The structure of heptabismuth tritantalum octadecaoxide, Bi7Ta3O18, has been solved and refined using single-crystal X-ray diffraction data collected at a synchrotron source in conjunction with unit-cell and symmetry information derived from electron diffraction. The space-group symmetry is triclinic C1 but is very close to monoclinic C2/m. A twin component observed during data collection was successfully modelled in the refinement. The C2/m prototype fitted all the Rietveld-refinable features of a medium-resolution neutron powder diffraction pattern. The metal-atom array is approximately face-centred cubic (fluorite type), punctuated by regularly spaced displacement faults perpendicular to the [111]fluorite direction every 2.5 fluorite unit cells. The metal-atom populations and O-atom positions are fully ordered. The Ta5+ cations are octahedrally coordinated, with TaO6 octahedra forming columns. The remaining O atoms occupy distorted fluorite positions. The Bi3+ cations occupy octahedral, square pyramidal or trigonal prismatic sites within the O-atom array; strain in the latter coordination environment appears to be responsible for the lowering of symmetry from monoclinic to triclinic.
Supporting information
| Crystallographic Information File (CIF) Contains datablocks xtl, global, pow |
| Rietveld powder data file (CIF format) Contains datablock pow |
| Structure factor file (SHELXL table format) Supplementary material |
Data reduction: Xtal DIFDAT SORTRF ADDREF ABSORB for xtl. Program(s) used to solve structure: Xtal for xtl. Program(s) used to refine structure: Xtal LSLS for xtl; GSAS for pow. Molecular graphics: Xtal for xtl. Software used to prepare material for publication: Xtal CIFIO for xtl.
(xtl) bismuth tantalum oxide
top
Crystal data top
Bi7O18Ta3 | Z = 4 |
Mr = 2293.71 | F(000) = 3776 |
Triclinic, C1 | Dx = 9.4 Mg m−3 |
Hall symbol: C 1 | Synchrotron radiation, λ = 0.9580 (4) Å |
a = 34.005 (3) Å | Cell parameters from 25 reflections |
b = 7.6024 (4) Å | θ = 22.8–38.0° |
c = 6.6358 (5) Å | µ = 85.4 mm−1 |
α = 90.086 (6)° | T = 293 K |
β = 109.127 (6)° | Plate, yellow |
γ = 90.043 (6)° | 0.02 × 0.02 × 0.002 mm |
V = 1620.8 (2) Å3 | |
Data collection top
Tsukuba diffractometer | Rint = 0.023 |
Radiation source: synchrotron | θmax = 50°, θmin = 1.7° |
Si monochromator | h = −54→54 |
Absorption correction: gaussian ? | k = −12→12 |
Tmin = 0.277, Tmax = 0.844 | l = −10→10 |
0.176040+05 measured reflections | 6 standard reflections every 200 reflections |
0.137980+05 independent reflections | intensity decay: none |
0.117960+05 reflections with refl observed if F2 > 3.000 σ(F2) | |
Refinement top
Refinement on F2 | 1 constraint |
Least-squares matrix: Full matrix | w = 1/σ2 |
R[F2 > 2σ(F2)] = 0.039 | (Δ/σ)max = 0.001 |
wR(F2) = 0.0337 | Δρmax = 5.80 e Å−3 |
0.117960+05 reflections | Δρmin = −5.61 e Å−3 |
