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Al+3-doped (Y,Ca)Ba2Cu3O7-y (YBCO) whiskers have been synthesized using a solid-state reaction technique. These materials are promising candidates for solid-state THz applications based on sequences of Josephson Junctions (IJJs). Alumina addition was systematically varied and the effect of aluminium incorporation on the structure has been investigated using single-crystal X-ray diffraction. Aluminium only replaces Cu atoms in the O-Cu-O-Cu chains and a gradual transition from orthorhombic to tetragonal space group occurs, thus increasing the Al content. A gradual modification of the coordination sphere of the copper site has also been observed. The Ca2+ ion substitutes mainly the Y3+ ion and also, to a small extent, the Ba2+ ion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520613029351/bp5058sup1.cif
Contains datablocks 1, 2, 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613029351/bp50581sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613029351/bp50582sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520613029351/bp50583sup4.hkl
Contains datablock 3

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520613029351/bp5058sup5.pdf
Figure with the electrical behavior(resistance versus temperature) and critical temperature values of tha analyzed structures

CCDC references: 968425; 968426; 968427

Computing details top

Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) for (2), (3). Cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) for (2), (3). Data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) for (2), (3). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
(1) top
Crystal data top
Ba2Ca0.07Cu3O6.85Y0.93Z = 1
Mr = 660.39F(000) = 291
Orthorhombic, PmmmDx = 6.362 Mg m3
a = 3.8114 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 3.8712 (3) ŵ = 28.11 mm1
c = 11.6824 (7) ÅT = 293 K
V = 172.37 (2) Å30.18 × 0.07 × 0.01 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
Rint = 0.044
Radiation source: fine-focus sealed tubeθmax = 26.3°, θmin = 7.0°
Graphite monochromatorh = 44
1081 measured reflectionsk = 44
234 independent reflectionsl = 1214
220 reflections with I > 2σ(I)
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032 w = 1/[σ2(Fo2) + (0.0609P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.083(Δ/σ)max < 0.001
S = 1.03Δρmax = 1.94 e Å3
234 reflectionsΔρmin = 1.32 e Å3
34 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.007 (2)
Crystal data top
Ba2Ca0.07Cu3O6.85Y0.93V = 172.37 (2) Å3
Mr = 660.39Z = 1
Orthorhombic, PmmmMo Kα radiation
a = 3.8114 (3) ŵ = 28.11 mm1
b = 3.8712 (3) ÅT = 293 K
c = 11.6824 (7) Å0.18 × 0.07 × 0.01 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
220 reflections with I > 2σ(I)
1081 measured reflectionsRint = 0.044
234 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03234 parameters
wR(F2) = 0.0830 restraints
S = 1.03Δρmax = 1.94 e Å3
234 reflectionsΔρmin = 1.32 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.00000.00000.00000.0133 (6)
Cu20.00000.00000.35530 (14)0.0100 (5)
Ba10.50000.50000.18455 (7)0.0137 (5)
Y10.50000.50000.50000.0113 (8)0.935 (9)
Ca10.50000.50000.50000.0113 (8)0.07
O10.00000.00000.1578 (8)0.020 (2)
O20.50000.00000.3778 (8)0.0153 (17)
O30.00000.50000.3777 (8)0.0161 (18)
O40.00000.50000.00000.024 (6)0.85 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0208 (12)0.0145 (11)0.0045 (12)0.0000.0000.000
Cu20.0124 (9)0.0104 (9)0.0072 (9)0.0000.0000.000
Ba10.0186 (6)0.0148 (6)0.0078 (6)0.0000.0000.000
Y10.0153 (11)0.0119 (10)0.0067 (12)0.0000.0000.000
Ca10.0153 (11)0.0119 (10)0.0067 (12)0.0000.0000.000
O10.026 (5)0.023 (4)0.010 (5)0.0000.0000.000
O20.017 (4)0.023 (4)0.007 (4)0.0000.0000.000
O30.027 (4)0.015 (4)0.006 (4)0.0000.0000.000
O40.031 (9)0.007 (8)0.034 (12)0.0000.0000.000
Geometric parameters (Å, º) top
Cu1—O1i1.843 (9)Ba1—O2ix2.974 (7)
Cu1—O11.843 (9)Ba1—O22.974 (7)
Cu1—O4ii1.9356 (2)Ba1—Cu2viii3.3700 (9)
Cu1—O41.9356 (2)Ba1—Cu2ix3.3700 (9)
Cu1—Ba1i3.4680 (5)Y1—O32.382 (6)
Cu1—Ba13.4680 (5)Y1—O3xi2.382 (6)
Cu1—Ba1iii3.4680 (5)Y1—O3x2.382 (6)
Cu1—Ba1iv3.4680 (5)Y1—O3xii2.382 (6)
Cu1—Ba1v3.4680 (5)Y1—O22.405 (5)
Cu1—Ba1vi3.4680 (5)Y1—O2xi2.405 (5)
Cu1—Ba1ii3.4680 (5)Y1—O2xiii2.405 (5)
Cu1—Ba1vii3.4680 (5)Y1—O2ix2.405 (5)
Cu2—O21.9237 (13)Y1—Cu2xi3.1994 (9)
Cu2—O2vi1.9237 (13)Y1—Cu2viii3.1994 (9)
Cu2—O31.9533 (13)Y1—Cu2xiv3.1994 (9)
Cu2—O3ii1.9533 (13)O1—Ba1vii2.7342 (10)
Cu2—O12.307 (9)O1—Ba1vi2.7342 (10)
Cu2—Y13.1994 (9)O1—Ba1ii2.7342 (10)
Cu2—Ca1vii3.1994 (9)O2—Cu2x1.9237 (13)
Cu2—Y1vii3.1994 (9)O2—Ca1ii2.405 (5)
Cu2—Ca1vi3.1994 (9)O2—Y1ii2.405 (5)
Cu2—Ca1ii3.1994 (9)O2—Ba1ii2.974 (7)
Cu2—Y1ii3.1994 (9)O3—Cu2ix1.9533 (13)
Ba1—O12.7342 (10)O3—Ca1vi2.382 (6)
Ba1—O1viii2.7342 (10)O3—Y1vi2.382 (6)
Ba1—O1ix2.7342 (10)O3—Ba1vi2.954 (7)
Ba1—O1x2.7342 (10)O4—Cu1ix1.9356 (2)
Ba1—O42.8775 (6)O4—Ba1iii2.8775 (6)
Ba1—O4x2.8775 (6)O4—Ba1v2.8775 (6)
Ba1—O3x2.954 (7)O4—Ba1vi2.8775 (6)
Ba1—O32.954 (7)
