Supporting information
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617009544/rm5005sup14.pdf | |
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617009544/rm5005sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Lasup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Cesup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Prsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Smsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Eusup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Tbsup7.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Dysup8.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Hosup9.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Ersup10.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Tmsup11.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Ybsup12.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617009544/rm5005Lusup13.hkl |
CCDC references: 1558797; 1558798; 1558799; 1558800; 1558801; 1558802; 1558803; 1558804; 1558805; 1558806; 1558807; 1558808
Data collection: Bruker APEX3 for La, Ce, Pr, Tb, Tm, Yb; CrystalClear (Rigaku/MSC, 2008) for Sm, Eu, Dy, Ho, Er, Lu. Cell refinement: Bruker SAINT for La, Ce, Pr, Tb, Tm, Yb; CrystalClear (Rigaku/MSC, 2008) for Sm, Eu, Dy, Ho, Er, Lu. Data reduction: Bruker SAINT for La, Ce, Pr, Tb, Tm, Yb; CrystalClear (Rigaku/MSC, 2008) for Sm, Eu, Dy, Ho, Er, Lu. Program(s) used to solve structure: SHELXT-2014 (Sheldrick 2014) for La, Ce, Pr, Tm, Yb; SHELXL2014/7 (Sheldrick, 2014) for Sm, Eu, Dy, Ho, Er, Lu; SHELXL2014 (Sheldrick 2014) for Tb. Program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2014) for La, Ce, Pr, Sm, Eu, Dy, Ho, Er, Tm, Yb, Lu; SHELXL2014 (Sheldrick 2014) for Tb. For all structures, molecular graphics: DIAMOND (Bradenburg, 1999). Software used to prepare material for publication: Bruker SHELXTL for La, Ce, Pr, Tb, Tm, Yb; SHELXL2014/7 (Sheldrick, 2014) for Sm, Eu, Dy, Ho, Er, Lu.
Ba2La2O13Si4 | Z = 2 |
Mr = 872.86 | F(000) = 772 |
Triclinic, P1 | Dx = 4.900 Mg m−3 |
a = 6.7327 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.9894 (4) Å | Cell parameters from 9900 reflections |
c = 10.2191 (4) Å | θ = 2.3–28.3° |
α = 86.6588 (12)° | µ = 14.12 mm−1 |
β = 73.5660 (12)° | T = 300 K |
γ = 86.5873 (13)° | Block, colourless |
V = 591.62 (4) Å3 | 0.11 × 0.10 × 0.10 mm |
Bruker Photon 100 diffractometer | 2218 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.025 |
φ and ω scans | θmax = 26.0°, θmin = 2.1° |
Absorption correction: multi-scan SADABS, Bruker | h = −8→8 |
Tmin = 0.788, Tmax = 1.000 | k = −11→11 |
10742 measured reflections | l = −11→12 |
2309 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.020 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.3644P] where P = (Fo2 + 2Fc2)/3 |
S = 1.17 | (Δ/σ)max = 0.001 |
2309 reflections | Δρmax = 0.82 e Å−3 |
190 parameters | Δρmin = −1.66 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.22533 (4) | 0.33341 (3) | 0.55665 (3) | 0.00891 (9) | |
Ba2 | 0.75458 (4) | 0.82796 (3) | 1.07751 (3) | 0.00716 (8) | |
La1 | 0.81221 (4) | 0.10920 (3) | 0.39581 (2) | 0.00386 (8) | |
La2 | 0.30909 (4) | 0.62200 (3) | 0.89937 (2) | 0.00425 (8) | |
Si1 | 0.60732 (18) | −0.06006 (13) | 0.68725 (12) | 0.0043 (2) | |
Si2 | 0.80176 (18) | 0.12284 (13) | 0.84381 (12) | 0.0041 (2) | |
Si3 | 0.67842 (19) | 0.38603 (13) | 0.67805 (12) | 0.0046 (2) | |
Si4 | 0.88817 (18) | 0.56862 (13) | 0.82408 (12) | 0.0042 (2) | |
O1 | 1.0252 (5) | 0.7155 (3) | 0.7977 (3) | 0.0074 (6) | |
O2 | 0.4722 (5) | −0.2071 (3) | 0.7079 (3) | 0.0085 (6) | |
O3 | 0.6661 (5) | 0.5978 (3) | 0.9374 (3) | 0.0067 (6) | |
O4 | 0.8275 (5) | −0.0886 (3) | 0.5745 (3) | 0.0062 (6) | |
O5 | 0.6538 (5) | −0.0149 (3) | 0.8324 (3) | 0.0060 (6) | |
O6 | 0.8401 (5) | 0.5183 (3) | 0.6825 (3) | 0.0071 (6) | |
O7 | 0.4754 (5) | 0.0757 (3) | 0.6342 (3) | 0.0095 (7) | |
O8 | 1.0170 (5) | 0.4307 (3) | 0.8770 (3) | 0.0099 (6) | |
O9 | 1.0278 (5) | 0.1091 (3) | 0.7395 (3) | 0.0072 (6) | |
O10 | 0.4491 (5) | 0.4562 (3) | 0.7009 (3) | 0.0112 (7) | |
O11 | 0.7875 (5) | 0.3186 (3) | 0.5334 (3) | 0.0134 (7) | |
O12 | 0.8067 (5) | 0.1263 (3) | 0.9992 (3) | 0.0067 (6) | |
O13 | 0.6693 (5) | 0.2739 (3) | 0.8127 (3) | 0.0068 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.01094 (15) | 0.00768 (14) | 0.00945 (15) | −0.00219 (10) | −0.00487 (11) | 0.00072 (10) |
Ba2 | 0.00642 (14) | 0.00674 (14) | 0.00898 (14) | −0.00069 (10) | −0.00304 (11) | −0.00087 (10) |
La1 | 0.00369 (14) | 0.00387 (13) | 0.00421 (14) | −0.00021 (9) | −0.00145 (10) | 0.00009 (9) |
La2 | 0.00397 (14) | 0.00427 (13) | 0.00442 (14) | −0.00006 (9) | −0.00126 (10) | 0.00099 (9) |
Si1 | 0.0042 (6) | 0.0053 (5) | 0.0037 (6) | −0.0013 (4) | −0.0012 (5) | −0.0002 (4) |
Si2 | 0.0039 (6) | 0.0047 (5) | 0.0033 (6) | −0.0005 (4) | −0.0003 (5) | −0.0004 (4) |
Si3 | 0.0060 (6) | 0.0048 (5) | 0.0033 (6) | −0.0008 (4) | −0.0017 (5) | −0.0007 (4) |
Si4 | 0.0039 (6) | 0.0054 (5) | 0.0037 (5) | −0.0013 (4) | −0.0014 (5) | −0.0001 (4) |
O1 | 0.0074 (16) | 0.0081 (15) | 0.0077 (16) | −0.0041 (12) | −0.0035 (13) | 0.0023 (12) |
O2 | 0.0095 (16) | 0.0097 (15) | 0.0066 (16) | −0.0047 (12) | −0.0025 (13) | 0.0023 (12) |
O3 | 0.0049 (15) | 0.0074 (15) | 0.0079 (15) | −0.0007 (12) | −0.0020 (12) | 0.0000 (12) |
O4 | 0.0053 (15) | 0.0073 (14) | 0.0065 (15) | −0.0007 (11) | −0.0025 (12) | −0.0011 (12) |
O5 | 0.0087 (16) | 0.0060 (14) | 0.0042 (15) | −0.0029 (12) | −0.0028 (12) | −0.0001 (11) |
O6 | 0.0085 (16) | 0.0077 (15) | 0.0056 (15) | −0.0036 (12) | −0.0025 (13) | 0.0002 (12) |
O7 | 0.0074 (16) | 0.0102 (15) | 0.0119 (17) | 0.0021 (12) | −0.0049 (13) | 0.0002 (13) |
O8 | 0.0092 (16) | 0.0092 (15) | 0.0122 (16) | 0.0019 (12) | −0.0052 (13) | 0.0004 (12) |
O9 | 0.0056 (15) | 0.0087 (15) | 0.0069 (15) | −0.0002 (12) | −0.0005 (13) | −0.0027 (12) |
O10 | 0.0094 (17) | 0.0109 (16) | 0.0150 (17) | 0.0015 (13) | −0.0063 (14) | −0.0035 (13) |
O11 | 0.0183 (18) | 0.0096 (16) | 0.0096 (17) | −0.0027 (13) | 0.0019 (14) | −0.0055 (13) |
O12 | 0.0080 (16) | 0.0085 (15) | 0.0040 (15) | −0.0023 (12) | −0.0023 (12) | 0.0005 (11) |
O13 | 0.0055 (15) | 0.0067 (14) | 0.0059 (15) | 0.0002 (11) | 0.0015 (12) | 0.0017 (11) |
Ba1—O10 | 2.703 (3) | Si1—La1i | 3.2315 (12) |
Ba1—O4i | 2.734 (3) | Si1—Ba1i | 3.5093 (12) |
Ba1—O9ii | 2.793 (3) | Si1—Ba2vi | 3.5685 (12) |
Ba1—O6iii | 2.847 (3) | Si2—O9 | 1.595 (3) |
Ba1—O7 | 2.984 (3) | Si2—O12 | 1.599 (3) |
Ba1—O6ii | 2.998 (3) | Si2—O13 | 1.645 (3) |
Ba1—O11ii | 3.035 (4) | Si2—O5 | 1.664 (3) |
Ba1—O2i | 3.116 (3) | Si2—Ba2v | 3.3647 (12) |
Ba1—O11iii | 3.212 (3) | Si2—Ba2ix | 3.4299 (12) |
Ba1—O8ii | 3.322 (3) | Si2—La2vi | 3.4778 (12) |
Ba1—Si3iii | 3.3381 (12) | Si2—Ba2vi | 3.6073 (12) |
Ba1—Si1i | 3.5093 (12) | Si3—O11 | 1.590 (3) |
Ba2—O12iv | 2.768 (3) | Si3—O10 | 1.592 (3) |
Ba2—O3 | 2.768 (3) | Si3—O13 | 1.647 (3) |
Ba2—O9v | 2.782 (3) | Si3—O6 | 1.670 (3) |
Ba2—O8v | 2.800 (3) | Si3—Ba1iii | 3.3381 (12) |
Ba2—O12v | 2.882 (3) | Si3—Ba1x | 3.5494 (13) |
Ba2—O13vi | 2.936 (3) | Si3—Ba2vi | 3.7981 (12) |
Ba2—O5iv | 3.027 (3) | Si4—O1 | 1.622 (3) |
Ba2—O7vi | 3.063 (3) | Si4—O8 | 1.625 (3) |
Ba2—O5vi | 3.071 (3) | Si4—O3 | 1.629 (3) |
Ba2—O1 | 3.112 (3) | Si4—O6 | 1.662 (3) |
Ba2—Si2v | 3.3648 (12) | Si4—La2vi | 3.2046 (12) |
Ba2—Si2iv | 3.4299 (12) | Si4—La2x | 3.2081 (12) |
La1—O11 | 2.385 (3) | Si4—Ba1x | 3.6992 (12) |
La1—O9vii | 2.478 (3) | O1—La1viii | 2.492 (3) |
La1—O1viii | 2.492 (3) | O1—La2x | 2.503 (3) |
La1—O4 | 2.492 (3) | O2—La2ix | 2.455 (3) |
La1—O4vii | 2.523 (3) | O2—La1i | 2.530 (3) |
