.209 (2) | GeB—Caii | 3.341 (2) |
Ca—GeBii | 3.341 (2) | GeB—Caviii | 3.353 (2) |
Ca—GeBiv | 3.353 (2) | GeB—Cax | 3.464 (2) |
Ca—Cu | 3.374 (2) | O1A—Cuv | 1.9491 (11) |
Cu—O1Bii | 1.9436 (11) | O1A—Cuxi | 2.3108 (10) |
Cu—O1Av | 1.9491 (11) | O1A—Cai | 2.455 (7) |
Cu—O2A | 1.977 (6) | O1B—Cuii | 1.9436 (11) |
Cu—O1Bvi | 2.118 (6) | O1B—Cuxii | 2.118 (6) |
Cu—O1Avii | 2.3108 (10) | O1B—Caii | 2.466 (6) |
Cu—O2B | 2.436 (8) | O2B—GeBii | 2.185 (4) |
Cu—GeBii | 2.9727 (14) | O2B—Caviii | 2.530 (2) |
Cu—Caviii | 3.209 (2) | O2B—Caii | 3.059 (9) |
Cu—Caix | 3.620 (2) | O3A—GeAiii | 1.782 (3) |
GeA—O2A | 1.714 (2) | O3A—Cax | 2.498 (2) |
GeA—O1A | 1.725 (5) | O3B—GeBiii | 1.877 (7) |
GeA—O3Ax | 1.782 (3) | O3B—Cax | 2.496 (7) |
| | | |
O2A—Ca—O1Ai | 79.06 (18) | O1Av—Cu—Caix | 101.10 (12) |
O2A—Ca—O1Bii | 68.94 (13) | O2A—Cu—Caix | 146.0 (2) |
O1Ai—Ca—O1Bii | 73.00 (16) | O1Bvi—Cu—Caix | 41.36 (17) |
O2A—Ca—O3Biii | 138.7 (2) | O1Avii—Cu—Caix | 42.07 (16) |
O1Ai—Ca—O3Biii | 132.1 (2) | O2B—Cu—Caix | 115.10 (17) |
O1Bii—Ca—O3Biii | 137.7 (2) | GeBii—Cu—Caix | 83.75 (4) |
O2A—Ca—O3Aiii | 92.8 (2) | Caviii—Cu—Caix | 126.49 (7) |
O1Ai—Ca—O3Aiii | 78.57 (13) | Ca—Cu—Caix | 121.40 (7) |
O1Bii—Ca—O3Aiii | 148.5 (2) | O2A—GeA—O1A | 119.8 (3) |
O3Biii—Ca—O3Aiii | 72.7 (2) | O2A—GeA—O3Ax | 109.6 (3) |
O2A—Ca—O2Biv | 156.8 (2) | O1A—GeA—O3Ax | 108.5 (2) |
O1Ai—Ca—O2Biv | 85.10 (19) | O2A—GeA—O3A | 104.4 (3) |
O1Bii—Ca—O2Biv | 90.35 (19) | O1A—GeA—O3A | 110.47 (18) |
O3Biii—Ca—O2Biv | 64.2 (2) | O3Ax—GeA—O3A | 102.71 (15) |
O3Aiii—Ca—O2Biv | 100.6 (2) | O2A—GeA—Ca | 36.2 (2) |
O2A—Ca—O3B | 85.1 (2) | O1A—GeA—Ca | 129.89 (14) |
O1Ai—Ca—O3B | 164.07 (17) | O3Ax—GeA—Ca | 120.82 (16) |
O1Bii—Ca—O3B | 102.9 (2) | O3A—GeA—Ca | 68.4 (2) |
O3Biii—Ca—O3B | 61.17 (9) | O2A—GeA—Cax | 105.4 (2) |
O3Aiii—Ca—O3B | 100.77 (18) | O1A—GeA—Cax | 132.59 (14) |
O2Biv—Ca—O3B | 110.5 (2) | O3Ax—GeA—Cax | 65.0 (2) |
O2A—Ca—O2Bii | 103.5 (2) | O3A—GeA—Cax | 39.58 (9) |
O1Ai—Ca—O2Bii | 129.44 (15) | Ca—GeA—Cax | 80.14 (5) |
O1Bii—Ca—O2Bii | 61.97 (19) | O2B—GeB—O1B | 111.3 (3) |
O3Biii—Ca—O2Bii | 78.1 (2) | O2B—GeB—O3B | 120.2 (4) |
O3Aiii—Ca—O2Bii | 149.5 (2) | O1B—GeB—O3B | 126.2 (3) |
O2Biv—Ca—O2Bii | 73.9 (3) | O2B—GeB—O3Bx | 94.9 (2) |
O3B—Ca—O2Bii | 56.10 (18) | O1B—GeB—O3Bx | 98.7 (2) |
O2A—Ca—Cuiv | 116.12 (18) | O3B—GeB—O3Bx | 91.8 (2) |
O1Ai—Ca—Cuiv | 37.34 (4) | O2B—GeB—O2Bii | 81.07 (17) |
O1Bii—Ca—Cuiv | 83.57 (13) | O1B—GeB—O2Bii | 87.8 (2) |
O3Biii—Ca—Cuiv | 100.28 (18) | O3B—GeB—O2Bii | 85.7 (3) |
O3Aiii—Ca—Cuiv | 81.96 (8) | O3Bx—GeB—O2Bii | 173.3 (3) |
O2Biv—Ca—Cuiv | 48.48 (18) | O2B—GeB—Cuii | 116.26 (19) |
O3B—Ca—Cuiv | 158.58 (16) | O1B—GeB—Cuii | 38.73 (8) |
O2Bii—Ca—Cuiv | 112.36 (12) | O3B—GeB—Cuii | 100.5 (2) |
O2A—Ca—GeBii | 85.18 (17) | O3Bx—GeB—Cuii | 132.9 (2) |
O1Ai—Ca—GeBii | 101.51 (7) | O2Bii—GeB—Cuii | 53.8 (2) |
O1Bii—Ca—GeBii | 30.73 (14) | O2B—GeB—Caii | 65.4 (3) |
O3Biii—Ca—GeBii | 108.56 (17) | O1B—GeB—Caii | 45.90 (19) |
O3Aiii—Ca—GeBii | 177.95 (13) | O3B—GeB—Caii | 163.3 (2) |
O2Biv—Ca—GeBii | 81.5 (2) | O3Bx—GeB—Caii | 103.7 (2) |
O3B—Ca—GeBii | 78.58 (15) | O2Bii—GeB—Caii | 79.7 (2) |
O2Bii—Ca—GeBii | 31.25 (13) | Cuii—GeB—Caii | 64.30 (4) |
Cuiv—Ca—GeBii | 99.36 (6) | O2B—GeB—Caviii | 47.64 (10) |
O2A—Ca—GeBiv | 171.92 (16) | O1B—GeB—Caviii | 114.09 (12) |
O1Ai—Ca—GeBiv | 108.44 (8) | O3B—GeB—Caviii | 111.5 (2) |
O1Bii—Ca—GeBiv | 115.62 (8) | O3Bx—GeB—Caviii | 47.3 (2) |
O3Biii—Ca—GeBiv | 33.55 (16) | O2Bii—GeB—Caviii | 128.23 (18) |
O3Aiii—Ca—GeBiv | 85.88 (14) | Cuii—GeB—Caviii | 147.87 (5) |
O2Biv—Ca—GeBiv | 30.64 (16) | Caii—GeB—Caviii | 83.98 (5) |
O3B—Ca—GeBiv | 87.31 (16) | O2B—GeB—Cax | 122.7 (2) |
O2Bii—Ca—GeBiv | 74.34 (11) | O1B—GeB—Cax | 116.43 (19) |
Cuiv—Ca—GeBiv | 71.63 (5) | O3B—GeB—Cax | 43.5 (2) |
GeBii—Ca—GeBiv | 96.02 (5) | O3Bx—GeB—Cax | 49.1 (2) |
O2A—Ca—Cu | 34.84 (13) | O2Bii—GeB—Cax | 129.0 (2) |
O1Ai—Ca—Cu | 77.63 (6) | Cuii—GeB—Cax | 120.65 (5) |
O1Bii—Ca—Cu | 34.66 (5) | Caii—GeB—Cax | 149.47 (5) |
O3Biii—Ca—Cu | 150.03 (19) | Caviii—GeB—Cax | 84.03 (6) |
O3Aiii—Ca—Cu | 125.63 (15) | O2B—GeB—Ca | 78.8 (3) |
O2Biv—Ca—Cu | 124.96 (18) | O1B—GeB—Ca | 143.75 (10) |
O3B—Ca—Cu | 90.30 (17) | O3B—GeB—Ca | 45.7 (2) |
O2Bii—Ca—Cu | 78.06 (12) | O3Bx—GeB—Ca | 115.5 (2) |
Cuiv—Ca—Cu | 105.48 (6) | O2Bii—GeB—Ca | 58.6 (2) |
GeBii—Ca—Cu | 52.54 (4) | Cuii—GeB—Ca | 105.13 (5) |
GeBiv—Ca—Cu | 148.19 (7) | Caii—GeB—Ca | 128.60 (4) |
O1Bii—Cu—O1Av | 176.2 (3) | Caviii—GeB—Ca | 98.50 (5) |
O1Bii—Cu—O2A | 87.7 (2) | Cax—GeB—Ca | 80.98 (6) |
O1Av—Cu—O2A | 94.29 (17) | GeA—O1A—Cuv | 120.7 (3) |
O1Bii—Cu—O1Bvi | 92.08 (17) | GeA—O1A—Cuxi | 112.7 (2) |
O1Av—Cu—O1Bvi | 85.51 (8) | Cuv—O1A—Cuxi | 93.02 (6) |
O2A—Cu—O1Bvi | 172.0 (3) | GeA—O1A—Cai | 130.81 (15) |
O1Bii—Cu—O1Avii | 80.52 (18) | Cuv—O1A—Cai | 92.8 (2) |
O1Av—Cu—O1Avii | 102.0 (2) | Cuxi—O1A—Cai | 98.83 (19) |
O2A—Cu—O1Avii | 105.2 (3) | GeB—O1B—Cuii | 106.9 (3) |
O1Bvi—Cu—O1Avii | 82.6 (2) | GeB—O1B—Cuxii | 138.0 (3) |
O1Bii—Cu—O2B | 76.8 (2) | Cuii—O1B—Cuxii | 99.4 (2) |
O1Av—Cu—O2B | 99.9 (2) | GeB—O1B—Caii | 103.4 (2) |
O2A—Cu—O2B | 91.5 (3) | Cuii—O1B—Caii | 99.2 (2) |
O1Bvi—Cu—O2B | 80.7 (2) | Cuxii—O1B—Caii | 104.1 (3) |
O1Avii—Cu—O2B | 151.21 (16) | GeA—O2A—Cu | 133.5 (4) |
O1Bii—Cu—GeBii | 34.39 (19) | GeA—O2A—Ca | 118.0 (3) |
O1Av—Cu—GeBii | 141.86 (18) | Cu—O2A—Ca | 102.89 (15) |
O2A—Cu—GeBii | 102.43 (19) | GeB—O2B—GeBii | 98.93 (17) |
O1Bvi—Cu—GeBii | 73.32 (8) | GeB—O2B—Cu | 132.8 (5) |
O1Avii—Cu—GeBii | 106.15 (9) | GeBii—O2B—Cu | 79.9 (2) |
O2B—Cu—GeBii | 46.36 (8) | GeB—O2B—Caviii | 101.7 (2) |
O1Bii—Cu—Caviii | 127.25 (19) | GeBii—O2B—Caviii | 158.0 (3) |
O1Av—Cu—Caviii | 49.82 (19) | Cu—O2B—Caviii | 80.48 (17) |
O2A—Cu—Caviii | 86.4 (2) | GeB—O2B—Caii | 83.3 (3) |
O1Bvi—Cu—Caviii | 87.39 (15) | GeBii—O2B—Caii | 83.8 (2) |
O1Avii—Cu—Caviii | 150.92 (5) | Cu—O2B—Caii | 142.1 (3) |
O2B—Cu—Caviii | 51.04 (7) | Caviii—O2B—Caii | 106.1 (3) |
GeBii—Cu—Caviii | 96.90 (5) | GeAiii—O3A—GeA | 126.54 (16) |
O1Bii—Cu—Ca | 46.18 (18) | GeAiii—O3A—Cax | 120.36 (12) |
O1Av—Cu—Ca | 135.17 (9) | GeA—O3A—Cax | 113.08 (15) |
O2A—Cu—Ca | 42.28 (16) | GeB—O3B—GeBiii | 122.9 (3) |
O1Bvi—Cu—Ca | 135.60 (6) | GeB—O3B—Cax | 107.2 (3) |
O1Avii—Cu—Ca | 100.70 (10) | GeBiii—O3B—Cax | 99.1 (3) |
O2B—Cu—Ca | 75.90 (17) | GeB—O3B—Ca | 105.7 (3) |
GeBii—Cu—Ca | 63.15 (4) | GeBiii—O3B—Ca | 98.5 (3) |
Caviii—Cu—Ca | 105.48 (6) | Cax—O3B—Ca | 125.0 (3) |
O1Bii—Cu—Caix | 78.85 (17) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.808 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3292 reflections |
a = 10.2165 (12) Å | θ = 2.1–27.7° |
b = 9.2483 (7) Å | µ = 18.22 mm−1 |
c = 5.2429 (6) Å | T = 629 K |
β = 105.942 (12)° | Cuboid, pale green |
V = 476.32 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1053 independent reflections |
Plane graphite monochromator | 778 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.060 |
rotation method scans | θmax = 27.9°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −12→12 |
5005 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0265P)2 + 3.3784P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.047 | (Δ/σ)max < 0.001 |
wR(F2) = 0.085 | Δρmax = 0.97 e Å−3 |
S = 1.16 | Δρmin = −0.96 e Å−3 |
1053 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0055 (6) |
Crystal data top
CaCuGe2O6 | V = 476.32 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2165 (12) Å | µ = 18.22 mm−1 |
b = 9.2483 (7) Å | T = 629 K |
c = 5.2429 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.942 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1053 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 778 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0.060 |
5005 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.047 | 92 parameters |
wR(F2) = 0.085 | 0 restraints |
S = 1.16 | Δρmax = 0.97 e Å−3 |
1053 reflections | Δρmin = −0.96 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.2804 (2) | 0.4521 (2) | 0.8019 (4) | 0.0177 (4) | |
Cu | 0.22939 (11) | 0.66019 (12) | 0.2549 (2) | 0.0140 (3) | |
GeA | 0.04816 (8) | 0.34923 (11) | 0.21112 (19) | 0.0103 (2) | |
GeB | 0.48893 (9) | 0.34985 (11) | 0.3863 (2) | 0.0139 (3) | |
O1A | −0.1273 (2) | 0.3598 (2) | 0.1155 (8) | 0.0156 (14) | |
O1B | 0.6578 (2) | 0.3205 (2) | 0.3822 (3) | 0.0128 (14) | |
O2A | 0.1423 (5) | 0.4914 (5) | 0.3732 (8) | 0.0210 (17) | |
O2B | 0.4306 (5) | 0.5190 (7) | 0.2560 (16) | 0.0233 (17) | |
O3A | 0.1038 (6) | 0.1975 (7) | 0.4284 (15) | 0.0160 (15) | |
O3B | 0.4003 (6) | 0.2539 (8) | 0.5785 (15) | 0.0170 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0207 (9) | 0.0149 (8) | 0.0172 (10) | 0.0004 (8) | 0.0048 (8) | 0.0036 (8) |
Cu | 0.0159 (5) | 0.0128 (5) | 0.0112 (6) | −0.0028 (5) | 0.0000 (4) | 0.0003 (4) |
GeA | 0.0099 (4) | 0.0095 (4) | 0.0107 (5) | −0.0006 (4) | 0.0016 (3) | −0.0006 (4) |
GeB | 0.0119 (5) | 0.0106 (5) | 0.0206 (5) | 0.0016 (4) | 0.0068 (4) | 0.0045 (4) |
O1A | 0.013 (3) | 0.018 (3) | 0.015 (3) | 0.004 (3) | 0.003 (3) | 0.000 (3) |
O1B | 0.017 (3) | 0.010 (3) | 0.013 (4) | 0.002 (2) | 0.006 (3) | 0.004 (2) |