O1i—Cu1—O1180.0O3x—Ba1—O254.55 (11)
O1i—Cu1—O4ii90.0O3—Ba1—O254.55 (11)
O1—Cu1—O4ii90.0O2ix—Ba1—O281.2 (2)
O1i—Cu1—O490.0O1—Ba1—Cu2viii150.27 (19)
O1—Cu1—O490.0O1viii—Ba1—Cu2viii42.86 (19)
O4ii—Cu1—O4180.0O1ix—Ba1—Cu2viii93.16 (11)
O1i—Cu1—Ba1i51.560 (11)O1x—Ba1—Cu2viii94.60 (11)
O1—Cu1—Ba1i128.440 (11)O4—Ba1—Cu2viii144.884 (12)
O4ii—Cu1—Ba1i56.073 (6)O4x—Ba1—Cu2viii93.96 (2)
O4—Cu1—Ba1i123.927 (6)O3x—Ba1—Cu2viii35.208 (17)
O1i—Cu1—Ba1128.440 (11)O3—Ba1—Cu2viii84.99 (10)
O1—Cu1—Ba151.560 (11)O2ix—Ba1—Cu2viii34.594 (16)
O4ii—Cu1—Ba1123.927 (6)O2—Ba1—Cu2viii85.67 (10)
O4—Cu1—Ba156.073 (6)O1—Ba1—Cu2ix94.60 (11)
Ba1i—Cu1—Ba1180.00 (2)O1viii—Ba1—Cu2ix93.16 (11)
O1i—Cu1—Ba1iii51.560 (11)O1ix—Ba1—Cu2ix42.86 (19)
O1—Cu1—Ba1iii128.440 (11)O1x—Ba1—Cu2ix150.27 (19)
O4ii—Cu1—Ba1iii123.927 (6)O4—Ba1—Cu2ix93.96 (2)
O4—Cu1—Ba1iii56.073 (6)O4x—Ba1—Cu2ix144.884 (12)
Ba1i—Cu1—Ba1iii67.854 (12)O3x—Ba1—Cu2ix84.99 (10)
Ba1—Cu1—Ba1iii112.146 (12)O3—Ba1—Cu2ix35.208 (17)
O1i—Cu1—Ba1iv51.560 (11)O2ix—Ba1—Cu2ix34.594 (17)
O1—Cu1—Ba1iv128.440 (11)O2—Ba1—Cu2ix85.67 (10)
O4ii—Cu1—Ba1iv56.073 (6)Cu2viii—Ba1—Cu2ix68.87 (2)
O4—Cu1—Ba1iv123.927 (6)O3—Y1—O3xi180.0000 (10)
Ba1i—Cu1—Ba1iv66.668 (12)O3—Y1—O3x106.3 (4)
Ba1—Cu1—Ba1iv113.332 (12)O3xi—Y1—O3x73.7 (4)
Ba1iii—Cu1—Ba1iv103.12 (2)O3—Y1—O3xii73.7 (4)
O1i—Cu1—Ba1v51.560 (11)O3xi—Y1—O3xii106.3 (4)
O1—Cu1—Ba1v128.440 (11)O3x—Y1—O3xii180.0
O4ii—Cu1—Ba1v123.927 (6)O3—Y1—O269.14 (14)
O4—Cu1—Ba1v56.073 (6)O3xi—Y1—O2110.86 (14)
Ba1i—Cu1—Ba1v103.12 (2)O3x—Y1—O269.14 (14)
Ba1—Cu1—Ba1v76.88 (2)O3xii—Y1—O2110.86 (14)
Ba1iii—Cu1—Ba1v66.668 (12)O3—Y1—O2xi110.86 (14)
Ba1iv—Cu1—Ba1v67.854 (12)O3xi—Y1—O2xi69.14 (14)
O1i—Cu1—Ba1vi128.440 (11)O3x—Y1—O2xi110.86 (14)
O1—Cu1—Ba1vi51.560 (11)O3xii—Y1—O2xi69.14 (14)
O4ii—Cu1—Ba1vi123.927 (6)O2—Y1—O2xi180.0000 (10)
O4—Cu1—Ba1vi56.073 (6)O3—Y1—O2xiii110.86 (14)
Ba1i—Cu1—Ba1vi113.332 (12)O3xi—Y1—O2xiii69.14 (14)
Ba1—Cu1—Ba1vi66.668 (12)O3x—Y1—O2xiii110.86 (14)
Ba1iii—Cu1—Ba1vi76.88 (2)O3xii—Y1—O2xiii69.14 (14)
Ba1iv—Cu1—Ba1vi180.0O2—Y1—O2xiii72.8 (4)
Ba1v—Cu1—Ba1vi112.146 (12)O2xi—Y1—O2xiii107.2 (4)
O1i—Cu1—Ba1ii128.440 (11)O3—Y1—O2ix69.14 (14)
O1—Cu1—Ba1ii51.560 (11)O3xi—Y1—O2ix110.86 (14)
O4ii—Cu1—Ba1ii56.073 (6)O3x—Y1—O2ix69.14 (14)
O4—Cu1—Ba1ii123.927 (6)O3xii—Y1—O2ix110.86 (14)
Ba1i—Cu1—Ba1ii112.146 (12)O2—Y1—O2ix107.2 (4)
Ba1—Cu1—Ba1ii67.854 (12)O2xi—Y1—O2ix72.8 (4)
Ba1iii—Cu1—Ba1ii180.0O2xiii—Y1—O2ix180.0
Ba1iv—Cu1—Ba1ii76.88 (2)O3—Y1—Cu237.48 (2)
Ba1v—Cu1—Ba1ii113.332 (12)O3xi—Y1—Cu2142.52 (2)
Ba1vi—Cu1—Ba1ii103.12 (2)O3x—Y1—Cu299.19 (14)
O1i—Cu1—Ba1vii128.440 (11)O3xii—Y1—Cu280.81 (14)
O1—Cu1—Ba1vii51.560 (11)O2—Y1—Cu236.82 (2)
O4ii—Cu1—Ba1vii56.073 (6)O2xi—Y1—Cu2143.18 (2)
O4—Cu1—Ba1vii123.927 (6)O2xiii—Y1—Cu280.03 (14)
Ba1i—Cu1—Ba1vii76.88 (2)O2ix—Y1—Cu299.97 (14)
Ba1—Cu1—Ba1vii103.12 (2)O3—Y1—Cu2xi142.52 (2)
Ba1iii—Cu1—Ba1vii113.332 (12)O3xi—Y1—Cu2xi37.48 (2)
Ba1iv—Cu1—Ba1vii112.146 (12)O3x—Y1—Cu2xi80.81 (14)
Ba1v—Cu1—Ba1vii180.0O3xii—Y1—Cu2xi99.19 (14)
Ba1vi—Cu1—Ba1vii67.854 (12)O2—Y1—Cu2xi143.18 (2)
Ba1ii—Cu1—Ba1vii66.668 (12)O2xi—Y1—Cu2xi36.82 (2)
O2—Cu2—O2vi164.3 (5)O2xiii—Y1—Cu2xi99.97 (14)
O2—Cu2—O388.95 (6)O2ix—Y1—Cu2xi80.03 (14)
O2vi—Cu2—O388.95 (6)Cu2—Y1—Cu2xi180.0
O2—Cu2—O3ii88.95 (6)O3—Y1—Cu2viii99.19 (14)
O2vi—Cu2—O3ii88.95 (6)O3xi—Y1—Cu2viii80.81 (15)
O3—Cu2—O3ii164.6 (6)O3x—Y1—Cu2viii37.48 (2)
O2—Cu2—O197.8 (3)O3xii—Y1—Cu2viii142.52 (2)
O2vi—Cu2—O197.8 (3)O2—Y1—Cu2viii99.97 (14)
O3—Cu2—O197.7 (3)O2xi—Y1—Cu2viii80.03 (14)
O3ii—Cu2—O197.7 (3)O2xiii—Y1—Cu2viii143.18 (2)
O2—Cu2—Y148.53 (16)O2ix—Y1—Cu2viii36.82 (2)
O2vi—Cu2—Y1121.2 (2)Cu2—Y1—Cu2viii116.21 (5)
O3—Cu2—Y147.90 (16)Cu2xi—Y1—Cu2viii63.79 (5)
O3ii—Cu2—Y1121.9 (2)O3—Y1—Cu2xiv80.81 (14)
O1—Cu2—Y1121.90 (3)O3xi—Y1—Cu2xiv99.19 (15)
O2—Cu2—Ca1vii121.2 (2)O3x—Y1—Cu2xiv142.52 (2)
O2vi—Cu2—Ca1vii48.53 (16)O3xii—Y1—Cu2xiv37.48 (2)
O3—Cu2—Ca1vii121.9 (2)O2—Y1—Cu2xiv80.03 (14)
O3ii—Cu2—Ca1vii47.90 (17)O2xi—Y1—Cu2xiv99.97 (14)
O1—Cu2—Ca1vii121.90 (3)O2xiii—Y1—Cu2xiv36.82 (2)
Y1—Cu2—Ca1vii116.21 (5)O2ix—Y1—Cu2xiv143.18 (2)
O2—Cu2—Y1vii121.2 (2)Cu2—Y1—Cu2xiv63.79 (5)
O2vi—Cu2—Y1vii48.53 (16)Cu2xi—Y1—Cu2xiv116.21 (5)
O3—Cu2—Y1vii121.9 (2)Cu2viii—Y1—Cu2xiv180.0
O3ii—Cu2—Y1vii47.90 (17)Cu1—O1—Cu2180.0
O1—Cu2—Y1vii121.90 (3)Cu1—O1—Ba196.56 (18)
Y1—Cu2—Y1vii116.21 (5)Cu2—O1—Ba183.44 (18)
Ca1vii—Cu2—Y1vii0.0Cu1—O1—Ba1vii96.56 (18)
O2—Cu2—Ca1vi121.2 (2)Cu2—O1—Ba1vii83.44 (18)
O2vi—Cu2—Ca1vi48.53 (16)Ba1—O1—Ba1vii166.9 (4)
O3—Cu2—Ca1vi47.90 (17)Cu1—O1—Ba1vi96.56 (18)
O3ii—Cu2—Ca1vi121.9 (2)Cu2—O1—Ba1vi83.44 (18)
O1—Cu2—Ca1vi121.90 (3)Ba1—O1—Ba1vi88.37 (4)
Y1—Cu2—Ca1vi73.12 (2)Ba1vii—O1—Ba1vi90.13 (4)
Ca1vii—Cu2—Ca1vi74.46 (2)Cu1—O1—Ba1ii96.56 (18)
Y1vii—Cu2—Ca1vi74.46 (2)Cu2—O1—Ba1ii83.44 (18)
O2—Cu2—Ca1ii48.53 (16)Ba1—O1—Ba1ii90.13 (4)
O2vi—Cu2—Ca1ii121.2 (2)Ba1vii—O1—Ba1ii88.37 (4)
O3—Cu2—Ca1ii121.9 (2)Ba1vi—O1—Ba1ii166.9 (4)
O3ii—Cu2—Ca1ii47.90 (17)Cu2—O2—Cu2x164.3 (5)
O1—Cu2—Ca1ii121.90 (3)Cu2—O2—Y194.65 (14)
Y1—Cu2—Ca1ii74.46 (2)Cu2x—O2—Y194.65 (14)