La1—O2i | 2.530 (3) | O2—Ba1i | 3.116 (3) |
La1—O7i | 2.718 (3) | O3—La2vi | 2.540 (3) |
La1—O7 | 2.835 (3) | O4—La1vii | 2.523 (3) |
La1—Si1i | 3.2315 (12) | O4—Ba1i | 2.734 (3) |
La1—Si1 | 3.2381 (12) | O5—Ba2ix | 3.027 (3) |
La1—La2iii | 3.9893 (4) | O5—Ba2vi | 3.071 (3) |
La1—Ba1i | 3.9944 (4) | O6—Ba1iii | 2.847 (3) |
La2—O2iv | 2.455 (3) | O6—Ba1x | 2.998 (3) |
La2—O1ii | 2.503 (3) | O7—La1i | 2.718 (3) |
La2—O10 | 2.516 (3) | O7—Ba2vi | 3.063 (3) |
La2—O12vi | 2.531 (3) | O8—La2vi | 2.725 (3) |
La2—O3 | 2.536 (3) | O8—La2x | 2.753 (3) |
La2—O3vi | 2.540 (3) | O8—Ba2v | 2.800 (3) |
La2—O8vi | 2.725 (3) | O8—Ba1x | 3.322 (3) |
La2—O8ii | 2.753 (3) | O9—La1vii | 2.479 (3) |
La2—Si4vi | 3.2047 (12) | O9—Ba2v | 2.782 (3) |
La2—Si4ii | 3.2081 (12) | O9—Ba1x | 2.793 (3) |
La2—Si2vi | 3.4778 (12) | O11—Ba1x | 3.035 (4) |
La2—La1iii | 3.9893 (4) | O11—Ba1iii | 3.212 (3) |
Si1—O4 | 1.617 (3) | O12—La2vi | 2.531 (3) |
Si1—O2 | 1.619 (3) | O12—Ba2ix | 2.768 (3) |
Si1—O7 | 1.624 (3) | O12—Ba2v | 2.882 (3) |
Si1—O5 | 1.677 (3) | O13—Ba2vi | 2.936 (3) |
O10—Ba1—O4i | 146.42 (9) | O10—La2—Si4vi | 111.36 (8) |
O10—Ba1—O9ii | 101.89 (10) | O12vi—La2—Si4vi | 95.34 (7) |
O4i—Ba1—O9ii | 68.01 (9) | O3—La2—Si4vi | 91.75 (7) |
O10—Ba1—O6iii | 121.09 (9) | O3vi—La2—Si4vi | 30.22 (7) |
O4i—Ba1—O6iii | 81.50 (9) | O8vi—La2—Si4vi | 30.46 (7) |
O9ii—Ba1—O6iii | 134.80 (9) | O8ii—La2—Si4vi | 66.62 (7) |
O10—Ba1—O7 | 76.05 (9) | O2iv—La2—Si4ii | 99.63 (8) |
O4i—Ba1—O7 | 71.23 (9) | O1ii—La2—Si4ii | 29.87 (7) |
O9ii—Ba1—O7 | 60.21 (9) | O10—La2—Si4ii | 80.20 (8) |
O6iii—Ba1—O7 | 139.35 (9) | O12vi—La2—Si4ii | 95.84 (7) |
O10—Ba1—O6ii | 93.59 (9) | O3—La2—Si4ii | 165.41 (7) |
O4i—Ba1—O6ii | 116.02 (9) | O3vi—La2—Si4ii | 102.85 (7) |
O9ii—Ba1—O6ii | 84.14 (8) | O8vi—La2—Si4ii | 66.85 (7) |
O6iii—Ba1—O6ii | 80.14 (9) | O8ii—La2—Si4ii | 30.43 (7) |
O7—Ba1—O6ii | 138.85 (9) | Si4vi—La2—Si4ii | 85.76 (3) |
O10—Ba1—O11ii | 142.42 (9) | O2iv—La2—Si2vi | 97.73 (8) |
O4i—Ba1—O11ii | 67.09 (9) | O1ii—La2—Si2vi | 95.81 (7) |
O9ii—Ba1—O11ii | 71.76 (9) | O10—La2—Si2vi | 170.23 (8) |
O6iii—Ba1—O11ii | 65.81 (9) | O12vi—La2—Si2vi | 25.10 (7) |
O7—Ba1—O11ii | 125.04 (9) | O3—La2—Si2vi | 84.89 (7) |
O6ii—Ba1—O11ii | 49.44 (8) | O3vi—La2—Si2vi | 93.09 (7) |
O10—Ba1—O2i | 108.78 (9) | O8vi—La2—Si2vi | 62.40 (7) |
O4i—Ba1—O2i | 53.31 (8) | O8ii—La2—Si2vi | 121.30 (7) |
O9ii—Ba1—O2i | 112.54 (8) | Si4vi—La2—Si2vi | 74.89 (3) |
O6iii—Ba1—O2i | 68.39 (8) | Si4ii—La2—Si2vi | 108.22 (3) |
O7—Ba1—O2i | 71.17 (9) | O2iv—La2—La1iii | 37.51 (7) |
O6ii—Ba1—O2i | 147.61 (8) | O1ii—La2—La1iii | 36.91 (7) |
O11ii—Ba1—O2i | 107.69 (8) | O10—La2—La1iii | 80.85 (7) |
O10—Ba1—O11iii | 76.53 (9) | O12vi—La2—La1iii | 73.15 (7) |
O4i—Ba1—O11iii | 130.27 (9) | O3—La2—La1iii | 121.94 (7) |
O9ii—Ba1—O11iii | 145.59 (9) | O3vi—La2—La1iii | 164.63 (7) |
O6iii—Ba1—O11iii | 48.77 (8) | O8vi—La2—La1iii | 116.13 (7) |
O7—Ba1—O11iii | 146.40 (9) | O8ii—La2—La1iii | 90.30 (7) |
O6ii—Ba1—O11iii | 61.90 (8) | Si4vi—La2—La1iii | 145.29 (2) |
O11ii—Ba1—O11iii | 88.55 (8) | Si4ii—La2—La1iii | 63.73 (2) |
O2i—Ba1—O11iii | 100.06 (8) | Si2vi—La2—La1iii | 98.23 (2) |
O10—Ba1—O8ii | 57.99 (9) | O4—Si1—O2 | 109.76 (17) |
O4i—Ba1—O8ii | 130.80 (9) | O4—Si1—O7 | 109.94 (17) |
O9ii—Ba1—O8ii | 64.10 (8) | O2—Si1—O7 | 107.10 (17) |
O6iii—Ba1—O8ii | 126.75 (8) | O4—Si1—O5 | 108.22 (17) |
O7—Ba1—O8ii | 93.86 (8) | O2—Si1—O5 | 112.24 (17) |
O6ii—Ba1—O8ii | 49.29 (8) | O7—Si1—O5 | 109.58 (17) |
O11ii—Ba1—O8ii | 87.58 (8) | O4—Si1—La1i | 118.40 (12) |
O2i—Ba1—O8ii | 162.86 (8) | O2—Si1—La1i | 50.47 (12) |
O11iii—Ba1—O8ii | 87.78 (8) | O7—Si1—La1i | 57.16 (12) |
O10—Ba1—Si3iii | 91.25 (7) | O5—Si1—La1i | 133.33 (12) |
O4i—Ba1—Si3iii | 106.54 (7) | O4—Si1—La1 | 48.87 (11) |
O9ii—Ba1—Si3iii | 162.78 (7) | O2—Si1—La1 | 124.75 (12) |
O6iii—Ba1—Si3iii | 30.01 (6) | O7—Si1—La1 | 61.09 (12) |
O7—Ba1—Si3iii | 135.01 (7) | O5—Si1—La1 | 122.67 (12) |
O6ii—Ba1—Si3iii | 83.96 (6) | La1i—Si1—La1 | 91.55 (3) |
O11ii—Ba1—Si3iii | 91.04 (7) | O4—Si1—Ba1i | 48.93 (11) |
O2i—Ba1—Si3iii | 72.74 (6) | O2—Si1—Ba1i | 62.62 (12) |
O11iii—Ba1—Si3iii | 28.01 (6) | O7—Si1—Ba1i | 111.45 (12) |
O8ii—Ba1—Si3iii | 115.76 (6) | O5—Si1—Ba1i | 138.10 (12) |
O10—Ba1—Si1i | 127.68 (7) | La1i—Si1—Ba1i | 78.25 (3) |
O4i—Ba1—Si1i | 26.47 (7) | La1—Si1—Ba1i | 72.47 (2) |
O9ii—Ba1—Si1i | 87.55 (6) | O4—Si1—Ba2vi | 151.48 (12) |
O6iii—Ba1—Si1i | 77.51 (6) | O2—Si1—Ba2vi | 98.76 (12) |
O7—Ba1—Si1i | 64.56 (7) | O7—Si1—Ba2vi | 58.88 (12) |
O6ii—Ba1—Si1i | 138.72 (6) | O5—Si1—Ba2vi | 59.27 (11) |
O11ii—Ba1—Si1i | 89.60 (6) | La1i—Si1—Ba2vi | 79.34 (3) |
O2i—Ba1—Si1i | 27.48 (6) | La1—Si1—Ba2vi | 113.21 (3) |
O11iii—Ba1—Si1i | 121.10 (6) | Ba1i—Si1—Ba2vi | 157.04 (4) |
O8ii—Ba1—Si1i | 150.91 (6) | O9—Si2—O12 | 112.68 (17) |
Si3iii—Ba1—Si1i | 93.23 (3) | O9—Si2—O13 | 112.56 (16) |
O12iv—Ba2—O3 | 129.61 (9) | O12—Si2—O13 | 106.99 (16) |
O12iv—Ba2—O9v | 83.29 (9) | O9—Si2—O5 | 112.50 (16) |
O3—Ba2—O9v | 142.46 (9) | O12—Si2—O5 | 108.04 (16) |
O12iv—Ba2—O8v | 140.66 (9) | O13—Si2—O5 | 103.49 (16) |
O3—Ba2—O8v | 70.72 (9) | O9—Si2—Ba2v | 55.18 (11) |
O9v—Ba2—O8v | 71.87 (9) | O12—Si2—Ba2v | 58.81 (11) |
O12iv—Ba2—O12v | 72.81 (10) | O13—Si2—Ba2v | 117.04 (12) |
O3—Ba2—O12v | 111.09 (9) | O5—Si2—Ba2v | 139.37 (12) |
O9v—Ba2—O12v | 55.96 (9) | O9—Si2—Ba2ix | 107.75 (12) |
O8v—Ba2—O12v | 68.06 (9) | O12—Si2—Ba2ix | 52.61 (11) |
O12iv—Ba2—O13vi | 118.30 (8) | O13—Si2—Ba2ix | 139.59 (12) |
O3—Ba2—O13vi | 66.20 (9) | O5—Si2—Ba2ix | 61.94 (11) |
O9v—Ba2—O13vi | 118.40 (9) | Ba2v—Si2—Ba2ix | 84.02 (3) |
O8v—Ba2—O13vi | 100.45 (9) | O9—Si2—La2vi | 120.45 (12) |
O12v—Ba2—O13vi | 168.01 (8) | O12—Si2—La2vi | 42.16 (11) |
O12iv—Ba2—O5iv | 54.00 (8) | O13—Si2—La2vi | 65.92 (11) |
O3—Ba2—O5iv | 76.31 (8) | O5—Si2—La2vi | 126.03 (12) |
O9v—Ba2—O5iv | 136.47 (8) | Ba2v—Si2—La2vi | 72.56 (2) |
O8v—Ba2—O5iv | 135.74 (9) | Ba2ix—Si2—La2vi | 91.57 (3) |
O12v—Ba2—O5iv | 98.55 (8) | O9—Si2—Ba2vi | 152.49 (13) |
O13vi—Ba2—O5iv | 92.17 (8) | O12—Si2—Ba2vi | 94.69 (12) |
O12iv—Ba2—O7vi | 88.28 (9) | O13—Si2—Ba2vi | 53.28 (11) |
O3—Ba2—O7vi | 128.03 (9) | O5—Si2—Ba2vi | 58.06 (11) |
O9v—Ba2—O7vi | 59.32 (9) | Ba2v—Si2—Ba2vi | 149.87 (4) |
O8v—Ba2—O7vi | 103.69 (9) | Ba2ix—Si2—Ba2vi | 90.67 (3) |
O12v—Ba2—O7vi | 113.90 (8) | La2vi—Si2—Ba2vi | 77.98 (2) |
O13vi—Ba2—O7vi | 64.31 (8) | O11—Si3—O10 | 116.92 (19) |
O5iv—Ba2—O7vi | 119.90 (8) | O11—Si3—O13 | 116.30 (17) |
O12iv—Ba2—O5vi | 68.01 (8) | O10—Si3—O13 | 105.46 (17) |
O3—Ba2—O5vi | 104.80 (9) | O11—Si3—O6 | 101.40 (17) |
O9v—Ba2—O5vi | 104.65 (8) | O10—Si3—O6 | 110.23 (17) |
O8v—Ba2—O5vi | 147.03 (9) | O13—Si3—O6 | 105.97 (16) |
O12v—Ba2—O5vi | 138.23 (8) | O11—Si3—Ba1iii | 71.57 (12) |
O13vi—Ba2—O5vi | 51.20 (8) | O10—Si3—Ba1iii | 80.69 (13) |
O5iv—Ba2—O5vi | 69.62 (9) | O13—Si3—Ba1iii | 164.37 (12) |
O7vi—Ba2—O5vi | 52.17 (8) | O6—Si3—Ba1iii | 58.48 (11) |
O12iv—Ba2—O1 | 94.06 (8) | O11—Si3—Ba1x | 58.39 (13) |
O3—Ba2—O1 | 53.82 (8) | O10—Si3—Ba1x | 161.53 (13) |
O9v—Ba2—O1 | 115.32 (8) | O13—Si3—Ba1x | 91.81 (11) |
O8v—Ba2—O1 | 71.02 (9) | O6—Si3—Ba1x | 57.35 (11) |
O12v—Ba2—O1 | 61.65 (8) | Ba1iii—Si3—Ba1x | 80.96 (3) |
O13vi—Ba2—O1 | 119.04 (8) | O11—Si3—Ba1 | 79.41 (14) |
O5iv—Ba2—O1 | 65.81 (8) | O10—Si3—Ba1 | 41.97 (12) |
O7vi—Ba2—O1 | 173.89 (8) | O13—Si3—Ba1 | 109.24 (12) |
O5vi—Ba2—O1 | 133.92 (8) | O6—Si3—Ba1 | 140.04 (12) |
O12iv—Ba2—Si2v | 80.21 (7) | Ba1iii—Si3—Ba1 | 85.05 (3) |
O3—Ba2—Si2v | 127.81 (7) | Ba1x—Si3—Ba1 | 137.78 (4) |
O9v—Ba2—Si2v | 28.08 (6) | O11—Si3—Ba2vi | 117.95 (13) |
