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CBN crystals show a one- and a two-dimensionally modulated modification. The former is isotypic with orthorhombic Ba4Na2Nb10O30 and the latter with the tetragonal tungsten bronze type of crystal structure. The orthorhombic form irreversibly transforms to the tetragonal polymorph at the ferroelectric phase transition near 603 K. Orthorhombic and tetragonal CBN24 slightly differ in the distribution of the Ba and Ca atoms over the incompletely filled Me1 and Me2 sites. The tetragonal symmetry is further broken in orthorhombic CBN24 by different amplitudes of the positional modulations of O atoms which are symmetrically equivalent in the TTB structure. A similar orthorhombic phase of CBN31 could be obtained by quenching from 1473 K.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614011676/dk5023sup1.cif
Contains datablocks global, cbn24ort, cbn24tet, cbn31

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn24ortsup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn24tetsup3.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011676/dk5023cbn31sup4.hkl
Contains datablock I

B-IncStrDB reference: 9692EcLKMW

Computing details top

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.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
(cbn24ort) top
Crystal data top
Ba0.761Ca0.239Nb2O6F(000) = 3553
Mr = 395.9Dx = 5.328 Mg m3
Orthorhombic, X2mm(00γ)000†Mo Kα radiation, λ = 0.71069 Å
q = 0.663800c*Cell parameters from 10368 reflections
a = 7.9429 (3) Åθ = 2.9–23.3°
b = 17.6240 (5) ŵ = 10.75 mm1
c = 17.6229 (6) ÅT = 293 K
V = 2466.95 (14) Å3Plate-like, colourless
Z = 200.40 × 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.

Data collection top
Xcalibur, Sapphire2, large Be window
diffractometer
3449 independent reflections
Radiation source: Enhance (Mo) X-ray Source2633 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.030
Detector resolution: 8.2495 pixels mm-1θmax = 31.7°, θmin = 3.0°
ω and π scansh = 1111
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 = 2524
Tmin = 0.081, Tmax = 0.672l = 2523
20132 measured reflections
Refinement top
Refinement on FWeighting 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) = 0.036Δρmax = 1.16 e Å3
S = 1.42Δρmin = 0.86 e Å3
3449 reflectionsExtinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
212 parametersExtinction coefficient: 271 (9)
0 restraintsAbsolute structure: 1605 of Friedel pairs used in the refinement
45 constraintsAbsolute structure parameter: 0.47 (3)
Crystal data top
Ba0.761Ca0.239Nb2O6V = 2466.95 (14) Å3
Mr = 395.9Z = 20
Orthorhombic, X2mm(00γ)000†Mo Kα radiation
q = 0.663800c*µ = 10.75 mm1
a = 7.9429 (3) ÅT = 293 K
b = 17.6240 (5) Å0.40 × 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.