Ca1vii—Cu2—Ca1ii73.12 (2)Cu2—O2—Ca1ii94.65 (14)
Y1vii—Cu2—Ca1ii73.12 (2)Cu2x—O2—Ca1ii94.65 (14)
Ca1vi—Cu2—Ca1ii116.21 (5)Y1—O2—Ca1ii107.2 (4)
O2—Cu2—Y1ii48.53 (16)Cu2—O2—Y1ii94.65 (14)
O2vi—Cu2—Y1ii121.2 (2)Cu2x—O2—Y1ii94.65 (14)
O3—Cu2—Y1ii121.9 (2)Y1—O2—Y1ii107.2 (4)
O3ii—Cu2—Y1ii47.90 (17)Ca1ii—O2—Y1ii0.0
O1—Cu2—Y1ii121.90 (3)Cu2—O2—Ba1ii84.1 (2)
Y1—Cu2—Y1ii74.46 (2)Cu2x—O2—Ba1ii84.1 (2)
Ca1vii—Cu2—Y1ii73.12 (2)Y1—O2—Ba1ii167.0 (3)
Y1vii—Cu2—Y1ii73.12 (2)Ca1ii—O2—Ba1ii85.80 (6)
Ca1vi—Cu2—Y1ii116.21 (5)Y1ii—O2—Ba1ii85.80 (6)
Ca1ii—Cu2—Y1ii0.0Cu2—O2—Ba184.1 (2)
O1—Ba1—O1viii166.9 (4)Cu2x—O2—Ba184.1 (2)
O1—Ba1—O1ix90.13 (4)Y1—O2—Ba185.80 (6)
O1viii—Ba1—O1ix88.37 (4)Ca1ii—O2—Ba1167.0 (3)
O1—Ba1—O1x88.37 (4)Y1ii—O2—Ba1167.0 (3)
O1viii—Ba1—O1x90.13 (4)Ba1ii—O2—Ba181.2 (2)
O1ix—Ba1—O1x166.9 (4)Cu2—O3—Cu2ix164.6 (6)
O1—Ba1—O456.82 (15)Cu2—O3—Y194.62 (15)
O1viii—Ba1—O4112.08 (16)Cu2ix—O3—Y194.62 (15)
O1ix—Ba1—O456.82 (15)Cu2—O3—Ca1vi94.62 (15)
O1x—Ba1—O4112.08 (16)Cu2ix—O3—Ca1vi94.62 (15)
O1—Ba1—O4x112.08 (16)Y1—O3—Ca1vi106.3 (4)
O1viii—Ba1—O4x56.82 (15)Cu2—O3—Y1vi94.62 (15)
O1ix—Ba1—O4x112.08 (16)Cu2ix—O3—Y1vi94.62 (15)
O1x—Ba1—O4x56.82 (15)Y1—O3—Y1vi106.3 (4)
O4—Ba1—O4x82.95 (2)Ca1vi—O3—Y1vi0.0
O1—Ba1—O3x122.48 (17)Cu2—O3—Ba1vi84.1 (2)
O1viii—Ba1—O3x68.76 (18)Cu2ix—O3—Ba1vi84.1 (2)
O1ix—Ba1—O3x122.48 (17)Y1—O3—Ba1vi167.0 (3)
O1x—Ba1—O3x68.76 (18)Ca1vi—O3—Ba1vi86.67 (7)
O4—Ba1—O3x178.71 (12)Y1vi—O3—Ba1vi86.67 (7)
O4x—Ba1—O3x98.35 (12)Cu2—O3—Ba184.1 (2)
O1—Ba1—O368.76 (18)Cu2ix—O3—Ba184.1 (2)
O1viii—Ba1—O3122.48 (17)Y1—O3—Ba186.67 (7)
O1ix—Ba1—O368.76 (18)Ca1vi—O3—Ba1167.0 (3)
O1x—Ba1—O3122.48 (17)Y1vi—O3—Ba1167.0 (3)
O4—Ba1—O398.35 (12)Ba1vi—O3—Ba180.4 (2)
O4x—Ba1—O3178.71 (12)Cu1ix—O4—Cu1180.0
O3x—Ba1—O380.4 (2)Cu1ix—O4—Ba1iii90.0
O1—Ba1—O2ix123.20 (17)Cu1—O4—Ba1iii90.0
O1viii—Ba1—O2ix68.04 (17)Cu1ix—O4—Ba190.0
O1ix—Ba1—O2ix68.04 (17)Cu1—O4—Ba190.0
O1x—Ba1—O2ix123.20 (17)Ba1iii—O4—Ba1180.00 (2)
O4—Ba1—O2ix124.67 (7)Cu1ix—O4—Ba1v90.0
O4x—Ba1—O2ix124.67 (7)Cu1—O4—Ba1v90.0
O3x—Ba1—O2ix54.55 (11)Ba1iii—O4—Ba1v82.95 (2)
O3—Ba1—O2ix54.55 (11)Ba1—O4—Ba1v97.05 (2)
O1—Ba1—O268.04 (17)Cu1ix—O4—Ba1vi90.0
O1viii—Ba1—O2123.20 (17)Cu1—O4—Ba1vi90.0
O1ix—Ba1—O2123.20 (17)Ba1iii—O4—Ba1vi97.05 (2)
O1x—Ba1—O268.04 (17)Ba1—O4—Ba1vi82.95 (2)
O4—Ba1—O2124.67 (7)Ba1v—O4—Ba1vi180.0
O4x—Ba1—O2124.67 (7)
Symmetry codes: (i) x, y, z; (ii) x, y1, z; (iii) x, y+1, z; (iv) x+1, y, z; (v) x+1, y+1, z; (vi) x1, y, z; (vii) x1, y1, z; (viii) x+1, y+1, z; (ix) x, y+1, z; (x) x+1, y, z; (xi) x+1, y+1, z+1; (xii) x, y+1, z+1; (xiii) x+1, y, z+1; (xiv) x, y, z+1.
(2) top
Crystal data top
Al0.06Cu2.94O6Y0.94·0.81(O)·2(Ba)·0.06(Ca)F(000) = 290
Mr = 657.80Dx = 6.285 Mg m3
Orthorhombic, PmmmMo Kα radiation, λ = 0.71073 Å
a = 3.8380 (2) ÅCell parameters from 1360 reflections
b = 3.8735 (2) Åθ = 6.3–30.4°
c = 11.6947 (5) ŵ = 27.77 mm1
V = 173.86 (2) Å3T = 293 K
Z = 10.21 × 0.04 × 0.02 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
353 independent reflections
Radiation source: Enhance (Mo) X-ray Source337 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
Detector resolution: 10.2890 pixels mm-1θmax = 30.5°, θmin = 6.3°
Absorption correction: analytical
?
h = 45
Tmin = 0.326, Tmax = 0.639k = 55
1677 measured reflectionsl = 1616
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.018Secondary atom site location: difference Fourier map
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0361P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max < 0.001
353 reflectionsΔρmax = 0.90 e Å3
34 parametersΔρmin = 0.86 e Å3
Crystal data top
Al0.06Cu2.94O6Y0.94·0.81(O)·2(Ba)·0.06(Ca)V = 173.86 (2) Å3
Mr = 657.80Z = 1
Orthorhombic, PmmmMo Kα radiation
a = 3.8380 (2) ŵ = 27.77 mm1
b = 3.8735 (2) ÅT = 293 K
c = 11.6947 (5) Å0.21 × 0.04 × 0.02 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
353 independent reflections
Absorption correction: analytical
?
337 reflections with I > 2σ(I)
Tmin = 0.326, Tmax = 0.639Rint = 0.026
1677 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01834 parameters
wR(F2) = 0.0510 restraints
S = 1.08Δρmax = 0.90 e Å3
353 reflectionsΔρmin = 0.86 e Å3
Special details top

Experimental. CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20–01-2012 CrysAlis171. NET) (compiled Jan 23 2012,18:06:46) 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)

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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.00000.00000.00000.0113 (3)0.943 (5)
Cu20.00000.00000.35628 (6)0.00776 (17)
Y10.50000.50000.50000.0081 (2)0.935 (4)
Ba10.50000.50000.18585 (3)0.01198 (14)
Ca10.50000.50000.50000.0081 (2)0.06
Al10.00000.00000.35628 (6)0.00776 (17)0.03
O10.00000.00000.1584 (4)0.0212 (8)
O20.50000.00000.3777 (4)0.0098 (6)
O30.00000.50000.3775 (4)0.0106 (7)
O40.00000.50000.00000.017 (3)0.65 (2)
O50.50000.00000.00000.012 (6)*0.16
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0136 (5)0.0126 (5)0.0079 (5)0.0000.0000.000
Cu20.0059 (3)0.0062 (3)0.0112 (4)0.0000.0000.000