O8v—Ba2—Si2v | 63.45 (7) | O10—Si3—Ba2vi | 63.26 (12) |
O12v—Ba2—Si2v | 28.34 (6) | O13—Si3—Ba2vi | 47.10 (11) |
O13vi—Ba2—Si2v | 143.88 (6) | O6—Si3—Ba2vi | 138.88 (12) |
O5iv—Ba2—Si2v | 122.36 (6) | Ba1iii—Si3—Ba2vi | 143.34 (4) |
O7vi—Ba2—Si2v | 87.26 (6) | Ba1x—Si3—Ba2vi | 135.21 (3) |
O5vi—Ba2—Si2v | 127.21 (6) | Ba1—Si3—Ba2vi | 64.15 (2) |
O1—Ba2—Si2v | 87.58 (6) | O1—Si4—O8 | 108.70 (17) |
O12iv—Ba2—Si2iv | 27.33 (6) | O1—Si4—O3 | 111.01 (17) |
O3—Ba2—Si2iv | 102.45 (7) | O8—Si4—O3 | 109.70 (17) |
O9v—Ba2—Si2iv | 107.51 (7) | O1—Si4—O6 | 112.10 (17) |
O8v—Ba2—Si2iv | 138.46 (7) | O8—Si4—O6 | 107.59 (17) |
O12v—Ba2—Si2iv | 77.57 (6) | O3—Si4—O6 | 107.67 (17) |
O13vi—Ba2—Si2iv | 114.34 (6) | O1—Si4—La2vi | 130.34 (12) |
O5iv—Ba2—Si2iv | 29.02 (6) | O8—Si4—La2vi | 58.23 (12) |
O7vi—Ba2—Si2iv | 111.29 (6) | O3—Si4—La2vi | 51.68 (11) |
O5vi—Ba2—Si2iv | 74.41 (6) | O6—Si4—La2vi | 117.52 (12) |
O1—Ba2—Si2iv | 72.52 (6) | O1—Si4—La2x | 50.24 (11) |
Si2v—Ba2—Si2iv | 95.98 (3) | O8—Si4—La2x | 59.10 (12) |
O11—La1—O9vii | 158.40 (11) | O3—Si4—La2x | 119.48 (12) |
O11—La1—O1viii | 84.67 (10) | O6—Si4—La2x | 132.82 (12) |
O9vii—La1—O1viii | 91.28 (10) | La2vi—Si4—La2x | 94.24 (3) |
O11—La1—O4 | 97.32 (11) | O1—Si4—Ba2 | 63.51 (12) |
O9vii—La1—O4 | 76.91 (10) | O8—Si4—Ba2 | 107.49 (13) |
O1viii—La1—O4 | 152.85 (10) | O3—Si4—Ba2 | 51.31 (11) |
O11—La1—O4vii | 81.24 (11) | O6—Si4—Ba2 | 143.86 (12) |
O9vii—La1—O4vii | 77.20 (10) | La2vi—Si4—Ba2 | 75.13 (3) |
O1viii—La1—O4vii | 83.02 (10) | La2x—Si4—Ba2 | 74.46 (3) |
O4—La1—O4vii | 70.63 (11) | O1—Si4—Ba1x | 99.23 (12) |
O11—La1—O2i | 94.69 (11) | O8—Si4—Ba1x | 63.92 (12) |
O9vii—La1—O2i | 104.48 (10) | O3—Si4—Ba1x | 149.16 (12) |
O1viii—La1—O2i | 73.32 (10) | O6—Si4—Ba1x | 52.67 (11) |
O4—La1—O2i | 133.06 (10) | La2vi—Si4—Ba1x | 111.85 (3) |
O4vii—La1—O2i | 156.28 (10) | La2x—Si4—Ba1x | 84.41 (3) |
O11—La1—O7i | 132.34 (11) | Ba2—Si4—Ba1x | 158.33 (4) |
O9vii—La1—O7i | 67.73 (10) | Si4—O1—La1viii | 138.33 (17) |
O1viii—La1—O7i | 118.87 (10) | Si4—O1—La2x | 99.89 (14) |
O4—La1—O7i | 79.49 (10) | La1viii—O1—La2x | 105.99 (11) |
O4vii—La1—O7i | 138.09 (9) | Si4—O1—Ba2 | 88.69 (13) |
O2i—La1—O7i | 59.49 (9) | La1viii—O1—Ba2 | 121.99 (11) |
O11—La1—O7 | 70.90 (10) | La2x—O1—Ba2 | 91.65 (9) |
O9vii—La1—O7 | 120.82 (9) | Si1—O2—La2ix | 136.27 (17) |
O1viii—La1—O7 | 144.12 (10) | Si1—O2—La1i | 99.96 (15) |
O4—La1—O7 | 59.33 (9) | La2ix—O2—La1i | 106.28 (12) |
O4vii—La1—O7 | 117.27 (10) | Si1—O2—Ba1i | 89.89 (13) |
O2i—La1—O7 | 82.69 (10) | La2ix—O2—Ba1i | 119.91 (11) |
O7i—La1—O7 | 66.82 (11) | La1i—O2—Ba1i | 97.38 (10) |
O11—La1—Si1i | 113.56 (9) | Si4—O3—La2 | 127.76 (17) |
O9vii—La1—Si1i | 88.01 (7) | Si4—O3—La2vi | 98.10 (14) |
O1viii—La1—Si1i | 97.93 (7) | La2—O3—La2vi | 110.74 (11) |
O4—La1—Si1i | 105.87 (7) | Si4—O3—Ba2 | 101.33 (14) |
O4vii—La1—Si1i | 165.20 (7) | La2—O3—Ba2 | 114.35 (11) |
O2i—La1—Si1i | 29.58 (7) | La2vi—O3—Ba2 | 100.36 (10) |
O7i—La1—Si1i | 30.14 (7) | Si1—O4—La1 | 101.89 (14) |
O7—La1—Si1i | 70.03 (7) | Si1—O4—La1vii | 129.33 (17) |
O11—La1—Si1 | 83.11 (8) | La1—O4—La1vii | 109.37 (11) |
O9vii—La1—Si1 | 99.50 (7) | Si1—O4—Ba1i | 104.60 (14) |
O1viii—La1—Si1 | 167.68 (7) | La1—O4—Ba1i | 99.59 (10) |
O4—La1—Si1 | 29.24 (7) | La1vii—O4—Ba1i | 108.16 (11) |
O4vii—La1—Si1 | 93.50 (7) | Si2—O5—Si1 | 124.30 (19) |
O2i—La1—Si1 | 109.29 (7) | Si2—O5—Ba2ix | 89.04 (12) |
O7i—La1—Si1 | 71.28 (7) | Si1—O5—Ba2ix | 138.28 (15) |
O7—La1—Si1 | 30.10 (6) | Si2—O5—Ba2vi | 94.57 (13) |
Si1i—La1—Si1 | 88.45 (3) | Si1—O5—Ba2vi | 92.74 (13) |
O11—La1—La2iii | 89.93 (8) | Ba2ix—O5—Ba2vi | 110.38 (9) |
O9vii—La1—La2iii | 99.60 (7) | Si4—O6—Si3 | 124.18 (19) |
O1viii—La1—La2iii | 37.10 (7) | Si4—O6—Ba1iii | 136.26 (16) |
O4—La1—La2iii | 168.04 (7) | Si3—O6—Ba1iii | 91.51 (13) |
O4vii—La1—La2iii | 120.12 (7) | Si4—O6—Ba1x | 101.18 (14) |
O2i—La1—La2iii | 36.21 (7) | Si3—O6—Ba1x | 94.68 (13) |
O7i—La1—La2iii | 88.60 (7) | Ba1iii—O6—Ba1x | 99.86 (9) |
O7—La1—La2iii | 114.94 (6) | Si1—O7—La1i | 92.70 (14) |
Si1i—La1—La2iii | 62.36 (2) | Si1—O7—La1 | 88.81 (14) |
Si1—La1—La2iii | 144.24 (2) | La1i—O7—La1 | 113.18 (11) |
O11—La1—Ba1i | 138.64 (8) | Si1—O7—Ba1 | 175.96 (18) |
O9vii—La1—Ba1i | 43.77 (7) | La1i—O7—Ba1 | 88.80 (9) |
O1viii—La1—Ba1i | 134.65 (7) | La1—O7—Ba1 | 94.05 (9) |
O4—La1—Ba1i | 42.44 (7) | Si1—O7—Ba2vi | 94.12 (14) |
O4vii—La1—Ba1i | 90.36 (7) | La1i—O7—Ba2vi | 97.40 (10) |
O2i—La1—Ba1i | 107.33 (7) | La1—O7—Ba2vi | 149.13 (12) |
O7i—La1—Ba1i | 48.33 (6) | Ba1—O7—Ba2vi | 81.96 (8) |
O7—La1—Ba1i | 77.58 (6) | Si4—O8—La2vi | 91.31 (14) |
Si1i—La1—Ba1i | 78.42 (2) | Si4—O8—La2x | 90.47 (14) |
Si1—La1—Ba1i | 56.90 (2) | La2vi—O8—La2x | 118.14 (12) |
La2iii—La1—Ba1i | 128.156 (8) | Si4—O8—Ba2v | 169.68 (19) |
O2iv—La2—O1ii | 74.42 (11) | La2vi—O8—Ba2v | 94.27 (10) |
O2iv—La2—O10 | 75.56 (10) | La2x—O8—Ba2v | 94.54 (10) |
O1ii—La2—O10 | 89.27 (10) | Si4—O8—Ba1x | 90.03 (13) |
O2iv—La2—O12vi | 78.35 (10) | La2vi—O8—Ba1x | 142.23 (12) |
O1ii—La2—O12vi | 75.38 (10) | La2x—O8—Ba1x | 99.59 (10) |
O10—La2—O12vi | 152.49 (10) | Ba2v—O8—Ba1x | 80.25 (8) |
O2iv—La2—O3 | 84.47 (10) | Si2—O9—La1vii | 127.06 (16) |
O1ii—La2—O3 | 158.79 (10) | Si2—O9—Ba2v | 96.74 (14) |
O10—La2—O3 | 87.37 (10) | La1vii—O9—Ba2v | 111.40 (11) |
O12vi—La2—O3 | 98.70 (10) | Si2—O9—Ba1x | 126.06 (16) |
O2iv—La2—O3vi | 150.54 (10) | La1vii—O9—Ba1x | 98.36 (10) |
O1ii—La2—O3vi | 131.70 (10) | Ba2v—O9—Ba1x | 90.71 (9) |
O10—La2—O3vi | 89.72 (10) | Si3—O10—La2 | 117.40 (16) |
O12vi—La2—O3vi | 117.57 (10) | Si3—O10—Ba1 | 114.84 (16) |
O3—La2—O3vi | 69.26 (11) | La2—O10—Ba1 | 126.21 (13) |
O2iv—La2—O8vi | 147.75 (10) | Si3—O11—La1 | 144.91 (19) |
O1ii—La2—O8vi | 82.27 (10) | Si3—O11—Ba1x | 95.11 (15) |
O10—La2—O8vi | 126.77 (10) | La1—O11—Ba1x | 102.94 (11) |
O12vi—La2—O8vi | 74.36 (9) | Si3—O11—Ba1iii | 80.42 (12) |
O3—La2—O8vi | 116.22 (10) | La1—O11—Ba1iii | 128.16 (13) |
O3vi—La2—O8vi | 60.59 (10) | Ba1x—O11—Ba1iii | 91.45 (8) |
O2iv—La2—O8ii | 120.71 (10) | Si2—O12—La2vi | 112.74 (15) |
O1ii—La2—O8ii | 60.03 (9) | Si2—O12—Ba2ix | 100.05 (14) |
O10—La2—O8ii | 68.47 (10) | La2vi—O12—Ba2ix | 138.21 (12) |
O12vi—La2—O8ii | 119.59 (10) | Si2—O12—Ba2v | 92.84 (13) |
O3—La2—O8ii | 136.56 (9) | La2vi—O12—Ba2v | 96.65 (9) |
O3vi—La2—O8ii | 74.89 (9) | Ba2ix—O12—Ba2v | 107.19 (10) |
O8vi—La2—O8ii | 61.86 (12) | Si2—O13—Si3 | 135.1 (2) |
O2iv—La2—Si4vi | 172.02 (8) | Si2—O13—Ba2vi | 100.05 (13) |
O1ii—La2—Si4vi | 108.94 (7) | Si3—O13—Ba2vi | 108.65 (14) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z; (v) −x+2, −y+1, −z+2; (vi) −x+1, −y+1, −z+2; (vii) −x+2, −y, −z+1; (viii) −x+2, −y+1, −z+1; (ix) x, y−1, z; (x) x+1, y, z. |
Ba2Ce2O13Si4 | Z = 2 |
Mr = 875.28 | F(000) = 776 |
Triclinic, P1 | Dx = 4.974 Mg m−3 |
a = 6.7062 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.9719 (4) Å | Cell parameters from 9144 reflections |
c = 10.1565 (5) Å | θ = 3.0–28.3° |
α = 86.6118 (16)° | µ = 14.77 mm−1 |
β = 73.5658 (15)° | T = 300 K |
γ = 86.4609 (16)° | Block, purple |
V = 584.45 (5) Å3 | 0.07 × 0.06 × 0.06 mm |
Bruker Photon 100 diffractometer | 2274 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.033 |
φ and ω scans | θmax = 26.5°, θmin = 2.1° |
Absorption correction: multi-scan SADABS, Bruker | h = −8→8 |
Tmin = 0.680, Tmax = 1.000 | k = −11→11 |
22454 measured reflections | l = −12→12 |
2433 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.019 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.045 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.3644P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.002 |