O2A | 0.027 (4) | 0.012 (3) | 0.021 (4) | −0.011 (3) | 0.002 (3) | −0.001 (3) |
O2B | 0.036 (4) | 0.015 (3) | 0.019 (4) | 0.005 (3) | 0.008 (3) | 0.004 (3) |
O3A | 0.015 (3) | 0.016 (3) | 0.018 (4) | 0.005 (2) | 0.008 (3) | 0.003 (3) |
O3B | 0.012 (3) | 0.023 (4) | 0.017 (4) | −0.006 (2) | 0.007 (3) | 0.001 (3) |
Geometric parameters (Å, º) top
Ca—O2A | 2.331 (2) | GeA—O3A | 1.799 (7) |
Ca—O1Ai | 2.4563 (19) | GeA—Cax | 3.605 (2) |
Ca—O1Bii | 2.467 (2) | GeB—O2B | 1.745 (6) |
Ca—O3Biii | 2.501 (7) | GeB—O1B | 1.753 (2) |
Ca—O3Aiii | 2.502 (7) | GeB—O3B | 1.768 (7) |
Ca—O2Biv | 2.530 (8) | GeB—O3Bx | 1.882 (7) |
Ca—O3B | 2.650 (8) | GeB—O2Bii | 2.195 (8) |
Ca—O2Bii | 3.062 (5) | GeB—Cuii | 2.9759 (14) |
Ca—Cuiv | 3.209 (3) | GeB—Caii | 3.341 (2) |
Ca—GeBii | 3.341 (2) | GeB—Caviii | 3.352 (2) |
Ca—GeBiv | 3.352 (2) | GeB—Cax | 3.466 (2) |
Ca—Cu | 3.373 (2) | O1A—Cuv | 1.944 (4) |
Cu—O1Bii | 1.9433 (11) | O1A—Cuxi | 2.3120 (10) |
Cu—O1Av | 1.944 (4) | O1A—Cai | 2.4563 (19) |
Cu—O2A | 1.9787 (10) | O1B—Cuii | 1.9433 (11) |
Cu—O1Bvi | 2.1208 (10) | O1B—Cuxii | 2.1208 (10) |
Cu—O1Avii | 2.3120 (10) | O1B—Caii | 2.467 (2) |
Cu—O2B | 2.4343 (11) | O2B—GeBii | 2.195 (8) |
Cu—GeBii | 2.9759 (14) | O2B—Caviii | 2.530 (8) |
Cu—Caviii | 3.209 (3) | O2B—Caii | 3.062 (5) |
Cu—Caix | 3.622 (2) | O3A—GeAiii | 1.781 (8) |
GeA—O2A | 1.711 (4) | O3A—Cax | 2.502 (7) |
GeA—O1A | 1.7266 (19) | O3B—GeBiii | 1.882 (7) |
GeA—O3Ax | 1.781 (8) | O3B—Cax | 2.501 (7) |
| | | |
O2A—Ca—O1Ai | 79.3 (2) | O1Av—Cu—Caix | 100.93 (8) |
O2A—Ca—O1Bii | 69.01 (9) | O2A—Cu—Caix | 145.9 (2) |
O1Ai—Ca—O1Bii | 73.07 (8) | O1Bvi—Cu—Caix | 41.37 (7) |
O2A—Ca—O3Biii | 138.5 (2) | O1Avii—Cu—Caix | 42.07 (6) |
O1Ai—Ca—O3Biii | 132.2 (2) | O2B—Cu—Caix | 115.17 (18) |
O1Bii—Ca—O3Biii | 137.61 (18) | GeBii—Cu—Caix | 83.79 (4) |
O2A—Ca—O3Aiii | 93.03 (18) | Caviii—Cu—Caix | 126.49 (7) |
O1Ai—Ca—O3Aiii | 78.75 (17) | Ca—Cu—Caix | 121.42 (7) |
O1Bii—Ca—O3Aiii | 148.79 (18) | O2A—GeA—O1A | 119.9 (3) |
O3Biii—Ca—O3Aiii | 72.5 (2) | O2A—GeA—O3Ax | 109.6 (3) |
O2A—Ca—O2Biv | 156.8 (2) | O1A—GeA—O3Ax | 108.4 (2) |
O1Ai—Ca—O2Biv | 84.93 (11) | O2A—GeA—O3A | 104.4 (2) |
O1Bii—Ca—O2Biv | 90.29 (18) | O1A—GeA—O3A | 110.5 (2) |
O3Biii—Ca—O2Biv | 64.3 (2) | O3Ax—GeA—O3A | 102.7 (2) |
O3Aiii—Ca—O2Biv | 100.4 (2) | O2A—GeA—Ca | 36.34 (9) |
O2A—Ca—O3B | 85.0 (3) | O1A—GeA—Ca | 130.04 (14) |
O1Ai—Ca—O3B | 164.2 (2) | O3Ax—GeA—Ca | 120.8 (2) |
O1Bii—Ca—O3B | 102.57 (18) | O3A—GeA—Ca | 68.2 (2) |
O3Biii—Ca—O3B | 61.13 (9) | O2A—GeA—Cax | 105.6 (2) |
O3Aiii—Ca—O3B | 100.9 (2) | O1A—GeA—Cax | 132.46 (10) |
O2Biv—Ca—O3B | 110.52 (16) | O3Ax—GeA—Cax | 64.7 (2) |
O2A—Ca—O2Bii | 103.6 (2) | O3A—GeA—Cax | 39.8 (2) |
O1Ai—Ca—O2Bii | 129.31 (14) | Ca—GeA—Cax | 80.25 (5) |
O1Bii—Ca—O2Bii | 61.92 (13) | O2B—GeB—O1B | 111.4 (2) |
O3Biii—Ca—O2Bii | 78.0 (2) | O2B—GeB—O3B | 120.0 (3) |
O3Aiii—Ca—O2Bii | 149.2 (2) | O1B—GeB—O3B | 126.1 (2) |
O2Biv—Ca—O2Bii | 73.7 (2) | O2B—GeB—O3Bx | 95.1 (3) |
O3B—Ca—O2Bii | 56.02 (19) | O1B—GeB—O3Bx | 98.9 (2) |
O2A—Ca—Cuiv | 116.2 (2) | O3B—GeB—O3Bx | 91.8 (2) |
O1Ai—Ca—Cuiv | 37.23 (10) | O2B—GeB—O2Bii | 81.2 (3) |
O1Bii—Ca—Cuiv | 83.63 (6) | O1B—GeB—O2Bii | 87.55 (10) |
O3Biii—Ca—Cuiv | 100.42 (19) | O3B—GeB—O2Bii | 85.4 (3) |
O3Aiii—Ca—Cuiv | 81.95 (18) | O3Bx—GeB—O2Bii | 173.4 (2) |
O2Biv—Ca—Cuiv | 48.44 (6) | O2B—GeB—Cuii | 116.2 (2) |
O3B—Ca—Cuiv | 158.57 (17) | O1B—GeB—Cuii | 38.61 (5) |
O2Bii—Ca—Cuiv | 112.20 (14) | O3B—GeB—Cuii | 100.5 (2) |
O2A—Ca—GeBii | 85.34 (10) | O3Bx—GeB—Cuii | 132.9 (2) |
O1Ai—Ca—GeBii | 101.44 (7) | O2Bii—GeB—Cuii | 53.63 (5) |
O1Bii—Ca—GeBii | 30.69 (5) | O2B—GeB—Caii | 65.51 (18) |
O3Biii—Ca—GeBii | 108.41 (17) | O1B—GeB—Caii | 45.93 (8) |
O3Aiii—Ca—GeBii | 178.28 (18) | O3B—GeB—Caii | 163.2 (2) |
O2Biv—Ca—GeBii | 81.29 (17) | O3Bx—GeB—Caii | 103.8 (2) |
O3B—Ca—GeBii | 78.43 (16) | O2Bii—GeB—Caii | 79.65 (19) |
O2Bii—Ca—GeBii | 31.25 (12) | Cuii—GeB—Caii | 64.25 (4) |
Cuiv—Ca—GeBii | 99.24 (6) | O2B—GeB—Caviii | 47.7 (3) |
O2A—Ca—GeBiv | 171.9 (2) | O1B—GeB—Caviii | 114.41 (8) |
O1Ai—Ca—GeBiv | 108.31 (11) | O3B—GeB—Caviii | 111.5 (2) |
O1Bii—Ca—GeBiv | 115.54 (7) | O3Bx—GeB—Caviii | 47.5 (2) |
O3Biii—Ca—GeBiv | 33.70 (17) | O2Bii—GeB—Caviii | 128.32 (15) |
O3Aiii—Ca—GeBiv | 85.71 (17) | Cuii—GeB—Caviii | 148.02 (6) |
O2Biv—Ca—GeBiv | 30.65 (13) | Caii—GeB—Caviii | 84.17 (5) |
O3B—Ca—GeBiv | 87.36 (16) | O2B—GeB—Cax | 122.7 (2) |
O2Bii—Ca—GeBiv | 74.16 (15) | O1B—GeB—Cax | 116.53 (11) |
Cuiv—Ca—GeBiv | 71.59 (5) | O3B—GeB—Cax | 43.5 (2) |
GeBii—Ca—GeBiv | 95.83 (5) | O3Bx—GeB—Cax | 49.1 (2) |
O2A—Ca—Cu | 34.90 (5) | O2Bii—GeB—Cax | 128.8 (2) |
O1Ai—Ca—Cu | 77.80 (9) | Cuii—GeB—Cax | 120.63 (5) |
O1Bii—Ca—Cu | 34.67 (4) | Caii—GeB—Cax | 149.64 (5) |
O3Biii—Ca—Cu | 149.78 (19) | Caviii—GeB—Cax | 84.05 (6) |
O3Aiii—Ca—Cu | 125.91 (17) | O2B—GeB—Ca | 78.7 (2) |
O2Biv—Ca—Cu | 124.92 (18) | O1B—GeB—Ca | 143.47 (7) |
O3B—Ca—Cu | 90.06 (17) | O3B—GeB—Ca | 45.5 (2) |
O2Bii—Ca—Cu | 78.10 (15) | O3Bx—GeB—Ca | 115.5 (2) |
Cuiv—Ca—Cu | 105.57 (6) | O2Bii—GeB—Ca | 58.53 (13) |
GeBii—Ca—Cu | 52.61 (4) | Cuii—GeB—Ca | 104.96 (5) |
GeBiv—Ca—Cu | 148.09 (7) | Caii—GeB—Ca | 128.54 (5) |
O1Bii—Cu—O1Av | 176.28 (9) | Caviii—GeB—Ca | 98.46 (5) |
O1Bii—Cu—O2A | 87.83 (14) | Cax—GeB—Ca | 80.91 (6) |
O1Av—Cu—O2A | 94.26 (12) | GeA—O1A—Cuv | 120.93 (19) |
O1Bii—Cu—O1Bvi | 92.08 (8) | GeA—O1A—Cuxi | 112.69 (11) |
O1Av—Cu—O1Bvi | 85.43 (7) | Cuv—O1A—Cuxi | 93.23 (12) |
O2A—Cu—O1Bvi | 172.1 (2) | GeA—O1A—Cai | 130.48 (18) |
O1Bii—Cu—O1Avii | 80.38 (11) | Cuv—O1A—Cai | 92.91 (11) |
O1Av—Cu—O1Avii | 102.00 (11) | Cuxi—O1A—Cai | 98.83 (9) |
O2A—Cu—O1Avii | 105.0 (2) | GeB—O1B—Cuii | 107.14 (9) |
O1Bvi—Cu—O1Avii | 82.67 (11) | GeB—O1B—Cuxii | 137.79 (13) |
O1Bii—Cu—O2B | 76.9 (2) | Cuii—O1B—Cuxii | 99.48 (7) |
O1Av—Cu—O2B | 99.9 (2) | GeB—O1B—Caii | 103.39 (10) |
O2A—Cu—O2B | 91.6 (3) | Cuii—O1B—Caii | 99.09 (11) |
O1Bvi—Cu—O2B | 80.71 (19) | Cuxii—O1B—Caii | 104.02 (11) |
O1Avii—Cu—O2B | 151.20 (19) | GeA—O2A—Cu | 133.7 (2) |
O1Bii—Cu—GeBii | 34.25 (6) | GeA—O2A—Ca | 117.87 (16) |
O1Av—Cu—GeBii | 142.07 (8) | Cu—O2A—Ca | 102.74 (12) |
O2A—Cu—GeBii | 102.54 (12) | GeB—O2B—GeBii | 98.8 (3) |
O1Bvi—Cu—GeBii | 73.44 (5) | GeB—O2B—Cu | 132.8 (4) |
O1Avii—Cu—GeBii | 105.96 (8) | GeBii—O2B—Cu | 79.83 (15) |
O2B—Cu—GeBii | 46.54 (18) | GeB—O2B—Caviii | 101.7 (3) |
O1Bii—Cu—Caviii | 127.35 (7) | GeBii—O2B—Caviii | 158.03 (18) |
O1Av—Cu—Caviii | 49.86 (8) | Cu—O2B—Caviii | 80.51 (16) |
O2A—Cu—Caviii | 86.4 (2) | GeB—O2B—Caii | 83.25 (10) |
O1Bvi—Cu—Caviii | 87.42 (10) | GeBii—O2B—Caii | 83.8 (2) |
O1Avii—Cu—Caviii | 150.98 (12) | Cu—O2B—Caii | 142.2 (3) |
O2B—Cu—Caviii | 51.05 (19) | Caviii—O2B—Caii | 106.3 (2) |
GeBii—Cu—Caviii | 97.12 (5) | GeAiii—O3A—GeA | 126.8 (4) |
O1Bii—Cu—Ca | 46.24 (8) | GeAiii—O3A—Cax | 120.3 (3) |
O1Av—Cu—Ca | 135.24 (9) | GeA—O3A—Cax | 112.9 (4) |
O2A—Cu—Ca | 42.37 (8) | GeB—O3B—GeBiii | 122.9 (3) |
O1Bvi—Cu—Ca | 135.69 (5) | GeB—O3B—Cax | 107.3 (3) |
O1Avii—Cu—Ca | 100.51 (13) | GeBiii—O3B—Cax | 98.8 (3) |
O2B—Cu—Ca | 76.04 (19) | GeB—O3B—Ca | 106.0 (3) |
GeBii—Cu—Ca | 63.13 (4) | GeBiii—O3B—Ca | 98.4 (3) |
Caviii—Cu—Ca | 105.57 (6) | Cax—O3B—Ca | 124.8 (3) |
O1Bii—Cu—Caix | 78.87 (8) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.805 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2243 reflections |
a = 10.2170 (12) Å | θ = 2.1–27.7° |
b = 9.2515 (7) Å | µ = 17.98 mm−1 |
c = 5.2446 (6) Å | T = 646 K |
β = 105.964 (12)° | Cuboid, pale green |
V = 476.61 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 1020 independent reflections |
Plane graphite monochromator | 764 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.060 |
rotation method scans | θmax = 27.8°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −12→12 |
4880 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.031P)2 + 3.7693P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.045 | (Δ/σ)max < 0.001 |
wR(F2) = 0.086 | Δρmax = 1.05 e Å−3 |
S = 1.10 | Δρmin = −1.04 e Å−3 |
1020 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0058 (7) |
Crystal data top
CaCuGe2O6 | V = 476.61 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2170 (12) Å | µ = 17.98 mm−1 |
b = 9.2515 (7) Å | T = 646 K |
c = 5.2446 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.964 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 1020 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 764 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0.060 |
4880 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | 92 parameters |
wR(F2) = 0.086 | 0 restraints |
S = 1.10 | Δρmax = 1.05 e Å−3 |
1020 reflections | Δρmin = −1.04 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.2800 (2) | 0.4521 (2) | 0.8015 (4) | 0.0168 (4) | |
Cu | 0.22967 (11) | 0.66017 (13) | 0.2548 (2) | 0.0126 (3) | |
GeA | 0.04796 (9) | 0.34941 (11) | 0.21112 (19) | 0.0089 (2) | |
GeB | 0.48868 (9) | 0.34967 (11) | 0.3851 (2) | 0.0129 (3) | |
O1A | −0.1274 (6) | 0.3595 (8) | 0.1154 (13) | 0.0140 (14) | |
O1B | 0.6574 (6) | 0.3206 (6) | 0.3824 (13) | 0.0106 (13) | |
O2A | 0.1427 (8) | 0.4920 (7) | 0.3743 (16) | 0.0210 (18) | |
