Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614011676/dk5023sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn24ortsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn24tetsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn31sup4.hkl |
B-IncStrDB reference: 9692EcLKMW
Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) for cbn24ort, cbn24tet; CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) for cbn31. Cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) for cbn24ort, cbn24tet; CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) for cbn31. Data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) for cbn24ort, cbn24tet; CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) for cbn31. Program(s) used to solve structure: Jana2006 for cbn24ort. Program(s) used to refine structure: Jana2006 for cbn24ort. Molecular graphics: Diamond 3.0 for cbn24ort. Software used to prepare material for publication: Jana2006 for cbn24ort.
Ba0.761Ca0.239Nb2O6 | F(000) = 3553 |
Mr = 395.9 | Dx = 5.328 Mg m−3 |
Orthorhombic, X2mm(00γ)000† | Mo Kα radiation, λ = 0.71069 Å |
q = 0.663800c* | Cell parameters from 10368 reflections |
a = 7.9429 (3) Å | θ = 2.9–23.3° |
b = 17.6240 (5) Å | µ = 10.75 mm−1 |
c = 17.6229 (6) Å | T = 293 K |
V = 2466.95 (14) Å3 | Plate-like, colourless |
Z = 20 | 0.40 × 0.34 × 0.04 mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) x1, −x2, x3, x4; (3) x1, x2, −x3, −x4; (4) x1, −x2, −x3, −x4; (5) x1, x2+1/2, x3+1/2, x4; (6) x1, −x2+1/2, x3+1/2, x4; (7) x1, x2+1/2, −x3+1/2, −x4; (8) x1, −x2+1/2, −x3+1/2, −x4; (9) x1+1/2, x2, x3, x4+1/2; (10) x1+1/2, −x2, x3, x4+1/2; (11) x1+1/2, x2, −x3, −x4+1/2; (12) x1+1/2, −x2, −x3, −x4+1/2; (13) x1+1/2, x2+1/2, x3+1/2, x4+1/2; (14) x1+1/2, −x2+1/2, x3+1/2, x4+1/2; (15) x1+1/2, x2+1/2, −x3+1/2, −x4+1/2; (16) x1+1/2, −x2+1/2, −x3+1/2, −x4+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 3449 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 2633 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 8.2495 pixels mm-1 | θmax = 31.7°, θmin = 3.0° |
ω and π scans | h = −11→11 |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | k = −25→24 |
Tmin = 0.081, Tmax = 0.672 | l = −25→23 |
20132 measured reflections |
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max = 0.045 |
wR(F2) = 0.036 | Δρmax = 1.16 e Å−3 |
S = 1.42 | Δρmin = −0.86 e Å−3 |
3449 reflections | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
212 parameters | Extinction coefficient: 271 (9) |
0 restraints | Absolute structure: 1605 of Friedel pairs used in the refinement |
45 constraints | Absolute structure parameter: 0.47 (3) |
Ba0.761Ca0.239Nb2O6 | V = 2466.95 (14) Å3 |
Mr = 395.9 | Z = 20 |
Orthorhombic, X2mm(00γ)000† | Mo Kα radiation |
q = 0.663800c* | µ = 10.75 mm−1 |
a = 7.9429 (3) Å | T = 293 K |
b = 17.6240 (5) Å | 0.40 × 0.34 × 0.04 mm |
c = 17.6229 (6) Å |
† Symmetry operations: (1) x1, x2, x3, x4; (2) x1, −x2, x3, x4; (3) x1, x2, −x3, −x4; (4) x1, −x2, −x3, −x4; (5) x1, x2+1/2, x3+1/2, x4; (6) x1, −x2+1/2, x3+1/2, x4; (7) x1, x2+1/2, −x3+1/2, −x4; (8) x1, −x2+1/2, −x3+1/2, −x4; (9) x1+1/2, x2, x3, x4+1/2; (10) x1+1/2, −x2, x3, x4+1/2; (11) x1+1/2, x2, −x3, −x4+1/2; (12) x1+1/2, −x2, −x3, −x4+1/2; (13) x1+1/2, x2+1/2, x3+1/2, x4+1/2; (14) x1+1/2, −x2+1/2, x3+1/2, x4+1/2; (15) x1+1/2, x2+1/2, −x3+1/2, −x4+1/2; (16) x1+1/2, −x2+1/2, −x3+1/2, −x4+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 3449 independent reflections |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | 2633 reflections with I > 3σ(I) |
Tmin = 0.081, Tmax = 0.672 | Rint = 0.030 |
20132 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.036 | Δρmax = 1.16 e Å−3 |
S = 1.42 | Δρmin = −0.86 e Å−3 |
3449 reflections | Absolute structure: 1605 of Friedel pairs used in the refinement |