2433 reflections | Δρmax = 0.67 e Å−3 |
190 parameters | Δρmin = −1.71 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.22932 (4) | 0.33177 (3) | 0.55628 (3) | 0.01095 (7) | |
Ba2 | 0.75497 (4) | 0.82700 (3) | 1.07632 (2) | 0.00868 (7) | |
Ce1 | 0.81453 (3) | 0.10888 (2) | 0.39455 (2) | 0.00558 (7) | |
Ce2 | 0.30991 (3) | 0.62213 (2) | 0.89848 (2) | 0.00600 (7) | |
Si1 | 0.60533 (17) | −0.05978 (12) | 0.68762 (11) | 0.0059 (2) | |
Si2 | 0.80096 (17) | 0.12232 (12) | 0.84495 (11) | 0.0058 (2) | |
Si3 | 0.67875 (17) | 0.38547 (12) | 0.67667 (11) | 0.0063 (2) | |
Si4 | 0.88969 (17) | 0.56702 (12) | 0.82318 (11) | 0.0057 (2) | |
O1 | 1.0257 (4) | 0.7141 (3) | 0.7968 (3) | 0.0092 (6) | |
O2 | 0.4718 (4) | −0.2078 (3) | 0.7076 (3) | 0.0098 (6) | |
O3 | 0.6655 (4) | 0.5960 (3) | 0.9359 (3) | 0.0082 (6) | |
O4 | 0.8278 (4) | −0.0869 (3) | 0.5742 (3) | 0.0082 (6) | |
O5 | 0.6519 (4) | −0.0158 (3) | 0.8335 (3) | 0.0080 (6) | |
O6 | 0.8441 (4) | 0.5163 (3) | 0.6802 (3) | 0.0077 (6) | |
O7 | 0.4719 (5) | 0.0755 (3) | 0.6349 (3) | 0.0119 (6) | |
O8 | 1.0179 (5) | 0.4293 (3) | 0.8775 (3) | 0.0114 (6) | |
O9 | 1.0275 (4) | 0.1068 (3) | 0.7399 (3) | 0.0093 (6) | |
O10 | 0.4496 (5) | 0.4585 (3) | 0.7013 (3) | 0.0135 (6) | |
O11 | 0.7835 (5) | 0.3161 (3) | 0.5320 (3) | 0.0161 (7) | |
O12 | 0.8059 (4) | 0.1275 (3) | 1.0008 (3) | 0.0092 (6) | |
O13 | 0.6683 (4) | 0.2731 (3) | 0.8127 (3) | 0.0086 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.01260 (14) | 0.00951 (13) | 0.01181 (13) | −0.00132 (9) | −0.00506 (10) | −0.00002 (9) |
Ba2 | 0.00725 (13) | 0.00832 (13) | 0.01090 (13) | 0.00008 (9) | −0.00312 (10) | −0.00161 (9) |
Ce1 | 0.00482 (12) | 0.00544 (12) | 0.00655 (12) | 0.00046 (8) | −0.00180 (9) | −0.00057 (8) |
Ce2 | 0.00489 (12) | 0.00595 (12) | 0.00684 (12) | 0.00069 (8) | −0.00148 (9) | 0.00040 (8) |
Si1 | 0.0050 (5) | 0.0066 (5) | 0.0063 (5) | −0.0009 (4) | −0.0019 (4) | −0.0007 (4) |
Si2 | 0.0049 (5) | 0.0062 (5) | 0.0057 (5) | 0.0001 (4) | −0.0007 (4) | −0.0010 (4) |
Si3 | 0.0064 (5) | 0.0061 (5) | 0.0065 (5) | −0.0001 (4) | −0.0015 (4) | −0.0012 (4) |
Si4 | 0.0040 (5) | 0.0069 (5) | 0.0060 (5) | −0.0014 (4) | −0.0012 (4) | −0.0006 (4) |
O1 | 0.0092 (15) | 0.0080 (14) | 0.0114 (15) | −0.0030 (11) | −0.0044 (12) | 0.0018 (11) |
O2 | 0.0096 (15) | 0.0098 (14) | 0.0104 (15) | −0.0036 (11) | −0.0032 (12) | 0.0006 (11) |
O3 | 0.0050 (14) | 0.0101 (14) | 0.0092 (14) | −0.0012 (11) | −0.0013 (11) | −0.0004 (11) |
O4 | 0.0044 (14) | 0.0103 (14) | 0.0100 (14) | 0.0000 (11) | −0.0020 (11) | −0.0017 (11) |
O5 | 0.0083 (14) | 0.0080 (13) | 0.0081 (14) | 0.0000 (11) | −0.0029 (11) | −0.0014 (11) |
O6 | 0.0092 (14) | 0.0087 (14) | 0.0058 (13) | −0.0031 (11) | −0.0024 (11) | −0.0012 (11) |
O7 | 0.0120 (15) | 0.0095 (14) | 0.0156 (16) | 0.0018 (11) | −0.0066 (13) | −0.0010 (12) |
O8 | 0.0112 (15) | 0.0091 (14) | 0.0149 (15) | 0.0016 (11) | −0.0055 (12) | −0.0005 (11) |
O9 | 0.0070 (14) | 0.0111 (14) | 0.0088 (14) | −0.0008 (11) | 0.0002 (12) | −0.0038 (11) |
O10 | 0.0116 (16) | 0.0131 (15) | 0.0180 (16) | 0.0032 (12) | −0.0076 (13) | −0.0044 (12) |
O11 | 0.0199 (17) | 0.0135 (15) | 0.0118 (15) | −0.0045 (12) | 0.0020 (13) | −0.0053 (12) |
O12 | 0.0107 (15) | 0.0091 (14) | 0.0079 (14) | 0.0005 (11) | −0.0028 (12) | −0.0009 (11) |
O13 | 0.0073 (14) | 0.0077 (13) | 0.0094 (14) | 0.0013 (11) | −0.0008 (11) | 0.0015 (11) |
Ba1—O10 | 2.698 (3) | Si1—Ce1i | 3.2164 (11) |
Ba1—O4i | 2.732 (3) | Si1—Ba1i | 3.4853 (11) |
Ba1—O9ii | 2.801 (3) | Si1—Ba2vi | 3.5551 (11) |
Ba1—O6iii | 2.841 (3) | Si2—O9 | 1.594 (3) |
Ba1—O7 | 2.937 (3) | Si2—O12 | 1.596 (3) |
Ba1—O6ii | 2.979 (3) | Si2—O13 | 1.641 (3) |
Ba1—O11ii | 3.081 (3) | Si2—O5 | 1.669 (3) |
Ba1—O2i | 3.078 (3) | Si2—Ba2v | 3.3573 (11) |
Ba1—O11iii | 3.235 (3) | Si2—Ba2ix | 3.4047 (11) |
Ba1—O8ii | 3.315 (3) | Si2—Ce2vi | 3.4640 (11) |
Ba1—Si3iii | 3.3274 (11) | Si2—Ba2vi | 3.5906 (11) |
Ba1—Si1i | 3.4854 (11) | Si3—O11 | 1.584 (3) |
Ba2—O3 | 2.770 (3) | Si3—O10 | 1.591 (3) |
Ba2—O12iv | 2.774 (3) | Si3—O13 | 1.649 (3) |
Ba2—O9v | 2.783 (3) | Si3—O6 | 1.672 (3) |
Ba2—O8v | 2.770 (3) | Si3—Ba1iii | 3.3275 (11) |
Ba2—O12v | 2.874 (3) | Si3—Ba1x | 3.5574 (12) |
Ba2—O13vi | 2.919 (3) | Si3—Ba2vi | 3.7919 (12) |
Ba2—O5iv | 2.997 (3) | Si4—O8 | 1.621 (3) |
Ba2—O7vi | 3.049 (3) | Si4—O1 | 1.616 (3) |
Ba2—O5vi | 3.058 (3) | Si4—O3 | 1.628 (3) |
Ba2—O1 | 3.095 (3) | Si4—O6 | 1.660 (3) |
Ba2—Si2v | 3.3574 (11) | Si4—Ce2vi | 3.1993 (11) |
Ba2—Si2iv | 3.4047 (11) | Si4—Ce2x | 3.1949 (11) |
Ce1—O11 | 2.355 (3) | Si4—Ba1x | 3.6851 (11) |
Ce1—O9vii | 2.444 (3) | O1—Ce1viii | 2.473 (3) |
Ce1—O4 | 2.473 (3) | O1—Ce2x | 2.490 (3) |
Ce1—O1viii | 2.473 (3) | O2—Ce2ix | 2.435 (3) |
Ce1—O4vii | 2.501 (3) | O2—Ce1i | 2.522 (3) |
Ce1—O2i | 2.522 (3) | O2—Ba1i | 3.078 (3) |
Ce1—O7i | 2.700 (3) | O3—Ce2vi | 2.533 (3) |
Ce1—O7 | 2.855 (3) | O4—Ce1vii | 2.501 (3) |
Ce1—Si1i | 3.2163 (11) | O4—Ba1i | 2.732 (3) |
Ce1—Si1 | 3.2381 (11) | O5—Ba2ix | 2.997 (3) |
Ce1—Ce2iii | 3.9605 (3) | O5—Ba2vi | 3.058 (3) |
Ce1—Ba1i | 3.9741 (4) | O6—Ba1iii | 2.841 (3) |
Ce2—O2iv | 2.435 (3) | O6—Ba1x | 2.979 (3) |
Ce2—O1ii | 2.490 (3) | O7—Ce1i | 2.701 (3) |
Ce2—O10 | 2.482 (3) | O7—Ba2vi | 3.049 (3) |
Ce2—O12vi | 2.510 (3) | O8—Ce2vi | 2.719 (3) |
Ce2—O3 | 2.514 (3) | O8—Ce2x | 2.751 (3) |
Ce2—O3vi | 2.533 (3) | O8—Ba2v | 2.770 (3) |
Ce2—O8vi | 2.719 (3) | O8—Ba1x | 3.315 (3) |
Ce2—O8ii | 2.751 (3) | O9—Ce1vii | 2.444 (3) |
Ce2—Si4vi | 3.1993 (11) | O9—Ba2v | 2.783 (3) |
Ce2—Si4ii | 3.1949 (11) | O9—Ba1x | 2.801 (3) |
Ce2—Si2vi | 3.4640 (11) | O11—Ba1x | 3.081 (3) |
Ce2—Ce1iii | 3.9605 (3) | O11—Ba1iii | 3.235 (3) |
Si1—O4 | 1.622 (3) | O12—Ce2vi | 2.510 (3) |
Si1—O2 | 1.618 (3) | O12—Ba2ix | 2.774 (3) |
Si1—O7 | 1.619 (3) | O12—Ba2v | 2.874 (3) |
Si1—O5 | 1.672 (3) | O13—Ba2vi | 2.919 (3) |
O10—Ba1—O4i | 147.78 (8) | O10—Ce2—Si4vi | 111.72 (7) |
O10—Ba1—O9ii | 102.71 (9) | O12vi—Ce2—Si4vi | 95.14 (7) |
O4i—Ba1—O9ii | 67.45 (8) | O3—Ce2—Si4vi | 91.88 (7) |
O10—Ba1—O6iii | 120.38 (9) | O3vi—Ce2—Si4vi | 30.26 (6) |
O4i—Ba1—O6iii | 82.14 (8) | O8vi—Ce2—Si4vi | 30.43 (6) |
O9ii—Ba1—O6iii | 133.92 (8) | O8ii—Ce2—Si4vi | 66.22 (6) |
O10—Ba1—O7 | 77.36 (8) | O2iv—Ce2—Si4ii | 99.85 (7) |
O4i—Ba1—O7 | 71.22 (8) | O1ii—Ce2—Si4ii | 29.88 (7) |
O9ii—Ba1—O7 | 59.95 (8) | O10—Ce2—Si4ii | 80.10 (7) |
O6iii—Ba1—O7 | 140.87 (8) | O12vi—Ce2—Si4ii | 96.09 (7) |
O10—Ba1—O6ii | 93.08 (8) | O3—Ce2—Si4ii | 164.70 (7) |
O4i—Ba1—O6ii | 115.19 (8) | O3vi—Ce2—Si4ii | 102.74 (7) |
O9ii—Ba1—O6ii | 84.00 (8) | O8vi—Ce2—Si4ii | 66.62 (7) |
O6iii—Ba1—O6ii | 78.51 (8) | O8ii—Ce2—Si4ii | 30.49 (6) |
O7—Ba1—O6ii | 138.65 (8) | Si4vi—Ce2—Si4ii | 85.43 (3) |
O10—Ba1—O11ii | 141.87 (8) | O2iv—Ce2—Si2vi | 97.48 (7) |
O4i—Ba1—O11ii | 66.32 (8) | O1ii—Ce2—Si2vi | 95.93 (7) |
O9ii—Ba1—O11ii | 71.17 (8) | O10—Ce2—Si2vi | 170.00 (7) |
O6iii—Ba1—O11ii | 65.05 (8) | O12vi—Ce2—Si2vi | 25.06 (7) |
O7—Ba1—O11ii | 124.23 (8) | O3—Ce2—Si2vi | 85.24 (7) |
O6ii—Ba1—O11ii | 49.36 (7) | O3vi—Ce2—Si2vi | 92.75 (7) |
O10—Ba1—O2i | 109.51 (8) | O8vi—Ce2—Si2vi | 62.47 (6) |
O4i—Ba1—O2i | 53.90 (8) | O8ii—Ce2—Si2vi | 121.34 (6) |
O9ii—Ba1—O2i | 112.80 (8) | Si4vi—Ce2—Si2vi | 74.83 (3) |
O6iii—Ba1—O2i | 69.31 (8) | Si4ii—Ce2—Si2vi | 108.46 (3) |
O7—Ba1—O2i | 71.86 (8) | O2iv—Ce2—Ce1iii | 37.72 (7) |
O6ii—Ba1—O2i | 146.90 (8) | O1ii—Ce2—Ce1iii | 36.91 (7) |
O11ii—Ba1—O2i | 107.32 (8) | O10—Ce2—Ce1iii | 81.17 (7) |
O10—Ba1—O11iii | 75.19 (8) | O12vi—Ce2—Ce1iii | 72.71 (6) |
O4i—Ba1—O11iii | 130.87 (8) | O3—Ce2—Ce1iii | 122.32 (6) |