O2B | 0.4301 (8) | 0.5180 (7) | 0.2543 (16) | 0.0229 (17) | |
O3A | 0.1039 (7) | 0.1973 (7) | 0.4294 (15) | 0.0162 (16) | |
O3B | 0.3999 (7) | 0.2542 (8) | 0.5773 (15) | 0.0161 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0187 (9) | 0.0144 (8) | 0.0166 (10) | 0.0017 (8) | 0.0037 (8) | 0.0028 (8) |
Cu | 0.0138 (5) | 0.0108 (5) | 0.0106 (6) | −0.0032 (5) | −0.0010 (4) | −0.0002 (4) |
GeA | 0.0076 (4) | 0.0081 (4) | 0.0098 (5) | −0.0010 (4) | 0.0003 (3) | −0.0009 (4) |
GeB | 0.0098 (5) | 0.0091 (5) | 0.0210 (5) | 0.0020 (4) | 0.0059 (4) | 0.0043 (4) |
O1A | 0.012 (3) | 0.015 (3) | 0.014 (3) | 0.004 (3) | 0.002 (3) | −0.002 (3) |
O1B | 0.013 (3) | 0.007 (3) | 0.010 (3) | 0.001 (2) | 0.001 (3) | 0.000 (2) |
O2A | 0.030 (4) | 0.012 (3) | 0.019 (4) | −0.014 (3) | 0.001 (3) | −0.001 (3) |
O2B | 0.034 (4) | 0.012 (3) | 0.021 (4) | 0.004 (3) | 0.005 (3) | 0.002 (3) |
O3A | 0.012 (3) | 0.020 (4) | 0.017 (4) | 0.004 (2) | 0.005 (3) | 0.004 (3) |
O3B | 0.014 (3) | 0.021 (4) | 0.016 (4) | −0.007 (3) | 0.008 (3) | 0.001 (3) |
Geometric parameters (Å, º) top
Ca—O2A | 2.323 (8) | GeA—O3A | 1.805 (7) |
Ca—O1Ai | 2.456 (7) | GeA—Cax | 3.607 (2) |
Ca—O1Bii | 2.469 (7) | GeB—O2B | 1.740 (7) |
Ca—O3Biii | 2.502 (7) | GeB—O1B | 1.749 (7) |
Ca—O3Aiii | 2.502 (7) | GeB—O3B | 1.767 (7) |
Ca—O2Biv | 2.522 (8) | GeB—O3Bx | 1.883 (7) |
Ca—O3B | 2.651 (8) | GeB—O2Bii | 2.214 (8) |
Ca—O2Bii | 3.068 (9) | GeB—Cuii | 2.9777 (15) |
Ca—Cuiv | 3.208 (3) | GeB—Caii | 3.343 (2) |
Ca—GeBii | 3.343 (2) | GeB—Caviii | 3.350 (2) |
Ca—GeBiv | 3.350 (2) | GeB—Cax | 3.467 (2) |
Ca—Cu | 3.373 (2) | O1A—Cuv | 1.944 (6) |
Cu—O1Bii | 1.943 (6) | O1A—Cuxi | 2.312 (7) |
Cu—O1Av | 1.944 (6) | O1A—Cai | 2.456 (7) |
Cu—O2A | 1.978 (7) | O1B—Cuii | 1.943 (6) |
Cu—O1Bvi | 2.123 (7) | O1B—Cuxii | 2.123 (7) |
Cu—O1Avii | 2.312 (7) | O1B—Caii | 2.469 (7) |
Cu—O2B | 2.434 (8) | O2B—GeBii | 2.214 (8) |
Cu—GeBii | 2.9777 (15) | O2B—Caviii | 2.522 (8) |
Cu—Caviii | 3.208 (3) | O2B—Caii | 3.068 (9) |
Cu—Caix | 3.622 (2) | O3A—GeAiii | 1.778 (8) |
GeA—O2A | 1.718 (7) | O3A—Cax | 2.502 (7) |
GeA—O1A | 1.725 (6) | O3B—GeBiii | 1.883 (7) |
GeA—O3Ax | 1.778 (8) | O3B—Cax | 2.502 (7) |
| | | |
O2A—Ca—O1Ai | 79.3 (3) | O1Av—Cu—Caix | 100.8 (2) |
O2A—Ca—O1Bii | 68.9 (2) | O2A—Cu—Caix | 145.7 (3) |
O1Ai—Ca—O1Bii | 73.2 (2) | O1Bvi—Cu—Caix | 41.44 (18) |
O2A—Ca—O3Biii | 138.5 (3) | O1Avii—Cu—Caix | 42.07 (17) |
O1Ai—Ca—O3Biii | 132.3 (3) | O2B—Cu—Caix | 115.55 (18) |
O1Bii—Ca—O3Biii | 137.5 (2) | GeBii—Cu—Caix | 83.85 (5) |
O2A—Ca—O3Aiii | 93.3 (3) | Caviii—Cu—Caix | 126.54 (8) |
O1Ai—Ca—O3Aiii | 78.8 (2) | Ca—Cu—Caix | 121.46 (7) |
O1Bii—Ca—O3Aiii | 149.0 (2) | O2A—GeA—O1A | 120.1 (4) |
O3Biii—Ca—O3Aiii | 72.4 (2) | O2A—GeA—O3Ax | 109.6 (4) |
O2A—Ca—O2Biv | 156.9 (2) | O1A—GeA—O3Ax | 108.5 (3) |
O1Ai—Ca—O2Biv | 85.0 (2) | O2A—GeA—O3A | 104.2 (3) |
O1Bii—Ca—O2Biv | 90.4 (2) | O1A—GeA—O3A | 110.4 (3) |
O3Biii—Ca—O2Biv | 64.3 (2) | O3Ax—GeA—O3A | 102.7 (2) |
O3Aiii—Ca—O2Biv | 100.2 (3) | O2A—GeA—Ca | 36.2 (3) |
O2A—Ca—O3B | 85.0 (3) | O1A—GeA—Ca | 130.1 (2) |
O1Ai—Ca—O3B | 164.2 (2) | O3Ax—GeA—Ca | 120.7 (2) |
O1Bii—Ca—O3B | 102.4 (2) | O3A—GeA—Ca | 68.2 (2) |
O3Biii—Ca—O3B | 61.12 (10) | O2A—GeA—Cax | 105.6 (3) |
O3Aiii—Ca—O3B | 101.0 (2) | O1A—GeA—Cax | 132.3 (2) |
O2Biv—Ca—O3B | 110.4 (2) | O3Ax—GeA—Cax | 64.6 (2) |
O2A—Ca—O2Bii | 103.7 (3) | O3A—GeA—Cax | 39.8 (2) |
O1Ai—Ca—O2Bii | 129.0 (2) | Ca—GeA—Cax | 80.31 (6) |
O1Bii—Ca—O2Bii | 61.7 (2) | O2B—GeB—O1B | 111.6 (4) |
O3Biii—Ca—O2Bii | 78.0 (2) | O2B—GeB—O3B | 119.8 (4) |
O3Aiii—Ca—O2Bii | 149.3 (2) | O1B—GeB—O3B | 126.1 (3) |
O2Biv—Ca—O2Bii | 73.5 (3) | O2B—GeB—O3Bx | 95.0 (3) |
O3B—Ca—O2Bii | 56.2 (2) | O1B—GeB—O3Bx | 99.1 (3) |
O2A—Ca—Cuiv | 116.2 (2) | O3B—GeB—O3Bx | 91.8 (2) |
O1Ai—Ca—Cuiv | 37.24 (15) | O2B—GeB—O2Bii | 81.3 (4) |
O1Bii—Ca—Cuiv | 83.70 (17) | O1B—GeB—O2Bii | 87.3 (3) |
O3Biii—Ca—Cuiv | 100.49 (19) | O3B—GeB—O2Bii | 85.4 (3) |
O3Aiii—Ca—Cuiv | 81.90 (18) | O3Bx—GeB—O2Bii | 173.4 (3) |
O2Biv—Ca—Cuiv | 48.47 (19) | O2B—GeB—Cuii | 116.4 (3) |
O3B—Ca—Cuiv | 158.56 (17) | O1B—GeB—Cuii | 38.5 (2) |
O2Bii—Ca—Cuiv | 111.87 (16) | O3B—GeB—Cuii | 100.4 (2) |
O2A—Ca—GeBii | 85.3 (2) | O3Bx—GeB—Cuii | 133.0 (2) |
O1Ai—Ca—GeBii | 101.37 (18) | O2Bii—GeB—Cuii | 53.5 (2) |
O1Bii—Ca—GeBii | 30.57 (15) | O2B—GeB—Caii | 65.7 (3) |
O3Biii—Ca—GeBii | 108.33 (18) | O1B—GeB—Caii | 45.9 (2) |
O3Aiii—Ca—GeBii | 178.59 (18) | O3B—GeB—Caii | 163.0 (2) |
O2Biv—Ca—GeBii | 81.2 (2) | O3Bx—GeB—Caii | 104.0 (2) |
O3B—Ca—GeBii | 78.40 (16) | O2Bii—GeB—Caii | 79.5 (2) |
O2Bii—Ca—GeBii | 31.12 (13) | Cuii—GeB—Caii | 64.20 (5) |
Cuiv—Ca—GeBii | 99.10 (6) | O2B—GeB—Caviii | 47.4 (3) |
O2A—Ca—GeBiv | 171.9 (2) | O1B—GeB—Caviii | 114.7 (2) |
O1Ai—Ca—GeBiv | 108.32 (17) | O3B—GeB—Caviii | 111.4 (2) |
O1Bii—Ca—GeBiv | 115.45 (15) | O3Bx—GeB—Caviii | 47.6 (2) |
O3Biii—Ca—GeBiv | 33.76 (17) | O2Bii—GeB—Caviii | 128.24 (19) |
O3Aiii—Ca—GeBiv | 85.56 (17) | Cuii—GeB—Caviii | 148.14 (6) |
O2Biv—Ca—GeBiv | 30.53 (16) | Caii—GeB—Caviii | 84.31 (6) |
O3B—Ca—GeBiv | 87.37 (16) | O2B—GeB—Cax | 122.5 (3) |
O2Bii—Ca—GeBiv | 73.99 (15) | O1B—GeB—Cax | 116.7 (2) |
Cuiv—Ca—GeBiv | 71.59 (5) | O3B—GeB—Cax | 43.5 (2) |
GeBii—Ca—GeBiv | 95.69 (6) | O3Bx—GeB—Cax | 49.2 (2) |
O2A—Ca—Cu | 34.83 (18) | O2Bii—GeB—Cax | 128.8 (2) |
O1Ai—Ca—Cu | 77.88 (17) | Cuii—GeB—Cax | 120.59 (5) |
O1Bii—Ca—Cu | 34.66 (14) | Caii—GeB—Cax | 149.81 (5) |
O3Biii—Ca—Cu | 149.6 (2) | Caviii—GeB—Cax | 84.13 (6) |
O3Aiii—Ca—Cu | 126.18 (17) | O2B—GeB—Ca | 78.7 (3) |
O2Biv—Ca—Cu | 125.01 (19) | O1B—GeB—Ca | 143.2 (2) |
O3B—Ca—Cu | 89.90 (17) | O3B—GeB—Ca | 45.4 (3) |
O2Bii—Ca—Cu | 78.05 (15) | O3Bx—GeB—Ca | 115.6 (2) |
Cuiv—Ca—Cu | 105.64 (6) | O2Bii—GeB—Ca | 58.5 (2) |
GeBii—Ca—Cu | 52.63 (4) | Cuii—GeB—Ca | 104.79 (5) |
GeBiv—Ca—Cu | 147.99 (7) | Caii—GeB—Ca | 128.46 (5) |
O1Bii—Cu—O1Av | 176.3 (3) | Caviii—GeB—Ca | 98.42 (6) |
O1Bii—Cu—O2A | 87.7 (3) | Cax—GeB—Ca | 80.87 (6) |
O1Av—Cu—O2A | 94.5 (3) | GeA—O1A—Cuv | 121.0 (4) |
O1Bii—Cu—O1Bvi | 92.1 (2) | GeA—O1A—Cuxi | 112.9 (3) |
O1Av—Cu—O1Bvi | 85.4 (3) | Cuv—O1A—Cuxi | 93.3 (3) |
O2A—Cu—O1Bvi | 172.3 (3) | GeA—O1A—Cai | 130.2 (4) |
O1Bii—Cu—O1Avii | 80.4 (2) | Cuv—O1A—Cai | 92.9 (2) |
O1Av—Cu—O1Avii | 101.9 (3) | Cuxi—O1A—Cai | 98.8 (3) |
O2A—Cu—O1Avii | 104.8 (3) | GeB—O1B—Cuii | 107.4 (4) |
O1Bvi—Cu—O1Avii | 82.7 (2) | GeB—O1B—Cuxii | 137.6 (3) |
O1Bii—Cu—O2B | 77.1 (3) | Cuii—O1B—Cuxii | 99.5 (3) |
O1Av—Cu—O2B | 99.8 (3) | GeB—O1B—Caii | 103.5 (3) |
O2A—Cu—O2B | 91.5 (3) | Cuii—O1B—Caii | 99.0 (2) |
O1Bvi—Cu—O2B | 80.9 (3) | Cuxii—O1B—Caii | 103.9 (3) |
O1Avii—Cu—O2B | 151.6 (2) | GeA—O2A—Cu | 133.4 (5) |
O1Bii—Cu—GeBii | 34.1 (2) | GeA—O2A—Ca | 117.8 (4) |
O1Av—Cu—GeBii | 142.3 (2) | Cu—O2A—Ca | 103.0 (3) |
O2A—Cu—GeBii | 102.4 (2) | GeB—O2B—GeBii | 98.7 (3) |
O1Bvi—Cu—GeBii | 73.51 (16) | GeB—O2B—Cu | 133.0 (5) |
O1Avii—Cu—GeBii | 105.89 (15) | GeBii—O2B—Cu | 79.5 (3) |
O2B—Cu—GeBii | 46.98 (18) | GeB—O2B—Caviii | 102.1 (3) |
O1Bii—Cu—Caviii | 127.4 (2) | GeBii—O2B—Caviii | 157.8 (3) |
O1Av—Cu—Caviii | 49.9 (2) | Cu—O2B—Caviii | 80.7 (2) |
O2A—Cu—Caviii | 86.6 (2) | GeB—O2B—Caii | 83.2 (3) |
O1Bvi—Cu—Caviii | 87.45 (19) | GeBii—O2B—Caii | 83.5 (2) |
O1Avii—Cu—Caviii | 150.93 (17) | Cu—O2B—Caii | 141.8 (3) |
O2B—Cu—Caviii | 50.86 (19) | Caviii—O2B—Caii | 106.5 (3) |
GeBii—Cu—Caviii | 97.34 (5) | GeAiii—O3A—GeA | 126.8 (4) |
O1Bii—Cu—Ca | 46.30 (19) | GeAiii—O3A—Cax | 120.5 (3) |
O1Av—Cu—Ca | 135.2 (2) | GeA—O3A—Cax | 112.7 (4) |
O2A—Cu—Ca | 42.1 (2) | GeB—O3B—GeBiii | 122.8 (4) |
O1Bvi—Cu—Ca | 135.81 (17) | GeB—O3B—Cax | 107.3 (3) |
O1Avii—Cu—Ca | 100.40 (18) | GeBiii—O3B—Cax | 98.6 (3) |
O2B—Cu—Ca | 76.2 (2) | GeB—O3B—Ca | 106.3 (3) |
GeBii—Cu—Ca | 63.17 (4) | GeBiii—O3B—Ca | 98.3 (3) |
Caviii—Cu—Ca | 105.64 (6) | Cax—O3B—Ca | 124.8 (3) |
O1Bii—Cu—Caix | 78.95 (18) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.802 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2373 reflections |
a = 10.2180 (12) Å | θ = 2.1–27.7° |
b = 9.2536 (7) Å | µ = 17.97 mm−1 |
c = 5.2468 (6) Å | T = 654 K |
β = 105.975 (12)° | Cuboid, pale green |
V = 476.94 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 3717 independent reflections |
Plane graphite monochromator | 2406 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0 |
rotation method scans | θmax = 27.9°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | h = −13→13 |
Tmin = 0.094, Tmax = 0.158 | k = −12→12 |
3717 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0374P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.048 | (Δ/σ)max < 0.001 |
wR(F2) = 0.095 | Δρmax = 1.03 e Å−3 |
S = 0.94 | Δρmin = −0.97 e Å−3 |
3717 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
92 parameters | Extinction coefficient: 0.0061 (4) |
Crystal data top
CaCuGe2O6 | V = 476.94 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2180 (12) Å | µ = 17.97 mm−1 |
b = 9.2536 (7) Å | T = 654 K |
c = 5.2468 (6) Å | 0.14 × 0.13 × 0.10 mm |
β = 105.975 (12)° | |
Data collection top
STOE IPDS 1 diffractometer | 3717 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 2406 reflections with I > 2σ(I) |
Tmin = 0.094, Tmax = 0.158 | Rint = 0 |