212 parameters | Absolute structure parameter: 0.47 (3) |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ba2a | 0.23955 | 0 | 0.32733 (2) | 0.01729 (14) | 0.9596 (19) |
Ba2b | 0.24174 (12) | 0.171915 (19) | 0 | 0.01627 (14) | 0.9294 (19) |
Nb2a | −0.00389 (13) | 0.181810 (18) | 0.39127 (2) | 0.00714 (12) | |
Nb2b | −0.00462 (13) | 0.10878 (2) | 0.181611 (19) | 0.00707 (12) | |
Nb1a | 0.0004 (2) | 0 | 0 | 0.0062 (2) | |
Nb1b | −0.0010 (2) | 0.5 | 0 | 0.0059 (2) | |
Ca1 | 0.2495 (6) | 0.25 | 0.25 | 0.0117 (6) | 0.532 (5) |
O1a | −0.0195 (10) | 0.2155 (2) | 0.5 | 0.0104 (13) | |
O5a | 0.2253 (7) | 0.18531 (19) | 0.3895 (2) | 0.0288 (12) | |
O5b | −0.2740 (6) | 0.11246 (18) | 0.18543 (19) | 0.0228 (12) | |
O1b | −0.0252 (9) | 0 | 0.2143 (3) | 0.0089 (13) | |
O2a | −0.0346 (6) | 0.14432 (19) | 0.28490 (18) | 0.0223 (12) | |
O3b | −0.0255 (6) | 0.07503 (16) | 0.41884 (19) | 0.0167 (10) | |
O2b | −0.0278 (7) | 0.21477 (17) | 0.1461 (2) | 0.0284 (12) | |
O3a | −0.0280 (6) | 0.08193 (17) | 0.07499 (18) | 0.0152 (9) | |
O4a | 0.2201 (11) | 0.5 | 0 | 0.019 (2) | |
O4b | 0.2401 (14) | 0 | 0 | 0.024 (2) | |
Ca2a | 0.23955 | 0 | 0.32733 (2) | 0.01729 (14) | 0.0272 |
Ca2b | 0.24174 (12) | 0.171915 (19) | 0 | 0.01627 (14) | 0.0304 |
Ba1 | 0.2495 (6) | 0.25 | 0.25 | 0.0117 (6) | 0.0274 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba2a | 0.0113 (2) | 0.0299 (3) | 0.0106 (2) | 0 | −0.0026 (4) | 0 |
Ba2b | 0.0112 (2) | 0.0088 (2) | 0.0288 (3) | −0.0008 (4) | 0 | 0 |
Nb2a | 0.0074 (2) | 0.0057 (2) | 0.0082 (2) | −0.0005 (4) | −0.0014 (4) | 0.00006 (13) |
Nb2b | 0.0077 (2) | 0.0078 (2) | 0.0057 (2) | −0.0004 (4) | −0.0009 (4) | −0.00007 (13) |
Nb1a | 0.0058 (4) | 0.0060 (3) | 0.0068 (4) | 0 | 0 | 0 |
Nb1b | 0.0063 (4) | 0.0063 (3) | 0.0051 (4) | 0 | 0 | 0 |
Ca1 | 0.0130 (11) | 0.0115 (10) | 0.0107 (11) | 0 | 0 | −0.0023 (7) |
O1a | 0.019 (2) | 0.0076 (19) | 0.004 (2) | 0.007 (3) | 0 | 0 |
O5a | 0.014 (2) | 0.054 (2) | 0.019 (2) | 0.007 (2) | −0.001 (2) | 0.0022 (16) |
O5b | 0.0111 (19) | 0.0252 (18) | 0.032 (2) | −0.009 (2) | −0.006 (2) | −0.0115 (14) |
O1b | 0.007 (2) | 0.011 (2) | 0.009 (2) | 0 | 0.003 (3) | 0 |
O2a | 0.031 (2) | 0.0289 (19) | 0.0070 (18) | 0.001 (2) | 0.002 (2) | −0.0084 (15) |
O3b | 0.028 (2) | 0.0055 (13) | 0.0165 (17) | −0.007 (2) | −0.001 (2) | −0.0032 (12) |
O2b | 0.046 (2) | 0.0101 (16) | 0.029 (2) | 0.009 (2) | 0.010 (3) | 0.0067 (16) |
O3a | 0.0223 (18) | 0.0127 (14) | 0.0106 (16) | 0.0076 (19) | 0.000 (2) | −0.0052 (13) |
O4a | 0.002 (4) | 0.032 (4) | 0.024 (4) | 0 | 0 | 0 |
O4b | 0.024 (4) | 0.027 (3) | 0.021 (4) | 0 | 0 | 0 |
Ca2a | 0.0113 (2) | 0.0299 (3) | 0.0106 (2) | 0 | −0.0026 (4) | 0 |
Ca2b | 0.0112 (2) | 0.0088 (2) | 0.0288 (3) | −0.0008 (4) | 0 | 0 |
Ba1 | 0.0130 (11) | 0.0115 (10) | 0.0107 (11) | 0 | 0 | −0.0023 (7) |
Average | Minimum | Maximum | |
Ba2a—O5bi | 3.194 (5) | 2.861 (5) | 3.528 (5) |
Ba2a—O5bii | 3.194 (5) | 2.861 (5) | 3.528 (5) |
Ba2a—O1b | 2.898 (9) | 2.795 (9) | 3.000 (9) |
Ba2a—O1bi | 2.733 (9) | 2.693 (9) | 2.774 (9) |
Ba2a—O3b | 2.965 (6) | 2.830 (6) | 3.100 (6) |
Ba2a—O3bi | 2.801 (6) | 2.720 (6) | 2.885 (6) |
Ba2a—O3biii | 2.965 (6) | 2.830 (6) | 3.100 (6) |
Ba2a—O3bii | 2.801 (6) | 2.720 (6) | 2.885 (6) |
Ba2a—O4aiv | 3.045 (4) | 2.808 (8) | 3.286 (8) |
Ba2b—O1av | 2.873 (7) | 2.807 (9) | 2.938 (9) |
Ba2b—O1avi | 2.746 (7) | 2.691 (9) | 2.803 (9) |
Ba2b—O5av | 3.187 (5) | 2.843 (5) | 3.526 (5) |
Ba2b—O5avii | 3.187 (5) | 2.843 (5) | 3.526 (5) |
Ba2b—O3ai | 2.762 (6) | 2.691 (6) | 2.840 (6) |
Ba2b—O3aviii | 2.762 (6) | 2.691 (6) | 2.840 (6) |
Nb2a—O1a | 2.012 (5) | 1.981 (8) | 2.039 (8) |
Nb2a—O5a | 1.833 (8) | 1.824 (8) | 1.849 (8) |
Nb2a—O3b | 1.955 (6) | 1.947 (6) | 1.963 (6) |
Nb2a—O2bvii | 1.956 (6) | 1.946 (6) | 1.966 (6) |
Nb2b—O5bi | 1.848 (8) | 1.829 (8) | 1.866 (8) |