327 parameters | Extinction correction: Zachariasen (1968), Eq22 p292 "Cryst. Comp." Munksgaard 1970 |
0 restraints | Extinction coefficient: 1828 (30) |
Crystal data top
Bi7O18Ta3 | γ = 90.043 (6)° |
Mr = 2293.71 | V = 1620.8 (2) Å3 |
Triclinic, C1 | Z = 4 |
a = 34.005 (3) Å | Synchrotron radiation, λ = 0.9580 (4) Å |
b = 7.6024 (4) Å | µ = 85.4 mm−1 |
c = 6.6358 (5) Å | T = 293 K |
α = 90.086 (6)° | 0.02 × 0.02 × 0.002 mm |
β = 109.127 (6)° | |
Data collection top
Tsukuba diffractometer | 0.117960+05 reflections with refl observed if F2 > 3.000 σ(F2) |
Absorption correction: gaussian ? | Rint = 0.023 |
Tmin = 0.277, Tmax = 0.844 | 6 standard reflections every 200 reflections |
0.176040+05 measured reflections | intensity decay: none |
0.137980+05 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.0337 | Δρmax = 5.80 e Å−3 |
0.117960+05 reflections | Δρmin = −5.61 e Å−3 |
327 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Bi1 | 0.34035 (3) | 0.23954 (9) | 0.48808 (13) | 0.0175 (4) | |
Bi2 | 0.338481 (19) | −0.49941 (8) | −0.03295 (9) | 0.0077 (3) | |
Bi3 | 0.352745 (18) | 0.00191 (8) | 0.00818 (8) | 0.0078 (3) | |
Ta4 | 0.439500 (19) | 0.25362 (8) | −0.02517 (10) | 0.0053 (2) | |
Bi5 | 0.13920 (2) | 0.25045 (8) | 0.42381 (9) | 0.0084 (3) | |
Ta6 | 0.44073 (2) | −0.24841 (8) | −0.01788 (10) | 0.0052 (3) | |
Bi7 | 0.145987 (18) | −0.49905 (7) | −0.03491 (8) | 0.0074 (3) | |
Ta8 | 0.25045 (2) | −0.25148 (9) | 0.00335 (10) | 0.0055 (2) | |
Bi9 | 0.13846 (2) | −0.25211 (8) | 0.42799 (10) | 0.0106 (3) | |
Bi10 | 0.35341 (2) | −0.25195 (9) | −0.49329 (11) | 0.0149 (4) | |
Bi11 | 0.44582 (2) | 0.01013 (9) | −0.47120 (9) | 0.0108 (3) | |
Ta12 | 0.051995 (18) | −0.25145 (7) | −0.03194 (9) | 0.0052 (3) | |
Bi13 | 0.249612 (19) | −0.00439 (8) | −0.47642 (9) | 0.0076 (3) | |
Bi14 | 0.05081 (2) | 0.00216 (9) | −0.50979 (10) | 0.0095 (3) | |
Ta15 | 0.24956 (2) | 0.25148 (9) | −0.00335 (11) | 0.0059 (2) | |
Bi16 | 0.246719 (19) | −0.49654 (9) | 0.46346 (9) | 0.0090 (3) | |
Bi17 | 0.045577 (19) | −0.49984 (8) | 0.42758 (9) | 0.0097 (3) | |
Ta18 | 0.052326 (18) | 0.25109 (7) | −0.03323 (9) | 0.0049 (3) | |
Bi19 | 0.158172 (19) | −0.00140 (8) | −0.00700 (8) | 0.0088 (3) | |
Bi20 | 0.44170 (2) | −0.50124 (8) | 0.46484 (9) | 0.0079 (3) | |
O1 | 0.4279 (3) | 0.0028 (12) | −0.1082 (13) | 0.0066 (14)* | |
O2 | 0.3787 (3) | −0.2898 (13) | −0.1112 (15) | 0.0104 (16)* | |
O3 | 0.1165 (3) | −0.2130 (12) | 0.0673 (14) | 0.0084 (15)* | |
O4 | 0.3789 (3) | 0.2971 (13) | −0.1083 (15) | 0.0117 (17)* | |
O5 | 0.1162 (3) | 0.2103 (11) | 0.0686 (13) | 0.0053 (14)* | |
O6 | 0.0674 (3) | 0.2152 (12) | 0.2988 (14) | 0.0068 (15)* | |
O7 | 0.4455 (3) | 0.2042 (13) | 0.2681 (15) | 0.0127 (17)* | |
O8 | 0.4476 (3) | −0.1953 (13) | 0.2686 (16) | 0.0137 (18)* | |
O9 | 0.4247 (3) | −0.2881 (12) | −0.3500 (14) | 0.0096 (16)* | |
O10 | 0.4971 (3) | −0.2166 (12) | −0.0312 (14) | 0.0087 (15)* | |