3717 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.048 | 92 parameters |
wR(F2) = 0.095 | 0 restraints |
S = 0.94 | Δρmax = 1.03 e Å−3 |
3717 reflections | Δρmin = −0.97 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.27995 (13) | 0.45221 (13) | 0.8007 (3) | 0.0179 (3) | |
Cu | 0.22971 (7) | 0.65993 (8) | 0.25470 (13) | 0.01462 (19) | |
GeA | 0.04801 (5) | 0.34921 (7) | 0.21127 (12) | 0.01001 (15) | |
GeB | 0.48866 (6) | 0.34967 (7) | 0.38415 (13) | 0.01411 (16) | |
O1A | −0.1279 (4) | 0.3597 (5) | 0.1153 (8) | 0.0167 (9) | |
O1B | 0.6579 (4) | 0.3203 (4) | 0.3833 (8) | 0.0117 (9) | |
O2A | 0.1426 (5) | 0.4910 (5) | 0.3712 (10) | 0.0222 (12) | |
O2B | 0.4299 (5) | 0.5192 (4) | 0.2562 (10) | 0.0235 (11) | |
O3A | 0.1040 (4) | 0.1987 (5) | 0.4301 (9) | 0.0163 (10) | |
O3B | 0.4004 (4) | 0.2542 (5) | 0.5776 (9) | 0.0153 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0200 (6) | 0.0172 (5) | 0.0164 (7) | 0.0011 (5) | 0.0047 (5) | 0.0022 (5) |
Cu | 0.0157 (3) | 0.0146 (3) | 0.0108 (4) | −0.0029 (3) | −0.0011 (3) | −0.0001 (3) |
GeA | 0.0091 (3) | 0.0104 (3) | 0.0096 (3) | −0.0011 (2) | 0.0009 (2) | −0.0002 (2) |
GeB | 0.0114 (3) | 0.0118 (3) | 0.0206 (3) | 0.0021 (2) | 0.0069 (2) | 0.0045 (3) |
O1A | 0.0096 (17) | 0.022 (2) | 0.015 (2) | 0.0052 (17) | −0.0032 (16) | −0.0025 (19) |
O1B | 0.0112 (17) | 0.013 (2) | 0.010 (2) | 0.0003 (13) | 0.0020 (16) | −0.0019 (14) |
O2A | 0.032 (3) | 0.015 (2) | 0.016 (3) | −0.0145 (17) | 0.000 (2) | −0.0045 (17) |
O2B | 0.036 (3) | 0.013 (2) | 0.022 (3) | 0.0045 (18) | 0.009 (2) | 0.0065 (18) |
O3A | 0.020 (2) | 0.021 (2) | 0.010 (2) | 0.0029 (15) | 0.0065 (19) | 0.0052 (16) |
O3B | 0.0131 (19) | 0.023 (2) | 0.010 (2) | −0.0066 (15) | 0.0030 (18) | 0.0025 (16) |
Geometric parameters (Å, º) top
Ca—O2A | 2.332 (5) | GeA—O3A | 1.796 (4) |
Ca—O1Ai | 2.452 (4) | GeA—Cax | 3.6062 (14) |
Ca—O1Bii | 2.471 (4) | GeB—O2B | 1.747 (4) |
Ca—O3Biii | 2.507 (4) | GeB—O1B | 1.751 (4) |
Ca—O3Aiii | 2.512 (5) | GeB—O3B | 1.769 (5) |
Ca—O2Biv | 2.535 (5) | GeB—O3Bx | 1.878 (4) |
Ca—O3B | 2.652 (5) | GeB—O2Bii | 2.204 (5) |
Ca—O2Bii | 3.072 (5) | GeB—Cuii | 2.9797 (10) |
Ca—Cuiv | 3.2101 (17) | GeB—Caii | 3.3399 (15) |
Ca—GeBii | 3.3399 (15) | GeB—Caviii | 3.3503 (15) |
Ca—GeBiv | 3.3503 (15) | GeB—Cax | 3.4683 (14) |
Ca—Cu | 3.3700 (16) | O1A—Cuv | 1.942 (4) |
Cu—O1Bii | 1.939 (4) | O1A—Cuxi | 2.314 (5) |
Cu—O1Av | 1.942 (4) | O1A—Cai | 2.452 (4) |
Cu—O2A | 1.977 (5) | O1B—Cuii | 1.939 (4) |
Cu—O1Bvi | 2.122 (4) | O1B—Cuxii | 2.122 (4) |
Cu—O1Avii | 2.314 (5) | O1B—Caii | 2.471 (4) |
Cu—O2B | 2.423 (5) | O2B—GeBii | 2.204 (5) |
Cu—GeBii | 2.9797 (10) | O2B—Caviii | 2.535 (5) |
Cu—Caviii | 3.2101 (17) | O2B—Caii | 3.072 (5) |
Cu—Caix | 3.6242 (13) | O3A—GeAiii | 1.779 (5) |
GeA—O2A | 1.707 (4) | O3A—Cax | 2.512 (5) |
GeA—O1A | 1.731 (4) | O3B—GeBiii | 1.878 (4) |
GeA—O3Ax | 1.779 (5) | O3B—Cax | 2.507 (4) |
| | | |
O2A—Ca—O1Ai | 79.75 (16) | O1Av—Cu—Caix | 100.75 (14) |
O2A—Ca—O1Bii | 69.04 (14) | O2A—Cu—Caix | 146.11 (16) |
O1Ai—Ca—O1Bii | 73.11 (15) | O1Bvi—Cu—Caix | 41.43 (12) |
O2A—Ca—O3Biii | 138.24 (16) | O1Avii—Cu—Caix | 41.94 (11) |
O1Ai—Ca—O3Biii | 132.11 (16) | O2B—Cu—Caix | 115.33 (11) |
O1Bii—Ca—O3Biii | 137.50 (14) | GeBii—Cu—Caix | 83.85 (3) |
O2A—Ca—O3Aiii | 93.53 (16) | Caviii—Cu—Caix | 126.43 (5) |
O1Ai—Ca—O3Aiii | 79.05 (16) | Ca—Cu—Caix | 121.50 (5) |
O1Bii—Ca—O3Aiii | 149.21 (14) | O2A—GeA—O1A | 120.1 (2) |
O3Biii—Ca—O3Aiii | 72.17 (14) | O2A—GeA—O3Ax | 109.3 (2) |
O2A—Ca—O2Biv | 156.97 (15) | O1A—GeA—O3Ax | 108.55 (19) |
O1Ai—Ca—O2Biv | 84.58 (15) | O2A—GeA—O3A | 104.1 (2) |
O1Bii—Ca—O2Biv | 90.36 (15) | O1A—GeA—O3A | 110.6 (2) |
O3Biii—Ca—O2Biv | 64.37 (14) | O3Ax—GeA—O3A | 102.61 (15) |
O3Aiii—Ca—O2Biv | 99.97 (16) | O2A—GeA—Ca | 36.46 (16) |
O2A—Ca—O3B | 84.75 (16) | O1A—GeA—Ca | 130.04 (15) |
O1Ai—Ca—O3B | 164.45 (14) | O3Ax—GeA—Ca | 120.70 (13) |
O1Bii—Ca—O3B | 102.45 (15) | O3A—GeA—Ca | 67.93 (14) |
O3Biii—Ca—O3B | 61.07 (6) | O2A—GeA—Cax | 105.51 (17) |
O3Aiii—Ca—O3B | 100.87 (14) | O1A—GeA—Cax | 132.38 (16) |
O2Biv—Ca—O3B | 110.59 (15) | O3Ax—GeA—Cax | 64.25 (14) |
O2A—Ca—O2Bii | 103.46 (17) | O3A—GeA—Cax | 40.03 (16) |
O1Ai—Ca—O2Bii | 129.25 (14) | Ca—GeA—Cax | 80.41 (4) |
O1Bii—Ca—O2Bii | 61.95 (12) | O2B—GeB—O1B | 111.9 (2) |
O3Biii—Ca—O2Bii | 77.82 (14) | O2B—GeB—O3B | 119.6 (2) |
O3Aiii—Ca—O2Bii | 148.82 (13) | O1B—GeB—O3B | 125.71 (19) |
O2Biv—Ca—O2Bii | 73.83 (19) | O2B—GeB—O3Bx | 95.6 (2) |
O3B—Ca—O2Bii | 55.89 (12) | O1B—GeB—O3Bx | 99.23 (19) |
O2A—Ca—Cuiv | 116.65 (14) | O3B—GeB—O3Bx | 92.01 (12) |
O1Ai—Ca—Cuiv | 37.17 (9) | O2B—GeB—O2Bii | 81.0 (2) |
O1Bii—Ca—Cuiv | 83.72 (11) | O1B—GeB—O2Bii | 86.98 (19) |
O3Biii—Ca—Cuiv | 100.34 (11) | O3B—GeB—O2Bii | 85.2 (2) |
O3Aiii—Ca—Cuiv | 81.95 (11) | O3Bx—GeB—O2Bii | 173.70 (18) |
O2Biv—Ca—Cuiv | 48.14 (12) | O2B—GeB—Cuii | 116.15 (16) |
O3B—Ca—Cuiv | 158.37 (10) | O1B—GeB—Cuii | 38.34 (13) |
O2Bii—Ca—Cuiv | 112.11 (10) | O3B—GeB—Cuii | 100.14 (13) |
O2A—Ca—GeBii | 85.44 (13) | O3Bx—GeB—Cuii | 132.98 (13) |
O1Ai—Ca—GeBii | 101.35 (12) | O2Bii—GeB—Cuii | 53.21 (13) |
O1Bii—Ca—GeBii | 30.69 (9) | O2B—GeB—Caii | 65.87 (18) |
O3Biii—Ca—GeBii | 108.22 (11) | O1B—GeB—Caii | 46.07 (13) |
O3Aiii—Ca—GeBii | 178.81 (11) | O3B—GeB—Caii | 162.65 (13) |
O2Biv—Ca—GeBii | 81.20 (12) | O3Bx—GeB—Caii | 104.11 (15) |
O3B—Ca—GeBii | 78.44 (10) | O2Bii—GeB—Caii | 79.40 (14) |
O2Bii—Ca—GeBii | 31.26 (8) | Cuii—GeB—Caii | 64.16 (3) |
Cuiv—Ca—GeBii | 99.06 (4) | O2B—GeB—Caviii | 47.90 (16) |
O2A—Ca—GeBiv | 171.54 (13) | O1B—GeB—Caviii | 114.97 (14) |
O1Ai—Ca—GeBiv | 108.20 (11) | O3B—GeB—Caviii | 111.64 (13) |
O1Bii—Ca—GeBiv | 115.52 (9) | O3Bx—GeB—Caviii | 47.73 (13) |
O3Biii—Ca—GeBiv | 33.65 (10) | O2Bii—GeB—Caviii | 128.43 (11) |
O3Aiii—Ca—GeBiv | 85.34 (10) | Cuii—GeB—Caviii | 148.21 (4) |
O2Biv—Ca—GeBiv | 30.74 (10) | Caii—GeB—Caviii | 84.41 (4) |
O3B—Ca—GeBiv | 87.23 (10) | O2B—GeB—Cax | 122.73 (16) |
O2Bii—Ca—GeBiv | 74.02 (10) | O1B—GeB—Cax | 116.60 (13) |
Cuiv—Ca—GeBiv | 71.53 (3) | O3B—GeB—Cax | 43.70 (14) |
GeBii—Ca—GeBiv | 95.59 (4) | O3Bx—GeB—Cax | 49.15 (15) |
O2A—Ca—Cu | 34.93 (11) | O2Bii—GeB—Cax | 128.71 (14) |
O1Ai—Ca—Cu | 78.00 (11) | Cuii—GeB—Cax | 120.59 (3) |
O1Bii—Ca—Cu | 34.64 (9) | Caii—GeB—Cax | 149.92 (3) |
O3Biii—Ca—Cu | 149.61 (12) | Caviii—GeB—Cax | 84.16 (4) |
O3Aiii—Ca—Cu | 126.41 (10) | O2B—GeB—Ca | 78.28 (19) |
O2Biv—Ca—Cu | 124.96 (11) | O1B—GeB—Ca | 142.92 (14) |
O3B—Ca—Cu | 89.97 (10) | O3B—GeB—Ca | 45.40 (15) |
O2Bii—Ca—Cu | 78.08 (9) | O3Bx—GeB—Ca | 115.63 (14) |
Cuiv—Ca—Cu | 105.74 (4) | O2Bii—GeB—Ca | 58.60 (14) |
GeBii—Ca—Cu | 52.73 (3) | Cuii—GeB—Ca | 104.67 (3) |
GeBiv—Ca—Cu | 148.00 (5) | Caii—GeB—Ca | 128.37 (3) |
O1Bii—Cu—O1Av | 176.26 (18) | Caviii—GeB—Ca | 98.43 (4) |
O1Bii—Cu—O2A | 88.14 (18) | Cax—GeB—Ca | 80.88 (4) |
O1Av—Cu—O2A | 94.13 (19) | GeA—O1A—Cuv | 120.9 (3) |
O1Bii—Cu—O1Bvi | 92.17 (14) | GeA—O1A—Cuxi | 112.6 (2) |
O1Av—Cu—O1Bvi | 85.17 (17) | Cuv—O1A—Cuxi | 93.39 (17) |
O2A—Cu—O1Bvi | 172.0 (2) | GeA—O1A—Cai | 130.3 (2) |
O1Bii—Cu—O1Avii | 80.16 (15) | Cuv—O1A—Cai | 93.12 (15) |
O1Av—Cu—O1Avii | 102.06 (15) | Cuxi—O1A—Cai | 98.95 (16) |
O2A—Cu—O1Avii | 105.29 (19) | GeB—O1B—Cuii | 107.6 (2) |
O1Bvi—Cu—O1Avii | 82.61 (16) | GeB—O1B—Cuxii | 137.5 (2) |
O1Bii—Cu—O2B | 77.02 (17) | Cuii—O1B—Cuxii | 99.77 (16) |
O1Av—Cu—O2B | 99.93 (18) | GeB—O1B—Caii | 103.24 (17) |
O2A—Cu—O2B | 91.46 (19) | Cuii—O1B—Caii | 98.96 (15) |
O1Bvi—Cu—O2B | 80.85 (16) | Cuxii—O1B—Caii | 103.93 (18) |
O1Avii—Cu—O2B | 151.14 (15) | GeA—O2A—Cu | 134.3 (3) |
O1Bii—Cu—GeBii | 34.08 (13) | GeA—O2A—Ca | 117.8 (2) |
O1Av—Cu—GeBii | 142.25 (13) | Cu—O2A—Ca | 102.60 (18) |
O2A—Cu—GeBii | 102.58 (14) | GeB—O2B—GeBii | 99.0 (2) |
O1Bvi—Cu—GeBii | 73.68 (10) | GeB—O2B—Cu | 133.2 (3) |
O1Avii—Cu—GeBii | 105.68 (9) | GeBii—O2B—Cu | 80.01 (16) |
O2B—Cu—GeBii | 46.77 (12) | GeB—O2B—Caviii | 101.4 (2) |
O1Bii—Cu—Caviii | 127.64 (12) | GeBii—O2B—Caviii | 158.3 (2) |
O1Av—Cu—Caviii | 49.71 (13) | Cu—O2B—Caviii | 80.65 (14) |
O2A—Cu—Caviii | 86.17 (15) | GeB—O2B—Caii | 82.87 (18) |
O1Bvi—Cu—Caviii | 87.33 (12) | GeBii—O2B—Caii | 83.62 (15) |
O1Avii—Cu—Caviii | 150.89 (11) | Cu—O2B—Caii | 142.19 (17) |
O2B—Cu—Caviii | 51.20 (12) | Caviii—O2B—Caii | 106.17 (19) |
GeBii—Cu—Caviii | 97.49 (3) | GeAiii—O3A—GeA | 127.2 (3) |
O1Bii—Cu—Ca | 46.41 (12) | GeAiii—O3A—Cax | 120.2 (2) |
O1Av—Cu—Ca | 135.29 (15) | GeA—O3A—Cax | 112.6 (2) |
O2A—Cu—Ca | 42.47 (13) | GeB—O3B—GeBiii | 123.1 (2) |
O1Bvi—Cu—Ca | 135.95 (10) | GeB—O3B—Cax | 107.1 (2) |
O1Avii—Cu—Ca | 100.42 (11) | GeBiii—O3B—Cax | 98.62 (18) |
O2B—Cu—Ca | 76.10 (13) | GeB—O3B—Ca | 106.25 (19) |
GeBii—Cu—Ca | 63.12 (3) | GeBiii—O3B—Ca | 98.47 (19) |
Caviii—Cu—Ca | 105.74 (4) | Cax—O3B—Ca | 124.66 (17) |
O1Bii—Cu—Caix | 78.84 (11) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y, z+1; (v) −x, −y+1, −z; (vi) −x+1, y+1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (ix) x, −y+3/2, z−1/2; (x) x, −y+1/2, z−1/2; (xi) −x, y−1/2, −z+1/2; (xii) −x+1, y−1/2, −z+1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.688 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1683 reflections |