O9ii—Ba1—O11iii | 145.09 (8) | O3vi—Ce2—Ce1iii | 165.08 (6) |
O6iii—Ba1—O11iii | 48.73 (8) | O8vi—Ce2—Ce1iii | 115.49 (6) |
O7—Ba1—O11iii | 146.79 (8) | O8ii—Ce2—Ce1iii | 90.72 (6) |
O6ii—Ba1—O11iii | 61.61 (8) | Si4vi—Ce2—Ce1iii | 144.71 (2) |
O11ii—Ba1—O11iii | 88.98 (8) | Si4ii—Ce2—Ce1iii | 63.87 (2) |
O2i—Ba1—O11iii | 100.24 (8) | Si2vi—Ce2—Ce1iii | 97.755 (19) |
O10—Ba1—O8ii | 57.89 (8) | O4—Si1—O2 | 109.82 (15) |
O4i—Ba1—O8ii | 130.19 (8) | O4—Si1—O7 | 109.99 (16) |
O9ii—Ba1—O8ii | 64.14 (7) | O2—Si1—O7 | 107.14 (16) |
O6iii—Ba1—O8ii | 125.32 (7) | O4—Si1—O5 | 107.84 (15) |
O7—Ba1—O8ii | 93.80 (8) | O2—Si1—O5 | 112.15 (15) |
O6ii—Ba1—O8ii | 49.39 (7) | O7—Si1—O5 | 109.91 (15) |
O11ii—Ba1—O8ii | 87.41 (8) | O4—Si1—Ce1i | 118.93 (11) |
O2i—Ba1—O8ii | 163.46 (7) | O2—Si1—Ce1i | 50.61 (11) |
O11iii—Ba1—O8ii | 87.21 (7) | O7—Si1—Ce1i | 56.99 (11) |
O10—Ba1—Si3iii | 90.54 (7) | O5—Si1—Ce1i | 133.17 (11) |
O4i—Ba1—Si3iii | 107.17 (6) | O4—Si1—Ce1 | 48.21 (10) |
O9ii—Ba1—Si3iii | 161.95 (6) | O2—Si1—Ce1 | 124.67 (11) |
O6iii—Ba1—Si3iii | 30.17 (6) | O7—Si1—Ce1 | 61.80 (11) |
O7—Ba1—Si3iii | 136.25 (6) | O5—Si1—Ce1 | 122.69 (11) |
O6ii—Ba1—Si3iii | 83.08 (6) | Ce1i—Si1—Ce1 | 92.15 (3) |
O11ii—Ba1—Si3iii | 90.83 (6) | O4—Si1—Ba1i | 49.68 (10) |
O2i—Ba1—Si3iii | 73.14 (6) | O2—Si1—Ba1i | 62.01 (11) |
O11iii—Ba1—Si3iii | 27.89 (5) | O7—Si1—Ba1i | 111.31 (11) |
O8ii—Ba1—Si3iii | 115.09 (5) | O5—Si1—Ba1i | 138.03 (11) |
O10—Ba1—Si1i | 128.72 (6) | Ce1i—Si1—Ba1i | 78.10 (2) |
O4i—Ba1—Si1i | 26.91 (6) | Ce1—Si1—Ba1i | 72.36 (2) |
O9ii—Ba1—Si1i | 87.47 (6) | O4—Si1—Ba2vi | 150.66 (11) |
O6iii—Ba1—Si1i | 78.45 (6) | O2—Si1—Ba2vi | 99.51 (11) |
O7—Ba1—Si1i | 64.75 (6) | O7—Si1—Ba2vi | 58.81 (11) |
O6ii—Ba1—Si1i | 138.18 (6) | O5—Si1—Ba2vi | 59.23 (10) |
O11ii—Ba1—Si1i | 89.19 (6) | Ce1i—Si1—Ba2vi | 79.52 (2) |
O2i—Ba1—Si1i | 27.66 (5) | Ce1—Si1—Ba2vi | 113.43 (3) |
O11iii—Ba1—Si1i | 121.59 (6) | Ba1i—Si1—Ba2vi | 157.10 (3) |
O8ii—Ba1—Si1i | 150.93 (5) | O9—Si2—O12 | 112.84 (16) |
Si3iii—Ba1—Si1i | 93.81 (3) | O9—Si2—O13 | 112.73 (16) |
O3—Ba2—O12iv | 130.42 (8) | O12—Si2—O13 | 106.88 (15) |
O3—Ba2—O9v | 143.04 (8) | O9—Si2—O5 | 112.06 (15) |
O12iv—Ba2—O9v | 82.13 (8) | O12—Si2—O5 | 108.51 (15) |
O3—Ba2—O8v | 70.86 (8) | O13—Si2—O5 | 103.24 (15) |
O12iv—Ba2—O8v | 140.65 (9) | O9—Si2—Ba2v | 55.46 (11) |
O9v—Ba2—O8v | 72.32 (8) | O12—Si2—Ba2v | 58.75 (11) |
O3—Ba2—O12v | 111.21 (8) | O13—Si2—Ba2v | 116.94 (11) |
O12iv—Ba2—O12v | 72.89 (9) | O5—Si2—Ba2v | 139.73 (11) |
O9v—Ba2—O12v | 56.01 (8) | O9—Si2—Ba2ix | 107.18 (11) |
O8v—Ba2—O12v | 68.08 (8) | O12—Si2—Ba2ix | 53.64 (10) |
O3—Ba2—O13vi | 66.35 (8) | O13—Si2—Ba2ix | 140.06 (11) |
O12iv—Ba2—O13vi | 118.00 (8) | O5—Si2—Ba2ix | 61.65 (10) |
O9v—Ba2—O13vi | 118.27 (8) | Ba2v—Si2—Ba2ix | 84.44 (3) |
O8v—Ba2—O13vi | 100.55 (8) | O9—Si2—Ce2vi | 120.83 (11) |
O12v—Ba2—O13vi | 168.07 (8) | O12—Si2—Ce2vi | 41.77 (10) |
O3—Ba2—O5iv | 76.59 (8) | O13—Si2—Ce2vi | 66.17 (10) |
O12iv—Ba2—O5iv | 54.50 (8) | O5—Si2—Ce2vi | 126.09 (11) |
O9v—Ba2—O5iv | 135.88 (8) | Ba2v—Si2—Ce2vi | 72.39 (2) |
O8v—Ba2—O5iv | 136.30 (8) | Ba2ix—Si2—Ce2vi | 92.21 (3) |
O12v—Ba2—O5iv | 98.79 (8) | O9—Si2—Ba2vi | 152.41 (12) |
O13vi—Ba2—O5iv | 92.03 (8) | O12—Si2—Ba2vi | 94.63 (11) |
O3—Ba2—O7vi | 128.31 (8) | O13—Si2—Ba2vi | 53.15 (10) |
O12iv—Ba2—O7vi | 87.32 (8) | O5—Si2—Ba2vi | 58.15 (10) |
O9v—Ba2—O7vi | 58.73 (8) | Ba2v—Si2—Ba2vi | 149.66 (3) |
O8v—Ba2—O7vi | 103.47 (8) | Ba2ix—Si2—Ba2vi | 90.87 (3) |
O12v—Ba2—O7vi | 113.47 (8) | Ce2vi—Si2—Ba2vi | 77.88 (2) |
O13vi—Ba2—O7vi | 64.48 (8) | O11—Si3—O10 | 117.02 (17) |
O5iv—Ba2—O7vi | 119.60 (8) | O11—Si3—O13 | 116.17 (16) |
O3—Ba2—O5vi | 105.08 (8) | O10—Si3—O13 | 105.06 (16) |
O12iv—Ba2—O5vi | 67.36 (8) | O11—Si3—O6 | 102.04 (16) |
O9v—Ba2—O5vi | 103.98 (8) | O10—Si3—O6 | 110.02 (15) |
O8v—Ba2—O5vi | 147.20 (8) | O13—Si3—O6 | 105.99 (15) |
O12v—Ba2—O5vi | 137.81 (8) | O11—Si3—Ba1iii | 72.82 (12) |
O13vi—Ba2—O5vi | 51.40 (7) | O10—Si3—Ba1iii | 79.92 (12) |
O5iv—Ba2—O5vi | 69.16 (9) | O13—Si3—Ba1iii | 164.34 (11) |
O7vi—Ba2—O5vi | 52.35 (8) | O6—Si3—Ba1iii | 58.59 (10) |
O3—Ba2—O1 | 53.94 (8) | O11—Si3—Ba1x | 59.79 (12) |
O12iv—Ba2—O1 | 94.87 (8) | O10—Si3—Ba1x | 161.33 (13) |
O9v—Ba2—O1 | 115.45 (8) | O13—Si3—Ba1x | 91.85 (11) |
O8v—Ba2—O1 | 71.03 (8) | O6—Si3—Ba1x | 56.45 (10) |
O12v—Ba2—O1 | 61.61 (8) | Ba1iii—Si3—Ba1x | 81.71 (3) |
O13vi—Ba2—O1 | 119.34 (8) | O11—Si3—Ba1 | 78.24 (13) |
O5iv—Ba2—O1 | 66.37 (7) | O10—Si3—Ba1 | 43.30 (11) |
O7vi—Ba2—O1 | 173.49 (8) | O13—Si3—Ba1 | 108.75 (11) |
O5vi—Ba2—O1 | 134.10 (7) | O6—Si3—Ba1 | 140.87 (11) |
O3—Ba2—Si2v | 128.11 (6) | Ba1iii—Si3—Ba1 | 85.19 (3) |
O12iv—Ba2—Si2v | 79.66 (6) | Ba1x—Si3—Ba1 | 138.01 (3) |
O9v—Ba2—Si2v | 28.15 (6) | O11—Si3—Ba2vi | 117.06 (12) |
O8v—Ba2—Si2v | 63.64 (6) | O10—Si3—Ba2vi | 63.59 (12) |
O12v—Ba2—Si2v | 28.34 (6) | O13—Si3—Ba2vi | 46.68 (10) |
O13vi—Ba2—Si2v | 143.81 (6) | O6—Si3—Ba2vi | 139.01 (11) |
O5iv—Ba2—Si2v | 122.34 (6) | Ba1iii—Si3—Ba2vi | 142.92 (3) |
O7vi—Ba2—Si2v | 86.77 (6) | Ba1x—Si3—Ba2vi | 135.03 (3) |
O5vi—Ba2—Si2v | 126.65 (6) | Ba1—Si3—Ba2vi | 64.161 (19) |
O1—Ba2—Si2v | 87.60 (6) | O8—Si4—O1 | 109.00 (16) |
O3—Ba2—Si2iv | 103.01 (6) | O8—Si4—O3 | 109.58 (16) |
O12iv—Ba2—Si2iv | 27.60 (6) | O1—Si4—O3 | 111.10 (15) |
O9v—Ba2—Si2iv | 106.62 (6) | O8—Si4—O6 | 107.57 (15) |
O8v—Ba2—Si2iv | 138.83 (7) | O1—Si4—O6 | 111.85 (15) |
O12v—Ba2—Si2iv | 77.53 (6) | O3—Si4—O6 | 107.65 (15) |
O13vi—Ba2—Si2iv | 114.36 (6) | O8—Si4—Ce2vi | 58.17 (11) |
O5iv—Ba2—Si2iv | 29.35 (6) | O1—Si4—Ce2vi | 130.27 (11) |
O7vi—Ba2—Si2iv | 110.71 (6) | O3—Si4—Ce2vi | 51.59 (10) |
O5vi—Ba2—Si2iv | 73.93 (6) | O6—Si4—Ce2vi | 117.83 (11) |
O1—Ba2—Si2iv | 73.09 (5) | O8—Si4—Ce2x | 59.45 (11) |
Si2v—Ba2—Si2iv | 95.56 (3) | O1—Si4—Ce2x | 50.12 (10) |
O11—Ce1—O9vii | 159.49 (11) | O3—Si4—Ce2x | 119.97 (11) |
O11—Ce1—O4 | 97.12 (10) | O6—Si4—Ce2x | 132.34 (11) |
O9vii—Ce1—O4 | 77.35 (9) | Ce2vi—Si4—Ce2x | 94.57 (3) |
O11—Ce1—O1viii | 84.34 (10) | O8—Si4—Ba2 | 107.35 (11) |
O9vii—Ce1—O1viii | 92.01 (9) | O1—Si4—Ba2 | 63.27 (11) |
O4—Ce1—O1viii | 153.45 (9) | O3—Si4—Ba2 | 51.79 (10) |
O11—Ce1—O4vii | 82.16 (10) | O6—Si4—Ba2 | 144.10 (11) |
O9vii—Ce1—O4vii | 77.37 (9) | Ce2vi—Si4—Ba2 | 75.06 (2) |
O4—Ce1—O4vii | 70.45 (11) | Ce2x—Si4—Ba2 | 74.34 (2) |
O1viii—Ce1—O4vii | 83.58 (9) | O8—Si4—Ba1x | 64.09 (11) |
O11—Ce1—O2i | 93.55 (10) | O1—Si4—Ba1x | 99.32 (11) |
O9vii—Ce1—O2i | 104.76 (9) | O3—Si4—Ba1x | 148.91 (11) |
O4—Ce1—O2i | 132.62 (9) | O6—Si4—Ba1x | 52.43 (10) |
O1viii—Ce1—O2i | 73.41 (10) | Ce2vi—Si4—Ba1x | 112.05 (3) |
O4vii—Ce1—O2i | 156.92 (9) | Ce2x—Si4—Ba1x | 84.34 (2) |
O11—Ce1—O7i | 131.37 (10) | Ba2—Si4—Ba1x | 158.15 (3) |
O9vii—Ce1—O7i | 67.59 (9) | Si4—O1—Ce1viii | 138.86 (16) |
O4—Ce1—O7i | 79.27 (9) | Si4—O1—Ce2x | 99.99 (13) |
O1viii—Ce1—O7i | 119.38 (9) | Ce1viii—O1—Ce2x | 105.89 (11) |
O4vii—Ce1—O7i | 137.76 (9) | Si4—O1—Ba2 | 88.92 (12) |
O2i—Ce1—O7i | 59.72 (9) | Ce1viii—O1—Ba2 | 121.12 (10) |
O11—Ce1—O7 | 70.33 (10) | Ce2x—O1—Ba2 | 91.71 (8) |
O9vii—Ce1—O7 | 120.76 (9) | Si1—O2—Ce2ix | 136.12 (16) |
O4—Ce1—O7 | 59.24 (9) | Si1—O2—Ce1i | 99.65 (13) |
O1viii—Ce1—O7 | 143.28 (9) | Ce2ix—O2—Ce1i | 106.05 (11) |
O4vii—Ce1—O7 | 117.31 (9) | Si1—O2—Ba1i | 90.32 (12) |
O2i—Ce1—O7 | 81.86 (9) | Ce2ix—O2—Ba1i | 120.04 (10) |
O7i—Ce1—O7 | 66.42 (10) | Ce1i—O2—Ba1i | 97.55 (9) |
O11—Ce1—Si1i | 112.57 (8) | Si4—O3—Ce2 | 128.51 (15) |
O9vii—Ce1—Si1i | 87.92 (7) | Si4—O3—Ce2vi | 98.15 (13) |
O4—Ce1—Si1i | 105.55 (7) | Ce2—O3—Ce2vi | 111.04 (10) |
O1viii—Ce1—Si1i | 98.19 (7) | Si4—O3—Ba2 | 100.71 (13) |