Y10.0074 (3)0.0072 (3)0.0097 (4)0.0000.0000.000
Ba10.01263 (19)0.01116 (19)0.0122 (2)0.0000.0000.000
Ca10.0074 (3)0.0072 (3)0.0097 (4)0.0000.0000.000
Al10.0059 (3)0.0062 (3)0.0112 (4)0.0000.0000.000
O10.027 (2)0.0262 (19)0.011 (2)0.0000.0000.000
O20.0065 (12)0.0117 (13)0.0113 (17)0.0000.0000.000
O30.0117 (13)0.0061 (13)0.0141 (19)0.0000.0000.000
O40.027 (4)0.007 (4)0.018 (5)0.0000.0000.000
Geometric parameters (Å, º) top
Cu1—O11.852 (5)Ba1—O1viii2.7453 (5)
Cu1—O1i1.852 (5)Ba1—O1ix2.7453 (5)
Cu1—O5ii1.9190Ba1—O12.7453 (5)
Cu1—O51.9190Ba1—O4iii2.8994 (3)
Cu1—O41.9367Ba1—O4ix2.8994 (3)
Cu1—O4iii1.9367Ba1—O5iii2.9112 (3)
Cu1—Ba1iv3.4868 (2)Ba1—O52.9112 (3)
Cu1—Ba1v3.4868 (2)Ba1—O3ix2.950 (3)
Cu1—Ba1i3.4868 (2)Ba1—O3iii2.950 (3)
Cu1—Ba1vi3.4868 (2)Ba1—O2viii2.964 (3)
Cu1—Ba1vii3.4868 (2)Ba1—O2ix2.964 (3)
Cu1—Ba13.4868 (2)O1—Ba1v2.7453 (5)
Cu2—O2viii1.9352 (6)O1—Ba1ii2.7453 (5)
Cu2—O21.9352 (5)O1—Ba1xiii2.7453 (5)
Cu2—O31.9525 (6)O2—Al1ii1.9352 (5)
Cu2—O3iii1.9525 (6)O2—Cu2ii1.9352 (5)
Cu2—O12.314 (5)O2—Y1iii2.408 (2)
Cu2—Ca1viii3.2029 (4)O2—Ca1iii2.408 (2)
Cu2—Y1viii3.2029 (4)O2—Ba1ii2.964 (3)
Cu2—Ca1iii3.2029 (4)O2—Ba1xiii2.964 (3)
Cu2—Y1iii3.2029 (4)O3—Al1v1.9525 (6)
Cu2—Y13.2029 (4)O3—Cu2v1.9525 (6)
Cu2—Ca1ix3.2029 (4)O3—Ca1viii2.395 (3)
Y1—O3ii2.395 (3)O3—Y1viii2.395 (3)
Y1—O3x2.395 (3)O3—Ba1xiii2.950 (3)
Y1—O32.395 (3)O3—Ba1v2.950 (3)
Y1—O3xi2.395 (3)O4—Cu1v1.9367
Y1—O22.408 (2)O4—Ba1i2.8994 (3)
Y1—O2xi2.408 (2)O4—Ba1v2.8994 (3)
Y1—O2v2.408 (2)O4—Ba1vii2.8994 (3)
Y1—O2xii2.408 (2)O4—Ba1xiii2.8994 (3)
Y1—Cu2ii3.2029 (4)O5—Cu1viii1.9190
Y1—Al1x3.2029 (4)O5—Ba1vi2.9112 (3)
Y1—Al1ii3.2029 (4)O5—Ba1v2.9112 (3)
Y1—Cu2x3.2029 (4)O5—Ba1vii2.9112 (3)
Ba1—O1iii2.7453 (5)
O1—Cu1—O1i180.0O3x—Y1—Cu2x37.434 (9)
O1—Cu1—O5ii90.0O3—Y1—Cu2x80.44 (7)
O1i—Cu1—O5ii90.0O3xi—Y1—Cu2x99.56 (7)
O1—Cu1—O590.0O2—Y1—Cu2x142.956 (9)
O1i—Cu1—O590.0O2xi—Y1—Cu2x37.044 (9)
O5ii—Cu1—O5180.0O2v—Y1—Cu2x79.95 (6)
O1—Cu1—O490.0O2xii—Y1—Cu2x100.05 (6)
O1i—Cu1—O490.0Cu2ii—Y1—Cu2x180.0
O5ii—Cu1—O490.0Al1x—Y1—Cu2x0.00 (2)
O5—Cu1—O490.0Al1ii—Y1—Cu2x180.0
O1—Cu1—O4iii90.0O1iii—Ba1—O1viii166.56 (19)
O1i—Cu1—O4iii90.0O1iii—Ba1—O1ix88.70 (2)
O5ii—Cu1—O4iii90.0O1viii—Ba1—O1ix89.74 (2)
O5—Cu1—O4iii90.0O1iii—Ba1—O189.74 (2)
O4—Cu1—O4iii180.0O1viii—Ba1—O188.70 (2)
O1—Cu1—Ba1iv128.561 (5)O1ix—Ba1—O1166.56 (19)
O1i—Cu1—Ba1iv51.439 (5)O1iii—Ba1—O4iii56.61 (8)
O5ii—Cu1—Ba1iv56.608 (3)O1viii—Ba1—O4iii112.02 (8)
O5—Cu1—Ba1iv123.392 (3)O1ix—Ba1—O4iii112.02 (8)
O4—Cu1—Ba1iv123.742 (3)O1—Ba1—O4iii56.61 (8)
O4iii—Cu1—Ba1iv56.258 (3)O1iii—Ba1—O4ix112.02 (8)
O1—Cu1—Ba1v51.439 (5)O1viii—Ba1—O4ix56.61 (8)
O1i—Cu1—Ba1v128.561 (5)O1ix—Ba1—O4ix56.61 (8)
O5ii—Cu1—Ba1v123.392 (3)O1—Ba1—O4ix112.02 (8)
O5—Cu1—Ba1v56.608 (3)O4iii—Ba1—O4ix82.884 (10)
O4—Cu1—Ba1v56.258 (3)O1iii—Ba1—O5iii56.17 (8)
O4iii—Cu1—Ba1v123.742 (3)O1viii—Ba1—O5iii112.46 (8)
Ba1iv—Cu1—Ba1v180.0O1ix—Ba1—O5iii56.17 (8)
O1—Cu1—Ba1i128.561 (5)O1—Ba1—O5iii112.46 (8)
O1i—Cu1—Ba1i51.439 (5)O4iii—Ba1—O5iii55.967 (6)
O5ii—Cu1—Ba1i56.608 (3)O4ix—Ba1—O5iii55.967 (6)
O5—Cu1—Ba1i123.392 (3)O1iii—Ba1—O5112.46 (8)
O4—Cu1—Ba1i56.258 (3)O1viii—Ba1—O556.17 (8)
O4iii—Cu1—Ba1i123.742 (3)O1ix—Ba1—O5112.46 (8)
Ba1iv—Cu1—Ba1i67.485 (6)O1—Ba1—O556.17 (8)
Ba1v—Cu1—Ba1i112.515 (6)O4iii—Ba1—O555.967 (6)
O1—Cu1—Ba1vi128.561 (5)O4ix—Ba1—O555.967 (6)
O1i—Cu1—Ba1vi51.439 (5)O5iii—Ba1—O583.408 (10)
O5ii—Cu1—Ba1vi123.392 (3)O1iii—Ba1—O3ix122.93 (9)
O5—Cu1—Ba1vi56.608 (3)O1viii—Ba1—O3ix68.54 (9)
O4—Cu1—Ba1vi123.742 (3)O1ix—Ba1—O3ix68.54 (9)
O4iii—Cu1—Ba1vi56.258 (3)O1—Ba1—O3ix122.93 (9)
Ba1iv—Cu1—Ba1vi66.784 (6)O4iii—Ba1—O3ix179.13 (5)
Ba1v—Cu1—Ba1vi113.216 (6)O4ix—Ba1—O3ix97.98 (5)
Ba1i—Cu1—Ba1vi102.878 (10)O5iii—Ba1—O3ix124.55 (3)
O1—Cu1—Ba1vii128.561 (5)O5—Ba1—O3ix124.55 (3)
O1i—Cu1—Ba1vii51.439 (5)O1iii—Ba1—O3iii68.54 (9)
O5ii—Cu1—Ba1vii123.392 (3)O1viii—Ba1—O3iii122.93 (9)
O5—Cu1—Ba1vii56.608 (3)O1ix—Ba1—O3iii122.93 (9)
O4—Cu1—Ba1vii56.258 (3)O1—Ba1—O3iii68.54 (9)
O4iii—Cu1—Ba1vii123.742 (3)O4iii—Ba1—O3iii97.98 (5)
Ba1iv—Cu1—Ba1vii102.878 (10)O4ix—Ba1—O3iii179.13 (5)
Ba1v—Cu1—Ba1vii77.122 (10)O5iii—Ba1—O3iii124.55 (3)
Ba1i—Cu1—Ba1vii66.784 (6)O5—Ba1—O3iii124.55 (3)
Ba1vi—Cu1—Ba1vii67.485 (6)O3ix—Ba1—O3iii81.15 (11)
O1—Cu1—Ba151.439 (5)O1iii—Ba1—O2viii123.34 (8)
O1i—Cu1—Ba1128.561 (5)O1viii—Ba1—O2viii68.13 (9)
O5ii—Cu1—Ba1123.392 (3)O1ix—Ba1—O2viii123.34 (8)
O5—Cu1—Ba156.608 (3)O1—Ba1—O2viii68.13 (9)
O4—Cu1—Ba1123.742 (3)O4iii—Ba1—O2viii124.57 (3)
O4iii—Cu1—Ba156.258 (3)O4ix—Ba1—O2viii124.57 (3)
Ba1iv—Cu1—Ba1112.515 (6)O5iii—Ba1—O2viii179.10 (5)
Ba1v—Cu1—Ba167.485 (6)O5—Ba1—O2viii97.49 (5)
Ba1i—Cu1—Ba1180.0O3ix—Ba1—O2viii54.91 (5)
Ba1vi—Cu1—Ba177.122 (10)O3iii—Ba1—O2viii54.91 (5)
Ba1vii—Cu1—Ba1113.216 (6)O1iii—Ba1—O2ix68.13 (9)
O2viii—Cu2—O2165.2 (2)O1viii—Ba1—O2ix123.34 (8)
O2viii—Cu2—O389.06 (2)O1ix—Ba1—O2ix68.13 (9)
O2—Cu2—O389.06 (2)O1—Ba1—O2ix123.34 (8)
O2viii—Cu2—O3iii89.06 (2)O4iii—Ba1—O2ix124.57 (3)
O2—Cu2—O3iii89.06 (2)O4ix—Ba1—O2ix124.57 (3)
O3—Cu2—O3iii165.4 (3)O5iii—Ba1—O2ix97.49 (5)