a = 10.2453 (12) Å | θ = 3.0–27.8° |
b = 9.2118 (9) Å | µ = 17.54 mm−1 |
c = 5.4115 (7) Å | T = 717 K |
β = 106.931 (14)° | Cuboid, pale green |
V = 488.50 (10) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 510 independent reflections |
Plane graphite monochromator | 392 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.048 |
rotation method scans | θmax = 27.8°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) ? | h = −13→13 |
Tmin = 0.102, Tmax = 0.172 | k = −11→12 |
1629 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0471P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.034 | (Δ/σ)max < 0.001 |
wR(F2) = 0.085 | Δρmax = 0.80 e Å−3 |
S = 1.05 | Δρmin = −0.75 e Å−3 |
510 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
48 parameters | Extinction coefficient: 0.0057 (7) |
Crystal data top
CaCuGe2O6 | V = 488.50 (10) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.2453 (12) Å | µ = 17.54 mm−1 |
b = 9.2118 (9) Å | T = 717 K |
c = 5.4115 (7) Å | 0.14 × 0.13 × 0.10 mm |
β = 106.931 (14)° | |
Data collection top
STOE IPDS 1 diffractometer | 510 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 392 reflections with I > 2σ(I) |
Tmin = 0.102, Tmax = 0.172 | Rint = 0.048 |
1629 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 48 parameters |
wR(F2) = 0.085 | 0 restraints |
S = 1.05 | Δρmax = 0.80 e Å−3 |
510 reflections | Δρmin = −0.75 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0 | 0.3009 (2) | 0.25 | 0.0246 (5) | |
Cu | 0 | 0.90652 (14) | 0.25 | 0.0183 (3) | |
Ge | 0.28317 (7) | 0.09748 (8) | 0.21310 (14) | 0.0161 (2) | |
O1 | 0.1065 (5) | 0.0931 (7) | 0.1212 (10) | 0.0231 (11) | |
O2 | 0.3605 (6) | 0.2592 (6) | 0.3320 (12) | 0.0313 (14) | |
O3 | 0.3562 (5) | 0.0259 (6) | −0.0208 (11) | 0.0241 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0289 (10) | 0.0191 (10) | 0.0229 (11) | 0 | 0.0031 (9) | 0 |
Cu | 0.0170 (5) | 0.0200 (6) | 0.0152 (6) | 0 | 0.0006 (4) | 0 |
Ge | 0.0127 (3) | 0.0174 (4) | 0.0168 (4) | 0.0005 (3) | 0.0020 (2) | −0.0017 (3) |
O1 | 0.0112 (19) | 0.036 (3) | 0.019 (3) | 0.006 (2) | −0.0006 (19) | 0.000 (2) |
O2 | 0.041 (3) | 0.019 (3) | 0.033 (3) | −0.005 (2) | 0.008 (3) | −0.007 (2) |
O3 | 0.015 (2) | 0.032 (3) | 0.023 (3) | 0.000 (2) | 0.003 (2) | −0.008 (2) |
Geometric parameters (Å, º) top
Ca—O2i | 2.363 (6) | Cu—O1xii | 2.253 (6) |
Ca—O2ii | 2.363 (6) | Cu—Caviii | 3.3124 (16) |
Ca—O1iii | 2.405 (6) | Cu—Caix | 3.3124 (16) |
Ca—O1 | 2.405 (6) | Cu—Caxii | 3.633 (2) |
Ca—O3iv | 2.705 (6) | Ge—O2 | 1.722 (5) |
Ca—O3v | 2.705 (6) | Ge—O1 | 1.732 (4) |
Ca—O3vi | 2.712 (6) | Ge—O3 | 1.774 (6) |
Ca—O3vii | 2.712 (6) | Ge—O3xiii | 1.816 (5) |
Ca—Geii | 3.2391 (9) | Ge—Caii | 3.2391 (9) |
Ca—Gei | 3.2391 (9) | Ge—Caxiv | 3.4899 (19) |
Ca—Cuviii | 3.3124 (16) | O1—Cuviii | 1.987 (5) |
Ca—Cuix | 3.3124 (16) | O1—Cuxv | 2.253 (6) |
Cu—O1viii | 1.987 (5) | O2—Cuxiv | 2.109 (6) |
Cu—O1x | 1.987 (5) | O2—Caii | 2.363 (6) |
Cu—O2vii | 2.109 (6) | O3—Gexvi | 1.816 (5) |
Cu—O2vi | 2.109 (6) | O3—Cav | 2.705 (6) |
Cu—O1xi | 2.253 (6) | O3—Caxiv | 2.712 (6) |
| | | |
O2i—Ca—O2ii | 152.9 (3) | O1viii—Cu—O2vi | 89.7 (2) |
O2i—Ca—O1iii | 83.79 (19) | O1x—Cu—O2vi | 90.4 (2) |
O2ii—Ca—O1iii | 74.62 (18) | O2vii—Cu—O2vi | 99.9 (3) |
O2i—Ca—O1 | 74.62 (18) | O1viii—Cu—O1xi | 97.98 (18) |
O2ii—Ca—O1 | 83.79 (19) | O1x—Cu—O1xi | 81.9 (2) |
O1iii—Ca—O1 | 74.5 (3) | O2vii—Cu—O1xi | 90.4 (2) |
O2i—Ca—O3iv | 108.60 (18) | O2vi—Cu—O1xi | 167.12 (19) |
O2ii—Ca—O3iv | 87.58 (18) | O1viii—Cu—O1xii | 81.9 (2) |
O1iii—Ca—O3iv | 89.01 (18) | O1x—Cu—O1xii | 97.98 (18) |
O1—Ca—O3iv | 162.9 (2) | O2vii—Cu—O1xii | 167.12 (19) |
O2i—Ca—O3v | 87.58 (18) | O2vi—Cu—O1xii | 90.4 (2) |
O2ii—Ca—O3v | 108.60 (18) | O1xi—Cu—O1xii | 80.5 (3) |
O1iii—Ca—O3v | 162.9 (2) | O1viii—Cu—Caviii | 46.04 (16) |
O1—Ca—O3v | 89.01 (18) | O1x—Cu—Caviii | 134.10 (18) |
O3iv—Ca—O3v | 107.7 (2) | O2vii—Cu—Caviii | 87.82 (17) |
O2i—Ca—O3vi | 141.11 (19) | O2vi—Cu—Caviii | 45.24 (16) |
O2ii—Ca—O3vi | 65.17 (17) | O1xi—Cu—Caviii | 143.93 (12) |
O1iii—Ca—O3vi | 132.26 (18) | O1xii—Cu—Caviii | 94.15 (15) |
O1—Ca—O3vi | 122.95 (15) | O1viii—Cu—Caix | 134.10 (18) |
O3iv—Ca—O3vi | 65.44 (17) | O1x—Cu—Caix | 46.04 (16) |
O3v—Ca—O3vi | 60.94 (8) | O2vii—Cu—Caix | 45.24 (16) |
O2i—Ca—O3vii | 65.17 (17) | O2vi—Cu—Caix | 87.82 (17) |
O2ii—Ca—O3vii | 141.11 (19) | O1xi—Cu—Caix | 94.15 (15) |
O1iii—Ca—O3vii | 122.95 (15) | O1xii—Cu—Caix | 143.93 (12) |
O1—Ca—O3vii | 132.26 (18) | Caviii—Cu—Caix | 109.53 (8) |
O3iv—Ca—O3vii | 60.94 (8) | O1viii—Cu—Caxii | 89.91 (18) |
O3v—Ca—O3vii | 65.44 (17) | O1x—Cu—Caxii | 89.91 (18) |
O3vi—Ca—O3vii | 80.3 (2) | O2vii—Cu—Caxii | 130.04 (16) |
O2i—Ca—Geii | 172.75 (16) | O2vi—Cu—Caxii | 130.04 (16) |
O2ii—Ca—Geii | 31.08 (13) | O1xi—Cu—Caxii | 40.26 (14) |
O1iii—Ca—Geii | 102.74 (12) | O1xii—Cu—Caxii | 40.26 (14) |
O1—Ca—Geii | 103.85 (11) | Caviii—Cu—Caxii | 125.24 (4) |
O3iv—Ca—Geii | 75.00 (10) | Caix—Cu—Caxii | 125.24 (4) |
O3v—Ca—Geii | 85.30 (11) | O2—Ge—O1 | 117.1 (3) |
O3vi—Ca—Geii | 34.09 (11) | O2—Ge—O3 | 110.1 (3) |
O3vii—Ca—Geii | 112.74 (13) | O1—Ge—O3 | 114.1 (2) |
O2i—Ca—Gei | 31.08 (13) | O2—Ge—O3xiii | 101.9 (3) |
O2ii—Ca—Gei | 172.75 (16) | O1—Ge—O3xiii | 111.6 (3) |
O1iii—Ca—Gei | 103.85 (11) | O3—Ge—O3xiii | 99.85 (15) |
O1—Ca—Gei | 102.74 (12) | O2—Ge—Caii | 45.1 (2) |
O3iv—Ca—Gei | 85.30 (11) | O1—Ge—Caii | 130.59 (19) |
O3v—Ca—Gei | 75.00 (10) | O3—Ge—Caii | 115.19 (14) |
O3vi—Ca—Gei | 112.74 (13) | O3xiii—Ge—Caii | 56.84 (18) |
O3vii—Ca—Gei | 34.09 (11) | O2—Ge—Caxiv | 116.1 (2) |
Geii—Ca—Gei | 146.41 (8) | O1—Ge—Caxiv | 126.4 (2) |
O2i—Ca—Cuviii | 39.34 (15) | O3—Ge—Caxiv | 49.92 (18) |
O2ii—Ca—Cuviii | 120.18 (16) | O3xiii—Ge—Caxiv | 49.94 (19) |
O1iii—Ca—Cuviii | 83.43 (15) | Caii—Ge—Caxiv | 85.18 (5) |
O1—Ca—Cuviii | 36.49 (12) | O2—Ge—Ca | 79.3 (2) |
O3iv—Ca—Cuviii | 147.59 (10) | O1—Ge—Ca | 38.41 (19) |
O3v—Ca—Cuviii | 80.57 (12) | O3—Ge—Ca | 140.06 (16) |
O3vi—Ca—Cuviii | 138.84 (13) | O3xiii—Ge—Ca | 116.47 (18) |
O3vii—Ca—Cuviii | 97.40 (12) | Caii—Ge—Ca | 99.04 (2) |
Geii—Ca—Cuviii | 137.40 (3) | Caxiv—Ge—Ca | 159.74 (6) |
Gei—Ca—Cuviii | 66.250 (19) | Ge—O1—Cuviii | 120.7 (3) |
O2i—Ca—Cuix | 120.18 (16) | Ge—O1—Cuxv | 119.2 (3) |
O2ii—Ca—Cuix | 39.34 (15) | Cuviii—O1—Cuxv | 98.1 (2) |
O1iii—Ca—Cuix | 36.49 (12) | Ge—O1—Ca | 115.0 (3) |
O1—Ca—Cuix | 83.43 (15) | Cuviii—O1—Ca | 97.5 (2) |
O3iv—Ca—Cuix | 80.57 (12) | Cuxv—O1—Ca | 102.5 (2) |
O3v—Ca—Cuix | 147.59 (10) | Ge—O2—Cuxiv | 138.1 (4) |
O3vi—Ca—Cuix | 97.40 (12) | Ge—O2—Caii | 103.8 (3) |
O3vii—Ca—Cuix | 138.84 (13) | Cuxiv—O2—Caii | 95.4 (2) |
Geii—Ca—Cuix | 66.250 (19) | Ge—O3—Gexvi | 129.5 (3) |
Gei—Ca—Cuix | 137.40 (3) | Ge—O3—Cav | 120.5 (3) |
Cuviii—Ca—Cuix | 109.53 (8) | Gexvi—O3—Cav | 99.2 (3) |
O1viii—Cu—O1x | 179.8 (4) | Ge—O3—Caxiv | 100.0 (2) |
O1viii—Cu—O2vii | 90.4 (2) | Gexvi—O3—Caxiv | 89.1 (2) |
O1x—Cu—O2vii | 89.7 (2) | Cav—O3—Caxiv | 114.56 (17) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) −x+1/2, −y+1/2, −z; (vi) −x+1/2, y+1/2, −z+1/2; (vii) x−1/2, y+1/2, z; (viii) −x, −y+1, −z; (ix) −x, −y+1, −z+1; (x) x, −y+1, z+1/2; (xi) −x, y+1, −z+1/2; (xii) x, y+1, z; (xiii) x, −y, z+1/2; (xiv) x+1/2, y−1/2, z; (xv) x, y−1, z; (xvi) x, −y, z−1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.72 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1642 reflections |
a = 10.2405 (12) Å | θ = 3.0–27.8° |
b = 9.1780 (8) Å | µ = 17.66 mm−1 |
c = 5.4003 (7) Å | T = 729 K |
β = 107.072 (11)° | Cuboid, pale green |
V = 485.19 (9) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 500 independent reflections |
Plane graphite monochromator | 374 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.057 |
rotation method scans | θmax = 28.1°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) ? | h = −13→13 |
Tmin = 0.102, Tmax = 0.172 | k = −12→12 |
1641 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0203P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.026 | (Δ/σ)max < 0.001 |
wR(F2) = 0.052 | Δρmax = 0.73 e Å−3 |
S = 0.94 | Δρmin = −0.61 e Å−3 |
500 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
48 parameters | Extinction coefficient: 0.0055 (5) |
Crystal data top
CaCuGe2O6 | V = 485.19 (9) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.2405 (12) Å | µ = 17.66 mm−1 |
b = 9.1780 (8) Å | T = 729 K |
c = 5.4003 (7) Å | 0.14 × 0.13 × 0.10 mm |
β = 107.072 (11)° | |
Data collection top
STOE IPDS 1 diffractometer | 500 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 374 reflections with I > 2σ(I) |
Tmin = 0.102, Tmax = 0.172 | Rint = 0.057 |
1641 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.026 | 48 parameters |
wR(F2) = 0.052 | 0 restraints |
S = 0.94 | Δρmax = 0.73 e Å−3 |
500 reflections | Δρmin = −0.61 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0 | 0.30077 (17) | 0.25 | 0.0207 (4) | |
Cu | 0 | 0.90638 (11) | 0.25 | 0.0159 (2) | |
Ge | 0.28308 (5) | 0.09741 (6) | 0.21294 (11) | 0.01320 (19) | |
O1 | 0.1064 (3) | 0.0916 (5) | 0.1211 (8) | 0.0195 (8) | |
O2 | 0.3599 (4) | 0.2586 (4) | 0.3324 (9) | 0.0301 (11) | |