O11 | 0.2356 (3) | 0.0006 (13) | −0.0646 (15) | 0.0124 (16)* | |
O12 | 0.3814 (3) | −0.0066 (13) | 0.4020 (14) | 0.0095 (15)* | |
O13 | 0.2581 (3) | −0.2062 (13) | 0.3109 (15) | 0.0129 (17)* | |
O14 | 0.4506 (3) | −0.4968 (13) | 0.0500 (15) | 0.0119 (17)* | |
O15 | 0.2662 (3) | 0.2029 (11) | 0.3241 (13) | 0.0085 (14)* | |
O16 | 0.1632 (3) | −0.4978 (13) | 0.3090 (14) | 0.0100 (15)* | |
O17 | 0.3246 (3) | 0.0028 (14) | −0.3502 (15) | 0.0146 (17)* | |
O18 | 0.0456 (3) | −0.0030 (13) | −0.1058 (14) | 0.0110 (16)* | |
O19 | 0.3779 (3) | −0.4902 (14) | 0.3089 (15) | 0.0144 (17)* | |
O20 | 0.1917 (3) | 0.2938 (12) | −0.0200 (14) | 0.0117 (16)* | |
O21 | 0.1131 (3) | 0.0024 (14) | −0.3657 (15) | 0.0144 (17)* | |
O22 | 0.1907 (3) | −0.2977 (14) | −0.0463 (16) | 0.0158 (18)* | |
O23 | 0.0671 (3) | −0.5002 (13) | 0.0475 (13) | 0.0083 (15)* | |
O24 | 0.1805 (3) | 0.0085 (14) | 0.3466 (16) | 0.0142 (18)* | |
O25 | 0.1098 (3) | −0.4942 (14) | −0.4592 (16) | 0.0136 (17)* | |
O26 | 0.0476 (3) | 0.2990 (12) | −0.3211 (14) | 0.0094 (16)* | |
O27 | 0.0687 (3) | −0.2092 (13) | 0.2996 (15) | 0.0106 (16)* | |
O28 | 0.2646 (3) | −0.4973 (12) | 0.0867 (14) | 0.0105 (15)* | |
O29 | 0.4278 (3) | 0.2940 (13) | −0.3478 (15) | 0.0107 (16)* | |
O30 | 0.0448 (3) | −0.2963 (14) | −0.3225 (16) | 0.0148 (18)* | |
O31 | 0.3110 (3) | 0.2065 (13) | 0.0623 (15) | 0.0151 (18)* | |
O32 | 0.3111 (3) | −0.1971 (14) | 0.0691 (17) | 0.019 (2)* | |
O33 | 0.2428 (3) | 0.3012 (15) | −0.2909 (17) | 0.022 (2)* | |
O34 | 0.3141 (3) | −0.5071 (14) | −0.4091 (16) | 0.0153 (18)* | |
O35 | 0.2463 (3) | −0.3006 (14) | −0.2943 (17) | 0.019 (2)* | |
O36 | 0.4982 (3) | 0.2185 (13) | −0.0190 (14) | 0.0095 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Bi1 | 0.0304 (4) | 0.0088 (3) | 0.0224 (3) | 0.0040 (3) | 0.0180 (3) | 0.0028 (2) |
Bi2 | 0.0076 (2) | 0.0086 (2) | 0.0075 (2) | −0.0001 (2) | 0.00230 (19) | −0.0002 (2) |
Bi3 | 0.0068 (2) | 0.0082 (2) | 0.0083 (2) | 0.0004 (2) | 0.00184 (18) | −0.0001 (2) |
Ta4 | 0.0058 (2) | 0.0051 (2) | 0.0056 (2) | −0.00038 (16) | 0.00254 (16) | −0.00041 (15) |
Bi5 | 0.0111 (2) | 0.0093 (2) | 0.0085 (2) | −0.00057 (19) | 0.00229 (18) | −0.00022 (18) |
Ta6 | 0.0058 (2) | 0.0053 (2) | 0.0059 (2) | 0.00013 (16) | 0.00278 (16) | 0.00015 (15) |
Bi7 | 0.0073 (2) | 0.0080 (2) | 0.0074 (2) | −0.0010 (2) | 0.0023 (2) | −0.0004 (2) |
Ta8 | 0.0069 (2) | 0.00494 (17) | 0.0064 (2) | −0.00009 (16) | 0.00363 (18) | −0.00013 (16) |
Bi9 | 0.0107 (2) | 0.0099 (3) | 0.0100 (2) | −0.0000 (2) | 0.0031 (2) | 0.0000 (2) |
Bi10 | 0.0180 (3) | 0.0112 (3) | 0.0174 (3) | −0.0040 (3) | 0.0070 (3) | −0.0006 (2) |
Bi11 | 0.0073 (2) | 0.0139 (3) | 0.0099 (2) | 0.0003 (2) | 0.0017 (2) | 0.0002 (2) |
Ta12 | 0.0047 (2) | 0.0049 (2) | 0.0059 (2) | −0.00043 (17) | 0.00177 (17) | −0.00029 (16) |
Bi13 | 0.0071 (2) | 0.0086 (2) | 0.0071 (2) | 0.0006 (2) | 0.00201 (18) | −0.00056 (19) |