Data collection top
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 = 0.672Rint = 0.030
20132 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0270 restraints
wR(F2) = 0.036Δρmax = 1.16 e Å3
S = 1.42Δρmin = 0.86 e Å3
3449 reflectionsAbsolute structure: 1605 of Friedel pairs used in the refinement
212 parametersAbsolute structure parameter: 0.47 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba2a0.2395500.32733 (2)0.01729 (14)0.9596 (19)
Ba2b0.24174 (12)0.171915 (19)00.01627 (14)0.9294 (19)
Nb2a0.00389 (13)0.181810 (18)0.39127 (2)0.00714 (12)
Nb2b0.00462 (13)0.10878 (2)0.181611 (19)0.00707 (12)
Nb1a0.0004 (2)000.0062 (2)
Nb1b0.0010 (2)0.500.0059 (2)
Ca10.2495 (6)0.250.250.0117 (6)0.532 (5)
O1a0.0195 (10)0.2155 (2)0.50.0104 (13)
O5a0.2253 (7)0.18531 (19)0.3895 (2)0.0288 (12)
O5b0.2740 (6)0.11246 (18)0.18543 (19)0.0228 (12)
O1b0.0252 (9)00.2143 (3)0.0089 (13)
O2a0.0346 (6)0.14432 (19)0.28490 (18)0.0223 (12)
O3b0.0255 (6)0.07503 (16)0.41884 (19)0.0167 (10)
O2b0.0278 (7)0.21477 (17)0.1461 (2)0.0284 (12)
O3a0.0280 (6)0.08193 (17)0.07499 (18)0.0152 (9)
O4a0.2201 (11)0.500.019 (2)
O4b0.2401 (14)000.024 (2)
Ca2a0.2395500.32733 (2)0.01729 (14)0.0272
Ca2b0.24174 (12)0.171915 (19)00.01627 (14)0.0304
Ba10.2495 (6)0.250.250.0117 (6)0.0274
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba2a0.0113 (2)0.0299 (3)0.0106 (2)00.0026 (4)0
Ba2b0.0112 (2)0.0088 (2)0.0288 (3)0.0008 (4)00
Nb2a0.0074 (2)0.0057 (2)0.0082 (2)0.0005 (4)0.0014 (4)0.00006 (13)
Nb2b0.0077 (2)0.0078 (2)0.0057 (2)0.0004 (4)0.0009 (4)0.00007 (13)
Nb1a0.0058 (4)0.0060 (3)0.0068 (4)000
Nb1b0.0063 (4)0.0063 (3)0.0051 (4)000
Ca10.0130 (11)0.0115 (10)0.0107 (11)000.0023 (7)
O1a0.019 (2)0.0076 (19)0.004 (2)0.007 (3)00
O5a0.014 (2)0.054 (2)0.019 (2)0.007 (2)0.001 (2)0.0022 (16)
O5b0.0111 (19)0.0252 (18)0.032 (2)0.009 (2)0.006 (2)0.0115 (14)
O1b0.007 (2)0.011 (2)0.009 (2)00.003 (3)0
O2a0.031 (2)0.0289 (19)0.0070 (18)0.001 (2)0.002 (2)0.0084 (15)
O3b0.028 (2)0.0055 (13)0.0165 (17)0.007 (2)0.001 (2)0.0032 (12)
O2b0.046 (2)0.0101 (16)0.029 (2)0.009 (2)0.010 (3)0.0067 (16)
O3a0.0223 (18)0.0127 (14)0.0106 (16)0.0076 (19)0.000 (2)0.0052 (13)
O4a0.002 (4)0.032 (4)0.024 (4)000
O4b0.024 (4)0.027 (3)0.021 (4)000
Ca2a0.0113 (2)0.0299 (3)0.0106 (2)00.0026 (4)0
Ca2b0.0112 (2)0.0088 (2)0.0288 (3)0.0008 (4)00
Ba10.0130 (11)0.0115 (10)0.0107 (11)000.0023 (7)
Bond lengths (Å) top
AverageMinimumMaximum
Ba2a—O5bi3.194 (5)2.861 (5)3.528 (5)
Ba2a—O5bii3.194 (5)2.861 (5)3.528 (5)
Ba2a—O1b2.898 (9)2.795 (9)3.000 (9)
Ba2a—O1bi2.733 (9)2.693 (9)2.774 (9)
Ba2a—O3b2.965 (6)2.830 (6)3.100 (6)
Ba2a—O3bi2.801 (6)2.720 (6)2.885 (6)
Ba2a—O3biii2.965 (6)2.830 (6)3.100 (6)
Ba2a—O3bii2.801 (6)2.720 (6)2.885 (6)
Ba2a—O4aiv3.045 (4)2.808 (8)3.286 (8)
Ba2b—O1av2.873 (7)2.807 (9)2.938 (9)
Ba2b—O1avi2.746 (7)2.691 (9)2.803 (9)