O3 | 0.3558 (4) | 0.0266 (5) | −0.0208 (8) | 0.0204 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0253 (8) | 0.0193 (8) | 0.0164 (9) | 0 | 0.0045 (7) | 0 |
Cu | 0.0153 (4) | 0.0212 (4) | 0.0095 (5) | 0 | 0.0010 (4) | 0 |
Ge | 0.0111 (3) | 0.0172 (3) | 0.0112 (3) | 0.0004 (2) | 0.0030 (2) | −0.0016 (3) |
O1 | 0.0096 (14) | 0.035 (2) | 0.012 (2) | 0.0061 (17) | −0.0009 (15) | 0.0016 (18) |
O2 | 0.036 (2) | 0.023 (2) | 0.029 (3) | −0.0069 (16) | 0.005 (2) | −0.0091 (18) |
O3 | 0.0146 (17) | 0.031 (2) | 0.015 (2) | 0.0009 (15) | 0.0028 (17) | −0.0097 (17) |
Geometric parameters (Å, º) top
Ca—O2i | 2.354 (4) | Cu—O1xii | 2.237 (4) |
Ca—O2ii | 2.354 (4) | Cu—Caviii | 3.3023 (12) |
Ca—O1iii | 2.409 (4) | Cu—Caix | 3.3023 (12) |
Ca—O1 | 2.409 (4) | Cu—Caxi | 3.6197 (17) |
Ca—O3iv | 2.701 (4) | Ge—O2 | 1.710 (4) |
Ca—O3v | 2.701 (4) | Ge—O1 | 1.731 (3) |
Ca—O3vi | 2.711 (4) | Ge—O3 | 1.767 (4) |
Ca—O3vii | 2.711 (4) | Ge—O3xiii | 1.813 (4) |
Ca—Geii | 3.2306 (8) | Ge—Caii | 3.2306 (8) |
Ca—Gei | 3.2306 (8) | Ge—Caxiv | 3.4822 (13) |
Ca—Cuviii | 3.3023 (12) | O1—Cuviii | 1.980 (4) |
Ca—Cuix | 3.3023 (12) | O1—Cuxv | 2.237 (4) |
Cu—O1x | 1.980 (4) | O2—Cuxiv | 2.115 (4) |
Cu—O1viii | 1.980 (4) | O2—Caii | 2.354 (4) |
Cu—O2vii | 2.115 (5) | O3—Gexvi | 1.813 (4) |
Cu—O2vi | 2.115 (5) | O3—Caiv | 2.701 (4) |
Cu—O1xi | 2.237 (4) | O3—Caxiv | 2.711 (4) |
| | | |
O2i—Ca—O2ii | 153.2 (2) | O1x—Cu—O2vi | 90.76 (17) |
O2i—Ca—O1iii | 83.81 (15) | O1viii—Cu—O2vi | 89.94 (17) |
O2ii—Ca—O1iii | 74.87 (13) | O2vii—Cu—O2vi | 100.2 (2) |
O2i—Ca—O1 | 74.87 (13) | O1x—Cu—O1xi | 97.71 (13) |
O2ii—Ca—O1 | 83.81 (15) | O1viii—Cu—O1xi | 81.45 (15) |
O1iii—Ca—O1 | 74.3 (2) | O2vii—Cu—O1xi | 167.22 (14) |
O2i—Ca—O3iv | 87.61 (13) | O2vi—Cu—O1xi | 89.96 (16) |
O2ii—Ca—O3iv | 108.25 (13) | O1x—Cu—O1xii | 81.45 (15) |
O1iii—Ca—O3iv | 162.63 (14) | O1viii—Cu—O1xii | 97.71 (13) |
O1—Ca—O3iv | 88.90 (13) | O2vii—Cu—O1xii | 89.96 (16) |
O2i—Ca—O3v | 108.25 (13) | O2vi—Cu—O1xii | 167.22 (14) |
O2ii—Ca—O3v | 87.61 (13) | O1xi—Cu—O1xii | 81.1 (2) |
O1iii—Ca—O3v | 88.90 (13) | O1x—Cu—Caviii | 134.50 (12) |
O1—Ca—O3v | 162.62 (14) | O1viii—Cu—Caviii | 46.37 (12) |
O3iv—Ca—O3v | 108.17 (17) | O2vii—Cu—Caviii | 88.03 (13) |
O2i—Ca—O3vi | 140.91 (14) | O2vi—Cu—Caviii | 45.24 (12) |
O2ii—Ca—O3vi | 65.02 (12) | O1xi—Cu—Caviii | 93.79 (11) |
O1iii—Ca—O3vi | 132.42 (13) | O1xii—Cu—Caviii | 143.96 (9) |
O1—Ca—O3vi | 122.99 (11) | O1x—Cu—Caix | 46.37 (12) |
O3iv—Ca—O3vi | 60.93 (6) | O1viii—Cu—Caix | 134.50 (12) |
O3v—Ca—O3vi | 65.71 (13) | O2vii—Cu—Caix | 45.24 (12) |
O2i—Ca—O3vii | 65.02 (12) | O2vi—Cu—Caix | 88.03 (13) |
O2ii—Ca—O3vii | 140.91 (14) | O1xi—Cu—Caix | 143.96 (9) |
O1iii—Ca—O3vii | 122.99 (11) | O1xii—Cu—Caix | 93.79 (11) |
O1—Ca—O3vii | 132.42 (13) | Caviii—Cu—Caix | 109.70 (6) |
O3iv—Ca—O3vii | 65.71 (13) | O1x—Cu—Caxi | 89.46 (12) |
O3v—Ca—O3vii | 60.93 (6) | O1viii—Cu—Caxi | 89.46 (12) |
O3vi—Ca—O3vii | 80.25 (16) | O2vii—Cu—Caxi | 129.90 (12) |
O2i—Ca—Geii | 172.79 (12) | O2vi—Cu—Caxi | 129.90 (12) |
O2ii—Ca—Geii | 30.88 (10) | O1xi—Cu—Caxi | 40.56 (10) |
O1iii—Ca—Geii | 102.78 (9) | O1xii—Cu—Caxi | 40.56 (10) |
O1—Ca—Geii | 103.88 (8) | Caviii—Cu—Caxi | 125.15 (3) |
O3iv—Ca—Geii | 85.26 (8) | Caix—Cu—Caxi | 125.15 (3) |
O3v—Ca—Geii | 75.12 (8) | O2—Ge—O1 | 117.45 (19) |
O3vi—Ca—Geii | 34.14 (8) | O2—Ge—O3 | 110.1 (2) |
O3vii—Ca—Geii | 112.66 (9) | O1—Ge—O3 | 114.10 (18) |
O2i—Ca—Gei | 30.88 (10) | O2—Ge—O3xiii | 102.0 (2) |
O2ii—Ca—Gei | 172.79 (12) | O1—Ge—O3xiii | 111.05 (18) |
O1iii—Ca—Gei | 103.88 (8) | O3—Ge—O3xiii | 100.05 (12) |
O1—Ca—Gei | 102.78 (9) | O2—Ge—Caii | 44.96 (15) |
O3iv—Ca—Gei | 75.12 (8) | O1—Ge—Caii | 130.66 (14) |
O3v—Ca—Gei | 85.26 (8) | O3—Ge—Caii | 115.14 (11) |
O3vi—Ca—Gei | 112.66 (9) | O3xiii—Ge—Caii | 57.02 (13) |
O3vii—Ca—Gei | 34.14 (8) | O2—Ge—Caxiv | 116.09 (15) |
Geii—Ca—Gei | 146.37 (6) | O1—Ge—Caxiv | 126.00 (14) |
O2i—Ca—Cuviii | 39.63 (11) | O3—Ge—Caxiv | 50.06 (13) |
O2ii—Ca—Cuviii | 120.25 (12) | O3xiii—Ge—Caxiv | 49.99 (14) |
O1iii—Ca—Cuviii | 83.45 (11) | Caii—Ge—Caxiv | 85.16 (3) |
O1—Ca—Cuviii | 36.52 (9) | O2—Ge—Ca | 79.29 (15) |
O3iv—Ca—Cuviii | 80.32 (8) | O1—Ge—Ca | 38.71 (14) |
O3v—Ca—Cuviii | 147.52 (8) | O3—Ge—Ca | 140.02 (12) |
O3vi—Ca—Cuviii | 138.65 (9) | O3xiii—Ge—Ca | 116.31 (14) |
O3vii—Ca—Cuviii | 97.46 (8) | Caii—Ge—Ca | 99.036 (19) |
Geii—Ca—Cuviii | 137.35 (2) | Caxiv—Ge—Ca | 159.73 (4) |
Gei—Ca—Cuviii | 66.267 (17) | Ge—O1—Cuviii | 120.5 (2) |
O2i—Ca—Cuix | 120.25 (12) | Ge—O1—Cuxv | 119.9 (2) |
O2ii—Ca—Cuix | 39.63 (11) | Cuviii—O1—Cuxv | 98.55 (15) |
O1iii—Ca—Cuix | 36.52 (9) | Ge—O1—Ca | 114.6 (2) |
O1—Ca—Cuix | 83.45 (11) | Cuviii—O1—Ca | 97.11 (14) |
O3iv—Ca—Cuix | 147.52 (7) | Cuxv—O1—Ca | 102.29 (15) |
O3v—Ca—Cuix | 80.32 (8) | Ge—O2—Cuxiv | 137.8 (3) |
O3vi—Ca—Cuix | 97.46 (8) | Ge—O2—Caii | 104.2 (2) |
O3vii—Ca—Cuix | 138.65 (9) | Cuxiv—O2—Caii | 95.13 (15) |
Geii—Ca—Cuix | 66.268 (17) | Ge—O3—Gexvi | 129.5 (2) |
Gei—Ca—Cuix | 137.35 (2) | Ge—O3—Caiv | 120.88 (19) |
Cuviii—Ca—Cuix | 109.70 (6) | Gexvi—O3—Caiv | 99.06 (18) |
O1x—Cu—O1viii | 178.9 (2) | Ge—O3—Caxiv | 99.95 (18) |
O1x—Cu—O2vii | 89.94 (17) | Gexvi—O3—Caxiv | 88.84 (16) |
O1viii—Cu—O2vii | 90.76 (17) | Caiv—O3—Caxiv | 114.29 (13) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2; (iv) −x+1/2, −y+1/2, −z; (v) x−1/2, −y+1/2, z+1/2; (vi) −x+1/2, y+1/2, −z+1/2; (vii) x−1/2, y+1/2, z; (viii) −x, −y+1, −z; (ix) −x, −y+1, −z+1; (x) x, −y+1, z+1/2; (xi) x, y+1, z; (xii) −x, y+1, −z+1/2; (xiii) x, −y, z+1/2; (xiv) x+1/2, y−1/2, z; (xv) x, y−1, z; (xvi) x, −y, z−1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.716 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1974 reflections |
a = 10.2430 (12) Å | θ = 3.0–27.8° |
b = 9.1821 (8) Å | µ = 17.65 mm−1 |
c = 5.4015 (8) Å | T = 763 K |
β = 107.074 (10)° | Cuboid, pale green |
V = 485.63 (10) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 523 independent reflections |
Plane graphite monochromator | 398 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.043 |
rotation method scans | θmax = 28.2°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) ? | h = −13→13 |
Tmin = 0.104, Tmax = 0.170 | k = −12→12 |
2188 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0367P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.032 | (Δ/σ)max < 0.001 |
wR(F2) = 0.071 | Δρmax = 0.75 e Å−3 |
S = 1.07 | Δρmin = −0.80 e Å−3 |
523 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
48 parameters | Extinction coefficient: 0.0054 (6) |
Crystal data top
CaCuGe2O6 | V = 485.63 (10) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.2430 (12) Å | µ = 17.65 mm−1 |
b = 9.1821 (8) Å | T = 763 K |
c = 5.4015 (8) Å | 0.14 × 0.13 × 0.10 mm |
β = 107.074 (10)° | |
Data collection top
STOE IPDS 1 diffractometer | 523 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 398 reflections with I > 2σ(I) |
Tmin = 0.104, Tmax = 0.170 | Rint = 0.043 |
2188 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.032 | 48 parameters |
wR(F2) = 0.071 | 0 restraints |
S = 1.07 | Δρmax = 0.75 e Å−3 |
523 reflections | Δρmin = −0.80 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0 | 0.3006 (2) | 0.25 | 0.0244 (5) | |
Cu | 0 | 0.90627 (12) | 0.25 | 0.0187 (3) | |
Ge | 0.28312 (6) | 0.09730 (6) | 0.21289 (13) | 0.0161 (2) | |
O1 | 0.1062 (4) | 0.0915 (5) | 0.1198 (9) | 0.0219 (10) | |
O2 | 0.3588 (5) | 0.2586 (5) | 0.3323 (10) | 0.0336 (13) | |
O3 | 0.3560 (4) | 0.0259 (5) | −0.0209 (9) | 0.0225 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0289 (9) | 0.0207 (9) | 0.0216 (10) | 0 | 0.0045 (8) | 0 |
Cu | 0.0175 (5) | 0.0215 (5) | 0.0149 (6) | 0 | 0.0013 (4) | 0 |
Ge | 0.0132 (3) | 0.0188 (3) | 0.0155 (4) | 0.0011 (3) | 0.0030 (2) | −0.0012 (3) |
O1 | 0.0167 (19) | 0.032 (2) | 0.015 (2) | 0.0046 (19) | 0.0023 (17) | 0.002 (2) |
O2 | 0.044 (3) | 0.025 (3) | 0.029 (3) | −0.007 (2) | 0.006 (2) | −0.006 (2) |
O3 | 0.018 (2) | 0.032 (3) | 0.017 (2) | −0.0006 (17) | 0.0044 (19) | −0.0084 (19) |
Geometric parameters (Å, º) top
Ca—O2i | 2.358 (5) | Cu—O1xii | 2.241 (5) |
Ca—O2ii | 2.358 (5) | Cu—Caviii | 3.3016 (14) |
Ca—O1 | 2.411 (5) | Cu—Caix | 3.3016 (14) |
Ca—O1iii | 2.411 (5) | Cu—Caxi | 3.620 (2) |
Ca—O3iv | 2.705 (5) | Ge—O2 | 1.708 (5) |
Ca—O3v | 2.705 (5) | Ge—O1 | 1.733 (4) |
Ca—O3vi | 2.707 (5) | Ge—O3 | 1.771 (5) |
Ca—O3vii | 2.707 (5) | Ge—O3xiii | 1.810 (4) |
Ca—Geii | 3.2322 (9) | Ge—Caii | 3.2322 (9) |
Ca—Gei | 3.2322 (9) | Ge—Caxiv | 3.4839 (16) |
Ca—Cuviii | 3.3016 (14) | O1—Cuviii | 1.974 (4) |
Ca—Cuix | 3.3016 (14) | O1—Cuxv | 2.241 (5) |
Cu—O1x | 1.974 (4) | O2—Cuxiv | 2.122 (5) |
Cu—O1viii | 1.974 (4) | O2—Caii | 2.358 (5) |
Cu—O2vii | 2.122 (5) | O3—Gexvi | 1.810 (4) |
Cu—O2vi | 2.122 (5) | O3—Cav | 2.705 (5) |
Cu—O1xi | 2.241 (5) | O3—Caxiv | 2.707 (5) |
| | | |
O2i—Ca—O2ii | 153.4 (2) | O1x—Cu—O2vi | 90.67 (19) |
O2i—Ca—O1 | 74.92 (16) | O1viii—Cu—O2vi | 90.10 (19) |
O2ii—Ca—O1 | 83.87 (17) | O2vii—Cu—O2vi | 100.6 (3) |
O2i—Ca—O1iii | 83.87 (17) | O1x—Cu—O1xi | 97.79 (15) |
O2ii—Ca—O1iii | 74.92 (16) | O1viii—Cu—O1xi | 81.30 (18) |
O1—Ca—O1iii | 74.5 (2) | O2vii—Cu—O1xi | 166.95 (17) |
O2i—Ca—O3iv | 108.06 (15) | O2vi—Cu—O1xi | 89.75 (19) |