Bi14 | 0.0075 (2) | 0.0119 (3) | 0.0098 (2) | −0.0001 (2) | 0.00397 (18) | −0.0000 (2) |
Ta15 | 0.0073 (2) | 0.00481 (16) | 0.0070 (2) | −0.00018 (15) | 0.00411 (17) | 0.00023 (15) |
Bi16 | 0.0077 (3) | 0.0103 (2) | 0.0076 (2) | 0.0001 (2) | 0.0013 (2) | −0.0005 (2) |
Bi17 | 0.0081 (2) | 0.0118 (3) | 0.0094 (2) | −0.0001 (2) | 0.00276 (19) | −0.0003 (2) |
Ta18 | 0.0054 (2) | 0.0049 (2) | 0.0060 (2) | −0.00068 (17) | 0.00248 (17) | −0.00049 (16) |
Bi19 | 0.0085 (2) | 0.0101 (2) | 0.0069 (2) | −0.0005 (2) | 0.00247 (19) | −0.0000 (2) |
Bi20 | 0.0064 (2) | 0.0103 (2) | 0.0082 (2) | −0.0003 (2) | 0.00202 (19) | 0.0004 (2) |
Geometric parameters (Å, º) top
Bi1—O17i | 2.249 (11) | Bi11—O12v | 2.075 (9) |
Bi1—O34ii | 2.317 (11) | Bi11—O7v | 2.273 (11) |
Bi1—O15 | 2.413 (8) | Bi11—O8v | 2.341 (11) |
Bi2—O19 | 2.225 (9) | Bi11—O29 | 2.456 (10) |
Bi2—O4iii | 2.234 (11) | Ta12—O36vi | 1.873 (10) |
Bi2—O2 | 2.268 (11) | Ta12—O30 | 1.893 (11) |
Bi2—O34 | 2.359 (10) | Ta12—O18 | 1.947 (10) |
Bi3—O32 | 2.198 (12) | Ta12—O23 | 1.986 (9) |
Bi3—O31 | 2.213 (11) | Ta12—O3 | 2.092 (9) |
Bi3—O17 | 2.254 (9) | Ta12—O27 | 2.108 (10) |
Ta4—O7 | 1.927 (10) | Bi13—O13v | 2.166 (10) |
Ta4—O14iv | 1.966 (10) | Bi13—O15v | 2.247 (9) |
Ta4—O4 | 1.978 (10) | Bi13—O24v | 2.259 (10) |
Ta4—O1 | 1.987 (9) | Bi13—O17 | 2.409 (10) |
Ta4—O36 | 2.001 (10) | Bi14—O21 | 2.018 (9) |
Ta4—O29 | 2.069 (10) | Bi14—O6v | 2.243 (10) |
Bi5—O5 | 2.247 (8) | Bi14—O27v | 2.247 (10) |
Bi5—O16iv | 2.306 (10) | Ta15—O33 | 1.885 (12) |
Bi5—O6 | 2.322 (9) | Ta15—O20 | 1.962 (10) |
Bi5—O25ii | 2.424 (11) | Ta15—O11 | 1.975 (10) |
Ta6—O8 | 1.881 (11) | Ta15—O28iv | 2.015 (9) |
Ta6—O14 | 1.946 (10) | Ta15—O31 | 2.020 (10) |
Ta6—O10 | 1.962 (10) | Ta15—O15 | 2.092 (9) |
Ta6—O1 | 2.008 (9) | Bi16—O34i | 2.169 (10) |
Ta6—O2 | 2.019 (10) | Bi16—O35i | 2.193 (11) |
Ta6—O9 | 2.111 (9) | Bi16—O33vii | 2.277 (12) |
Bi7—O16 | 2.162 (9) | Bi17—O25i | 2.064 (10) |
Bi7—O22 | 2.174 (11) | Bi17—O26vii | 2.249 (10) |
Bi7—O20iii | 2.192 (10) | Bi17—O30i | 2.273 (11) |
Ta8—O28 | 1.965 (9) | Ta18—O10viii | 1.899 (10) |
Ta8—O35 | 1.969 (11) | Ta18—O26 | 1.900 (10) |
Ta8—O22 | 1.981 (11) | Ta18—O23iv | 1.984 (9) |
Ta8—O11 | 1.996 (10) | Ta18—O18 | 1.985 (10) |
Ta8—O13 | 2.000 (10) | Ta18—O5 | 2.077 (9) |
Ta8—O32 | 2.006 (11) | Ta18—O6 | 2.110 (9) |
Bi9—O27 | 2.268 (9) | Bi19—O24 | 2.218 (10) |
Bi9—O3 | 2.282 (9) | Bi19—O3 | 2.302 (10) |
Bi9—O16 | 2.292 (10) | Bi19—O5 | 2.313 (9) |
Bi9—O25i | 2.319 (11) | Bi19—O21 | 2.372 (9) |
Bi10—O12v | 2.303 (10) | Bi20—O19 | 2.078 (9) |
Bi10—O9 | 2.314 (9) | Bi20—O29vii | 2.141 (10) |
Bi10—O2 | 2.414 (9) | Bi20—O9i | 2.220 (10) |
| | | |
O17i—Bi1—O34ii | 110.5 (4) | O33—Ta15—O20 | 97.1 (4) |
O17i—Bi1—O15 | 75.3 (3) | O33—Ta15—O11 | 92.6 (4) |
O34ii—Bi1—O15 | 77.4 (3) | O33—Ta15—O28iv | 92.5 (4) |
O19—Bi2—O4iii | 92.3 (4) | O33—Ta15—O31 | 91.5 (5) |
O19iii—Bi2—O2 | 90.4 (4) | O33—Ta15—O15 | 171.7 (4) |