Ba2b—O5av3.187 (5)2.843 (5)3.526 (5)
Ba2b—O5avii3.187 (5)2.843 (5)3.526 (5)
Ba2b—O3ai2.762 (6)2.691 (6)2.840 (6)
Ba2b—O3aviii2.762 (6)2.691 (6)2.840 (6)
Nb2a—O1a2.012 (5)1.981 (8)2.039 (8)
Nb2a—O5a1.833 (8)1.824 (8)1.849 (8)
Nb2a—O3b1.955 (6)1.947 (6)1.963 (6)
Nb2a—O2bvii1.956 (6)1.946 (6)1.966 (6)
Nb2b—O5bi1.848 (8)1.829 (8)1.866 (8)
Nb2b—O2a1.948 (7)1.934 (7)1.960 (7)
Nb2b—O2b1.985 (6)1.977 (6)1.998 (6)
Nb2b—O3a1.951 (7)1.944 (7)1.963 (7)
Nb1a—O3a1.976 (6)1.965 (6)1.988 (6)
Nb1a—O3aiii1.976 (6)1.965 (6)1.988 (6)
Nb1a—O3aix1.976 (6)1.965 (6)1.988 (6)
Nb1a—O3ax1.976 (6)1.965 (6)1.988 (6)
Nb1a—O4b1.917 (14)1.893 (17)1.930 (12)
Nb1b—O3bxi1.961 (6)1.956 (7)1.970 (6)
Nb1b—O3bv1.961 (6)1.956 (7)1.970 (6)
Nb1b—O3bxii1.961 (6)1.956 (7)1.970 (6)
Nb1b—O3bvii1.961 (6)1.956 (7)1.970 (6)
Nb1b—O4a1.764 (11)1.755 (13)1.771 (9)
O5a—Ba12.725 (5)2.583 (6)2.852 (6)
O5b—Ba1xiii2.695 (5)2.658 (5)2.738 (5)
O2a—Ba12.991 (7)2.776 (7)3.207 (8)
O2a—Ba1xiii2.610 (7)2.487 (7)2.738 (7)
O2b—Ba12.930 (8)2.687 (8)3.176 (8)
O2b—Ba1xiii2.625 (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, x21/2, x3+1/2, x4; (v) x1, x2+1/2, x31/2, x4; (vi) x1+1/2, x2+1/2, x31/2, 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, x31/2, x4; (xii) x1, x2+1/2, x3+1/2, x4; (xiii) x11/2, x2, x3, x4+1/2.
(cbn24tet) top
Crystal data top
Ba0.761Ca0.239Nb2O6F(000) = 1773
Mr = 395.9Dx = 5.349 Mg m3
Tetragonal, X4bmMo 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) Åθ = 2.8–42.5°
c = 7.9291 (4) ŵ = 10.83 mm1
V = 1228.56 (8) Å3T = 293 K
Z = 100.38 × 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.

Data collection top
Xcalibur, Sapphire2, large Be window
diffractometer
2905 independent reflections
Radiation source: Enhance (Mo) X-ray Source2299 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 8.2495 pixels mm-1θmax = 42.6°, θmin = 2.9°
ω and π scansh = 1923
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 = 2223
Tmin = 0.11, Tmax = 0.654l = 1413
59030 measured reflections
Refinement top
Refinement on FWeighting 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) = 0.039Δρmax = 0.00 e Å3
S = 1.48Δρmin = 0.58 e Å3
2905 reflectionsExtinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
152 parametersExtinction coefficient: 198 (14)
0 restraintsAbsolute structure: 1407 of Friedel pairs used in the refinement
3 constraintsAbsolute structure parameter: 0.45 (3)
Crystal data top
Ba0.761Ca0.239Nb2O6V = 1228.56 (8) Å3
Mr = 395.9Z = 10
Tetragonal, X4bmMo Kα radiation
q1 = 0.309425a* + 0.309425b*; q2 = -0.309425a* + 0.309425b*µ = 10.83 mm1
a = 12.4476 (4) ÅT = 293 K
c = 7.9291 (4) Å0.38 × 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.

Data collection top
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 = 0.654Rint = 0.038