O2ii—Ca—O3iv | 87.79 (16) | O1x—Cu—O1xii | 81.30 (18) |
O1—Ca—O3iv | 162.91 (16) | O1viii—Cu—O1xii | 97.79 (15) |
O1iii—Ca—O3iv | 88.98 (15) | O2vii—Cu—O1xii | 89.75 (19) |
O2i—Ca—O3v | 87.79 (16) | O2vi—Cu—O1xii | 166.95 (17) |
O2ii—Ca—O3v | 108.06 (16) | O1xi—Cu—O1xii | 81.2 (2) |
O1—Ca—O3v | 88.98 (15) | O1x—Cu—Caviii | 134.52 (14) |
O1iii—Ca—O3v | 162.91 (16) | O1viii—Cu—Caviii | 46.43 (13) |
O3iv—Ca—O3v | 107.8 (2) | O2vii—Cu—Caviii | 88.14 (15) |
O2i—Ca—O3vi | 140.98 (16) | O2vi—Cu—Caviii | 45.37 (14) |
O2ii—Ca—O3vi | 64.87 (15) | O1xi—Cu—Caviii | 93.62 (12) |
O1—Ca—O3vi | 123.05 (13) | O1xii—Cu—Caviii | 144.10 (11) |
O1iii—Ca—O3vi | 132.19 (15) | O1x—Cu—Caix | 46.43 (13) |
O3iv—Ca—O3vi | 65.55 (15) | O1viii—Cu—Caix | 134.52 (14) |
O3v—Ca—O3vi | 60.89 (7) | O2vii—Cu—Caix | 45.37 (14) |
O2i—Ca—O3vii | 64.87 (15) | O2vi—Cu—Caix | 88.14 (15) |
O2ii—Ca—O3vii | 140.98 (16) | O1xi—Cu—Caix | 144.10 (11) |
O1—Ca—O3vii | 132.19 (15) | O1xii—Cu—Caix | 93.62 (12) |
O1iii—Ca—O3vii | 123.05 (13) | Caviii—Cu—Caix | 109.77 (7) |
O3iv—Ca—O3vii | 60.89 (7) | O1x—Cu—Caxi | 89.40 (14) |
O3v—Ca—O3vii | 65.55 (15) | O1viii—Cu—Caxi | 89.40 (14) |
O3vi—Ca—O3vii | 80.32 (18) | O2vii—Cu—Caxi | 129.71 (14) |
O2i—Ca—Geii | 172.94 (14) | O2vi—Cu—Caxi | 129.71 (14) |
O2ii—Ca—Geii | 30.83 (11) | O1xi—Cu—Caxi | 40.62 (12) |
O1—Ca—Geii | 104.05 (10) | O1xii—Cu—Caxi | 40.62 (12) |
O1iii—Ca—Geii | 102.67 (10) | Caviii—Cu—Caxi | 125.11 (3) |
O3iv—Ca—Geii | 75.03 (9) | Caix—Cu—Caxi | 125.11 (3) |
O3v—Ca—Geii | 85.20 (9) | O2—Ge—O1 | 117.2 (2) |
O3vi—Ca—Geii | 34.04 (9) | O2—Ge—O3 | 110.5 (2) |
O3vii—Ca—Geii | 112.65 (11) | O1—Ge—O3 | 113.9 (2) |
O2i—Ca—Gei | 30.83 (11) | O2—Ge—O3xiii | 101.9 (2) |
O2ii—Ca—Gei | 172.94 (14) | O1—Ge—O3xiii | 111.3 (2) |
O1—Ca—Gei | 102.67 (10) | O3—Ge—O3xiii | 99.97 (13) |
O1iii—Ca—Gei | 104.05 (10) | O2—Ge—Caii | 45.02 (18) |
O3iv—Ca—Gei | 85.20 (9) | O1—Ge—Caii | 130.84 (16) |
O3v—Ca—Gei | 75.03 (9) | O3—Ge—Caii | 115.14 (13) |
O3vi—Ca—Gei | 112.65 (11) | O3xiii—Ge—Caii | 56.87 (15) |
O3vii—Ca—Gei | 34.04 (9) | O2—Ge—Caxiv | 116.44 (17) |
Geii—Ca—Gei | 146.26 (7) | O1—Ge—Caxiv | 125.97 (16) |
O2i—Ca—Cuviii | 39.83 (13) | O3—Ge—Caxiv | 49.92 (15) |
O2ii—Ca—Cuviii | 120.19 (14) | O3xiii—Ge—Caxiv | 50.05 (16) |
O1—Ca—Cuviii | 36.39 (10) | Caii—Ge—Caxiv | 85.22 (4) |
O1iii—Ca—Cuviii | 83.63 (13) | O2—Ge—Ca | 78.94 (18) |
O3iv—Ca—Cuviii | 147.57 (9) | O1—Ge—Ca | 38.79 (16) |
O3v—Ca—Cuviii | 80.43 (10) | O3—Ge—Ca | 140.13 (14) |
O3vi—Ca—Cuviii | 138.67 (10) | O3xiii—Ge—Ca | 116.30 (15) |
O3vii—Ca—Cuviii | 97.37 (10) | Caii—Ge—Ca | 99.00 (2) |
Geii—Ca—Cuviii | 137.40 (3) | Caxiv—Ge—Ca | 159.69 (5) |
Gei—Ca—Cuviii | 66.280 (19) | Ge—O1—Cuviii | 120.8 (3) |
O2i—Ca—Cuix | 120.19 (14) | Ge—O1—Cuxv | 119.7 (2) |
O2ii—Ca—Cuix | 39.83 (13) | Cuviii—O1—Cuxv | 98.70 (18) |
O1—Ca—Cuix | 83.63 (13) | Ge—O1—Ca | 114.4 (2) |
O1iii—Ca—Cuix | 36.39 (10) | Cuviii—O1—Ca | 97.18 (16) |
O3iv—Ca—Cuix | 80.43 (10) | Cuxv—O1—Ca | 102.14 (18) |
O3v—Ca—Cuix | 147.57 (9) | Ge—O2—Cuxiv | 137.4 (3) |
O3vi—Ca—Cuix | 97.37 (10) | Ge—O2—Caii | 104.2 (2) |
O3vii—Ca—Cuix | 138.67 (10) | Cuxiv—O2—Caii | 94.80 (18) |
Geii—Ca—Cuix | 66.280 (19) | Ge—O3—Gexvi | 129.5 (2) |
Gei—Ca—Cuix | 137.40 (3) | Ge—O3—Cav | 120.6 (2) |
Cuviii—Ca—Cuix | 109.77 (7) | Gexvi—O3—Cav | 99.1 (2) |
O1x—Cu—O1viii | 178.8 (3) | Ge—O3—Caxiv | 100.0 (2) |
O1x—Cu—O2vii | 90.10 (19) | Gexvi—O3—Caxiv | 89.09 (18) |
O1viii—Cu—O2vii | 90.67 (19) | Cav—O3—Caxiv | 114.45 (15) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) −x+1/2, −y+1/2, −z; (vi) −x+1/2, y+1/2, −z+1/2; (vii) x−1/2, y+1/2, z; (viii) −x, −y+1, −z; (ix) −x, −y+1, −z+1; (x) x, −y+1, z+1/2; (xi) x, y+1, z; (xii) −x, y+1, −z+1/2; (xiii) x, −y, z+1/2; (xiv) x+1/2, y−1/2, z; (xv) x, y−1, z; (xvi) x, −y, z−1/2. |
Crystal data top
CaCuGe2O6 | F(000) = 644 |
Mr = 344.8 | Dx = 4.711 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1823 reflections |
a = 10.2448 (12) Å | θ = 2.2–28.0° |
b = 9.1898 (9) Å | µ = 17.63 mm−1 |
c = 5.4023 (7) Å | T = 796 K |
β = 107.090 (14)° | Cuboid, pale green |
V = 486.16 (10) Å3 | 0.14 × 0.13 × 0.10 mm |
Z = 4 | |
Data collection top
STOE IPDS 1 diffractometer | 493 independent reflections |
Plane graphite monochromator | 407 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.034 |
rotation method scans | θmax = 28.0°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) ? | h = −13→13 |
Tmin = 0.102, Tmax = 0.172 | k = −12→12 |
1633 measured reflections | l = −6→6 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.028P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.031 | (Δ/σ)max < 0.001 |
wR(F2) = 0.059 | Δρmax = 0.63 e Å−3 |
S = 1.07 | Δρmin = −0.58 e Å−3 |
493 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
48 parameters | Extinction coefficient: 0.0063 (5) |
Crystal data top
CaCuGe2O6 | V = 486.16 (10) Å3 |
Mr = 344.8 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.2448 (12) Å | µ = 17.63 mm−1 |
b = 9.1898 (9) Å | T = 796 K |
c = 5.4023 (7) Å | 0.14 × 0.13 × 0.10 mm |
β = 107.090 (14)° | |
Data collection top
STOE IPDS 1 diffractometer | 493 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 407 reflections with I > 2σ(I) |
Tmin = 0.102, Tmax = 0.172 | Rint = 0.034 |
1633 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.031 | 48 parameters |
wR(F2) = 0.059 | 0 restraints |
S = 1.07 | Δρmax = 0.63 e Å−3 |
493 reflections | Δρmin = −0.58 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0 | 0.3008 (2) | 0.25 | 0.0243 (4) | |
Cu | 0 | 0.90668 (13) | 0.25 | 0.0180 (3) | |
Ge | 0.28310 (6) | 0.09739 (6) | 0.21290 (12) | 0.0154 (2) | |
O1 | 0.1062 (4) | 0.0921 (6) | 0.1196 (3) | 0.0223 (9) | |
O2 | 0.3591 (4) | 0.2581 (4) | 0.3332 (10) | 0.0342 (12) | |
O3 | 0.3563 (4) | 0.0253 (5) | −0.0207 (9) | 0.0232 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0292 (9) | 0.0212 (9) | 0.0201 (10) | 0 | 0.0037 (8) | 0 |
Cu | 0.0171 (4) | 0.0220 (5) | 0.0128 (5) | 0 | 0.0012 (4) | 0 |
Ge | 0.0126 (3) | 0.0196 (3) | 0.0136 (3) | 0.0003 (3) | 0.0030 (2) | −0.0019 (3) |
O1 | 0.0115 (17) | 0.037 (2) | 0.016 (2) | 0.0088 (19) | 0.0007 (16) | −0.001 (2) |
O2 | 0.041 (3) | 0.025 (2) | 0.034 (3) | −0.004 (2) | 0.006 (2) | −0.005 (2) |
O3 | 0.019 (2) | 0.034 (3) | 0.016 (2) | −0.0032 (18) | 0.0044 (18) | −0.0079 (19) |
Geometric parameters (Å, º) top
Ca—O2i | 2.353 (5) | Cu—O1xii | 2.244 (5) |
Ca—O2ii | 2.353 (5) | Cu—Caviii | 3.3066 (15) |
Ca—O1iii | 2.410 (5) | Cu—Caix | 3.3066 (15) |
Ca—O1 | 2.410 (5) | Cu—Caxii | 3.6223 (19) |
Ca—O3iv | 2.701 (5) | Ge—O2 | 1.707 (4) |
Ca—O3v | 2.701 (5) | Ge—O1 | 1.733 (4) |
Ca—O3vi | 2.706 (5) | Ge—O3 | 1.775 (5) |
Ca—O3vii | 2.706 (5) | Ge—O3xiii | 1.809 (4) |
Ca—Geii | 3.2314 (9) | Ge—Caii | 3.2314 (9) |
Ca—Gei | 3.2314 (9) | Ge—Caxiv | 3.4846 (16) |
Ca—Cuviii | 3.3066 (15) | O1—Cuviii | 1.9731 (11) |
Ca—Cuix | 3.3066 (15) | O1—Cuxv | 2.244 (5) |
Cu—O1viii | 1.9731 (11) | O2—Cuxiv | 2.1288 (10) |
Cu—O1x | 1.9731 (11) | O2—Caii | 2.353 (5) |
Cu—O2v | 2.1288 (11) | O3—Gexvi | 1.809 (4) |
Cu—O2iv | 2.1288 (11) | O3—Caxiv | 2.701 (5) |
Cu—O1xi | 2.244 (5) | O3—Cavi | 2.706 (5) |
| | | |
O2i—Ca—O2ii | 153.4 (2) | O1viii—Cu—O2iv | 89.8 (2) |
O2i—Ca—O1iii | 83.90 (14) | O1x—Cu—O2iv | 90.6 (2) |
O2ii—Ca—O1iii | 74.91 (7) | O2v—Cu—O2iv | 100.2 (3) |
O2i—Ca—O1 | 74.91 (7) | O1viii—Cu—O1xi | 98.03 (13) |
O2ii—Ca—O1 | 83.90 (14) | O1x—Cu—O1xi | 81.49 (17) |
O1iii—Ca—O1 | 74.5 (2) | O2v—Cu—O1xi | 89.96 (18) |
O2i—Ca—O3iv | 141.03 (17) | O2iv—Cu—O1xi | 167.12 (16) |
O2ii—Ca—O3iv | 64.81 (12) | O1viii—Cu—O1xii | 81.49 (17) |
O1iii—Ca—O3iv | 132.11 (11) | O1x—Cu—O1xii | 98.03 (13) |
O1—Ca—O3iv | 123.04 (13) | O2v—Cu—O1xii | 167.12 (16) |
O2i—Ca—O3v | 64.81 (12) | O2iv—Cu—O1xii | 89.96 (18) |
O2ii—Ca—O3v | 141.03 (17) | O1xi—Cu—O1xii | 81.2 (2) |
O1iii—Ca—O3v | 123.04 (13) | O1viii—Cu—Caviii | 46.28 (13) |
O1—Ca—O3v | 132.11 (11) | O1x—Cu—Caviii | 134.22 (15) |
O3iv—Ca—O3v | 80.40 (18) | O2v—Cu—Caviii | 88.02 (15) |
O2i—Ca—O3vi | 87.78 (15) | O2iv—Cu—Caviii | 45.15 (14) |
O2ii—Ca—O3vi | 108.10 (10) | O1xi—Cu—Caviii | 144.19 (4) |
O1iii—Ca—O3vi | 163.02 (15) | O1xii—Cu—Caviii | 93.74 (9) |
O1—Ca—O3vi | 89.03 (15) | O1viii—Cu—Caix | 134.22 (15) |
O3iv—Ca—O3vi | 60.91 (7) | O1x—Cu—Caix | 46.28 (13) |
O3v—Ca—O3vi | 65.45 (16) | O2v—Cu—Caix | 45.15 (14) |
O2i—Ca—O3vii | 108.10 (10) | O2iv—Cu—Caix | 88.02 (15) |
O2ii—Ca—O3vii | 87.78 (15) | O1xi—Cu—Caix | 93.74 (9) |
O1iii—Ca—O3vii | 89.03 (15) | O1xii—Cu—Caix | 144.19 (4) |
O1—Ca—O3vii | 163.02 (15) | Caviii—Cu—Caix | 109.55 (7) |
O3iv—Ca—O3vii | 65.45 (16) | O1viii—Cu—Caxii | 89.68 (15) |
O3v—Ca—O3vii | 60.91 (7) | O1x—Cu—Caxii | 89.68 (15) |
O3vi—Ca—O3vii | 107.7 (2) | O2v—Cu—Caxii | 129.89 (14) |
O2i—Ca—Geii | 172.97 (13) | O2iv—Cu—Caxii | 129.89 (14) |
O2ii—Ca—Geii | 30.78 (9) | O1xi—Cu—Caxii | 40.58 (11) |
O1iii—Ca—Geii | 102.60 (4) | O1xii—Cu—Caxii | 40.58 (11) |
O1—Ca—Geii | 104.03 (5) | Caviii—Cu—Caxii | 125.22 (4) |
O3iv—Ca—Geii | 34.04 (9) | Caix—Cu—Caxii | 125.22 (4) |
O3v—Ca—Geii | 112.74 (11) | O2—Ge—O1 | 117.1 (2) |
O3vi—Ca—Geii | 85.25 (10) | O2—Ge—O3 | 110.7 (2) |
O3vii—Ca—Geii | 75.00 (9) | O1—Ge—O3 | 114.03 (16) |