O19iii—Bi2—O34 | 164.7 (4) | O20—Ta15—O11 | 88.8 (4) |
O4iii—Bi2—O2 | 88.5 (4) | O20—Ta15—O28iv | 90.7 (4) |
O4iii—Bi2—O34 | 77.0 (4) | O20—Ta15—O31 | 171.3 (4) |
O2—Bi2—O34 | 78.6 (4) | O20—Ta15—O15 | 90.7 (4) |
O32—Bi3—O31 | 88.2 (4) | O11—Ta15—O28iv | 174.9 (4) |
O32—Bi3—O17 | 97.0 (4) | O11—Ta15—O31 | 92.4 (4) |
O31—Bi3—O17 | 95.4 (4) | O11—Ta15—O15 | 90.4 (4) |
O7iv—Ta4—O14 | 89.1 (4) | O28iv—Ta15—O31 | 87.3 (4) |
O7—Ta4—O4 | 94.0 (4) | O28iv—Ta15—O15 | 84.5 (3) |
O7—Ta4—O1 | 92.2 (4) | O31—Ta15—O15 | 80.6 (4) |
O7—Ta4—O36 | 100.3 (4) | O34i—Bi16—O35i | 90.0 (4) |
O7—Ta4—O29 | 174.6 (4) | O34i—Bi16—O33vii | 89.8 (4) |
O14iv—Ta4—O4 | 90.2 (4) | O35i—Bi16—O33vii | 85.3 (4) |
O14iv—Ta4—O1 | 178.7 (4) | O25i—Bi17—O26vii | 88.4 (4) |
O14iv—Ta4—O36 | 91.0 (4) | O25i—Bi17—O30i | 89.1 (4) |
O14iv—Ta4—O29 | 94.2 (4) | O26vii—Bi17—O30i | 85.8 (4) |
O4—Ta4—O1 | 89.5 (4) | O10viii—Ta18—O26 | 103.0 (4) |
O4—Ta4—O36 | 165.6 (4) | O10viii—Ta18—O23iv | 92.2 (4) |
O4—Ta4—O29 | 81.7 (4) | O10viii—Ta18—O18 | 95.3 (4) |
O1—Ta4—O36 | 89.0 (4) | O10viii—Ta18—O5 | 161.6 (4) |
O1—Ta4—O29 | 84.4 (4) | O10viii—Ta18—O6 | 85.0 (4) |
O36—Ta4—O29 | 83.9 (4) | O26—Ta18—O23iv | 91.0 (4) |
O5—Bi5—O16iv | 78.7 (3) | O26—Ta18—O18 | 88.8 (4) |
O5—Bi5—O6 | 69.3 (3) | O26—Ta18—O5 | 95.2 (4) |
O5—Bi5—O25ii | 113.9 (3) | O26—Ta18—O6 | 170.7 (4) |
O16iv—Bi5—O6 | 114.9 (3) | O23iv—Ta18—O18 | 172.4 (4) |
O16iv—Bi5—O25ii | 70.7 (4) | O23iv—Ta18—O5 | 84.8 (3) |
O6—Bi5—O25ii | 73.2 (3) | O23iv—Ta18—O6 | 83.7 (3) |
O8—Ta6—O14 | 91.0 (4) | O18—Ta18—O5 | 87.6 (4) |
O8—Ta6—O10 | 102.7 (4) | O18—Ta18—O6 | 95.4 (4) |
O8—Ta6—O1 | 92.4 (4) | O5—Ta18—O6 | 76.7 (4) |
O8—Ta6—O2 | 96.5 (4) | O24—Bi19—O3 | 79.5 (4) |
O8—Ta6—O9 | 171.6 (4) | O24—Bi19—O5 | 76.7 (3) |
O14—Ta6—O10 | 91.9 (4) | O24—Bi19—O21 | 161.1 (4) |
O14—Ta6—O1 | 176.0 (3) | O3—Bi19—O5 | 88.4 (3) |
O14—Ta6—O2 | 90.2 (4) | O3—Bi19—O21 | 89.1 (3) |
O14—Ta6—O9 | 94.1 (4) | O5—Bi19—O21 | 88.1 (3) |
O10—Ta6—O1 | 89.4 (4) | O19—Bi20—O29vii | 85.7 (4) |
O10—Ta6—O2 | 160.6 (4) | O19—Bi20—O9i | 80.0 (4) |
O10—Ta6—O9 | 83.8 (4) | O29vii—Bi20—O9i | 93.6 (4) |
O1—Ta6—O2 | 87.3 (4) | Ta4—O1—Ta6 | 145.7 (4) |
O1—Ta6—O9 | 82.3 (4) | Ta6—O2—Bi2 | 133.3 (4) |
O2—Ta6—O9 | 76.8 (4) | Ta6—O2—Bi10 | 106.2 (5) |
O16—Bi7—O22 | 94.8 (4) | Bi2—O2—Bi10 | 107.0 (3) |
O16—Bi7—O20iii | 90.7 (3) | Ta12—O3—Bi9 | 105.1 (5) |
O22—Bi7—O20iii | 90.8 (4) | Ta12—O3—Bi19 | 133.2 (4) |
O28—Ta8—O35 | 91.9 (4) | Bi9—O3—Bi19 | 107.7 (3) |
O28—Ta8—O22 | 91.3 (4) | Ta4—O4—Bi2iv | 135.7 (5) |
O28—Ta8—O11 | 176.6 (4) | Ta18—O5—Bi5 | 106.8 (4) |
O28—Ta8—O13 | 86.4 (4) | Ta18—O5—Bi19 | 133.5 (4) |
O28—Ta8—O32 | 89.7 (4) | Bi5—O5—Bi19 | 107.1 (3) |
O35—Ta8—O22 | 93.9 (4) | Ta18—O6—Bi14i | 131.7 (4) |
O35—Ta8—O11 | 91.4 (4) | Ta18—O6—Bi5 | 103.0 (4) |
O35—Ta8—O13 | 176.7 (4) | Bi14i—O6—Bi5 | 108.1 (3) |
O35—Ta8—O32 | 89.3 (5) | Ta4—O7—Bi11i | 150.4 (5) |