59030 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0270 restraints
wR(F2) = 0.039Δρmax = 0.00 e Å3
S = 1.48Δρmin = 0.58 e Å3
2905 reflectionsAbsolute structure: 1407 of Friedel pairs used in the refinement
152 parametersAbsolute structure parameter: 0.45 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba20.172267 (15)0.672267 (15)0.250.01616 (9)0.9382 (8)
Ca1000.2583 (6)0.0105 (6)0.524 (2)
Nb100.50.00929 (17)0.00571 (13)
Nb20.07295 (2)0.20951 (2)0.00540 (11)0.00674 (10)
O10.21501 (17)0.28499 (17)0.0113 (9)0.0098 (8)
O20.1401 (2)0.0697 (2)0.0210 (6)0.0236 (9)
O30.00673 (18)0.34333 (18)0.0176 (5)0.0133 (7)
O400.50.2381 (11)0.0192 (12)
O50.07402 (19)0.2031 (2)0.2350 (5)0.0188 (8)
Ca20.172267 (15)0.672267 (15)0.250.01616 (9)0.0322
Ba1000.2583 (6)0.0105 (6)0.0261 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba20.01854 (15)0.01854 (15)0.01139 (18)0.00959 (11)0.0005 (2)0.0005 (2)
Ca10.0100 (8)0.0100 (8)0.0113 (12)000
Nb10.00524 (18)0.00524 (18)0.0067 (3)0.00036 (19)00
Nb20.00611 (17)0.00623 (17)0.0079 (2)0.00114 (9)0.0003 (3)0.0003 (3)
O10.0077 (9)0.0077 (9)0.0140 (19)0.0024 (11)0.0023 (15)0.0023 (15)
O20.0233 (15)0.0124 (13)0.0350 (19)0.0118 (11)0.0029 (17)0.0065 (16)
O30.0111 (11)0.0108 (12)0.0179 (13)0.0057 (8)0.0055 (13)0.0001 (14)
O40.0222 (15)0.0222 (15)0.013 (3)0.0023 (18)00
O50.0245 (14)0.0196 (13)0.0124 (16)0.0054 (10)0.0044 (16)0.0044 (16)
Ca20.01854 (15)0.01854 (15)0.01139 (18)0.00959 (11)0.0005 (2)0.0005 (2)
Ba10.0100 (8)0.0100 (8)0.0113 (12)000
Bond lengths (Å) top
AverageMinimumMaximum
Ba2—O1i2.856 (8)2.826 (8)2.915 (8)
Ba2—O1ii2.734 (8)2.715 (8)2.771 (8)
Ba2—O2i3.441 (9)3.384 (8)3.468 (9)
Ba2—O2ii3.204 (9)3.154 (9)3.303 (9)
Ba2—O2iii3.438 (9)3.380 (8)3.468 (9)
Ba2—O2iv3.241 (9)3.179 (9)3.275 (9)
Ba2—O3v2.962 (7)2.836 (7)3.106 (7)
Ba2—O3vi2.772 (7)2.702 (7)2.861 (7)
Ba2—O3vii2.917 (7)2.817 (7)3.123 (7)
Ba2—O3viii2.746 (7)2.689 (7)2.872 (7)
Ba2—O43.083 (5)2.864 (5)3.208 (5)
Ba2—O5i3.256 (7)2.878 (7)3.490 (7)
Ba2—O5v3.370 (6)3.076 (6)3.803 (6)
Ba2—O5vii3.563 (6)3.068 (6)3.811 (6)
Ba2—O5iii3.145 (7)3.067 (7)3.303 (7)
Ba2—Ca2000
Ca1—Nb23.412 (4)3.401 (4)3.425 (4)
Ca1—Nb2ix3.385 (4)3.382 (4)3.390 (4)
Ca1—Nb2x3.412 (4)3.401 (4)3.425 (4)
Ca1—Nb2xi3.385 (4)3.382 (4)3.390 (4)
Ca1—Nb2xii3.412 (4)3.401 (4)3.425 (4)
Ca1—Nb2xiii3.385 (4)3.382 (4)3.390 (4)
Ca1—Nb2xiv3.412 (4)3.401 (4)3.425 (4)
Ca1—Nb2xv3.385 (4)3.382 (4)3.390 (4)
Ca1—O22.956 (10)2.632 (10)3.273 (10)
Ca1—O2ix2.626 (9)2.508 (9)2.766 (10)
Ca1—O2x2.956 (10)2.632 (10)3.273 (10)
Ca1—O2xi2.626 (9)2.508 (9)2.766 (10)
Ca1—O2xii2.956 (10)2.632 (10)3.273 (10)
Ca1—O2xiii2.626 (9)2.508 (9)2.766 (10)
Ca1—O2xiv2.956 (10)2.632 (10)3.273 (10)
Ca1—O2xv2.626 (9)2.508 (9)2.766 (10)
Ca1—O52.712 (6)2.693 (6)2.764 (6)
Ca1—O5x2.712 (6)2.693 (6)2.764 (6)
Ca1—O5xii2.712 (6)2.693 (6)2.764 (6)