O2viii—Cu2—O197.42 (12)O5—Ba1—O2ix179.10 (5)
O2—Cu2—O197.42 (12)O3ix—Ba1—O2ix54.91 (5)
O3—Cu2—O197.29 (13)O3iii—Ba1—O2ix54.91 (5)
O3iii—Cu2—O197.29 (13)O2viii—Ba1—O2ix81.62 (10)
O2viii—Cu2—Ca1viii48.55 (7)Cu1—O1—Cu2180.0
O2—Cu2—Ca1viii121.76 (9)Cu1—O1—Ba1v96.72 (9)
O3—Cu2—Ca1viii48.21 (7)Cu2—O1—Ba1v83.28 (9)
O3iii—Cu2—Ca1viii122.22 (9)Cu1—O1—Ba1ii96.72 (9)
O1—Cu2—Ca1viii121.652 (11)Cu2—O1—Ba1ii83.28 (9)
O2viii—Cu2—Y1viii48.55 (7)Ba1v—O1—Ba1ii166.56 (19)
O2—Cu2—Y1viii121.76 (9)Cu1—O1—Ba196.72 (9)
O3—Cu2—Y1viii48.21 (7)Cu2—O1—Ba183.28 (9)
O3iii—Cu2—Y1viii122.22 (9)Ba1v—O1—Ba189.74 (2)
O1—Cu2—Y1viii121.652 (11)Ba1ii—O1—Ba188.70 (2)
Ca1viii—Cu2—Y1viii0.0Cu1—O1—Ba1xiii96.72 (9)
O2viii—Cu2—Ca1iii121.76 (9)Cu2—O1—Ba1xiii83.28 (9)
O2—Cu2—Ca1iii48.55 (7)Ba1v—O1—Ba1xiii88.70 (2)
O3—Cu2—Ca1iii122.22 (9)Ba1ii—O1—Ba1xiii89.74 (2)
O3iii—Cu2—Ca1iii48.21 (7)Ba1—O1—Ba1xiii166.56 (19)
O1—Cu2—Ca1iii121.652 (11)Al1ii—O2—Cu2ii0.00 (4)
Ca1viii—Cu2—Ca1iii116.70 (2)Al1ii—O2—Cu2165.2 (2)
Y1viii—Cu2—Ca1iii116.70 (2)Cu2ii—O2—Cu2165.2 (2)
O2viii—Cu2—Y1iii121.76 (9)Al1ii—O2—Y194.40 (6)
O2—Cu2—Y1iii48.55 (7)Cu2ii—O2—Y194.40 (6)
O3—Cu2—Y1iii122.22 (9)Cu2—O2—Y194.40 (6)
O3iii—Cu2—Y1iii48.21 (7)Al1ii—O2—Y1iii94.40 (6)
O1—Cu2—Y1iii121.652 (11)Cu2ii—O2—Y1iii94.40 (6)
Ca1viii—Cu2—Y1iii116.70 (2)Cu2—O2—Y1iii94.40 (6)
Y1viii—Cu2—Y1iii116.70 (2)Y1—O2—Y1iii107.09 (16)
Ca1iii—Cu2—Y1iii0.0Al1ii—O2—Ca1iii94.40 (6)
O2viii—Cu2—Y1121.76 (9)Cu2ii—O2—Ca1iii94.40 (6)
O2—Cu2—Y148.55 (7)Cu2—O2—Ca1iii94.40 (6)
O3—Cu2—Y148.21 (7)Y1—O2—Ca1iii107.09 (16)
O3iii—Cu2—Y1122.22 (9)Y1iii—O2—Ca1iii0.0
O1—Cu2—Y1121.652 (11)Al1ii—O2—Ba1ii84.39 (10)
Ca1viii—Cu2—Y173.617 (11)Cu2ii—O2—Ba1ii84.39 (10)
Y1viii—Cu2—Y173.617 (11)Cu2—O2—Ba1ii84.39 (10)
Ca1iii—Cu2—Y174.413 (11)Y1—O2—Ba1ii167.26 (13)
Y1iii—Cu2—Y174.413 (11)Y1iii—O2—Ba1ii85.65 (3)
O2viii—Cu2—Ca1ix48.55 (7)Ca1iii—O2—Ba1ii85.65 (3)
O2—Cu2—Ca1ix121.76 (9)Al1ii—O2—Ba1xiii84.39 (10)
O3—Cu2—Ca1ix122.22 (9)Cu2ii—O2—Ba1xiii84.39 (10)
O3iii—Cu2—Ca1ix48.21 (7)Cu2—O2—Ba1xiii84.39 (10)
O1—Cu2—Ca1ix121.652 (11)Y1—O2—Ba1xiii85.65 (3)
Ca1viii—Cu2—Ca1ix74.413 (11)Y1iii—O2—Ba1xiii167.26 (13)
Y1viii—Cu2—Ca1ix74.413 (11)Ca1iii—O2—Ba1xiii167.26 (13)
Ca1iii—Cu2—Ca1ix73.617 (11)Ba1ii—O2—Ba1xiii81.62 (10)
Y1iii—Cu2—Ca1ix73.617 (11)Cu2—O3—Al1v165.4 (3)
Y1—Cu2—Ca1ix116.70 (2)Cu2—O3—Cu2v165.4 (3)
O3ii—Y1—O3x180.00 (16)Al1v—O3—Cu2v0.00 (4)
O3ii—Y1—O3106.50 (16)Cu2—O3—Ca1viii94.35 (7)
O3x—Y1—O373.50 (16)Al1v—O3—Ca1viii94.35 (7)
O3ii—Y1—O3xi73.50 (16)Cu2v—O3—Ca1viii94.35 (7)
O3x—Y1—O3xi106.50 (16)Cu2—O3—Y1viii94.35 (7)
O3—Y1—O3xi180.0Al1v—O3—Y1viii94.35 (7)
O3ii—Y1—O269.17 (6)Cu2v—O3—Y1viii94.35 (7)
O3x—Y1—O2110.83 (6)Ca1viii—O3—Y1viii0.0
O3—Y1—O269.17 (6)Cu2—O3—Y194.35 (7)
O3xi—Y1—O2110.83 (6)Al1v—O3—Y194.35 (7)
O3ii—Y1—O2xi110.83 (6)Cu2v—O3—Y194.35 (7)
O3x—Y1—O2xi69.17 (6)Ca1viii—O3—Y1106.50 (16)
O3—Y1—O2xi110.83 (6)Y1viii—O3—Y1106.50 (16)
O3xi—Y1—O2xi69.17 (6)Cu2—O3—Ba1xiii84.47 (10)
O2—Y1—O2xi180.00 (16)Al1v—O3—Ba1xiii84.47 (10)
O3ii—Y1—O2v69.17 (6)Cu2v—O3—Ba1xiii84.47 (10)
O3x—Y1—O2v110.83 (6)Ca1viii—O3—Ba1xiii167.33 (14)
O3—Y1—O2v69.17 (6)Y1viii—O3—Ba1xiii167.33 (14)
O3xi—Y1—O2v110.83 (6)Y1—O3—Ba1xiii86.18 (3)
O2—Y1—O2v107.09 (16)Cu2—O3—Ba1v84.47 (10)
O2xi—Y1—O2v72.91 (16)Al1v—O3—Ba1v84.47 (10)
O3ii—Y1—O2xii110.83 (6)Cu2v—O3—Ba1v84.47 (10)
O3x—Y1—O2xii69.17 (6)Ca1viii—O3—Ba1v86.18 (3)
O3—Y1—O2xii110.83 (6)Y1viii—O3—Ba1v86.18 (3)
O3xi—Y1—O2xii69.17 (6)Y1—O3—Ba1v167.33 (14)
O2—Y1—O2xii72.91 (16)Ba1xiii—O3—Ba1v81.15 (11)
O2xi—Y1—O2xii107.09 (16)Cu1v—O4—Cu1180.0
O2v—Y1—O2xii180.0Cu1v—O4—Ba1i90.0
O3ii—Y1—Cu2ii37.434 (10)Cu1—O4—Ba1i90.0
O3x—Y1—Cu2ii142.566 (9)Cu1v—O4—Ba1v90.0
O3—Y1—Cu2ii99.56 (7)Cu1—O4—Ba1v90.0
O3xi—Y1—Cu2ii80.44 (7)Ba1i—O4—Ba1v180.000 (9)
O2—Y1—Cu2ii37.044 (9)Cu1v—O4—Ba1vii90.0
O2xi—Y1—Cu2ii142.956 (9)Cu1—O4—Ba1vii90.0
O2v—Y1—Cu2ii100.05 (6)Ba1i—O4—Ba1vii82.884 (10)
O2xii—Y1—Cu2ii79.95 (6)Ba1v—O4—Ba1vii97.116 (10)
O3ii—Y1—Al1x142.566 (10)Cu1v—O4—Ba1xiii90.0
O3x—Y1—Al1x37.434 (9)Cu1—O4—Ba1xiii90.0
O3—Y1—Al1x80.44 (7)Ba1i—O4—Ba1xiii97.116 (10)
O3xi—Y1—Al1x99.56 (7)Ba1v—O4—Ba1xiii82.884 (10)
O2—Y1—Al1x142.956 (9)Ba1vii—O4—Ba1xiii180.0
O2xi—Y1—Al1x37.044 (9)Cu1viii—O5—Cu1180.0
O2v—Y1—Al1x79.95 (6)Cu1viii—O5—Ba1vi90.0
O2xii—Y1—Al1x100.05 (6)Cu1—O5—Ba1vi90.0
Cu2ii—Y1—Al1x180.0Cu1viii—O5—Ba1v90.0
O3ii—Y1—Al1ii37.434 (10)Cu1—O5—Ba1v90.0
O3x—Y1—Al1ii142.566 (9)Ba1vi—O5—Ba1v180.000 (9)
O3—Y1—Al1ii99.56 (7)Cu1viii—O5—Ba1vii90.0
O3xi—Y1—Al1ii80.44 (7)Cu1—O5—Ba1vii90.0
O2—Y1—Al1ii37.044 (9)Ba1vi—O5—Ba1vii83.408 (10)
O2xi—Y1—Al1ii142.956 (9)Ba1v—O5—Ba1vii96.592 (10)
O2v—Y1—Al1ii100.05 (6)Cu1viii—O5—Ba190.0
O2xii—Y1—Al1ii79.95 (6)Cu1—O5—Ba190.0
Cu2ii—Y1—Al1ii0.0Ba1vi—O5—Ba196.592 (10)
Al1x—Y1—Al1ii180.0Ba1v—O5—Ba183.408 (10)
O3ii—Y1—Cu2x142.566 (10)Ba1vii—O5—Ba1180.000 (9)
Symmetry codes: (i) x, y, z; (ii) x1, y, z; (iii) x, y1, z; (iv) x, y1, z; (v) x, y+1, z; (vi) x+1, y1, z; (vii) x+1, y, z; (viii) x+1, y, z; (ix) x+1, y1, z; (x) x, y+1, z+1; (xi) x1, y+1, z+1; (xii) x1, y, z+1; (xiii) x1, y+1, z.