Nb2b—O2a | 1.948 (7) | 1.934 (7) | 1.960 (7) |
Nb2b—O2b | 1.985 (6) | 1.977 (6) | 1.998 (6) |
Nb2b—O3a | 1.951 (7) | 1.944 (7) | 1.963 (7) |
Nb1a—O3a | 1.976 (6) | 1.965 (6) | 1.988 (6) |
Nb1a—O3aiii | 1.976 (6) | 1.965 (6) | 1.988 (6) |
Nb1a—O3aix | 1.976 (6) | 1.965 (6) | 1.988 (6) |
Nb1a—O3ax | 1.976 (6) | 1.965 (6) | 1.988 (6) |
Nb1a—O4b | 1.917 (14) | 1.893 (17) | 1.930 (12) |
Nb1b—O3bxi | 1.961 (6) | 1.956 (7) | 1.970 (6) |
Nb1b—O3bv | 1.961 (6) | 1.956 (7) | 1.970 (6) |
Nb1b—O3bxii | 1.961 (6) | 1.956 (7) | 1.970 (6) |
Nb1b—O3bvii | 1.961 (6) | 1.956 (7) | 1.970 (6) |
Nb1b—O4a | 1.764 (11) | 1.755 (13) | 1.771 (9) |
O5a—Ba1 | 2.725 (5) | 2.583 (6) | 2.852 (6) |
O5b—Ba1xiii | 2.695 (5) | 2.658 (5) | 2.738 (5) |
O2a—Ba1 | 2.991 (7) | 2.776 (7) | 3.207 (8) |
O2a—Ba1xiii | 2.610 (7) | 2.487 (7) | 2.738 (7) |
O2b—Ba1 | 2.930 (8) | 2.687 (8) | 3.176 (8) |
O2b—Ba1xiii | 2.625 (8) | 2.545 (8) | 2.715 (8) |
Symmetry codes: (i) x1+1/2, x2, x3, x4+1/2; (ii) x1+1/2, −x2, x3, x4+1/2; (iii) x1, −x2, x3, x4; (iv) x1, x2−1/2, x3+1/2, x4; (v) x1, −x2+1/2, x3−1/2, x4; (vi) x1+1/2, −x2+1/2, x3−1/2, x4+1/2; (vii) x1, −x2+1/2, −x3+1/2, −x4; (viii) x1+1/2, x2, −x3, −x4+1/2; (ix) x1, x2, −x3, −x4; (x) x1, −x2, −x3, −x4; (xi) x1, x2+1/2, x3−1/2, x4; (xii) x1, x2+1/2, −x3+1/2, −x4; (xiii) x1−1/2, x2, x3, x4+1/2. |
Ba0.761Ca0.239Nb2O6 | F(000) = 1773 |
Mr = 395.9 | Dx = 5.349 Mg m−3 |
Tetragonal, X4bm† | Mo Kα radiation, λ = 0.7107 Å |
q1 = 0.309425a* + 0.309425b*; q2 = -0.309425a* + 0.309425b* | Cell parameters from 14376 reflections |
a = 12.4476 (4) Å | θ = 2.8–42.5° |
c = 7.9291 (4) Å | µ = 10.83 mm−1 |
V = 1228.56 (8) Å3 | T = 293 K |
Z = 10 | 0.38 × 0.23 × 0.07 mm |
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 2905 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 2299 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: 8.2495 pixels mm-1 | θmax = 42.6°, θmin = 2.9° |
ω and π scans | h = −19→23 |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | k = −22→23 |
Tmin = 0.11, Tmax = 0.654 | l = −14→13 |
59030 measured reflections |
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max = 0.021 |
wR(F2) = 0.039 | Δρmax = 0.00 e Å−3 |
S = 1.48 | Δρmin = −0.58 e Å−3 |
2905 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
152 parameters | Extinction coefficient: 198 (14) |
0 restraints | Absolute structure: 1407 of Friedel pairs used in the refinement |
3 constraints | Absolute structure parameter: 0.45 (3) |
Ba0.761Ca0.239Nb2O6 | V = 1228.56 (8) Å3 |
Mr = 395.9 | Z = 10 |
Tetragonal, X4bm† | Mo Kα radiation |
q1 = 0.309425a* + 0.309425b*; q2 = -0.309425a* + 0.309425b* | µ = 10.83 mm−1 |
a = 12.4476 (4) Å | T = 293 K |
c = 7.9291 (4) Å | 0.38 × 0.23 × 0.07 mm |
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 2905 independent reflections |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | 2299 reflections with I > 3σ(I) |
Tmin = 0.11, Tmax = 0.654 | Rint = 0.038 |
59030 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.039 | Δρmax = 0.00 e Å−3 |
S = 1.48 | Δρmin = −0.58 e Å−3 |
2905 reflections | Absolute structure: 1407 of Friedel pairs used in the refinement |
152 parameters | Absolute structure parameter: 0.45 (3) |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ba2 | 0.172267 (15) | 0.672267 (15) | 0.25 | 0.01616 (9) | 0.9382 (8) |
Ca1 | 0 | 0 | 0.2583 (6) | 0.0105 (6) | 0.524 (2) |
Nb1 | 0 | 0.5 | 0.00929 (17) | 0.00571 (13) | |
Nb2 | 0.07295 (2) | 0.20951 (2) | 0.00540 (11) | 0.00674 (10) | |
O1 | 0.21501 (17) | 0.28499 (17) | −0.0113 (9) | 0.0098 (8) | |
O2 | 0.1401 (2) | 0.0697 (2) | −0.0210 (6) | 0.0236 (9) | |
O3 | −0.00673 (18) | 0.34333 (18) | −0.0176 (5) | 0.0133 (7) | |
O4 | 0 | 0.5 | 0.2381 (11) | 0.0192 (12) | |
O5 | 0.07402 (19) | 0.2031 (2) | 0.2350 (5) | 0.0188 (8) | |