Ca1—O5xiv2.712 (6)2.693 (6)2.764 (6)
Ca1—Ba1000
Nb1—O31.969 (8)1.961 (8)1.985 (8)
Nb1—O3v1.971 (8)1.959 (8)1.980 (8)
Nb1—O3vii1.972 (8)1.962 (8)1.980 (8)
Nb1—O3xvi1.971 (8)1.955 (8)1.979 (8)
Nb1—O41.831 (10)1.819 (10)1.840 (10)
Nb1—O4xvii2.163 (10)2.161 (10)2.166 (10)
Nb2—O12.003 (8)1.987 (8)2.027 (8)
Nb2—O21.956 (9)1.942 (9)1.978 (9)
Nb2—O2x1.998 (9)1.983 (9)2.027 (9)
Nb2—O31.955 (8)1.944 (8)1.969 (8)
Nb2—O51.841 (9)1.821 (9)1.878 (9)
Nb2—O5xvii2.173 (9)2.137 (9)2.207 (9)
Nb2—Ba13.412 (4)3.401 (4)3.425 (4)
Nb2—Ba1xvii3.387 (4)3.382 (4)3.390 (4)
O1—O22.839 (12)2.792 (12)2.903 (12)
O1—O2vii2.834 (12)2.812 (12)2.893 (12)
O1—O32.858 (11)2.831 (11)2.879 (11)
O1—O3vii2.866 (11)2.827 (11)2.891 (11)
O1—O52.835 (11)2.778 (12)2.934 (11)
O1—O5xvii2.864 (11)2.788 (12)2.990 (11)
O1—O5vii2.820 (11)2.788 (12)2.873 (11)
O1—O5xviii2.889 (11)2.812 (12)2.933 (11)
O1—Ca2xix2.886 (8)2.764 (8)2.979 (8)
O1—Ca2xx2.740 (8)2.686 (8)2.805 (8)
O2—O2xvii3.960 (11)3.324 (11)4.620 (11)
O2—O2ix3.976 (11)3.324 (11)4.620 (11)
O2—O2x2.795 (13)2.739 (13)2.838 (13)
O2—O2xiv2.795 (13)2.739 (13)2.838 (13)
O2—O3xiv2.648 (12)2.607 (12)2.697 (12)
O2—O52.770 (11)2.745 (11)2.812 (12)
O2—O5xvii2.711 (11)2.674 (11)2.753 (11)
O2—O5xiv2.840 (12)2.801 (12)2.883 (12)
O2—O5xxi2.777 (12)2.738 (12)2.841 (12)
O2—Ca2xix3.451 (9)3.360 (9)3.499 (8)
O2—Ca2xx3.201 (9)3.018 (9)3.445 (9)
O2—Ba12.956 (10)2.632 (10)3.273 (10)
O2—Ba1xvii2.627 (9)2.508 (9)2.766 (10)
O3—O3vii2.896 (11)2.838 (11)2.929 (11)
O3—O3xvi2.652 (11)2.650 (11)2.655 (11)
O3—O42.829 (11)2.815 (11)2.856 (11)
O3—O4xvii2.764 (11)2.746 (11)2.791 (11)
O3—O52.859 (11)2.796 (11)2.972 (11)
O3—O5xvii2.833 (11)2.762 (11)2.944 (11)
O3—Ca2v2.971 (7)2.804 (7)3.137 (7)
O3—Ca2xxii2.773 (7)2.681 (8)2.879 (7)
O4—O53.852 (8)3.318 (8)4.327 (8)
O4—O5v3.782 (8)3.309 (8)4.313 (8)
O4—O5vii3.986 (8)3.315 (8)4.309 (8)
O4—O5xvi3.648 (8)3.311 (8)4.330 (8)
O4—Ca23.083 (5)2.864 (5)3.208 (5)
O4—Ca2v2.983 (5)2.877 (5)3.196 (5)
O5—O5x3.804 (9)3.187 (9)4.425 (9)
O5—O5xiv3.804 (9)3.187 (9)4.425 (9)
O5—Ca2xix3.199 (7)2.708 (7)3.661 (7)
O5—Ca2v3.465 (6)2.934 (7)3.942 (6)
O5—Ba12.712 (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) x21/2, x1+1/2, x3, x4, x5; (xvii) x1, x2, x31/2, x4+1/2, x5+1/2; (xviii) x2+1/2, x1+1/2, x31/2, x4+1/2, x5+1/2; (xix) x2+1, x1, x3, x5, x4; (xx) x2+1, x1, x31/2, x5+1/2, x4+1/2; (xxi) x2, x1, x31/2, x5+1/2, x4+1/2; (xxii) x1, x2+1, x31/2, x4+1/2, x5+1/2.
(cbn31) top
Crystal data top
Ba0.693Ca0.307Nb2O6Dx = 5.256 Mg m3
Mr = 389.3Mo Kα radiation, λ = 0.7107 Å
Tetragonal, X4bmCell parameters from 18477 reflections
q1 = 0.294200a* + 0.294200b*; q2 = -0.294200a* + 0.294200b*θ = 3.1–36.8°
a = 12.4608 (5) ŵ = 10.37 mm1
c = 7.9185 (7) ÅT = 293 K
V = 1229.52 (13) Å3'3.08', 3.08
Z = 100.34 × 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.