O22—Ta8—O11 | 87.9 (4) | Ta6—O8—Bi11i | 149.6 (5) |
O22—Ta8—O13 | 89.1 (4) | Ta6—O9—Bi20v | 131.0 (4) |
O22—Ta8—O32 | 176.7 (4) | Ta6—O9—Bi10 | 106.8 (5) |
O11—Ta8—O13 | 90.3 (4) | Bi20v—O9—Bi10 | 106.7 (3) |
O11—Ta8—O32 | 91.0 (4) | Ta18ix—O10—Ta6 | 165.3 (6) |
O13—Ta8—O32 | 87.8 (4) | Ta15—O11—Ta8 | 148.8 (4) |
O27—Bi9—O3 | 69.1 (4) | Bi11i—O12—Bi10i | 114.3 (4) |
O27—Bi9—O16 | 116.5 (3) | Ta8—O13—Bi13i | 141.7 (5) |
O27—Bi9—O25i | 74.8 (3) | Ta6—O14—Ta4iii | 150.9 (5) |
O3—Bi9—O16 | 77.1 (3) | Ta15—O15—Bi13i | 134.6 (4) |
O3—Bi9—O25i | 114.5 (3) | Ta15—O15—Bi1 | 109.6 (4) |
O16—Bi9—O25i | 72.8 (4) | Bi13i—O15—Bi1 | 104.0 (3) |
O12v—Bi10—O9 | 74.9 (3) | Bi7—O16—Bi9 | 111.3 (4) |
O12v—Bi10—O2 | 112.0 (3) | Bi7—O16—Bi5iii | 110.1 (4) |
O9—Bi10—O2 | 65.8 (4) | Bi9—O16—Bi5iii | 110.7 (4) |
O12v—Bi11—O7v | 89.3 (4) | Bi1v—O17—Bi3 | 115.0 (4) |
O12v—Bi11—O8v | 86.5 (4) | Bi1v—O17—Bi13 | 104.0 (4) |
O12v—Bi11—O29 | 80.9 (3) | Bi3—O17—Bi13 | 113.7 (5) |
O7v—Bi11—O8v | 82.3 (4) | Ta12—O18—Ta18 | 152.7 (5) |
O7v—Bi11—O29 | 75.1 (4) | Bi20—O19—Bi2 | 133.4 (6) |
O8v—Bi11—O29 | 154.2 (3) | Ta15—O20—Bi7iv | 143.5 (5) |
O36vi—Ta12—O30 | 102.9 (4) | Bi14—O21—Bi19 | 135.1 (6) |
O36vi—Ta12—O18 | 95.6 (4) | Ta8—O22—Bi7 | 144.0 (5) |
O36vi—Ta12—O23 | 92.5 (4) | Ta18iii—O23—Ta12 | 144.6 (4) |
O36vi—Ta12—O3 | 160.2 (4) | Bi19—O24—Bi13i | 119.1 (5) |
O36vi—Ta12—O27 | 84.4 (4) | Bi17v—O25—Bi9v | 113.9 (4) |
O30—Ta12—O18 | 87.2 (4) | Bi17v—O25—Bi5x | 111.5 (4) |
O30—Ta12—O23 | 92.1 (4) | Bi9v—O25—Bi5x | 105.7 (5) |
O30—Ta12—O3 | 96.7 (4) | Ta18—O26—Bi17xi | 148.1 (5) |
O30—Ta12—O27 | 172.2 (4) | Ta12—O27—Bi14i | 131.7 (4) |
O18—Ta12—O23 | 171.7 (4) | Ta12—O27—Bi9 | 105.1 (5) |
O18—Ta12—O3 | 88.0 (4) | Bi14i—O27—Bi9 | 109.6 (4) |
O18—Ta12—O27 | 94.9 (4) | Ta8—O28—Ta15iii | 143.4 (4) |
O23—Ta12—O3 | 83.9 (4) | Ta4—O29—Bi20xi | 134.9 (5) |
O23—Ta12—O27 | 84.8 (4) | Ta4—O29—Bi11 | 103.2 (4) |
O3—Ta12—O27 | 75.8 (4) | Bi20xi—O29—Bi11 | 108.6 (5) |
O13v—Bi13—O15v | 90.0 (4) | Ta12—O30—Bi17v | 146.7 (5) |
O13v—Bi13—O24v | 91.8 (4) | Ta15—O31—Bi3 | 139.3 (5) |
O13v—Bi13—O17 | 83.7 (4) | Ta8—O32—Bi3 | 141.2 (5) |
O15v—Bi13—O24v | 94.6 (3) | Ta15—O33—Bi16xi | 147.7 (6) |
O15v—Bi13—O17 | 75.4 (3) | Bi16v—O34—Bi1x | 112.1 (4) |
O24v—Bi13—O17 | 169.0 (4) | Bi16v—O34—Bi2 | 111.8 (5) |
O21—Bi14—O6v | 81.3 (4) | Bi1x—O34—Bi2 | 107.2 (4) |
O21—Bi14—O27v | 80.3 (4) | Ta8—O35—Bi16v | 147.9 (6) |
O6v—Bi14—O27v | 91.9 (4) | Ta12xii—O36—Ta4 | 164.9 (6) |
Symmetry codes: (i) x, y, z+1; (ii) x, y+1, z+1; (iii) x, y−1, z; (iv) x, y+1, z; (v) x, y, z−1; (vi) x−1/2, y−1/2, z; (vii) x, y−1, z+1; (viii) x−1/2, y+1/2, z; (ix) x+1/2, y−1/2, z; (x) x, y−1, z−1; (xi) x, y+1, z−1; (xii) x+1/2, y+1/2, z. |
(pow) bismuth tantalum oxide
top
Crystal data top
Bi7Ta3O18 | Z = 4 |
Mr = 2293.71 | Neutron radiation, λ = ? Å |
Monoclinic, C2/m | T = 293 K |
a = 34.0084 (9) Å | Particle morphology: plate |
b = 7.6069 (2) Å | yellow |