Ca2 | 0.172267 (15) | 0.672267 (15) | 0.25 | 0.01616 (9) | 0.0322 |
Ba1 | 0 | 0 | 0.2583 (6) | 0.0105 (6) | 0.0261 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba2 | 0.01854 (15) | 0.01854 (15) | 0.01139 (18) | −0.00959 (11) | 0.0005 (2) | 0.0005 (2) |
Ca1 | 0.0100 (8) | 0.0100 (8) | 0.0113 (12) | 0 | 0 | 0 |
Nb1 | 0.00524 (18) | 0.00524 (18) | 0.0067 (3) | −0.00036 (19) | 0 | 0 |
Nb2 | 0.00611 (17) | 0.00623 (17) | 0.0079 (2) | 0.00114 (9) | 0.0003 (3) | 0.0003 (3) |
O1 | 0.0077 (9) | 0.0077 (9) | 0.0140 (19) | 0.0024 (11) | 0.0023 (15) | −0.0023 (15) |
O2 | 0.0233 (15) | 0.0124 (13) | 0.0350 (19) | 0.0118 (11) | −0.0029 (17) | −0.0065 (16) |
O3 | 0.0111 (11) | 0.0108 (12) | 0.0179 (13) | 0.0057 (8) | −0.0055 (13) | −0.0001 (14) |
O4 | 0.0222 (15) | 0.0222 (15) | 0.013 (3) | −0.0023 (18) | 0 | 0 |
O5 | 0.0245 (14) | 0.0196 (13) | 0.0124 (16) | −0.0054 (10) | 0.0044 (16) | 0.0044 (16) |
Ca2 | 0.01854 (15) | 0.01854 (15) | 0.01139 (18) | −0.00959 (11) | 0.0005 (2) | 0.0005 (2) |
Ba1 | 0.0100 (8) | 0.0100 (8) | 0.0113 (12) | 0 | 0 | 0 |
Average | Minimum | Maximum | |
Ba2—O1i | 2.856 (8) | 2.826 (8) | 2.915 (8) |
Ba2—O1ii | 2.734 (8) | 2.715 (8) | 2.771 (8) |
Ba2—O2i | 3.441 (9) | 3.384 (8) | 3.468 (9) |
Ba2—O2ii | 3.204 (9) | 3.154 (9) | 3.303 (9) |
Ba2—O2iii | 3.438 (9) | 3.380 (8) | 3.468 (9) |
Ba2—O2iv | 3.241 (9) | 3.179 (9) | 3.275 (9) |
Ba2—O3v | 2.962 (7) | 2.836 (7) | 3.106 (7) |
Ba2—O3vi | 2.772 (7) | 2.702 (7) | 2.861 (7) |
Ba2—O3vii | 2.917 (7) | 2.817 (7) | 3.123 (7) |
Ba2—O3viii | 2.746 (7) | 2.689 (7) | 2.872 (7) |
Ba2—O4 | 3.083 (5) | 2.864 (5) | 3.208 (5) |
Ba2—O5i | 3.256 (7) | 2.878 (7) | 3.490 (7) |
Ba2—O5v | 3.370 (6) | 3.076 (6) | 3.803 (6) |
Ba2—O5vii | 3.563 (6) | 3.068 (6) | 3.811 (6) |
Ba2—O5iii | 3.145 (7) | 3.067 (7) | 3.303 (7) |
Ba2—Ca2 | 0 | 0 | 0 |
Ca1—Nb2 | 3.412 (4) | 3.401 (4) | 3.425 (4) |
Ca1—Nb2ix | 3.385 (4) | 3.382 (4) | 3.390 (4) |
Ca1—Nb2x | 3.412 (4) | 3.401 (4) | 3.425 (4) |
Ca1—Nb2xi | 3.385 (4) | 3.382 (4) | 3.390 (4) |
Ca1—Nb2xii | 3.412 (4) | 3.401 (4) | 3.425 (4) |
Ca1—Nb2xiii | 3.385 (4) | 3.382 (4) | 3.390 (4) |
Ca1—Nb2xiv | 3.412 (4) | 3.401 (4) | 3.425 (4) |
Ca1—Nb2xv | 3.385 (4) | 3.382 (4) | 3.390 (4) |
Ca1—O2 | 2.956 (10) | 2.632 (10) | 3.273 (10) |
Ca1—O2ix | 2.626 (9) | 2.508 (9) | 2.766 (10) |
Ca1—O2x | 2.956 (10) | 2.632 (10) | 3.273 (10) |
Ca1—O2xi | 2.626 (9) | 2.508 (9) | 2.766 (10) |
Ca1—O2xii | 2.956 (10) | 2.632 (10) | 3.273 (10) |
Ca1—O2xiii | 2.626 (9) | 2.508 (9) | 2.766 (10) |
Ca1—O2xiv | 2.956 (10) | 2.632 (10) | 3.273 (10) |
Ca1—O2xv | 2.626 (9) | 2.508 (9) | 2.766 (10) |
Ca1—O5 | 2.712 (6) | 2.693 (6) | 2.764 (6) |
Ca1—O5x | 2.712 (6) | 2.693 (6) | 2.764 (6) |
Ca1—O5xii | 2.712 (6) | 2.693 (6) | 2.764 (6) |
Ca1—O5xiv | 2.712 (6) | 2.693 (6) | 2.764 (6) |
Ca1—Ba1 | 0 | 0 | 0 |
Nb1—O3 | 1.969 (8) | 1.961 (8) | 1.985 (8) |
Nb1—O3v | 1.971 (8) | 1.959 (8) | 1.980 (8) |
Nb1—O3vii | 1.972 (8) | 1.962 (8) | 1.980 (8) |
Nb1—O3xvi | 1.971 (8) | 1.955 (8) | 1.979 (8) |
Nb1—O4 | 1.831 (10) | 1.819 (10) | 1.840 (10) |
Nb1—O4xvii | 2.163 (10) | 2.161 (10) | 2.166 (10) |
Nb2—O1 | 2.003 (8) | 1.987 (8) | 2.027 (8) |
Nb2—O2 | 1.956 (9) | 1.942 (9) | 1.978 (9) |
Nb2—O2x | 1.998 (9) | 1.983 (9) | 2.027 (9) |
Nb2—O3 | 1.955 (8) | 1.944 (8) | 1.969 (8) |
Nb2—O5 | 1.841 (9) | 1.821 (9) | 1.878 (9) |
Nb2—O5xvii | 2.173 (9) | 2.137 (9) | 2.207 (9) |
Nb2—Ba1 | 3.412 (4) | 3.401 (4) | 3.425 (4) |
Nb2—Ba1xvii | 3.387 (4) | 3.382 (4) | 3.390 (4) |
O1—O2 | 2.839 (12) | 2.792 (12) | 2.903 (12) |
O1—O2vii | 2.834 (12) | 2.812 (12) | 2.893 (12) |
O1—O3 | 2.858 (11) | 2.831 (11) | 2.879 (11) |
O1—O3vii | 2.866 (11) | 2.827 (11) | 2.891 (11) |
O1—O5 | 2.835 (11) | 2.778 (12) | 2.934 (11) |
O1—O5xvii | 2.864 (11) | 2.788 (12) | 2.990 (11) |
O1—O5vii | 2.820 (11) | 2.788 (12) | 2.873 (11) |