Data collection top
Xcalibur, Sapphire2, large Be window
diffractometer
2905 independent reflections
Radiation source: Enhance (Mo) X-ray Source2580 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.026
Detector resolution: 8.2495 pixels mm-1θmax = 36.3°, θmin = 2.9°
ω and π scansh = 2020
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 = 1920
Tmin = 0.198, Tmax = 0.556l = 1312
52003 measured reflections
Refinement top
Refinement on FWeighting 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) = 0.047Δρmax = 0.00 e Å3
S = 2.02Δρmin = 0.66 e Å3
2905 reflectionsExtinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
151 parametersExtinction coefficient: 330 (20)
0 restraintsAbsolute structure: 1406 of Friedel pairs used in the refinement
0 constraintsAbsolute structure parameter: 0.47 (3)
Crystal data top
Ba0.693Ca0.307Nb2O6V = 1229.52 (13) Å3
Mr = 389.3Z = 10
Tetragonal, X4bmMo Kα radiation
q1 = 0.294200a* + 0.294200b*; q2 = -0.294200a* + 0.294200b*µ = 10.37 mm1
a = 12.4608 (5) ÅT = 293 K
c = 7.9185 (7) Å0.34 × 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.

Data collection top
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 = 0.556Rint = 0.026
52003 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.047Δρmax = 0.00 e Å3
S = 2.02Δρmin = 0.66 e Å3
2905 reflectionsAbsolute structure: 1406 of Friedel pairs used in the refinement
151 parametersAbsolute structure parameter: 0.47 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba20.172006 (17)0.672006 (17)0.250.01488 (11)0.8542
Ca1000.2575 (6)0.0105 (5)0.5904
Nb100.50.01060 (18)0.00572 (15)
Nb20.07330 (2)0.21001 (2)0.00552 (12)0.00671 (12)
O10.21579 (18)0.28421 (18)0.0103 (9)0.0092 (8)
O20.1391 (2)0.0688 (2)0.0208 (5)0.0215 (9)
O30.00672 (19)0.34339 (18)0.0150 (5)0.0142 (7)
O400.50.2382 (11)0.0179 (12)
O50.07371 (18)0.20251 (19)0.2375 (5)0.0190 (8)
Ca20.172006 (17)0.672006 (17)0.250.01488 (11)0.0882
Ba1000.2575 (6)0.0105 (5)0.028
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba20.01669 (17)0.01669 (17)0.0112 (2)0.00931 (12)0.0004 (2)0.0004 (2)
Ca10.0092 (6)0.0092 (6)0.0132 (11)000
Nb10.0054 (2)0.0054 (2)0.0064 (3)0.0004 (2)00
Nb20.00595 (18)0.00593 (19)0.0082 (2)0.00098 (9)0.0003 (3)0.0018 (3)
O10.0081 (9)0.0081 (9)0.0114 (19)0.0021 (12)0.0016 (16)0.0016 (16)
O20.0220 (15)0.0121 (13)0.0306 (18)0.0105 (11)0.0041 (16)0.0064 (15)
O30.0125 (12)0.0094 (12)0.0208 (14)0.0048 (8)0.0018 (15)0.0007 (15)
O40.0231 (15)0.0231 (15)0.008 (3)0.0018 (18)00
O50.0213 (13)0.0222 (12)0.0135 (17)0.0034 (9)0.0039 (17)0.0004 (17)
Ca20.01669 (17)0.01669 (17)0.0112 (2)0.00931 (12)0.0004 (2)0.0004 (2)