c = 6.63644 (17) Å | cylinder, 25 × 8 mm |
β = 109.2375 (11)° | Specimen preparation: Prepared at 1173 K and 101.3 kPa |
V = 1620.94 (7) Å3 | |
Data collection top
3He gas and ZnS scintillation counters diffractometer | Specimen mounting: vanadium can |
Radiation source: spallation | |
Refinement top
Rp = 0.046 | ? data points |
Rwp = 0.034 | Profile function: exponential pseudo-Voigt convolution Von Dreele 1990 (unpublished) |
Rexp = ? | 116 parameters |
χ2 = 29.268 | |
Crystal data top
Bi7Ta3O18 | β = 109.2375 (11)° |
Mr = 2293.71 | V = 1620.94 (7) Å3 |
Monoclinic, C2/m | Z = 4 |
a = 34.0084 (9) Å | Neutron radiation, λ = ? Å |
b = 7.6069 (2) Å | T = 293 K |
c = 6.63644 (17) Å | cylinder, 25 × 8 mm |
Data collection top
3He gas and ZnS scintillation counters diffractometer | Specimen mounting: vanadium can |
Refinement top
Rp = 0.046 | χ2 = 29.268 |
Rwp = 0.034 | ? data points |
Rexp = ? | 116 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Bi1 | 0.24592 (12) | 0.5 | 0.4693 (6) | 0.0114 (7)* | |
Bi2 | 0.14509 (7) | 0.2522 (4) | 0.4641 (3) | 0.0154 (5)* | |
Bi3 | 0.14788 (9) | 0.5 | 0.9794 (5) | 0.0019 (6)* | |
Ta4 | 0.05535 (7) | 0.2490 (3) | 0.9919 (4) | 0.0011 (4)* | |
Bi5 | 0.04985 (10) | 0.5 | 0.4544 (6) | 0.0234 (11)* | |
Ta6 | 0.25 | 0.25 | 0.0 | 0.0032 (8)* | |
Bi7 | 0.16126 (10) | 0.0 | 0.0205 (5) | 0.0119 (6)* | |
Bi8 | 0.05314 (9) | 0.0 | 0.5117 (5) | 0.0043 (6)* | |
O9 | 0.07053 (12) | 0.5 | 0.0872 (5) | 0.0016 (8)* | |
O10 | 0.11913 (9) | 0.2017 (4) | 0.0979 (5) | 0.0085 (7)* | |
O11 | 0.04957 (9) | 0.2973 (4) | 0.7019 (4) | 0.0064 (6)* | |
O12 | 0.07096 (9) | 0.2109 (5) | 0.3232 (5) | 0.0106 (7)* | |
O13 | 0.04746 (14) | 0.0 | 0.9260 (7) | 0.0098 (10)* | |
O14 | 0.0 | 0.2889 (5) | 0.0 | 0.0026 (7)* | |
O15 | 0.23936 (13) | 0.2937 (7) | 0.6883 (7) | 0.0436 (13)* | |
O16 | 0.23930 (15) | 0.0 | 0.9454 (8) | 0.0140 (10)* | |
O17 | 0.16979 (15) | 0.5 | 0.3363 (8) | 0.0131 (10)* | |
O18 | 0.18926 (11) | 0.2898 (5) | 0.9466 (6) | 0.0223 (9)* | |
O19 | 0.11791 (16) | 0.0 | 0.6697 (8) | 0.0206 (12)* | |
O20 | 0.11376 (13) | 0.5 | 0.5550 (7) | 0.0035 (8)* | |
O21 | 0.18336 (13) | 0.0 | 0.3733 (7) | 0.0086 (8)* | |
Experimental details
| (XTL) | (pow) |
Crystal data |
Chemical formula | Bi7O18Ta3 | Bi7Ta3O18 |
Mr | 2293.71 | 2293.71 |
Crystal system, space group | Triclinic, C1 | Monoclinic, C2/m |
Temperature (K) | 293 | 293 |
a, b, c (Å) | 34.005 (3), 7.6024 (4), 6.6358 (5) | 34.0084 (9), 7.6069 (2), 6.63644 (17) |
α, β, γ (°) | 90.086 (6), 109.127 (6), 90.043 (6) | 90, 109.2375 (11), 90 |
V (Å3) | 1620.8 (2) | 1620.94 (7) |
Z | 4 | 4 |
Radiation type | Synchrotron, λ = 0.9580 (4) Å | Neutron, λ = ? Å |
µ (mm−1) | 85.4 | – |
Specimen shape, size (mm) | 0.02 × 0.02 × 0.002 | Cylinder, 25 × 8 |
|
Data collection |
Diffractometer | Tsukuba diffractometer | 3He gas and ZnS scintillation counters diffractometer |