O1—O5xviii | 2.889 (11) | 2.812 (12) | 2.933 (11) |
O1—Ca2xix | 2.886 (8) | 2.764 (8) | 2.979 (8) |
O1—Ca2xx | 2.740 (8) | 2.686 (8) | 2.805 (8) |
O2—O2xvii | 3.960 (11) | 3.324 (11) | 4.620 (11) |
O2—O2ix | 3.976 (11) | 3.324 (11) | 4.620 (11) |
O2—O2x | 2.795 (13) | 2.739 (13) | 2.838 (13) |
O2—O2xiv | 2.795 (13) | 2.739 (13) | 2.838 (13) |
O2—O3xiv | 2.648 (12) | 2.607 (12) | 2.697 (12) |
O2—O5 | 2.770 (11) | 2.745 (11) | 2.812 (12) |
O2—O5xvii | 2.711 (11) | 2.674 (11) | 2.753 (11) |
O2—O5xiv | 2.840 (12) | 2.801 (12) | 2.883 (12) |
O2—O5xxi | 2.777 (12) | 2.738 (12) | 2.841 (12) |
O2—Ca2xix | 3.451 (9) | 3.360 (9) | 3.499 (8) |
O2—Ca2xx | 3.201 (9) | 3.018 (9) | 3.445 (9) |
O2—Ba1 | 2.956 (10) | 2.632 (10) | 3.273 (10) |
O2—Ba1xvii | 2.627 (9) | 2.508 (9) | 2.766 (10) |
O3—O3vii | 2.896 (11) | 2.838 (11) | 2.929 (11) |
O3—O3xvi | 2.652 (11) | 2.650 (11) | 2.655 (11) |
O3—O4 | 2.829 (11) | 2.815 (11) | 2.856 (11) |
O3—O4xvii | 2.764 (11) | 2.746 (11) | 2.791 (11) |
O3—O5 | 2.859 (11) | 2.796 (11) | 2.972 (11) |
O3—O5xvii | 2.833 (11) | 2.762 (11) | 2.944 (11) |
O3—Ca2v | 2.971 (7) | 2.804 (7) | 3.137 (7) |
O3—Ca2xxii | 2.773 (7) | 2.681 (8) | 2.879 (7) |
O4—O5 | 3.852 (8) | 3.318 (8) | 4.327 (8) |
O4—O5v | 3.782 (8) | 3.309 (8) | 4.313 (8) |
O4—O5vii | 3.986 (8) | 3.315 (8) | 4.309 (8) |
O4—O5xvi | 3.648 (8) | 3.311 (8) | 4.330 (8) |
O4—Ca2 | 3.083 (5) | 2.864 (5) | 3.208 (5) |
O4—Ca2v | 2.983 (5) | 2.877 (5) | 3.196 (5) |
O5—O5x | 3.804 (9) | 3.187 (9) | 4.425 (9) |
O5—O5xiv | 3.804 (9) | 3.187 (9) | 4.425 (9) |
O5—Ca2xix | 3.199 (7) | 2.708 (7) | 3.661 (7) |
O5—Ca2v | 3.465 (6) | 2.934 (7) | 3.942 (6) |
O5—Ba1 | 2.712 (6) | 2.693 (6) | 2.764 (6) |
Symmetry codes: (i) −x1+1/2, x2+1/2, x3, x5, x4; (ii) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (iii) x2, −x1+1, x3, x5, −x4; (iv) x2, −x1+1, x3+1/2, x5+1/2, −x4+1/2; (v) −x1, −x2+1, x3, −x4, −x5; (vi) −x1, −x2+1, x3+1/2, −x4+1/2, −x5+1/2; (vii) −x2+1/2, −x1+1/2, x3, −x4, x5; (viii) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (ix) x1, x2, x3+1/2, x4+1/2, x5+1/2; (x) −x2, x1, x3, −x5, x4; (xi) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (xii) −x1, −x2, x3, −x4, −x5; (xiii) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (xiv) x2, −x1, x3, x5, −x4; (xv) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (xvi) x2−1/2, x1+1/2, x3, x4, −x5; (xvii) x1, x2, x3−1/2, x4+1/2, x5+1/2; (xviii) −x2+1/2, −x1+1/2, x3−1/2, −x4+1/2, x5+1/2; (xix) −x2+1, x1, x3, −x5, x4; (xx) −x2+1, x1, x3−1/2, −x5+1/2, x4+1/2; (xxi) x2, −x1, x3−1/2, x5+1/2, −x4+1/2; (xxii) −x1, −x2+1, x3−1/2, −x4+1/2, −x5+1/2. |
Ba0.693Ca0.307Nb2O6 | Dx = 5.256 Mg m−3 |
Mr = 389.3 | Mo Kα radiation, λ = 0.7107 Å |
Tetragonal, X4bm† | Cell parameters from 18477 reflections |
q1 = 0.294200a* + 0.294200b*; q2 = -0.294200a* + 0.294200b* | θ = 3.1–36.8° |
a = 12.4608 (5) Å | µ = 10.37 mm−1 |
c = 7.9185 (7) Å | T = 293 K |
V = 1229.52 (13) Å3 | '3.08', 3.08 |
Z = 10 | 0.34 × 0.25 × 0.09 mm |
F(000) = 1750 |
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 2905 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 2580 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.026 |
Detector resolution: 8.2495 pixels mm-1 | θmax = 36.3°, θmin = 2.9° |
ω and π scans | h = −20→20 |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | k = −19→20 |
Tmin = 0.198, Tmax = 0.556 | l = −13→12 |
52003 measured reflections |
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
R[F2 > 2σ(F2)] = 0.030 | (Δ/σ)max = 0.026 |
wR(F2) = 0.047 | Δρmax = 0.00 e Å−3 |
S = 2.02 | Δρmin = −0.66 e Å−3 |
2905 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
151 parameters | Extinction coefficient: 330 (20) |
0 restraints | Absolute structure: 1406 of Friedel pairs used in the refinement |