Ba10.0092 (6)0.0092 (6)0.0132 (11)000
Bond lengths (Å) top
AverageMinimumMaximum
Ba2—O1i2.845 (8)2.820 (8)2.895 (8)
Ba2—O1ii2.733 (8)2.714 (8)2.771 (8)
Ba2—O2i3.463 (8)3.367 (8)3.506 (8)
Ba2—O2ii3.236 (8)3.161 (8)3.329 (8)
Ba2—O2iii3.450 (8)3.366 (8)3.504 (8)
Ba2—O2iv3.260 (8)3.188 (8)3.299 (8)
Ba2—O3v2.950 (7)2.833 (7)3.075 (7)
Ba2—O3vi2.787 (7)2.707 (7)2.877 (7)
Ba2—O3vii2.905 (7)2.815 (7)3.092 (7)
Ba2—O3viii2.754 (7)2.690 (7)2.891 (7)
Ba2—O43.071 (5)2.888 (5)3.181 (5)
Ba2—O5i3.257 (6)2.850 (6)3.537 (6)
Ba2—O5v3.361 (6)3.106 (6)3.778 (6)
Ba2—O5vii3.556 (6)3.099 (6)3.786 (6)
Ba2—O5iii3.154 (6)3.076 (6)3.313 (6)
Ba2—Ca2000
Ca1—Nb23.415 (4)3.405 (4)3.426 (4)
Ca1—Nb2ix3.395 (3)3.392 (3)3.402 (3)
Ca1—Nb2x3.415 (4)3.405 (4)3.426 (4)
Ca1—Nb2xi3.395 (3)3.392 (3)3.402 (3)
Ca1—Nb2xii3.415 (4)3.405 (4)3.426 (4)
Ca1—Nb2xiii3.395 (3)3.392 (3)3.402 (3)
Ca1—Nb2xiv3.415 (4)3.405 (4)3.426 (4)
Ca1—Nb2xv3.395 (3)3.392 (3)3.402 (3)
Ca1—O22.947 (9)2.624 (9)3.246 (9)
Ca1—O2ix2.623 (9)2.503 (8)2.757 (9)
Ca1—O2x2.947 (9)2.624 (9)3.246 (9)
Ca1—O2xi2.623 (9)2.503 (8)2.757 (9)
Ca1—O2xii2.947 (9)2.624 (9)3.246 (9)
Ca1—O2xiii2.623 (9)2.503 (8)2.757 (9)
Ca1—O2xiv2.947 (9)2.624 (9)3.246 (9)
Ca1—O2xv2.623 (9)2.503 (8)2.757 (9)
Ca1—O52.694 (5)2.655 (5)2.751 (5)
Ca1—O5x2.694 (5)2.655 (5)2.751 (5)
Ca1—O5xii2.694 (5)2.655 (5)2.751 (5)
Ca1—O5xiv2.694 (5)2.655 (5)2.751 (5)
Ca1—Ba1000
Nb1—O31.970 (7)1.961 (8)1.991 (8)
Nb1—O3v1.972 (7)1.957 (7)1.977 (7)
Nb1—O3vii1.974 (7)1.963 (7)1.985 (7)
Nb1—O3xvi1.971 (7)1.953 (8)1.982 (8)
Nb1—O41.816 (10)1.814 (10)1.817 (10)
Nb1—O4xvii2.168 (10)2.164 (10)2.175 (10)
Nb2—O12.005 (7)1.995 (7)2.020 (7)
Nb2—O21.964 (8)1.950 (8)1.986 (8)
Nb2—O2x2.003 (8)1.985 (8)2.029 (8)
Nb2—O31.952 (8)1.943 (8)1.963 (8)
Nb2—O51.854 (9)1.830 (9)1.897 (9)
Nb2—O5xvii2.147 (9)2.123 (9)2.189 (9)
Nb2—Ba13.415 (4)3.405 (4)3.426 (4)
Nb2—Ba1xvii3.399 (3)3.392 (3)3.402 (3)
O1—O22.849 (11)2.797 (11)2.918 (11)
O1—O2vii2.843 (11)2.819 (11)2.909 (11)
O1—O32.876 (10)2.856 (10)2.905 (10)
O1—O3vii2.877 (10)2.849 (10)2.901 (10)
O1—O52.850 (11)2.794 (11)2.944 (10)
O1—O5xvii2.861 (11)2.785 (11)2.989 (10)
O1—O5vii2.838 (11)2.795 (11)2.892 (10)
O1—O5xviii2.884 (11)2.824 (11)2.916 (11)
O1—Ca2xix2.867 (8)2.758 (8)2.960 (8)
O1—Ca2xx2.740 (8)2.681 (8)2.809 (8)
O2—O2xvii3.939 (10)3.338 (10)4.594 (10)
O2—O2ix3.985 (10)3.338 (10)4.594 (10)
O2—O2x2.774 (11)2.719 (11)2.817 (11)
O2—O2xiv2.774 (11)2.719 (11)2.817 (11)
O2—O3xiv2.661 (11)2.619 (11)2.707 (11)
O2—O52.779 (11)2.757 (11)2.828 (11)
O2—O5xvii2.692 (11)2.660 (11)2.738 (10)
O2—O5xiv2.843 (11)2.809 (11)2.881 (11)
O2—O5xxi2.753 (11)2.712 (11)2.817 (11)
O2—Ca2xix3.469 (8)3.354 (8)3.514 (8)