(3) top
Crystal data top
Cu2O5.92Y0.88·0.84(O)·1.93(Ba)·0.69(Cu)·2.12(Ca0.04)Dx = 6.119 Mg m3
Mr = 639.18Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/mmmCell parameters from 2189 reflections
a = 3.8595 (2) Åθ = 6.3–32.7°
c = 11.6456 (8) ŵ = 26.38 mm1
V = 173.47 (2) Å3T = 293 K
Z = 10.24 × 0.04 × 0.02 mm
F(000) = 282.7
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
244 independent reflections
Radiation source: fine-focus sealed tube228 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
Detector resolution: 10.2890 pixels mm-1θmax = 32.8°, θmin = 6.3°
Absorption correction: analytical
CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) 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)
h = 55
Tmin = 0.304, Tmax = 0.642k = 55
3659 measured reflectionsl = 1617
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.016Secondary atom site location: difference Fourier map
wR(F2) = 0.039 w = 1/[σ2(Fo2) + (0.015P)2 + 0.187P]
where P = (Fo2 + 2Fc2)/3
S = 1.38(Δ/σ)max < 0.001
233 reflectionsΔρmax = 0.95 e Å3
26 parametersΔρmin = 1.19 e Å3
Crystal data top
Cu2O5.92Y0.88·0.84(O)·1.93(Ba)·0.69(Cu)·2.12(Ca0.04)Z = 1
Mr = 639.18Mo Kα radiation
Tetragonal, P4/mmmµ = 26.38 mm1
a = 3.8595 (2) ÅT = 293 K
c = 11.6456 (8) Å0.24 × 0.04 × 0.02 mm
V = 173.47 (2) Å3
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
244 independent reflections
Absorption correction: analytical
CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) 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)
228 reflections with I > 2σ(I)
Tmin = 0.304, Tmax = 0.642Rint = 0.040
3659 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01626 parameters
wR(F2) = 0.0390 restraints
S = 1.38Δρmax = 0.95 e Å3
233 reflectionsΔρmin = 1.19 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Y10.00000.00000.50000.0086 (3)0.884 (6)
Ca10.00000.00000.50000.0086 (3)0.12
Cu20.50000.50000.35723 (6)0.0088 (2)
Cu10.50000.50000.00000.0172 (5)0.695 (6)
Al10.50000.50000.00000.0172 (5)0.31
Ba10.00000.00000.18690 (3)0.01424 (13)0.964 (4)
Ca20.00000.00000.18690 (3)0.01424 (13)0.04
O10.50000.50000.1560 (5)0.032 (2)0.96 (3)
O20.50000.00000.00000.020 (3)0.42 (2)
O30.00000.50000.3767 (3)0.0123 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.0071 (3)0.0071 (3)0.0115 (4)0.0000.0000.000
Ca10.0071 (3)0.0071 (3)0.0115 (4)0.0000.0000.000
Cu20.0061 (3)0.0061 (3)0.0142 (4)0.0000.0000.000
Cu10.0207 (6)0.0207 (6)0.0102 (6)0.0000.0000.000
Al10.0207 (6)0.0207 (6)0.0102 (6)0.0000.0000.000
Ba10.01422 (15)0.01422 (15)0.0143 (2)0.0000.0000.000
Ca20.01422 (15)0.01422 (15)0.0143 (2)0.0000.0000.000
O10.038 (3)0.038 (3)0.020 (3)0.0000.0000.000
O20.035 (7)0.011 (5)0.015 (5)0.0000.0000.000
O30.0059 (12)0.0121 (13)0.0188 (13)0.0000.0000.000
Geometric parameters (Å, º) top
Y1—O3i2.4053 (19)Ba1—O1xvi2.7526 (8)
Y1—O3ii2.4053 (19)Ba1—O1xiii2.7526 (8)
Y1—O3iii2.4053 (19)Ba1—O1xvii2.7526 (8)
Y1—O3iv2.4053 (19)Ba1—O1xviii2.7526 (8)
Y1—O3v2.4053 (19)Ba1—O2xix2.9088 (3)
Y1—O32.4053 (19)Ba1—O2x2.9088 (3)
Y1—O3vi2.4053 (19)Ba1—O2i2.9088 (3)
Y1—O3vii2.4053 (19)Ba1—O22.9088 (3)
Y1—Cu2viii3.1956 (4)Ba1—O32.934 (2)
Y1—Cu2ix3.1956 (4)Ba1—O3iii2.934 (2)
Y1—Cu2x3.1956 (4)Ba1—O3i2.934 (2)
Y1—Cu2ii3.1956 (4)Ba1—O3ii2.934 (2)
Cu2—O3xi1.9430 (4)O1—Cu2xiii2.343 (6)
Cu2—O3xii1.9430 (4)O1—Ca2xvi2.7526 (8)
Cu2—O31.9430 (4)O1—Ba1xvi2.7526 (8)
Cu2—O3iii1.9430 (4)O1—Ca2xiii2.7526 (8)
Cu2—O1xiii2.343 (6)O1—Ba1xiii2.7526 (8)
Cu2—Ca1xiv3.1956 (4)O1—Ba1xvii2.7526 (8)
Cu2—Y1xiv3.1956 (4)O1—Ba1xviii2.7526 (8)
Cu2—Y1xv3.1956 (4)O1—Ca2xviii2.7526 (8)
Cu2—Ca1xv3.1956 (4)O1—Ca2xvii2.7526 (8)
Cu2—Y1xii3.1956 (4)O2—Al1ii1.9297
Cu1—O11.817 (6)O2—Cu1ii1.9297
Cu1—O1xiii1.817 (6)O2—Ca2xvi2.9088 (3)
Cu1—O2iii1.9297O2—Ba1xvi2.9088 (3)
Cu1—O2i1.9297O2—Ca2xviii2.9088 (3)
Cu1—O21.9297O2—Ba1xviii2.9088 (3)
Cu1—O2xv1.9297O2—Ba1xii2.9088 (3)
Cu1—Ca2xvi3.4907 (3)O2—Ca2xii2.9088 (3)
Cu1—Ba1xvi3.4907 (3)O3—Cu2x1.9430 (4)
Cu1—Ba1xiv3.4907 (3)O3—Ca1xv2.4053 (19)
Cu1—Ca2xiv3.4907 (3)O3—Y1xv2.4053 (19)
Cu1—Ca2xvii3.4907 (3)O3—Ca2xv2.934 (2)
Cu1—Ca2xviii3.4907 (3)O3—Ba1xv2.934 (2)
O3i—Y1—O3ii69.12 (6)Ca2xvii—Cu1—Ca2xviii102.851 (10)
O3i—Y1—O3iii106.70 (12)O1xvi—Ba1—O1xiii165.0 (2)
O3ii—Y1—O3iii69.12 (6)O1xvi—Ba1—O1xvii89.02 (3)
O3i—Y1—O3iv180.00 (12)O1xiii—Ba1—O1xvii89.02 (3)
O3ii—Y1—O3iv110.88 (6)O1xvi—Ba1—O1xviii89.02 (3)
O3iii—Y1—O3iv73.30 (12)O1xiii—Ba1—O1xviii89.02 (3)
O3i—Y1—O3v110.88 (6)O1xvii—Ba1—O1xviii165.0 (2)
O3ii—Y1—O3v180.00 (12)O1xvi—Ba1—O2xix55.75 (10)
O3iii—Y1—O3v110.88 (6)O1xiii—Ba1—O2xix111.56 (10)
O3iv—Y1—O3v69.12 (6)O1xvii—Ba1—O2xix111.56 (10)
O3i—Y1—O369.12 (6)O1xviii—Ba1—O2xix55.75 (10)
O3ii—Y1—O3106.70 (12)O1xvi—Ba1—O2x55.75 (10)
O3iii—Y1—O369.12 (6)O1xiii—Ba1—O2x111.56 (10)
O3iv—Y1—O3110.88 (6)O1xvii—Ba1—O2x55.75 (10)
O3v—Y1—O373.30 (12)O1xviii—Ba1—O2x111.56 (10)
O3i—Y1—O3vi73.30 (12)O2xix—Ba1—O2x55.951 (6)
O3ii—Y1—O3vi110.88 (6)O1xvi—Ba1—O2i111.56 (10)
O3iii—Y1—O3vi180.0O1xiii—Ba1—O2i55.75 (10)
O3iv—Y1—O3vi106.70 (12)O1xvii—Ba1—O2i55.75 (10)