O4vii—Ce1—Si1i | 165.25 (7) | Ce2—O3—Ba2 | 114.04 (10) |
O2i—Ce1—Si1i | 29.74 (7) | Ce2vi—O3—Ba2 | 100.00 (9) |
O7i—Ce1—Si1i | 30.18 (6) | Si1—O4—Ce1 | 102.52 (13) |
O7—Ce1—Si1i | 69.42 (6) | Si1—O4—Ce1vii | 129.27 (15) |
O11—Ce1—Si1 | 82.72 (8) | Ce1—O4—Ce1vii | 109.55 (11) |
O9vii—Ce1—Si1 | 99.73 (7) | Si1—O4—Ba1i | 103.42 (13) |
O4—Ce1—Si1 | 29.27 (7) | Ce1—O4—Ba1i | 99.43 (9) |
O1viii—Ce1—Si1 | 167.01 (7) | Ce1vii—O4—Ba1i | 108.67 (10) |
O4vii—Ce1—Si1 | 93.52 (7) | Si2—O5—Si1 | 124.05 (18) |
O2i—Ce1—Si1 | 108.49 (7) | Si2—O5—Ba2ix | 89.00 (11) |
O7i—Ce1—Si1 | 70.85 (7) | Si1—O5—Ba2ix | 138.38 (14) |
O7—Ce1—Si1 | 29.98 (6) | Si2—O5—Ba2vi | 94.24 (11) |
Si1i—Ce1—Si1 | 87.85 (3) | Si1—O5—Ba2vi | 92.76 (12) |
O11—Ce1—Ce2iii | 89.41 (8) | Ba2ix—O5—Ba2vi | 110.84 (9) |
O9vii—Ce1—Ce2iii | 99.86 (7) | Si4—O6—Si3 | 123.66 (18) |
O4—Ce1—Ce2iii | 167.88 (6) | Si4—O6—Ba1iii | 135.50 (14) |
O1viii—Ce1—Ce2iii | 37.20 (7) | Si3—O6—Ba1iii | 91.24 (12) |
O4vii—Ce1—Ce2iii | 120.78 (7) | Si4—O6—Ba1x | 101.36 (12) |
O2i—Ce1—Ce2iii | 36.22 (6) | Si3—O6—Ba1x | 95.66 (12) |
O7i—Ce1—Ce2iii | 88.74 (6) | Ba1iii—O6—Ba1x | 101.49 (8) |
O7—Ce1—Ce2iii | 114.21 (6) | Si1—O7—Ce1i | 92.83 (13) |
Si1i—Ce1—Ce2iii | 62.41 (2) | Si1—O7—Ce1 | 88.22 (13) |
Si1—Ce1—Ce2iii | 143.45 (2) | Ce1i—O7—Ce1 | 113.58 (10) |
O11—Ce1—Ba1i | 138.35 (8) | Si1—O7—Ba1 | 176.04 (16) |
O9vii—Ce1—Ba1i | 44.23 (7) | Ce1i—O7—Ba1 | 89.55 (8) |
O4—Ce1—Ba1i | 42.70 (6) | Ce1—O7—Ba1 | 93.74 (9) |
O1viii—Ce1—Ba1i | 135.77 (7) | Si1—O7—Ba2vi | 94.18 (13) |
O4vii—Ce1—Ba1i | 90.68 (6) | Ce1i—O7—Ba2vi | 97.79 (9) |
O2i—Ce1—Ba1i | 106.97 (6) | Ce1—O7—Ba2vi | 148.40 (11) |
O7i—Ce1—Ba1i | 47.65 (6) | Ba1—O7—Ba2vi | 82.35 (7) |
O7—Ce1—Ba1i | 77.08 (6) | Si4—O8—Ce2vi | 91.40 (13) |
Si1i—Ce1—Ba1i | 77.80 (2) | Si4—O8—Ce2x | 90.06 (12) |
Si1—Ce1—Ba1i | 56.698 (19) | Ce2vi—O8—Ce2x | 118.37 (10) |
Ce2iii—Ce1—Ba1i | 128.165 (8) | Si4—O8—Ba2v | 169.47 (17) |
O2iv—Ce2—O1ii | 74.62 (10) | Ce2vi—O8—Ba2v | 94.46 (9) |
O2iv—Ce2—O10 | 75.54 (10) | Ce2x—O8—Ba2v | 94.83 (9) |
O1ii—Ce2—O10 | 89.16 (9) | Si4—O8—Ba1x | 89.81 (12) |
O2iv—Ce2—O12vi | 78.17 (9) | Ce2vi—O8—Ba1x | 142.43 (11) |
O1ii—Ce2—O12vi | 75.54 (9) | Ce2x—O8—Ba1x | 99.17 (9) |
O10—Ce2—O12vi | 152.31 (10) | Ba2v—O8—Ba1x | 80.22 (7) |
O2iv—Ce2—O3 | 84.63 (9) | Si2—O9—Ce1vii | 127.51 (15) |
O1ii—Ce2—O3 | 159.21 (9) | Si2—O9—Ba2v | 96.40 (12) |
O10—Ce2—O3 | 86.96 (9) | Ce1vii—O9—Ba2v | 112.05 (10) |
O12vi—Ce2—O3 | 99.15 (9) | Si2—O9—Ba1x | 125.95 (15) |
O2iv—Ce2—O3vi | 150.77 (9) | Ce1vii—O9—Ba1x | 98.29 (9) |
O1ii—Ce2—O3vi | 131.52 (9) | Ba2v—O9—Ba1x | 89.81 (8) |
O10—Ce2—O3vi | 90.28 (9) | Si3—O10—Ce2 | 118.56 (15) |
O12vi—Ce2—O3vi | 117.18 (9) | Si3—O10—Ba1 | 112.84 (14) |
O3—Ce2—O3vi | 68.96 (10) | Ce2—O10—Ba1 | 126.81 (12) |
O2iv—Ce2—O8vi | 147.39 (9) | Si3—O11—Ce1 | 146.62 (18) |
O1ii—Ce2—O8vi | 81.87 (9) | Si3—O11—Ba1x | 93.84 (14) |
O10—Ce2—O8vi | 126.99 (9) | Ce1—O11—Ba1x | 102.16 (11) |
O12vi—Ce2—O8vi | 74.24 (9) | Si3—O11—Ba1iii | 79.30 (12) |
O3—Ce2—O8vi | 116.49 (9) | Ce1—O11—Ba1iii | 128.76 (12) |
O3vi—Ce2—O8vi | 60.61 (9) | Ba1x—O11—Ba1iii | 91.02 (8) |
O2iv—Ce2—O8ii | 121.14 (9) | Si2—O12—Ce2vi | 113.17 (14) |
O1ii—Ce2—O8ii | 60.13 (9) | Si2—O12—Ba2ix | 98.76 (13) |
O10—Ce2—O8ii | 68.66 (9) | Ce2vi—O12—Ba2ix | 138.97 (11) |
O12vi—Ce2—O8ii | 119.73 (9) | Si2—O12—Ba2v | 92.91 (13) |
O3—Ce2—O8ii | 135.84 (9) | Ce2vi—O12—Ba2v | 96.67 (9) |
O3vi—Ce2—O8ii | 74.73 (9) | Ba2ix—O12—Ba2v | 107.11 (9) |
O8vi—Ce2—O8ii | 61.63 (11) | Si3—O13—Si2 | 135.08 (18) |
O2iv—Ce2—Si4vi | 171.83 (7) | Si3—O13—Ba2vi | 109.05 (13) |
O1ii—Ce2—Si4vi | 108.50 (7) | Si2—O13—Ba2vi | 100.11 (12) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z; (v) −x+2, −y+1, −z+2; (vi) −x+1, −y+1, −z+2; (vii) −x+2, −y, −z+1; (viii) −x+2, −y+1, −z+1; (ix) x, y−1, z; (x) x+1, y, z. |
Ba2O13Pr2Si4 | Z = 2 |
Mr = 876.86 | F(000) = 780 |
Triclinic, P1 | Dx = 5.020 Mg m−3 |
a = 6.6880 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.9530 (4) Å | Cell parameters from 9962 reflections |
c = 10.1324 (4) Å | θ = 3.0–28.3° |
α = 86.5023 (13)° | µ = 15.43 mm−1 |
β = 73.5481 (13)° | T = 300 K |
γ = 86.2929 (15)° | Block, green |
V = 580.07 (4) Å3 | 0.07 × 0.06 × 0.06 mm |
Bruker Photon 100 diffractometer | 2147 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.031 |
φ and ω scans | θmax = 26.0°, θmin = 2.3° |
Absorption correction: multi-scan SADABS, Bruker | h = −8→8 |
Tmin = 0.774, Tmax = 1.000 | k = −11→11 |
11990 measured reflections | l = −12→11 |
2269 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.021 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.3644P] where P = (Fo2 + 2Fc2)/3 |
S = 1.17 | (Δ/σ)max = 0.001 |
2269 reflections | Δρmax = 0.86 e Å−3 |
190 parameters | Δρmin = −2.14 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.23060 (4) | 0.33073 (3) | 0.55602 (3) | 0.00879 (9) | |
Ba2 | 0.75491 (4) | 0.82697 (3) | 1.07556 (3) | 0.00663 (8) | |
Pr1 | 0.81448 (3) | 0.10886 (2) | 0.39470 (2) | 0.00403 (8) | |
Pr2 | 0.30991 (4) | 0.62219 (2) | 0.89810 (2) | 0.00470 (8) | |
Si1 | 0.60516 (18) | −0.05981 (13) | 0.68737 (12) | 0.0040 (2) | |
Si2 | 0.80098 (18) | 0.12217 (13) | 0.84505 (12) | 0.0039 (2) | |
Si3 | 0.67880 (19) | 0.38591 (13) | 0.67647 (12) | 0.0047 (2) | |
Si4 | 0.88985 (18) | 0.56690 (13) | 0.82303 (12) | 0.0040 (2) | |
O1 | 1.0269 (5) | 0.7142 (3) | 0.7971 (3) | 0.0075 (6) | |
O2 | 0.4706 (5) | −0.2074 (3) | 0.7077 (3) | 0.0082 (6) | |
O3 | 0.6645 (5) | 0.5952 (3) | 0.9360 (3) | 0.0073 (6) | |
O4 | 0.8282 (5) | −0.0867 (3) | 0.5743 (3) | 0.0054 (6) | |
O5 | 0.6516 (5) | −0.0157 (3) | 0.8339 (3) | 0.0053 (6) | |
O6 | 0.8453 (5) | 0.5158 (3) | 0.6797 (3) | 0.0066 (6) | |
O7 | 0.4712 (5) | 0.0758 (3) | 0.6341 (3) | 0.0103 (7) | |
O8 | 1.0182 (5) | 0.4291 (3) | 0.8781 (3) | 0.0108 (7) | |
O9 | 1.0274 (5) | 0.1054 (3) | 0.7403 (3) | 0.0081 (6) | |
O10 | 0.4495 (5) | 0.4605 (3) | 0.7012 (3) | 0.0119 (7) | |
O11 | 0.7830 (5) | 0.3160 (3) | 0.5313 (3) | 0.0141 (7) | |
O12 | 0.8048 (5) | 0.1285 (3) | 1.0016 (3) | 0.0072 (6) | |
O13 | 0.6678 (4) | 0.2737 (3) | 0.8127 (3) | 0.0064 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.01098 (15) | 0.00706 (14) | 0.00949 (15) | −0.00148 (10) | −0.00467 (11) | 0.00039 (10) |
Ba2 | 0.00573 (14) | 0.00606 (14) | 0.00867 (14) | −0.00025 (10) | −0.00284 (11) | −0.00097 (10) |
Pr1 | 0.00378 (13) | 0.00355 (13) | 0.00507 (13) | −0.00003 (9) | −0.00177 (10) | −0.00033 (9) |
Pr2 | 0.00444 (13) | 0.00414 (13) | 0.00543 (13) | 0.00033 (9) | −0.00157 (10) | 0.00080 (9) |
Si1 | 0.0038 (6) | 0.0045 (5) | 0.0037 (5) | −0.0015 (4) | −0.0008 (5) | −0.0007 (4) |
Si2 | 0.0036 (6) | 0.0036 (5) | 0.0041 (5) | −0.0011 (4) | −0.0003 (5) | −0.0003 (4) |
Si3 | 0.0060 (6) | 0.0036 (5) | 0.0046 (6) | −0.0011 (4) | −0.0015 (5) | −0.0009 (4) |
Si4 | 0.0035 (6) | 0.0044 (5) | 0.0044 (6) | −0.0014 (4) | −0.0013 (5) | −0.0006 (4) |
O1 | 0.0083 (16) | 0.0073 (15) | 0.0081 (15) | −0.0035 (12) | −0.0039 (13) | 0.0013 (12) |
O2 | 0.0088 (16) | 0.0076 (15) | 0.0087 (15) | −0.0049 (12) | −0.0026 (13) | 0.0010 (12) |
O3 | 0.0058 (15) | 0.0090 (15) | 0.0066 (15) | −0.0018 (12) | −0.0007 (12) | −0.0002 (12) |
O4 | 0.0039 (15) | 0.0076 (15) | 0.0046 (14) | −0.0003 (11) | −0.0008 (12) | −0.0016 (11) |
O5 | 0.0046 (15) | 0.0063 (14) | 0.0055 (15) | −0.0036 (11) | −0.0014 (12) | −0.0010 (11) |
O6 | 0.0068 (15) | 0.0095 (15) | 0.0045 (14) | −0.0041 (12) | −0.0025 (12) | −0.0006 (11) |
O7 | 0.0098 (16) | 0.0077 (15) | 0.0149 (17) | 0.0027 (12) | −0.0065 (13) | −0.0012 (12) |