O2—Ca2xx3.210 (8)3.049 (8)3.445 (8)
O2—Ba12.947 (9)2.624 (9)3.246 (9)
O2—Ba1xvii2.617 (9)2.503 (8)2.757 (9)
O3—O3xvii3.987 (9)3.492 (9)4.428 (9)
O3—O3ix3.933 (9)3.492 (9)4.428 (9)
O3—O3vii2.894 (11)2.849 (11)2.919 (11)
O3—O3xvi2.654 (11)2.636 (11)2.677 (11)
O3—O42.814 (10)2.808 (10)2.825 (10)
O3—O4xvii2.774 (10)2.747 (10)2.813 (11)
O3—O52.858 (10)2.807 (10)2.957 (10)
O3—O5xvii2.835 (10)2.772 (10)2.944 (10)
O3—Ca2v2.950 (7)2.802 (7)3.106 (7)
O3—Ca2xxii2.787 (7)2.678 (7)2.903 (7)
O4—O53.876 (7)3.349 (7)4.319 (7)
O4—O5v3.779 (7)3.330 (7)4.311 (7)
O4—O5vii3.991 (7)3.337 (7)4.306 (7)
O4—O5xvi3.664 (7)3.341 (7)4.323 (7)
O4—Ca23.071 (5)2.888 (5)3.181 (5)
O4—Ca2v2.989 (5)2.897 (5)3.172 (5)
O5—O5x3.781 (8)3.194 (8)4.402 (8)
O5—O5xiv3.781 (8)3.194 (8)4.402 (8)
O5—Ca2xix3.214 (6)2.721 (6)3.667 (6)
O5—Ca2v3.470 (6)2.941 (6)3.939 (6)
O5—Ba12.694 (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) x21/2, x1+1/2, x3, x4, x5; (xvii) x1, x2, x31/2, x4+1/2, x5+1/2; (xviii) x2+1/2, x1+1/2, x31/2, x4+1/2, x5+1/2; (xix) x2+1, x1, x3, x5, x4; (xx) x2+1, x1, x31/2, x5+1/2, x4+1/2; (xxi) x2, x1, x31/2, x5+1/2, x4+1/2; (xxii) x1, x2+1, x31/2, x4+1/2, x5+1/2.

Experimental details

(cbn24ort)(cbn24tet)(cbn31)
Crystal data
Chemical formulaBa0.761Ca0.239Nb2O6Ba0.761Ca0.239Nb2O6Ba0.693Ca0.307Nb2O6
Mr395.9395.9389.3
Crystal system, space groupOrthorhombic, X2mm(00γ)000†Tetragonal, X4bmTetragonal, X4bm§
Temperature (K)293293293
Wave vectorsq = 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, 9090, 90, 9090, 90, 90
V3)2466.95 (14)1228.56 (8)1229.52 (13)
Z201010
Radiation typeMo KαMo KαMo Kα
µ (mm1)10.7510.8310.37
Crystal size (mm)0.40 × 0.34 × 0.040.38 × 0.23 × 0.070.34 × 0.25 × 0.09
Data collection
DiffractometerXcalibur, Sapphire2, large Be window
diffractometer
Xcalibur, Sapphire2, large Be window
diffractometer
Xcalibur, Sapphire2, large Be window
diffractometer
Absorption correctionAnalytical
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, Tmax0.081, 0.6720.11, 0.6540.198, 0.556
No. of measured, independent and
observed [I > 3σ(I)] reflections
20132, 3449, 2633 59030, 2905, 2299 52003, 2905, 2580
Rint0.0300.0380.026
(sin θ/λ)max1)0.7400.9520.834
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 reflections344929052905
No. of parameters212152151
Δρmax, Δρmin (e Å3)1.16, 0.860.00, 0.580.00, 0.66
Absolute structure1605 of Friedel pairs used in the refinement1407 of Friedel pairs used in the refinement1406 of Friedel pairs used in the refinement
Absolute structure parameter0.47 (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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