0 constraints | Absolute structure parameter: 0.47 (3) |
Ba0.693Ca0.307Nb2O6 | V = 1229.52 (13) Å3 |
Mr = 389.3 | Z = 10 |
Tetragonal, X4bm† | Mo Kα radiation |
q1 = 0.294200a* + 0.294200b*; q2 = -0.294200a* + 0.294200b* | µ = 10.37 mm−1 |
a = 12.4608 (5) Å | T = 293 K |
c = 7.9185 (7) Å | 0.34 × 0.25 × 0.09 mm |
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2. |
Xcalibur, Sapphire2, large Be window diffractometer | 2905 independent reflections |
Absorption correction: analytical CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | 2580 reflections with I > 3σ(I) |
Tmin = 0.198, Tmax = 0.556 | Rint = 0.026 |
52003 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 0 restraints |
wR(F2) = 0.047 | Δρmax = 0.00 e Å−3 |
S = 2.02 | Δρmin = −0.66 e Å−3 |
2905 reflections | Absolute structure: 1406 of Friedel pairs used in the refinement |
151 parameters | Absolute structure parameter: 0.47 (3) |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ba2 | 0.172006 (17) | 0.672006 (17) | 0.25 | 0.01488 (11) | 0.8542 |
Ca1 | 0 | 0 | 0.2575 (6) | 0.0105 (5) | 0.5904 |
Nb1 | 0 | 0.5 | 0.01060 (18) | 0.00572 (15) | |
Nb2 | 0.07330 (2) | 0.21001 (2) | 0.00552 (12) | 0.00671 (12) | |
O1 | 0.21579 (18) | 0.28421 (18) | −0.0103 (9) | 0.0092 (8) | |
O2 | 0.1391 (2) | 0.0688 (2) | −0.0208 (5) | 0.0215 (9) | |
O3 | −0.00672 (19) | 0.34339 (18) | −0.0150 (5) | 0.0142 (7) | |
O4 | 0 | 0.5 | 0.2382 (11) | 0.0179 (12) | |
O5 | 0.07371 (18) | 0.20251 (19) | 0.2375 (5) | 0.0190 (8) | |
Ca2 | 0.172006 (17) | 0.672006 (17) | 0.25 | 0.01488 (11) | 0.0882 |
Ba1 | 0 | 0 | 0.2575 (6) | 0.0105 (5) | 0.028 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba2 | 0.01669 (17) | 0.01669 (17) | 0.0112 (2) | −0.00931 (12) | 0.0004 (2) | 0.0004 (2) |
Ca1 | 0.0092 (6) | 0.0092 (6) | 0.0132 (11) | 0 | 0 | 0 |
Nb1 | 0.0054 (2) | 0.0054 (2) | 0.0064 (3) | −0.0004 (2) | 0 | 0 |
Nb2 | 0.00595 (18) | 0.00593 (19) | 0.0082 (2) | 0.00098 (9) | 0.0003 (3) | −0.0018 (3) |
O1 | 0.0081 (9) | 0.0081 (9) | 0.0114 (19) | 0.0021 (12) | −0.0016 (16) | 0.0016 (16) |
O2 | 0.0220 (15) | 0.0121 (13) | 0.0306 (18) | 0.0105 (11) | −0.0041 (16) | −0.0064 (15) |
O3 | 0.0125 (12) | 0.0094 (12) | 0.0208 (14) | 0.0048 (8) | −0.0018 (15) | −0.0007 (15) |
O4 | 0.0231 (15) | 0.0231 (15) | 0.008 (3) | 0.0018 (18) | 0 | 0 |
O5 | 0.0213 (13) | 0.0222 (12) | 0.0135 (17) | −0.0034 (9) | 0.0039 (17) | −0.0004 (17) |
Ca2 | 0.01669 (17) | 0.01669 (17) | 0.0112 (2) | −0.00931 (12) | 0.0004 (2) | 0.0004 (2) |
Ba1 | 0.0092 (6) | 0.0092 (6) | 0.0132 (11) | 0 | 0 | 0 |
Average | Minimum | Maximum | |
Ba2—O1i | 2.845 (8) | 2.820 (8) | 2.895 (8) |
Ba2—O1ii | 2.733 (8) | 2.714 (8) | 2.771 (8) |
Ba2—O2i | 3.463 (8) | 3.367 (8) | 3.506 (8) |
Ba2—O2ii | 3.236 (8) | 3.161 (8) | 3.329 (8) |
Ba2—O2iii | 3.450 (8) | 3.366 (8) | 3.504 (8) |
Ba2—O2iv | 3.260 (8) | 3.188 (8) | 3.299 (8) |
Ba2—O3v | 2.950 (7) | 2.833 (7) | 3.075 (7) |
Ba2—O3vi | 2.787 (7) | 2.707 (7) | 2.877 (7) |
Ba2—O3vii | 2.905 (7) | 2.815 (7) | 3.092 (7) |
Ba2—O3viii | 2.754 (7) | 2.690 (7) | 2.891 (7) |
Ba2—O4 | 3.071 (5) | 2.888 (5) | 3.181 (5) |
Ba2—O5i | 3.257 (6) | 2.850 (6) | 3.537 (6) |
Ba2—O5v | 3.361 (6) | 3.106 (6) | 3.778 (6) |
Ba2—O5vii | 3.556 (6) | 3.099 (6) | 3.786 (6) |
Ba2—O5iii | 3.154 (6) | 3.076 (6) | 3.313 (6) |
Ba2—Ca2 | 0 | 0 | 0 |
Ca1—Nb2 | 3.415 (4) | 3.405 (4) | 3.426 (4) |
Ca1—Nb2ix | 3.395 (3) | 3.392 (3) | 3.402 (3) |
Ca1—Nb2x | 3.415 (4) | 3.405 (4) | 3.426 (4) |
Ca1—Nb2xi | 3.395 (3) | 3.392 (3) | 3.402 (3) |
Ca1—Nb2xii | 3.415 (4) | 3.405 (4) | 3.426 (4) |
Ca1—Nb2xiii | 3.395 (3) | 3.392 (3) | 3.402 (3) |
Ca1—Nb2xiv | 3.415 (4) | 3.405 (4) | 3.426 (4) |
Ca1—Nb2xv | 3.395 (3) | 3.392 (3) | 3.402 (3) |
Ca1—O2 | 2.947 (9) | 2.624 (9) | 3.246 (9) |
Ca1—O2ix | 2.623 (9) | 2.503 (8) | 2.757 (9) |
Ca1—O2x | 2.947 (9) | 2.624 (9) | 3.246 (9) |