O8 | 0.0119 (16) | 0.0090 (15) | 0.0138 (16) | 0.0019 (12) | −0.0079 (14) | −0.0009 (12) |
O9 | 0.0085 (15) | 0.0074 (15) | 0.0081 (15) | −0.0001 (12) | −0.0010 (13) | −0.0033 (11) |
O10 | 0.0112 (17) | 0.0083 (15) | 0.0187 (17) | 0.0020 (12) | −0.0077 (14) | −0.0053 (12) |
O11 | 0.0197 (18) | 0.0103 (16) | 0.0100 (16) | −0.0025 (13) | 0.0013 (14) | −0.0062 (12) |
O12 | 0.0092 (16) | 0.0076 (15) | 0.0049 (14) | −0.0014 (12) | −0.0021 (12) | −0.0002 (11) |
O13 | 0.0047 (14) | 0.0056 (14) | 0.0071 (15) | 0.0008 (11) | 0.0006 (12) | 0.0015 (11) |
Ba1—O10 | 2.703 (3) | Si1—Pr1i | 3.2073 (12) |
Ba1—O4i | 2.725 (3) | Si1—Ba1i | 3.4673 (12) |
Ba1—O9ii | 2.804 (3) | Si1—Ba2vi | 3.5497 (12) |
Ba1—O6iii | 2.837 (3) | Si2—O9 | 1.588 (3) |
Ba1—O7 | 2.907 (3) | Si2—O12 | 1.598 (3) |
Ba1—O6ii | 2.971 (3) | Si2—O13 | 1.642 (3) |
Ba1—O2i | 3.066 (3) | Si2—O5 | 1.666 (3) |
Ba1—O11ii | 3.086 (3) | Si2—Ba2iv | 3.3540 (12) |
Ba1—O11iii | 3.234 (3) | Si2—Ba2ix | 3.3881 (12) |
Ba1—O8ii | 3.318 (3) | Si2—Pr2vi | 3.4605 (12) |
Ba1—Si3iii | 3.3187 (12) | Si2—Ba2vi | 3.5788 (12) |
Ba1—Si1i | 3.4673 (12) | Si3—O11 | 1.586 (3) |
Ba2—O8iv | 2.757 (3) | Si3—O10 | 1.591 (3) |
Ba2—O3 | 2.771 (3) | Si3—O13 | 1.644 (3) |
Ba2—O12v | 2.773 (3) | Si3—O6 | 1.670 (3) |
Ba2—O9iv | 2.785 (3) | Si3—Ba1iii | 3.3187 (12) |
Ba2—O12iv | 2.872 (3) | Si3—Ba1x | 3.5553 (12) |
Ba2—O13vi | 2.912 (3) | Si3—Ba2vi | 3.7896 (12) |
Ba2—O5v | 2.977 (3) | Si4—O8 | 1.619 (3) |
Ba2—O5vi | 3.045 (3) | Si4—O1 | 1.620 (3) |
Ba2—O7vi | 3.053 (3) | Si4—O3 | 1.629 (3) |
Ba2—O1 | 3.081 (3) | Si4—O6 | 1.658 (3) |
Ba2—Si2iv | 3.3540 (12) | Si4—Pr2x | 3.1863 (12) |
Ba2—Si2v | 3.3881 (12) | Si4—Pr2vi | 3.1946 (12) |
Pr1—O11 | 2.345 (3) | Si4—Ba1x | 3.6832 (12) |
Pr1—O9vii | 2.431 (3) | O1—Pr1viii | 2.467 (3) |
Pr1—O4 | 2.463 (3) | O1—Pr2x | 2.471 (3) |
Pr1—O1viii | 2.467 (3) | O2—Pr2ix | 2.425 (3) |
Pr1—O4vii | 2.491 (3) | O2—Pr1i | 2.506 (3) |
Pr1—O2i | 2.506 (3) | O2—Ba1i | 3.066 (3) |
Pr1—O7i | 2.693 (3) | O3—Pr2vi | 2.522 (3) |
Pr1—O7 | 2.844 (3) | O4—Pr1vii | 2.491 (3) |
Pr1—Si1i | 3.2072 (12) | O4—Ba1i | 2.725 (3) |
Pr1—Si1 | 3.2264 (12) | O5—Ba2ix | 2.978 (3) |
Pr1—Pr2iii | 3.9445 (3) | O5—Ba2vi | 3.045 (3) |
Pr1—Ba1i | 3.9570 (4) | O6—Ba1iii | 2.837 (3) |
Pr2—O2v | 2.425 (3) | O6—Ba1x | 2.971 (3) |
Pr2—O10 | 2.463 (3) | O7—Pr1i | 2.693 (3) |
Pr2—O1ii | 2.471 (3) | O7—Ba2vi | 3.053 (3) |
Pr2—O12vi | 2.493 (3) | O8—Pr2vi | 2.711 (3) |
Pr2—O3 | 2.502 (3) | O8—Pr2x | 2.746 (3) |
Pr2—O3vi | 2.522 (3) | O8—Ba2iv | 2.757 (3) |
Pr2—O8vi | 2.711 (3) | O8—Ba1x | 3.318 (3) |
Pr2—O8ii | 2.746 (3) | O9—Pr1vii | 2.431 (3) |
Pr2—Si4ii | 3.1862 (12) | O9—Ba2iv | 2.785 (3) |
Pr2—Si4vi | 3.1947 (12) | O9—Ba1x | 2.804 (3) |
Pr2—Si2vi | 3.4605 (12) | O11—Ba1x | 3.086 (3) |
Pr2—Pr1iii | 3.9445 (3) | O11—Ba1iii | 3.234 (3) |
Si1—O4 | 1.617 (3) | O12—Pr2vi | 2.493 (3) |
Si1—O2 | 1.617 (3) | O12—Ba2ix | 2.773 (3) |
Si1—O7 | 1.619 (3) | O12—Ba2iv | 2.872 (3) |
Si1—O5 | 1.675 (3) | O13—Ba2vi | 2.912 (3) |
O10—Ba1—O4i | 148.68 (9) | O1ii—Pr2—Si4ii | 30.03 (7) |
O10—Ba1—O9ii | 103.11 (9) | O12vi—Pr2—Si4ii | 96.37 (7) |
O4i—Ba1—O9ii | 67.42 (9) | O3—Pr2—Si4ii | 164.53 (7) |
O10—Ba1—O6iii | 119.87 (9) | O3vi—Pr2—Si4ii | 102.81 (7) |
O4i—Ba1—O6iii | 82.18 (8) | O8vi—Pr2—Si4ii | 66.52 (7) |
O9ii—Ba1—O6iii | 133.70 (9) | O8ii—Pr2—Si4ii | 30.54 (6) |
O10—Ba1—O7 | 78.08 (9) | O2v—Pr2—Si4vi | 171.69 (8) |
O4i—Ba1—O7 | 71.38 (9) | O10—Pr2—Si4vi | 112.03 (8) |
O9ii—Ba1—O7 | 60.00 (9) | O1ii—Pr2—Si4vi | 108.48 (7) |
O6iii—Ba1—O7 | 141.22 (9) | O12vi—Pr2—Si4vi | 95.10 (7) |
O10—Ba1—O6ii | 92.53 (9) | O3—Pr2—Si4vi | 91.73 (7) |
O4i—Ba1—O6ii | 114.96 (8) | O3vi—Pr2—Si4vi | 30.30 (7) |
O9ii—Ba1—O6ii | 83.95 (8) | O8vi—Pr2—Si4vi | 30.44 (7) |
O6iii—Ba1—O6ii | 78.12 (9) | O8ii—Pr2—Si4vi | 66.03 (7) |
O7—Ba1—O6ii | 138.66 (8) | Si4ii—Pr2—Si4vi | 85.35 (3) |
O10—Ba1—O2i | 109.79 (9) | O2v—Pr2—Si2vi | 97.33 (7) |
O4i—Ba1—O2i | 54.15 (8) | O10—Pr2—Si2vi | 169.82 (8) |
O9ii—Ba1—O2i | 112.97 (8) | O1ii—Pr2—Si2vi | 95.96 (7) |
O6iii—Ba1—O2i | 69.58 (8) | O12vi—Pr2—Si2vi | 25.01 (7) |
O7—Ba1—O2i | 71.96 (8) | O3—Pr2—Si2vi | 85.15 (7) |
O6ii—Ba1—O2i | 146.82 (8) | O3vi—Pr2—Si2vi | 92.55 (7) |
O10—Ba1—O11ii | 141.44 (9) | O8vi—Pr2—Si2vi | 62.56 (7) |
O4i—Ba1—O11ii | 66.06 (8) | O8ii—Pr2—Si2vi | 121.33 (7) |
O9ii—Ba1—O11ii | 71.14 (9) | Si4ii—Pr2—Si2vi | 108.60 (3) |
O6iii—Ba1—O11ii | 64.73 (9) | Si4vi—Pr2—Si2vi | 74.79 (3) |
O7—Ba1—O11ii | 124.21 (9) | O2v—Pr2—Pr1iii | 37.59 (7) |
O6ii—Ba1—O11ii | 49.40 (8) | O10—Pr2—Pr1iii | 80.92 (7) |
O2i—Ba1—O11ii | 107.27 (8) | O1ii—Pr2—Pr1iii | 36.94 (7) |
O10—Ba1—O11iii | 74.41 (9) | O12vi—Pr2—Pr1iii | 72.80 (6) |
O4i—Ba1—O11iii | 130.97 (8) | O3—Pr2—Pr1iii | 122.45 (7) |
O9ii—Ba1—O11iii | 144.83 (8) | O3vi—Pr2—Pr1iii | 165.31 (7) |
O6iii—Ba1—O11iii | 48.79 (8) | O8vi—Pr2—Pr1iii | 115.46 (6) |
O7—Ba1—O11iii | 146.83 (9) | O8ii—Pr2—Pr1iii | 90.96 (6) |
O6ii—Ba1—O11iii | 61.43 (8) | Si4ii—Pr2—Pr1iii | 64.01 (2) |
O2i—Ba1—O11iii | 100.35 (8) | Si4vi—Pr2—Pr1iii | 144.72 (2) |
O11ii—Ba1—O11iii | 88.96 (8) | Si2vi—Pr2—Pr1iii | 97.80 (2) |
O10—Ba1—O8ii | 57.69 (9) | O4—Si1—O2 | 110.26 (16) |
O4i—Ba1—O8ii | 130.18 (8) | O4—Si1—O7 | 109.95 (17) |
O9ii—Ba1—O8ii | 64.20 (8) | O2—Si1—O7 | 106.85 (17) |
O6iii—Ba1—O8ii | 124.89 (8) | O4—Si1—O5 | 107.69 (16) |
O7—Ba1—O8ii | 93.89 (8) | O2—Si1—O5 | 112.13 (16) |
O6ii—Ba1—O8ii | 49.34 (8) | O7—Si1—O5 | 109.97 (16) |
O2i—Ba1—O8ii | 163.56 (8) | O4—Si1—Pr1i | 119.11 (12) |
O11ii—Ba1—O8ii | 87.46 (8) | O2—Si1—Pr1i | 50.33 (11) |
O11iii—Ba1—O8ii | 86.87 (8) | O7—Si1—Pr1i | 57.00 (12) |
O10—Ba1—Si3iii | 90.06 (7) | O5—Si1—Pr1i | 133.14 (12) |
O4i—Ba1—Si3iii | 107.21 (6) | O4—Si1—Pr1 | 48.19 (10) |
O9ii—Ba1—Si3iii | 161.74 (7) | O2—Si1—Pr1 | 124.81 (12) |
O6iii—Ba1—Si3iii | 30.20 (6) | O7—Si1—Pr1 | 61.77 (12) |
O7—Ba1—Si3iii | 136.45 (7) | O5—Si1—Pr1 | 122.62 (11) |
O6ii—Ba1—Si3iii | 82.88 (6) | Pr1i—Si1—Pr1 | 92.27 (3) |
O2i—Ba1—Si3iii | 73.19 (6) | O4—Si1—Ba1i | 49.99 (11) |
O11ii—Ba1—Si3iii | 90.66 (6) | O2—Si1—Ba1i | 62.17 (11) |
O11iii—Ba1—Si3iii | 27.98 (6) | O7—Si1—Ba1i | 111.05 (12) |
O8ii—Ba1—Si3iii | 114.85 (6) | O5—Si1—Ba1i | 138.25 (11) |
O10—Ba1—Si1i | 129.36 (7) | Pr1i—Si1—Ba1i | 77.89 (3) |
O4i—Ba1—Si1i | 27.03 (6) | Pr1—Si1—Ba1i | 72.38 (2) |
O9ii—Ba1—Si1i | 87.51 (6) | O4—Si1—Ba2vi | 150.43 (12) |
O6iii—Ba1—Si1i | 78.64 (6) | O2—Si1—Ba2vi | 99.31 (12) |
O7—Ba1—Si1i | 64.83 (7) | O7—Si1—Ba2vi | 59.11 (12) |
O6ii—Ba1—Si1i | 138.07 (6) | O5—Si1—Ba2vi | 58.95 (11) |
O2i—Ba1—Si1i | 27.80 (6) | Pr1i—Si1—Ba2vi | 79.76 (3) |
O11ii—Ba1—Si1i | 89.04 (6) | Pr1—Si1—Ba2vi | 113.54 (3) |
O11iii—Ba1—Si1i | 121.79 (6) | Ba1i—Si1—Ba2vi | 157.12 (4) |
O8ii—Ba1—Si1i | 151.06 (6) | O9—Si2—O12 | 113.03 (17) |
Si3iii—Ba1—Si1i | 93.90 (3) | O9—Si2—O13 | 113.07 (16) |
O8iv—Ba2—O3 | 70.79 (9) | O12—Si2—O13 | 106.35 (16) |
O8iv—Ba2—O12v | 140.68 (9) | O9—Si2—O5 | 111.89 (16) |
O3—Ba2—O12v | 130.98 (8) | O12—Si2—O5 | 108.61 (16) |
O8iv—Ba2—O9iv | 72.64 (9) | O13—Si2—O5 | 103.28 (15) |
O3—Ba2—O9iv | 143.27 (8) | O9—Si2—Ba2iv | 55.62 (11) |
O12v—Ba2—O9iv | 81.54 (9) | O12—Si2—Ba2iv | 58.80 (11) |
O8iv—Ba2—O12iv | 68.00 (9) | O13—Si2—Ba2iv | 116.75 (12) |
O3—Ba2—O12iv | 111.32 (9) | O5—Si2—Ba2iv | 139.88 (11) |
O12v—Ba2—O12iv | 73.05 (9) | O9—Si2—Ba2ix | 106.85 (11) |
O9iv—Ba2—O12iv | 56.00 (8) | O12—Si2—Ba2ix | 54.14 (11) |
O8iv—Ba2—O13vi | 100.30 (9) | O13—Si2—Ba2ix | 140.05 (11) |
O3—Ba2—O13vi | 66.12 (8) | O5—Si2—Ba2ix | 61.49 (10) |
O12v—Ba2—O13vi | 118.10 (8) | Ba2iv—Si2—Ba2ix | 84.58 (3) |
O9iv—Ba2—O13vi | 118.22 (8) | O9—Si2—Pr2vi | 121.00 (12) |
O12iv—Ba2—O13vi | 167.73 (8) | O12—Si2—Pr2vi | 41.28 (10) |