O3v—Y1—O3vi69.12 (6)O1xviii—Ba1—O2i111.56 (10)
O3—Y1—O3vi110.88 (6)O2xix—Ba1—O2i83.120 (10)
O3i—Y1—O3vii110.88 (6)O2x—Ba1—O2i55.951 (6)
O3ii—Y1—O3vii73.30 (12)O1xvi—Ba1—O2111.56 (10)
O3iii—Y1—O3vii110.88 (6)O1xiii—Ba1—O255.75 (10)
O3iv—Y1—O3vii69.12 (6)O1xvii—Ba1—O2111.56 (10)
O3v—Y1—O3vii106.70 (12)O1xviii—Ba1—O255.75 (10)
O3—Y1—O3vii180.0O2xix—Ba1—O255.951 (6)
O3vi—Y1—O3vii69.12 (6)O2x—Ba1—O283.120 (10)
O3i—Y1—Cu2viii37.340 (7)O2i—Ba1—O255.951 (6)
O3ii—Y1—Cu2viii37.340 (7)O1xvi—Ba1—O3124.01 (10)
O3iii—Y1—Cu2viii100.01 (5)O1xiii—Ba1—O368.73 (11)
O3iv—Y1—Cu2viii142.660 (7)O1xvii—Ba1—O368.73 (11)
O3v—Y1—Cu2viii142.660 (7)O1xviii—Ba1—O3124.01 (10)
O3—Y1—Cu2viii100.01 (5)O2xix—Ba1—O3179.56 (4)
O3vi—Y1—Cu2viii79.99 (5)O2x—Ba1—O3124.31 (2)
O3vii—Y1—Cu2viii79.99 (5)O2i—Ba1—O397.32 (4)
O3i—Y1—Cu2ix142.660 (7)O2—Ba1—O3124.31 (2)
O3ii—Y1—Cu2ix142.660 (7)O1xvi—Ba1—O3iii124.01 (10)
O3iii—Y1—Cu2ix79.99 (5)O1xiii—Ba1—O3iii68.73 (11)
O3iv—Y1—Cu2ix37.340 (7)O1xvii—Ba1—O3iii124.01 (10)
O3v—Y1—Cu2ix37.340 (7)O1xviii—Ba1—O3iii68.73 (11)
O3—Y1—Cu2ix79.99 (5)O2xix—Ba1—O3iii124.31 (2)
O3vi—Y1—Cu2ix100.01 (5)O2x—Ba1—O3iii179.56 (4)
O3vii—Y1—Cu2ix100.01 (5)O2i—Ba1—O3iii124.31 (2)
Cu2viii—Y1—Cu2ix180.00 (2)O2—Ba1—O3iii97.32 (4)
O3i—Y1—Cu2x37.340 (7)O3—Ba1—O3iii55.43 (5)
O3ii—Y1—Cu2x100.01 (5)O1xvi—Ba1—O3i68.73 (11)
O3iii—Y1—Cu2x100.01 (5)O1xiii—Ba1—O3i124.01 (10)
O3iv—Y1—Cu2x142.660 (7)O1xvii—Ba1—O3i68.73 (11)
O3v—Y1—Cu2x79.99 (5)O1xviii—Ba1—O3i124.01 (10)
O3—Y1—Cu2x37.340 (7)O2xix—Ba1—O3i124.31 (2)
O3vi—Y1—Cu2x79.99 (5)O2x—Ba1—O3i97.32 (4)
O3vii—Y1—Cu2x142.660 (7)O2i—Ba1—O3i124.31 (2)
Cu2viii—Y1—Cu2x74.295 (10)O2—Ba1—O3i179.56 (4)
Cu2ix—Y1—Cu2x105.705 (10)O3—Ba1—O3i55.43 (5)
O3i—Y1—Cu2ii100.01 (5)O3iii—Ba1—O3i82.24 (8)
O3ii—Y1—Cu2ii37.340 (7)O1xvi—Ba1—O3ii68.73 (11)
O3iii—Y1—Cu2ii37.340 (7)O1xiii—Ba1—O3ii124.01 (10)
O3iv—Y1—Cu2ii79.99 (5)O1xvii—Ba1—O3ii124.01 (10)
O3v—Y1—Cu2ii142.660 (7)O1xviii—Ba1—O3ii68.73 (11)
O3—Y1—Cu2ii100.01 (5)O2xix—Ba1—O3ii97.32 (4)
O3vi—Y1—Cu2ii142.660 (7)O2x—Ba1—O3ii124.31 (2)
O3vii—Y1—Cu2ii79.99 (5)O2i—Ba1—O3ii179.56 (4)
Cu2viii—Y1—Cu2ii74.295 (10)O2—Ba1—O3ii124.31 (2)
Cu2ix—Y1—Cu2ii105.705 (10)O3—Ba1—O3ii82.24 (8)
Cu2x—Y1—Cu2ii117.30 (2)O3iii—Ba1—O3ii55.43 (5)
O3xi—Cu2—O3xii89.22 (2)O3i—Ba1—O3ii55.43 (5)
O3xi—Cu2—O389.22 (2)Cu1—O1—Cu2xiii180.0
O3xii—Cu2—O3166.60 (19)Cu1—O1—Ca2xvi97.50 (12)
O3xi—Cu2—O3iii166.60 (19)Cu2xiii—O1—Ca2xvi82.50 (12)
O3xii—Cu2—O3iii89.22 (2)Cu1—O1—Ba1xvi97.50 (12)
O3—Cu2—O3iii89.22 (2)Cu2xiii—O1—Ba1xvi82.50 (12)
O3xi—Cu2—O1xiii96.70 (9)Ca2xvi—O1—Ba1xvi0.000 (14)
O3xii—Cu2—O1xiii96.70 (9)Cu1—O1—Ca2xiii97.50 (12)
O3—Cu2—O1xiii96.70 (9)Cu2xiii—O1—Ca2xiii82.50 (12)
O3iii—Cu2—O1xiii96.70 (9)Ca2xvi—O1—Ca2xiii165.0 (2)
O3xi—Cu2—Ca1xiv48.66 (5)Ba1xvi—O1—Ca2xiii165.0 (2)
O3xii—Cu2—Ca1xiv48.66 (5)Cu1—O1—Ba1xiii97.50 (12)
O3—Cu2—Ca1xiv122.62 (7)Cu2xiii—O1—Ba1xiii82.50 (12)
O3iii—Cu2—Ca1xiv122.62 (7)Ca2xvi—O1—Ba1xiii165.0 (2)
O1xiii—Cu2—Ca1xiv121.351 (11)Ba1xvi—O1—Ba1xiii165.0 (2)
O3xi—Cu2—Y1xiv48.66 (5)Ca2xiii—O1—Ba1xiii0.000 (14)
O3xii—Cu2—Y1xiv48.66 (5)Cu1—O1—Ba1xvii97.50 (12)
O3—Cu2—Y1xiv122.62 (7)Cu2xiii—O1—Ba1xvii82.50 (12)
O3iii—Cu2—Y1xiv122.62 (7)Ca2xvi—O1—Ba1xvii89.02 (3)
O1xiii—Cu2—Y1xiv121.351 (11)Ba1xvi—O1—Ba1xvii89.02 (3)
Ca1xiv—Cu2—Y1xiv0.0Ca2xiii—O1—Ba1xvii89.02 (3)
O3xi—Cu2—Y1122.62 (7)Ba1xiii—O1—Ba1xvii89.02 (3)
O3xii—Cu2—Y1122.62 (7)Cu1—O1—Ba1xviii97.50 (12)
O3—Cu2—Y148.66 (5)Cu2xiii—O1—Ba1xviii82.50 (12)
O3iii—Cu2—Y148.66 (5)Ca2xvi—O1—Ba1xviii89.02 (3)
O1xiii—Cu2—Y1121.351 (11)Ba1xvi—O1—Ba1xviii89.02 (3)
Ca1xiv—Cu2—Y1117.30 (2)Ca2xiii—O1—Ba1xviii89.02 (3)
Y1xiv—Cu2—Y1117.30 (2)Ba1xiii—O1—Ba1xviii89.02 (3)
O3xi—Cu2—Y1xv48.66 (6)Ba1xvii—O1—Ba1xviii165.0 (2)
O3xii—Cu2—Y1xv122.62 (7)Cu1—O1—Ca2xviii97.50 (12)
O3—Cu2—Y1xv48.66 (5)Cu2xiii—O1—Ca2xviii82.50 (12)
O3iii—Cu2—Y1xv122.62 (7)Ca2xvi—O1—Ca2xviii89.02 (3)
O1xiii—Cu2—Y1xv121.351 (11)Ba1xvi—O1—Ca2xviii89.02 (3)
Ca1xiv—Cu2—Y1xv74.295 (10)Ca2xiii—O1—Ca2xviii89.02 (3)
Y1xiv—Cu2—Y1xv74.295 (10)Ba1xiii—O1—Ca2xviii89.02 (3)
Y1—Cu2—Y1xv74.295 (10)Ba1xvii—O1—Ca2xviii165.0 (2)
O3xi—Cu2—Ca1xv48.66 (6)Ba1xviii—O1—Ca2xviii0.000 (14)
O3xii—Cu2—Ca1xv122.62 (7)Cu1—O1—Ca2xvii97.50 (12)
O3—Cu2—Ca1xv48.66 (5)Cu2xiii—O1—Ca2xvii82.50 (12)
O3iii—Cu2—Ca1xv122.62 (7)Ca2xvi—O1—Ca2xvii89.02 (3)
O1xiii—Cu2—Ca1xv121.351 (11)Ba1xvi—O1—Ca2xvii89.02 (3)
Ca1xiv—Cu2—Ca1xv74.295 (10)Ca2xiii—O1—Ca2xvii89.02 (3)
Y1xiv—Cu2—Ca1xv74.295 (10)Ba1xiii—O1—Ca2xvii89.02 (3)
Y1—Cu2—Ca1xv74.295 (10)Ba1xvii—O1—Ca2xvii0.000 (14)
Y1xv—Cu2—Ca1xv0.0Ba1xviii—O1—Ca2xvii165.0 (2)
O3xi—Cu2—Y1xii122.62 (7)Ca2xviii—O1—Ca2xvii165.0 (2)
O3xii—Cu2—Y1xii48.66 (5)Al1ii—O2—Cu1180.0
O3—Cu2—Y1xii122.62 (7)Al1ii—O2—Cu1ii0.0
O3iii—Cu2—Y1xii48.66 (5)Cu1—O2—Cu1ii180.0
O1xiii—Cu2—Y1xii121.351 (11)Al1ii—O2—Ca2xvi90.0
Ca1xiv—Cu2—Y1xii74.295 (10)Cu1—O2—Ca2xvi90.0
Y1xiv—Cu2—Y1xii74.295 (10)Cu1ii—O2—Ca2xvi90.0
Y1—Cu2—Y1xii74.295 (10)Al1ii—O2—Ba1xvi90.0
Y1xv—Cu2—Y1xii117.30 (2)Cu1—O2—Ba1xvi90.0