Ca1—O2xi | 2.623 (9) | 2.503 (8) | 2.757 (9) |
Ca1—O2xii | 2.947 (9) | 2.624 (9) | 3.246 (9) |
Ca1—O2xiii | 2.623 (9) | 2.503 (8) | 2.757 (9) |
Ca1—O2xiv | 2.947 (9) | 2.624 (9) | 3.246 (9) |
Ca1—O2xv | 2.623 (9) | 2.503 (8) | 2.757 (9) |
Ca1—O5 | 2.694 (5) | 2.655 (5) | 2.751 (5) |
Ca1—O5x | 2.694 (5) | 2.655 (5) | 2.751 (5) |
Ca1—O5xii | 2.694 (5) | 2.655 (5) | 2.751 (5) |
Ca1—O5xiv | 2.694 (5) | 2.655 (5) | 2.751 (5) |
Ca1—Ba1 | 0 | 0 | 0 |
Nb1—O3 | 1.970 (7) | 1.961 (8) | 1.991 (8) |
Nb1—O3v | 1.972 (7) | 1.957 (7) | 1.977 (7) |
Nb1—O3vii | 1.974 (7) | 1.963 (7) | 1.985 (7) |
Nb1—O3xvi | 1.971 (7) | 1.953 (8) | 1.982 (8) |
Nb1—O4 | 1.816 (10) | 1.814 (10) | 1.817 (10) |
Nb1—O4xvii | 2.168 (10) | 2.164 (10) | 2.175 (10) |
Nb2—O1 | 2.005 (7) | 1.995 (7) | 2.020 (7) |
Nb2—O2 | 1.964 (8) | 1.950 (8) | 1.986 (8) |
Nb2—O2x | 2.003 (8) | 1.985 (8) | 2.029 (8) |
Nb2—O3 | 1.952 (8) | 1.943 (8) | 1.963 (8) |
Nb2—O5 | 1.854 (9) | 1.830 (9) | 1.897 (9) |
Nb2—O5xvii | 2.147 (9) | 2.123 (9) | 2.189 (9) |
Nb2—Ba1 | 3.415 (4) | 3.405 (4) | 3.426 (4) |
Nb2—Ba1xvii | 3.399 (3) | 3.392 (3) | 3.402 (3) |
O1—O2 | 2.849 (11) | 2.797 (11) | 2.918 (11) |
O1—O2vii | 2.843 (11) | 2.819 (11) | 2.909 (11) |
O1—O3 | 2.876 (10) | 2.856 (10) | 2.905 (10) |
O1—O3vii | 2.877 (10) | 2.849 (10) | 2.901 (10) |
O1—O5 | 2.850 (11) | 2.794 (11) | 2.944 (10) |
O1—O5xvii | 2.861 (11) | 2.785 (11) | 2.989 (10) |
O1—O5vii | 2.838 (11) | 2.795 (11) | 2.892 (10) |
O1—O5xviii | 2.884 (11) | 2.824 (11) | 2.916 (11) |
O1—Ca2xix | 2.867 (8) | 2.758 (8) | 2.960 (8) |
O1—Ca2xx | 2.740 (8) | 2.681 (8) | 2.809 (8) |
O2—O2xvii | 3.939 (10) | 3.338 (10) | 4.594 (10) |
O2—O2ix | 3.985 (10) | 3.338 (10) | 4.594 (10) |
O2—O2x | 2.774 (11) | 2.719 (11) | 2.817 (11) |
O2—O2xiv | 2.774 (11) | 2.719 (11) | 2.817 (11) |
O2—O3xiv | 2.661 (11) | 2.619 (11) | 2.707 (11) |
O2—O5 | 2.779 (11) | 2.757 (11) | 2.828 (11) |
O2—O5xvii | 2.692 (11) | 2.660 (11) | 2.738 (10) |
O2—O5xiv | 2.843 (11) | 2.809 (11) | 2.881 (11) |
O2—O5xxi | 2.753 (11) | 2.712 (11) | 2.817 (11) |
O2—Ca2xix | 3.469 (8) | 3.354 (8) | 3.514 (8) |
O2—Ca2xx | 3.210 (8) | 3.049 (8) | 3.445 (8) |
O2—Ba1 | 2.947 (9) | 2.624 (9) | 3.246 (9) |
O2—Ba1xvii | 2.617 (9) | 2.503 (8) | 2.757 (9) |
O3—O3xvii | 3.987 (9) | 3.492 (9) | 4.428 (9) |
O3—O3ix | 3.933 (9) | 3.492 (9) | 4.428 (9) |
O3—O3vii | 2.894 (11) | 2.849 (11) | 2.919 (11) |
O3—O3xvi | 2.654 (11) | 2.636 (11) | 2.677 (11) |
O3—O4 | 2.814 (10) | 2.808 (10) | 2.825 (10) |
O3—O4xvii | 2.774 (10) | 2.747 (10) | 2.813 (11) |
O3—O5 | 2.858 (10) | 2.807 (10) | 2.957 (10) |
O3—O5xvii | 2.835 (10) | 2.772 (10) | 2.944 (10) |
O3—Ca2v | 2.950 (7) | 2.802 (7) | 3.106 (7) |
O3—Ca2xxii | 2.787 (7) | 2.678 (7) | 2.903 (7) |
O4—O5 | 3.876 (7) | 3.349 (7) | 4.319 (7) |
O4—O5v | 3.779 (7) | 3.330 (7) | 4.311 (7) |
O4—O5vii | 3.991 (7) | 3.337 (7) | 4.306 (7) |
O4—O5xvi | 3.664 (7) | 3.341 (7) | 4.323 (7) |
O4—Ca2 | 3.071 (5) | 2.888 (5) | 3.181 (5) |
O4—Ca2v | 2.989 (5) | 2.897 (5) | 3.172 (5) |
O5—O5x | 3.781 (8) | 3.194 (8) | 4.402 (8) |
O5—O5xiv | 3.781 (8) | 3.194 (8) | 4.402 (8) |
O5—Ca2xix | 3.214 (6) | 2.721 (6) | 3.667 (6) |
O5—Ca2v | 3.470 (6) | 2.941 (6) | 3.939 (6) |
O5—Ba1 | 2.694 (5) | 2.655 (5) | 2.751 (5) |
Symmetry codes: (i) −x1+1/2, x2+1/2, x3, x5, x4; (ii) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (iii) x2, −x1+1, x3, x5, −x4; (iv) x2, −x1+1, x3+1/2, x5+1/2, −x4+1/2; (v) −x1, −x2+1, x3, −x4, −x5; (vi) −x1, −x2+1, x3+1/2, −x4+1/2, −x5+1/2; (vii) −x2+1/2, −x1+1/2, x3, −x4, x5; (viii) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (ix) x1, x2, x3+1/2, x4+1/2, x5+1/2; (x) −x2, x1, x3, −x5, x4; (xi) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (xii) −x1, −x2, x3, −x4, −x5; (xiii) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (xiv) x2, −x1, x3, x5, −x4; (xv) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (xvi) x2−1/2, x1+1/2, x3, x4, −x5; (xvii) x1, x2, x3−1/2, x4+1/2, x5+1/2; (xviii) −x2+1/2, −x1+1/2, x3−1/2, −x4+1/2, x5+1/2; (xix) −x2+1, x1, x3, −x5, x4; (xx) −x2+1, x1, x3−1/2, −x5+1/2, x4+1/2; (xxi) x2, −x1, x3−1/2, x5+1/2, −x4+1/2; (xxii) −x1, −x2+1, x3−1/2, −x4+1/2, −x5+1/2. |