O2i—Ca—Gei | 30.78 (9) | O2—Ge—O3xiii | 101.6 (2) |
O2ii—Ca—Gei | 172.97 (13) | O1—Ge—O3xiii | 111.6 (2) |
O1iii—Ca—Gei | 104.03 (5) | O3—Ge—O3xiii | 99.79 (14) |
O1—Ca—Gei | 102.60 (4) | O2—Ge—Caii | 44.87 (17) |
O3iv—Ca—Gei | 112.74 (11) | O1—Ge—Caii | 130.81 (10) |
O3v—Ca—Gei | 34.04 (9) | O3—Ge—Caii | 115.06 (13) |
O3vi—Ca—Gei | 75.00 (9) | O3xiii—Ge—Caii | 56.70 (15) |
O3vii—Ca—Gei | 85.25 (10) | O2—Ge—Caxiv | 116.31 (16) |
Geii—Ca—Gei | 146.35 (7) | O1—Ge—Caxiv | 126.13 (17) |
O2i—Ca—Cuviii | 39.90 (4) | O3—Ge—Caxiv | 49.72 (15) |
O2ii—Ca—Cuviii | 120.10 (14) | O3xiii—Ge—Caxiv | 50.08 (16) |
O1iii—Ca—Cuviii | 83.58 (10) | Caii—Ge—Caxiv | 85.19 (4) |
O1—Ca—Cuviii | 36.28 (3) | O2—Ge—Ca | 78.99 (16) |
O3iv—Ca—Cuviii | 138.76 (11) | O1—Ge—Ca | 38.70 (15) |
O3v—Ca—Cuviii | 97.42 (10) | O3—Ge—Ca | 140.29 (14) |
O3vi—Ca—Cuviii | 80.56 (10) | O3xiii—Ge—Ca | 116.34 (16) |
O3vii—Ca—Cuviii | 147.67 (9) | Caii—Ge—Ca | 99.00 (2) |
Geii—Ca—Cuviii | 137.34 (3) | Caxiv—Ge—Ca | 159.74 (5) |
Gei—Ca—Cuviii | 66.328 (18) | Ge—O1—Cuviii | 120.8 (2) |
O2i—Ca—Cuix | 120.10 (14) | Ge—O1—Cuxv | 119.5 (2) |
O2ii—Ca—Cuix | 39.90 (4) | Cuviii—O1—Cuxv | 98.51 (16) |
O1iii—Ca—Cuix | 36.28 (3) | Ge—O1—Ca | 114.6 (2) |
O1—Ca—Cuix | 83.58 (10) | Cuviii—O1—Ca | 97.44 (15) |
O3iv—Ca—Cuix | 97.42 (10) | Cuxv—O1—Ca | 102.16 (16) |
O3v—Ca—Cuix | 138.76 (11) | Ge—O2—Cuxiv | 137.4 (3) |
O3vi—Ca—Cuix | 147.67 (9) | Ge—O2—Caii | 104.4 (2) |
O3vii—Ca—Cuix | 80.56 (10) | Cuxiv—O2—Caii | 94.95 (16) |
Geii—Ca—Cuix | 66.328 (18) | Ge—O3—Gexvi | 129.4 (3) |
Gei—Ca—Cuix | 137.34 (3) | Ge—O3—Caxiv | 100.2 (2) |
Cuviii—Ca—Cuix | 109.55 (7) | Gexvi—O3—Caxiv | 89.27 (18) |
O1viii—Cu—O1x | 179.4 (3) | Ge—O3—Cavi | 120.4 (2) |
O1viii—Cu—O2v | 90.6 (2) | Gexvi—O3—Cavi | 99.1 (2) |
O1x—Cu—O2v | 89.8 (2) | Caxiv—O3—Cavi | 114.55 (16) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x−1/2, y+1/2, z; (vi) −x+1/2, −y+1/2, −z; (vii) x−1/2, −y+1/2, z+1/2; (viii) −x, −y+1, −z; (ix) −x, −y+1, −z+1; (x) x, −y+1, z+1/2; (xi) −x, y+1, −z+1/2; (xii) x, y+1, z; (xiii) x, −y, z+1/2; (xiv) x+1/2, y−1/2, z; (xv) x, y−1, z; (xvi) x, −y, z−1/2. |
Experimental details
| (cacu_100K) | (cacu_150K) | (cacu_200K) | (cacu_250) |
Crystal data |
Chemical formula | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 |
Mr | 344.8 | 344.8 | 344.8 | 344.8 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 100 | 150 | 200 | 250 |
a, b, c (Å) | 10.1798 (12), 9.1869 (7), 5.1978 (6) | 10.1822 (12), 9.1912 (7), 5.1995 (6) | 10.1853 (12), 9.1959 (7), 5.2013 (6) | 10.1893 (12), 9.1996 (7), 5.2043 (6) |
β (°) | 105.614 (12) | 105.636 (12) | 105.649 (12) | 105.669 (12) |
V (Å3) | 468.16 (9) | 468.60 (9) | 469.11 (9) | 469.71 (9) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.22 | 18.29 | 18.22 | 18.25 |
Crystal size (mm) | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 |
|
Data collection |
Diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Empirical (using intensity measurements) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.097, 0.150 | 0.097, 0.150 | 0.084, 0.162 | 0.097, 0.150 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5815, 1616, 1415 | 5820, 1626, 1416 | 5828, 1626, 1415 | 5849, 1631, 1404 |
Rint | 0.039 | 0.040 | 0.037 | 0.040 |
(sin θ/λ)max (Å−1) | 0.750 | 0.750 | 0.749 | 0.750 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.056, 1.06 | 0.027, 0.061, 1.08 | 0.025, 0.052, 1.07 | 0.025, 0.055, 1.03 |
No. of reflections | 1616 | 1626 | 1626 | 1631 |
No. of parameters | 92 | 92 | 92 | 92 |
No. of restraints | 0 | 0 | 0 | 0 |
Δρmax, Δρmin (e Å−3) | 0.80, −0.91 | 0.88, −0.90 | 0.75, −0.81 | 0.74, −0.70 |
| (cacu_298K) | (cacu_328K) | (cacu_361K) | (cacu_470K) |
Crystal data |
Chemical formula | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 |
Mr | 344.8 | 344.8 | 344.8 | 344.8 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 298 | 328 | 361 | 470 |
a, b, c (Å) | 10.1930 (12), 9.2039 (7), 5.2078 (6) | 10.1944 (12), 9.2078 (7), 5.2103 (6) | 10.1957 (12), 9.2123 (7), 5.2142 (6) | 10.2047 (12), 9.2255 (7), 5.2249 (6) |
β (°) | 105.688 (12) | 105.699 (12) | 105.702 (12) | 105.785 (12) |
V (Å3) | 470.37 (9) | 470.84 (9) | 471.47 (9) | 473.34 (9) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.22 | 18.20 | 18.18 | 18.11 |
Crystal size (mm) | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 |
|
Data collection |
Diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer |
Absorption correction | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.093, 0.158 | 0.091, 0.161 | 0.089, 0.152 | 0.094, 0.158 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5565, 1622, 1438 | 3509, 1018, 827 | 3763, 1040, 820 | 3745, 1041, 814 |
Rint | 0.038 | 0.038 | 0.049 | 0.047 |
(sin θ/λ)max (Å−1) | 0.750 | 0.656 | 0.659 | 0.658 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.063, 1.1 | 0.035, 0.064, 1.16 | 0.038, 0.073, 1.11 | 0.040, 0.078, 1.14 |
No. of reflections | 1622 | 1018 | 1040 | 1041 |
No. of parameters | 92 | 92 | 92 | 92 |
No. of restraints | 0 | 5 | 3 | 4 |
Δρmax, Δρmin (e Å−3) | 0.85, −0.85 | 0.88, −0.90 | 0.93, −1.09 | 0.97, −0.89 |
| (cacu_570K) | (cacu_612K) | (cacu_629K) | (cacu_646K) |
Crystal data |
Chemical formula | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 |
Mr | 344.8 | 344.8 | 344.8 | 344.8 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 570 | 612 | 629 | 646 |
a, b, c (Å) | 10.2130 (12), 9.2385 (7), 5.2359 (6) | 10.2150 (12), 9.2455 (7), 5.2407 (6) | 10.2165 (12), 9.2483 (7), 5.2429 (6) | 10.2170 (12), 9.2515 (7), 5.2446 (6) |
β (°) | 105.870 (12) | 105.928 (12) | 105.942 (12) | 105.964 (12) |
V (Å3) | 475.19 (9) | 475.94 (9) | 476.32 (9) | 476.61 (9) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.04 | 18.01 | 18.22 | 17.98 |
Crystal size (mm) | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 |
|
Data collection |
Diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer |
Absorption correction | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.094, 0.158 | 0.094, 0.158 | 0.094, 0.158 | 0.094, 0.158 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3696, 1032, 795 | 4729, 1037, 777 | 5005, 1053, 778 | 4880, 1020, 764 |
Rint | 0.048 | 0.057 | 0.060 | 0.060 |
(sin θ/λ)max (Å−1) | 0.659 | 0.657 | 0.659 | 0.657 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.085, 1.11 | 0.047, 0.084, 1.11 | 0.047, 0.085, 1.16 | 0.045, 0.086, 1.10 |
No. of reflections | 1032 | 1037 | 1053 | 1020 |
No. of parameters | 92 | 92 | 92 | 92 |
No. of restraints | 5 | 2 | 0 | 0 |
Δρmax, Δρmin (e Å−3) | 1.15, −0.85 | 0.96, −0.85 | 0.97, −0.96 | 1.05, −1.04 |
| (cacu_654K) | (cacu_717K) | (cacu_729K) | (cacu_763K) |
Crystal data |
Chemical formula | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 | CaCuGe2O6 |
Mr | 344.8 | 344.8 | 344.8 | 344.8 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, C2/c | Monoclinic, C2/c | Monoclinic, C2/c |
Temperature (K) | 654 | 717 | 729 | 763 |
a, b, c (Å) | 10.2180 (12), 9.2536 (7), 5.2468 (6) | 10.2453 (12), 9.2118 (9), 5.4115 (7) | 10.2405 (12), 9.1780 (8), 5.4003 (7) | 10.2430 (12), 9.1821 (8), 5.4015 (8) |
β (°) | 105.975 (12) | 106.931 (14) | 107.072 (11) | 107.074 (10) |
V (Å3) | 476.94 (9) | 488.50 (10) | 485.19 (9) | 485.63 (10) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 17.97 | 17.54 | 17.66 | 17.65 |
Crystal size (mm) | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 | 0.14 × 0.13 × 0.10 |
|
Data collection |
Diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer | STOE IPDS 1 diffractometer |
Absorption correction | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) | Empirical (using intensity measurements) | Empirical (using intensity measurements) |
Tmin, Tmax | 0.094, 0.158 | 0.102, 0.172 | 0.102, 0.172 | 0.104, 0.170 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3717, 3717, 2406 | 1629, 510, 392 | 1641, 500, 374 | 2188, 523, 398 |
Rint | 0 | 0.048 | 0.057 | 0.043 |
(sin θ/λ)max (Å−1) | 0.659 | 0.656 | 0.662 | 0.664 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.095, 0.94 | 0.034, 0.085, 1.05 | 0.026, 0.052, 0.94 | 0.032, 0.071, 1.07 |
No. of reflections | 3717 | 510 | 500 | 523 |
No. of parameters | 92 | 48 | 48 | 48 |
No. of restraints | 0 | 0 | 0 | 0 |
Δρmax, Δρmin (e Å−3) | 1.03, −0.97 | 0.80, −0.75 | 0.73, −0.61 | 0.75, −0.80 |
| (cacu_796K) |
Crystal data |
Chemical formula | CaCuGe2O6 |
Mr | 344.8 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 796 |
a, b, c (Å) | 10.2448 (12), 9.1898 (9), 5.4023 (7) |
β (°) | 107.090 (14) |
V (Å3) | 486.16 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 17.63 |
Crystal size (mm) | 0.14 × 0.13 × 0.10 |
|
Data collection |
Diffractometer | STOE IPDS 1 diffractometer |
Absorption correction | Empirical (using intensity measurements) |
Tmin, Tmax | 0.102, 0.172 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1633, 493, 407 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.661 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.059, 1.07 |
No. of reflections | 493 |
No. of parameters | 48 |
No. of restraints | 0 |
Δρmax, Δρmin (e Å−3) | 0.63, −0.58 |
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