Ca1xv—Cu2—Y1xii117.30 (2)Cu1ii—O2—Ba1xvi90.0
O1—Cu1—O1xiii180.0Ca2xvi—O2—Ba1xvi0.000 (9)
O1—Cu1—O2iii90.0Al1ii—O2—Ca2xviii90.0
O1xiii—Cu1—O2iii90.0Cu1—O2—Ca2xviii90.0
O1—Cu1—O2i90.0Cu1ii—O2—Ca2xviii90.0
O1xiii—Cu1—O2i90.0Ca2xvi—O2—Ca2xviii83.120 (10)
O2iii—Cu1—O2i180.0Ba1xvi—O2—Ca2xviii83.120 (10)
O1—Cu1—O290.0Al1ii—O2—Ba1xviii90.0
O1xiii—Cu1—O290.0Cu1—O2—Ba1xviii90.0
O2iii—Cu1—O290.0Cu1ii—O2—Ba1xviii90.0
O2i—Cu1—O290.0Ca2xvi—O2—Ba1xviii83.120 (10)
O1—Cu1—O2xv90.0Ba1xvi—O2—Ba1xviii83.120 (10)
O1xiii—Cu1—O2xv90.0Ca2xviii—O2—Ba1xviii0.0
O2iii—Cu1—O2xv90.0Al1ii—O2—Ba1xii90.0
O2i—Cu1—O2xv90.0Cu1—O2—Ba1xii90.0
O2—Cu1—O2xv180.0Cu1ii—O2—Ba1xii90.0
O1—Cu1—Ca2xvi51.426 (5)Ca2xvi—O2—Ba1xii180.0
O1xiii—Cu1—Ca2xvi128.574 (5)Ba1xvi—O2—Ba1xii180.0
O2iii—Cu1—Ca2xvi123.560 (3)Ca2xviii—O2—Ba1xii96.880 (10)
O2i—Cu1—Ca2xvi56.440 (3)Ba1xviii—O2—Ba1xii96.880 (10)
O2—Cu1—Ca2xvi56.440 (3)Al1ii—O2—Ca2xii90.0
O2xv—Cu1—Ca2xvi123.560 (3)Cu1—O2—Ca2xii90.0
O1—Cu1—Ba1xvi51.426 (5)Cu1ii—O2—Ca2xii90.0
O1xiii—Cu1—Ba1xvi128.574 (5)Ca2xvi—O2—Ca2xii180.0
O2iii—Cu1—Ba1xvi123.560 (3)Ba1xvi—O2—Ca2xii180.0
O2i—Cu1—Ba1xvi56.440 (3)Ca2xviii—O2—Ca2xii96.880 (10)
O2—Cu1—Ba1xvi56.440 (3)Ba1xviii—O2—Ca2xii96.880 (10)
O2xv—Cu1—Ba1xvi123.560 (3)Ba1xii—O2—Ca2xii0.000 (9)
Ca2xvi—Cu1—Ba1xvi0.000 (9)Al1ii—O2—Ba190.0
O1—Cu1—Ba1xiv128.574 (5)Cu1—O2—Ba190.0
O1xiii—Cu1—Ba1xiv51.426 (5)Cu1ii—O2—Ba190.0
O2iii—Cu1—Ba1xiv56.440 (3)Ca2xvi—O2—Ba196.880 (10)
O2i—Cu1—Ba1xiv123.560 (3)Ba1xvi—O2—Ba196.880 (10)
O2—Cu1—Ba1xiv123.560 (3)Ca2xviii—O2—Ba1180.000 (9)
O2xv—Cu1—Ba1xiv56.440 (3)Ba1xviii—O2—Ba1180.000 (9)
Ca2xvi—Cu1—Ba1xiv180.000 (9)Ba1xii—O2—Ba183.120 (10)
Ba1xvi—Cu1—Ba1xiv180.000 (9)Ca2xii—O2—Ba183.120 (10)
O1—Cu1—Ca2xiv128.574 (5)Cu2x—O3—Cu2166.60 (19)
O1xiii—Cu1—Ca2xiv51.426 (5)Cu2x—O3—Ca1xv93.99 (5)
O2iii—Cu1—Ca2xiv56.440 (3)Cu2—O3—Ca1xv93.99 (5)
O2i—Cu1—Ca2xiv123.560 (3)Cu2x—O3—Y1xv93.99 (5)
O2—Cu1—Ca2xiv123.560 (3)Cu2—O3—Y1xv93.99 (5)
O2xv—Cu1—Ca2xiv56.440 (3)Ca1xv—O3—Y1xv0.0
Ca2xvi—Cu1—Ca2xiv180.000 (9)Cu2x—O3—Y193.99 (5)
Ba1xvi—Cu1—Ca2xiv180.000 (9)Cu2—O3—Y193.99 (5)
Ba1xiv—Cu1—Ca2xiv0.000 (9)Ca1xv—O3—Y1106.70 (12)
O1—Cu1—Ca2xvii51.426 (5)Y1xv—O3—Y1106.70 (12)
O1xiii—Cu1—Ca2xvii128.574 (5)Cu2x—O3—Ba184.96 (7)
O2iii—Cu1—Ca2xvii123.560 (3)Cu2—O3—Ba184.96 (7)
O2i—Cu1—Ca2xvii56.440 (3)Ca1xv—O3—Ba1167.77 (10)
O2—Cu1—Ca2xvii123.560 (3)Y1xv—O3—Ba1167.77 (10)
O2xv—Cu1—Ca2xvii56.440 (3)Y1—O3—Ba185.53 (2)
Ca2xvi—Cu1—Ca2xvii67.121 (5)Cu2x—O3—Ca2xv84.96 (7)
Ba1xvi—Cu1—Ca2xvii67.121 (5)Cu2—O3—Ca2xv84.96 (7)
Ba1xiv—Cu1—Ca2xvii112.879 (5)Ca1xv—O3—Ca2xv85.53 (2)
Ca2xiv—Cu1—Ca2xvii112.879 (5)Y1xv—O3—Ca2xv85.53 (2)
O1—Cu1—Ca2xviii51.426 (5)Y1—O3—Ca2xv167.77 (10)
O1xiii—Cu1—Ca2xviii128.574 (5)Ba1—O3—Ca2xv82.24 (8)
O2iii—Cu1—Ca2xviii56.440 (3)Cu2x—O3—Ba1xv84.96 (7)
O2i—Cu1—Ca2xviii123.560 (3)Cu2—O3—Ba1xv84.96 (7)
O2—Cu1—Ca2xviii56.440 (3)Ca1xv—O3—Ba1xv85.53 (2)
O2xv—Cu1—Ca2xviii123.560 (3)Y1xv—O3—Ba1xv85.53 (2)
Ca2xvi—Cu1—Ca2xviii67.121 (5)Y1—O3—Ba1xv167.77 (10)
Ba1xvi—Cu1—Ca2xviii67.121 (5)Ba1—O3—Ba1xv82.24 (8)
Ba1xiv—Cu1—Ca2xviii112.879 (5)Ca2xv—O3—Ba1xv0.000 (9)
Ca2xiv—Cu1—Ca2xviii112.879 (5)
Symmetry codes: (i) y, x, z; (ii) x, y1, z; (iii) y+1, x, z; (iv) y, x, z+1; (v) x, y+1, z+1; (vi) y1, x, z+1; (vii) x, y, z+1; (viii) x1, y1, z; (ix) x+1, y+1, z+1; (x) x1, y, z; (xi) y+1, x+1, z; (xii) x+1, y, z; (xiii) x+1, y+1, z; (xiv) x+1, y+1, z; (xv) x, y+1, z; (xvi) x, y, z; (xvii) x, y+1, z; (xviii) x+1, y, z; (xix) y, x1, z.

Experimental details

(1)(2)(3)
Crystal data
Chemical formulaBa2Ca0.07Cu3O6.85Y0.93Al0.06Cu2.94O6Y0.94·0.81(O)·2(Ba)·0.06(Ca)Cu2O5.92Y0.88·0.84(O)·1.93(Ba)·0.69(Cu)·2.12(Ca0.04)
Mr660.39657.80639.18
Crystal system, space groupOrthorhombic, PmmmOrthorhombic, PmmmTetragonal, P4/mmm
Temperature (K)293293293
a, b, c (Å)3.8114 (3), 3.8712 (3), 11.6824 (7)3.8380 (2), 3.8735 (2), 11.6947 (5)3.8595 (2), 3.8595 (2), 11.6456 (8)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 90
V3)172.37 (2)173.86 (2)173.47 (2)
Z111
Radiation typeMo KαMo KαMo Kα
µ (mm1)28.1127.7726.38
Crystal size (mm)0.18 × 0.07 × 0.010.21 × 0.04 × 0.020.24 × 0.04 × 0.02
Data collection
DiffractometerXcalibur, Ruby, Gemini ultra
diffractometer
Xcalibur, Ruby, Gemini ultra
diffractometer
Xcalibur, Ruby, Gemini ultra
diffractometer
Absorption correctionAnalyticalAnalytical
CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) 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, Tmax0.326, 0.6390.304, 0.642
No. of measured, independent and
observed [I > 2σ(I)] reflections
1081, 234, 220 1677, 353, 337 3659, 244, 228
Rint0.0440.0260.040
(sin θ/λ)max1)0.6240.7140.761
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.083, 1.03 0.018, 0.051, 1.08 0.016, 0.039, 1.38
No. of reflections234353233
No. of parameters343426
Δρmax, Δρmin (e Å3)1.94, 1.320.90, 0.860.95, 1.19

Computer programs: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).

 

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