Experimental details
(cbn24ort) | (cbn24tet) | (cbn31) | |
Crystal data | |||
Chemical formula | Ba0.761Ca0.239Nb2O6 | Ba0.761Ca0.239Nb2O6 | Ba0.693Ca0.307Nb2O6 |
Mr | 395.9 | 395.9 | 389.3 |
Crystal system, space group | Orthorhombic, X2mm(00γ)000† | Tetragonal, X4bm‡ | Tetragonal, X4bm§ |
Temperature (K) | 293 | 293 | 293 |
Wave vectors | q = 0.663800c* | q1 = 0.309425a* + 0.309425b*; q2 = -0.309425a* + 0.309425b* | q1 = 0.294200a* + 0.294200b*; q2 = -0.294200a* + 0.294200b* |
a, b, c (Å) | 7.9429 (3), 17.6240 (5), 17.6229 (6) | 12.4476 (4), 12.4476 (4), 7.9291 (4) | 12.4608 (5), 12.4608 (5), 7.9185 (7) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 2466.95 (14) | 1228.56 (8) | 1229.52 (13) |
Z | 20 | 10 | 10 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 10.75 | 10.83 | 10.37 |
Crystal size (mm) | 0.40 × 0.34 × 0.04 | 0.38 × 0.23 × 0.07 | 0.34 × 0.25 × 0.09 |
Data collection | |||
Diffractometer | Xcalibur, Sapphire2, large Be window diffractometer | Xcalibur, Sapphire2, large Be window diffractometer | Xcalibur, Sapphire2, large Be window diffractometer |
Absorption correction | Analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | Analytical CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | Analytical CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) |
Tmin, Tmax | 0.081, 0.672 | 0.11, 0.654 | 0.198, 0.556 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 20132, 3449, 2633 | 59030, 2905, 2299 | 52003, 2905, 2580 |
Rint | 0.030 | 0.038 | 0.026 |
(sin θ/λ)max (Å−1) | 0.740 | 0.952 | 0.834 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.036, 1.42 | 0.027, 0.039, 1.48 | 0.030, 0.047, 2.02 |
No. of reflections | 3449 | 2905 | 2905 |
No. of parameters | 212 | 152 | 151 |
Δρmax, Δρmin (e Å−3) | 1.16, −0.86 | 0.00, −0.58 | 0.00, −0.66 |
Absolute structure | 1605 of Friedel pairs used in the refinement | 1407 of Friedel pairs used in the refinement | 1406 of Friedel pairs used in the refinement |
Absolute structure parameter | 0.47 (3) | 0.45 (3) | 0.47 (3) |
† Symmetry operations: (1) x1, x2, x3, x4; (2) x1, −x2, x3, x4; (3) x1, x2, −x3, −x4; (4) x1, −x2, −x3, −x4; (5) x1, x2+1/2, x3+1/2, x4; (6) x1, −x2+1/2, x3+1/2, x4; (7) x1, x2+1/2, −x3+1/2, −x4; (8) x1, −x2+1/2, −x3+1/2, −x4; (9) x1+1/2, x2, x3, x4+1/2; (10) x1+1/2, −x2, x3, x4+1/2; (11) x1+1/2, x2, −x3, −x4+1/2; (12) x1+1/2, −x2, −x3, −x4+1/2; (13) x1+1/2, x2+1/2, x3+1/2, x4+1/2; (14) x1+1/2, −x2+1/2, x3+1/2, x4+1/2; (15) x1+1/2, x2+1/2, −x3+1/2, −x4+1/2; (16) x1+1/2, −x2+1/2, −x3+1/2, −x4+1/2.
‡ Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2.
§ Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x2, x1, x3, −x5, x4; (3) −x1+1/2, x2+1/2, x3, x5, x4; (4) −x1, −x2, x3, −x4, −x5; (5) −x2+1/2, −x1+1/2, x3, −x4, x5; (6) x2, −x1, x3, x5, −x4; (7) x1+1/2, −x2+1/2, x3, −x5, −x4; (8) x2+1/2, x1+1/2, x3, x4, −x5; (9) x1, x2, x3+1/2, x4+1/2, x5+1/2; (10) −x2, x1, x3+1/2, −x5+1/2, x4+1/2; (11) −x1+1/2, x2+1/2, x3+1/2, x5+1/2, x4+1/2; (12) −x1, −x2, x3+1/2, −x4+1/2, −x5+1/2; (13) −x2+1/2, −x1+1/2, x3+1/2, −x4+1/2, x5+1/2; (14) x2, −x1, x3+1/2, x5+1/2, −x4+1/2; (15) x1+1/2, −x2+1/2, x3+1/2, −x5+1/2, −x4+1/2; (16) x2+1/2, x1+1/2, x3+1/2, x4+1/2, −x5+1/2.
Computer programs: CrysAlis PRO, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25), CrysAlis PRO, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49), Jana2006, Diamond 3.0.
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