Specimen mounting | – | Vanadium can |
Data collection mode | – | ? |
Data collection method | ? | ? |
Absorption correction | Gaussian | – |
Tmin, Tmax | 0.277, 0.844 | – |
No. of measured, independent and observed [refl observed if F2 > 3.000 σ(F2)] reflections | 0.176040+05, 0.137980+05, 0.117960+05 | – |
Rint | 0.023 | – |
θ values (°) | θmax = 50, θmin = 1.7 | 2θmin = ? 2θmax = ? 2θstep = ? |
(sin θ/λ)max (Å−1) | 0.800 | – |
|
Refinement |
R factors and goodness of fit | R[F2 > 2σ(F2)] = 0.039, wR(F2) = 0.0337, S = ? | Rp = 0.046, Rwp = 0.034, Rexp = ?, χ2 = 29.268 |
No. of reflections/data points | 0.117960+05 | ? |
No. of parameters | 327 | 116 |
No. of restraints | 0 | ? |
Δρmax, Δρmin (e Å−3) | 5.80, −5.61 | – |
Selected bond lengths (Å) for (xtl) topBi1—O17i | 2.249 (11) | Bi11—O12v | 2.075 (9) |
Bi1—O34ii | 2.317 (11) | Bi11—O7v | 2.273 (11) |
Bi1—O15 | 2.413 (8) | Bi11—O8v | 2.341 (11) |
Bi2—O19 | 2.225 (9) | Bi11—O29 | 2.456 (10) |
Bi2—O4iii | 2.234 (11) | Ta12—O36vi | 1.873 (10) |
Bi2—O2 | 2.268 (11) | Ta12—O30 | 1.893 (11) |
Bi2—O34 | 2.359 (10) | Ta12—O18 | 1.947 (10) |
Bi3—O32 | 2.198 (12) | Ta12—O23 | 1.986 (9) |
Bi3—O31 | 2.213 (11) | Ta12—O3 | 2.092 (9) |
Bi3—O17 | 2.254 (9) | Ta12—O27 | 2.108 (10) |
Ta4—O7 | 1.927 (10) | Bi13—O13v | 2.166 (10) |
Ta4—O14iv | 1.966 (10) | Bi13—O15v | 2.247 (9) |
Ta4—O4 | 1.978 (10) | Bi13—O24v | 2.259 (10) |
Ta4—O1 | 1.987 (9) | Bi13—O17 | 2.409 (10) |
Ta4—O36 | 2.001 (10) | Bi14—O21 | 2.018 (9) |
Ta4—O29 | 2.069 (10) | Bi14—O6v | 2.243 (10) |
Bi5—O5 | 2.247 (8) | Bi14—O27v | 2.247 (10) |
Bi5—O16iv | 2.306 (10) | Ta15—O33 | 1.885 (12) |
Bi5—O6 | 2.322 (9) | Ta15—O20 | 1.962 (10) |
Bi5—O25ii | 2.424 (11) | Ta15—O11 | 1.975 (10) |
Ta6—O8 | 1.881 (11) | Ta15—O28iv | 2.015 (9) |
Ta6—O14 | 1.946 (10) | Ta15—O31 | 2.020 (10) |
Ta6—O10 | 1.962 (10) | Ta15—O15 | 2.092 (9) |
Ta6—O1 | 2.008 (9) | Bi16—O34i | 2.169 (10) |
Ta6—O2 | 2.019 (10) | Bi16—O35i | 2.193 (11) |
Ta6—O9 | 2.111 (9) | Bi16—O33vii | 2.277 (12) |
Bi7—O16 | 2.162 (9) | Bi17—O25i | 2.064 (10) |
Bi7—O22 | 2.174 (11) | Bi17—O26vii | 2.249 (10) |
Bi7—O20iii | 2.192 (10) | Bi17—O30i | 2.273 (11) |
Ta8—O28 | 1.965 (9) | Ta18—O10viii | 1.899 (10) |
Ta8—O35 | 1.969 (11) | Ta18—O26 | 1.900 (10) |
Ta8—O22 | 1.981 (11) | Ta18—O23iv | 1.984 (9) |
Ta8—O11 | 1.996 (10) | Ta18—O18 | 1.985 (10) |
Ta8—O13 | 2.000 (10) | Ta18—O5 | 2.077 (9) |
Ta8—O32 | 2.006 (11) | Ta18—O6 | 2.110 (9) |
Bi9—O27 | 2.268 (9) | Bi19—O24 | 2.218 (10) |
Bi9—O3 | 2.282 (9) | Bi19—O3 | 2.302 (10) |
Bi9—O16 | 2.292 (10) | Bi19—O5 | 2.313 (9) |
Bi9—O25i | 2.319 (11) | Bi19—O21 | 2.372 (9) |
Bi10—O12v | 2.303 (10) | Bi20—O19 | 2.078 (9) |
Bi10—O9 | 2.314 (9) | Bi20—O29vii | 2.141 (10) |
Bi10—O2 | 2.414 (9) | Bi20—O9i | 2.220 (10) |
Symmetry codes: (i) x, y, z+1; (ii) x, y+1, z+1; (iii) x, y−1, z; (iv) x, y+1, z; (v) x, y, z−1; (vi) x−1/2, y−1/2, z; (vii) x, y−1, z+1; (viii) x−1/2, y+1/2, z. |