O8iv—Ba2—O5v | 136.42 (9) | O13—Si2—Pr2vi | 66.14 (11) |
O3—Ba2—O5v | 76.84 (8) | O5—Si2—Pr2vi | 126.03 (11) |
O12v—Ba2—O5v | 54.76 (8) | Ba2iv—Si2—Pr2vi | 72.16 (2) |
O9iv—Ba2—O5v | 135.54 (8) | Ba2ix—Si2—Pr2vi | 92.31 (3) |
O12iv—Ba2—O5v | 98.91 (8) | O9—Si2—Ba2vi | 152.61 (12) |
O13vi—Ba2—O5v | 92.21 (8) | O12—Si2—Ba2vi | 94.25 (12) |
O8iv—Ba2—O5vi | 147.10 (9) | O13—Si2—Ba2vi | 53.28 (11) |
O3—Ba2—O5vi | 105.06 (8) | O5—Si2—Ba2vi | 58.04 (10) |
O12v—Ba2—O5vi | 67.24 (8) | Ba2iv—Si2—Ba2vi | 149.44 (4) |
O9iv—Ba2—O5vi | 103.67 (8) | Ba2ix—Si2—Ba2vi | 90.70 (3) |
O12iv—Ba2—O5vi | 137.90 (8) | Pr2vi—Si2—Ba2vi | 77.90 (2) |
O13vi—Ba2—O5vi | 51.57 (8) | O11—Si3—O10 | 116.96 (18) |
O5v—Ba2—O5vi | 69.18 (9) | O11—Si3—O13 | 116.30 (16) |
O8iv—Ba2—O7vi | 103.22 (8) | O10—Si3—O13 | 105.04 (16) |
O3—Ba2—O7vi | 128.18 (9) | O11—Si3—O6 | 102.11 (17) |
O12v—Ba2—O7vi | 87.02 (8) | O10—Si3—O6 | 109.95 (16) |
O9iv—Ba2—O7vi | 58.39 (9) | O13—Si3—O6 | 105.91 (15) |
O12iv—Ba2—O7vi | 113.24 (8) | O11—Si3—Ba1iii | 73.04 (12) |
O13vi—Ba2—O7vi | 64.64 (8) | O10—Si3—Ba1iii | 79.55 (12) |
O5v—Ba2—O7vi | 119.75 (8) | O13—Si3—Ba1iii | 164.30 (12) |
O5vi—Ba2—O7vi | 52.52 (8) | O6—Si3—Ba1iii | 58.72 (10) |
O8iv—Ba2—O1 | 70.92 (9) | O11—Si3—Ba1x | 60.04 (13) |
O3—Ba2—O1 | 54.31 (8) | O10—Si3—Ba1x | 161.15 (13) |
O12v—Ba2—O1 | 95.23 (8) | O13—Si3—Ba1x | 91.93 (11) |
O9iv—Ba2—O1 | 115.34 (8) | O6—Si3—Ba1x | 56.23 (11) |
O12iv—Ba2—O1 | 61.40 (8) | Ba1iii—Si3—Ba1x | 81.94 (3) |
O13vi—Ba2—O1 | 119.51 (8) | O11—Si3—Ba1 | 77.77 (13) |
O5v—Ba2—O1 | 66.62 (8) | O10—Si3—Ba1 | 43.92 (11) |
O5vi—Ba2—O1 | 134.40 (8) | O13—Si3—Ba1 | 108.49 (11) |
O7vi—Ba2—O1 | 173.01 (8) | O6—Si3—Ba1 | 141.40 (11) |
O8iv—Ba2—Si2iv | 63.77 (7) | Ba1iii—Si3—Ba1 | 85.37 (3) |
O3—Ba2—Si2iv | 128.32 (7) | Ba1x—Si3—Ba1 | 137.80 (4) |
O12v—Ba2—Si2iv | 79.45 (6) | O11—Si3—Ba2vi | 116.84 (13) |
O9iv—Ba2—Si2iv | 28.07 (6) | O10—Si3—Ba2vi | 63.97 (12) |
O12iv—Ba2—Si2iv | 28.41 (6) | O13—Si3—Ba2vi | 46.44 (11) |
O13vi—Ba2—Si2iv | 143.57 (6) | O6—Si3—Ba2vi | 139.07 (11) |
O5v—Ba2—Si2iv | 122.36 (6) | Ba1iii—Si3—Ba2vi | 142.91 (4) |
O5vi—Ba2—Si2iv | 126.42 (6) | Ba1x—Si3—Ba2vi | 134.82 (3) |
O7vi—Ba2—Si2iv | 86.37 (6) | Ba1—Si3—Ba2vi | 64.16 (2) |
O1—Ba2—Si2iv | 87.53 (6) | O8—Si4—O1 | 108.72 (17) |
O8iv—Ba2—Si2v | 138.85 (7) | O8—Si4—O3 | 109.25 (17) |
O3—Ba2—Si2v | 103.36 (6) | O1—Si4—O3 | 111.43 (16) |
O12v—Ba2—Si2v | 27.84 (6) | O8—Si4—O6 | 107.57 (16) |
O9iv—Ba2—Si2v | 106.20 (6) | O1—Si4—O6 | 112.08 (16) |
O12iv—Ba2—Si2v | 77.55 (6) | O3—Si4—O6 | 107.69 (16) |
O13vi—Ba2—Si2v | 114.67 (6) | O8—Si4—Pr2x | 59.51 (12) |
O5v—Ba2—Si2v | 29.44 (6) | O1—Si4—Pr2x | 49.73 (11) |
O5vi—Ba2—Si2v | 74.01 (6) | O3—Si4—Pr2x | 120.15 (12) |
O7vi—Ba2—Si2v | 110.77 (6) | O6—Si4—Pr2x | 132.13 (12) |
O1—Ba2—Si2v | 73.22 (6) | O8—Si4—Pr2vi | 58.04 (12) |
Si2iv—Ba2—Si2v | 95.42 (3) | O1—Si4—Pr2vi | 130.00 (12) |
O11—Pr1—O9vii | 159.60 (11) | O3—Si4—Pr2vi | 51.37 (11) |
O11—Pr1—O4 | 97.25 (10) | O6—Si4—Pr2vi | 117.88 (12) |
O9vii—Pr1—O4 | 77.69 (10) | Pr2x—Si4—Pr2vi | 94.65 (3) |
O11—Pr1—O1viii | 84.26 (10) | O8—Si4—Ba2 | 107.17 (12) |
O9vii—Pr1—O1viii | 91.71 (10) | O1—Si4—Ba2 | 63.11 (11) |
O4—Pr1—O1viii | 153.58 (10) | O3—Si4—Ba2 | 52.13 (11) |
O11—Pr1—O4vii | 82.23 (11) | O6—Si4—Ba2 | 144.31 (12) |
O9vii—Pr1—O4vii | 77.45 (10) | Pr2x—Si4—Ba2 | 74.27 (3) |
O4—Pr1—O4vii | 70.48 (11) | Pr2vi—Si4—Ba2 | 75.09 (3) |
O1viii—Pr1—O4vii | 83.69 (10) | O8—Si4—Ba1x | 64.27 (12) |
O11—Pr1—O2i | 93.57 (11) | O1—Si4—Ba1x | 99.40 (12) |
O9vii—Pr1—O2i | 104.42 (10) | O3—Si4—Ba1x | 148.55 (12) |
O4—Pr1—O2i | 132.70 (10) | O6—Si4—Ba1x | 52.20 (11) |
O1viii—Pr1—O2i | 73.18 (10) | Pr2x—Si4—Ba1x | 84.40 (3) |
O4vii—Pr1—O2i | 156.81 (10) | Pr2vi—Si4—Ba1x | 112.03 (3) |
O11—Pr1—O7i | 131.43 (11) | Ba2—Si4—Ba1x | 158.14 (4) |
O9vii—Pr1—O7i | 67.56 (10) | Si4—O1—Pr1viii | 138.47 (17) |
O4—Pr1—O7i | 79.15 (9) | Si4—O1—Pr2x | 100.24 (14) |
O1viii—Pr1—O7i | 119.36 (10) | Pr1viii—O1—Pr2x | 106.05 (11) |
O4vii—Pr1—O7i | 137.64 (9) | Si4—O1—Ba2 | 88.92 (13) |
O2i—Pr1—O7i | 59.85 (9) | Pr1viii—O1—Ba2 | 121.12 (11) |
O11—Pr1—O7 | 70.51 (10) | Pr2x—O1—Ba2 | 91.94 (9) |
O9vii—Pr1—O7 | 120.97 (9) | Si1—O2—Pr2ix | 136.22 (17) |
O4—Pr1—O7 | 59.38 (9) | Si1—O2—Pr1i | 99.88 (14) |
O1viii—Pr1—O7 | 143.13 (9) | Pr2ix—O2—Pr1i | 106.23 (11) |
O4vii—Pr1—O7 | 117.56 (9) | Si1—O2—Ba1i | 90.02 (13) |
O2i—Pr1—O7 | 81.79 (9) | Pr2ix—O2—Ba1i | 119.97 (11) |
O7i—Pr1—O7 | 66.23 (11) | Pr1i—O2—Ba1i | 97.33 (9) |
O11—Pr1—Si1i | 112.57 (9) | Si4—O3—Pr2 | 128.52 (16) |
O9vii—Pr1—Si1i | 87.78 (8) | Si4—O3—Pr2vi | 98.33 (14) |
O4—Pr1—Si1i | 105.52 (7) | Pr2—O3—Pr2vi | 111.35 (11) |
O1viii—Pr1—Si1i | 98.07 (7) | Si4—O3—Ba2 | 100.21 (14) |
O4vii—Pr1—Si1i | 165.18 (7) | Pr2—O3—Ba2 | 114.06 (11) |
O2i—Pr1—Si1i | 29.78 (7) | Pr2vi—O3—Ba2 | 99.98 (10) |
O7i—Pr1—Si1i | 30.27 (7) | Si1—O4—Pr1 | 102.51 (14) |
O7—Pr1—Si1i | 69.22 (7) | Si1—O4—Pr1vii | 129.49 (16) |
O11—Pr1—Si1 | 82.92 (8) | Pr1—O4—Pr1vii | 109.52 (11) |
O9vii—Pr1—Si1 | 100.00 (7) | Si1—O4—Ba1i | 102.98 (14) |
O4—Pr1—Si1 | 29.29 (7) | Pr1—O4—Ba1i | 99.26 (10) |
O1viii—Pr1—Si1 | 167.15 (7) | Pr1vii—O4—Ba1i | 108.97 (10) |
O4vii—Pr1—Si1 | 93.64 (7) | Si2—O5—Si1 | 123.98 (18) |
O2i—Pr1—Si1 | 108.53 (7) | Si2—O5—Ba2ix | 89.07 (12) |
O7i—Pr1—Si1 | 70.64 (7) | Si1—O5—Ba2ix | 138.24 (15) |
O7—Pr1—Si1 | 30.09 (6) | Si2—O5—Ba2vi | 94.31 (12) |
Si1i—Pr1—Si1 | 87.73 (3) | Si1—O5—Ba2vi | 92.93 (12) |
O11—Pr1—Pr2iii | 89.24 (8) | Ba2ix—O5—Ba2vi | 110.82 (9) |
O9vii—Pr1—Pr2iii | 99.55 (7) | Si4—O6—Si3 | 123.57 (18) |
O4—Pr1—Pr2iii | 167.94 (7) | Si4—O6—Ba1iii | 135.17 (15) |
O1viii—Pr1—Pr2iii | 37.01 (7) | Si3—O6—Ba1iii | 91.08 (12) |
O4vii—Pr1—Pr2iii | 120.70 (7) | Si4—O6—Ba1x | 101.64 (13) |
O2i—Pr1—Pr2iii | 36.18 (7) | Si3—O6—Ba1x | 95.92 (13) |
O7i—Pr1—Pr2iii | 88.93 (6) | Ba1iii—O6—Ba1x | 101.88 (9) |
O7—Pr1—Pr2iii | 114.07 (6) | Si1—O7—Pr1i | 92.73 (14) |
Si1i—Pr1—Pr2iii | 62.50 (2) | Si1—O7—Pr1 | 88.13 (13) |
Si1—Pr1—Pr2iii | 143.42 (2) | Pr1i—O7—Pr1 | 113.77 (11) |
O11—Pr1—Ba1i | 138.53 (8) | Si1—O7—Ba1 | 175.86 (18) |
O9vii—Pr1—Ba1i | 44.57 (7) | Pr1i—O7—Ba1 | 89.83 (9) |
O4—Pr1—Ba1i | 42.83 (7) | Pr1—O7—Ba1 | 93.82 (9) |
O1viii—Pr1—Ba1i | 135.78 (7) | Si1—O7—Ba2vi | 93.83 (13) |
O4vii—Pr1—Ba1i | 90.91 (7) | Pr1i—O7—Ba2vi | 97.93 (10) |
O2i—Pr1—Ba1i | 106.73 (7) | Pr1—O7—Ba2vi | 148.13 (12) |
O7i—Pr1—Ba1i | 47.29 (6) | Ba1—O7—Ba2vi | 82.58 (8) |
O7—Pr1—Ba1i | 76.98 (6) | Si4—O8—Pr2vi | 91.52 (14) |
Si1i—Pr1—Ba1i | 77.52 (2) | Si4—O8—Pr2x | 89.95 (14) |
Si1—Pr1—Ba1i | 56.63 (2) | Pr2vi—O8—Pr2x | 118.56 (11) |
Pr2iii—Pr1—Ba1i | 128.055 (8) | Si4—O8—Ba2iv | 169.25 (18) |
O2v—Pr2—O10 | 75.44 (10) | Pr2vi—O8—Ba2iv | 94.46 (9) |
O2v—Pr2—O1ii | 74.52 (11) | Pr2x—O8—Ba2iv | 95.00 (10) |
O10—Pr2—O1ii | 89.07 (10) | Si4—O8—Ba1x | 89.66 (13) |
O2v—Pr2—O12vi | 77.99 (10) | Pr2vi—O8—Ba1x | 142.32 (12) |
O10—Pr2—O12vi | 152.08 (10) | Pr2x—O8—Ba1x | 99.10 (10) |
O1ii—Pr2—O12vi | 75.67 (10) | Ba2iv—O8—Ba1x | 80.16 (8) |
O2v—Pr2—O3 | 84.89 (10) | Si2—O9—Pr1vii | 127.99 (16) |
O10—Pr2—O3 | 87.04 (10) | Si2—O9—Ba2iv | 96.31 (13) |
O1ii—Pr2—O3 | 159.37 (10) | Pr1vii—O9—Ba2iv | 112.47 (11) |
O12vi—Pr2—O3 | 99.03 (10) | Si2—O9—Ba1x | 125.70 (15) |
O2v—Pr2—O3vi | 150.85 (10) | Pr1vii—O9—Ba1x | 97.95 (10) |
O10—Pr2—O3vi | 90.68 (10) | Ba2iv—O9—Ba1x | 89.49 (9) |
O1ii—Pr2—O3vi | 131.69 (10) | Si3—O10—Pr2 | 118.75 (16) |
O12vi—Pr2—O3vi | 116.97 (9) | Si3—O10—Ba1 | 111.98 (15) |
O3—Pr2—O3vi | 68.65 (11) | Pr2—O10—Ba1 | 127.21 (12) |
O2v—Pr2—O8vi | 147.19 (10) | Si3—O11—Pr1 | 146.71 (19) |
O10—Pr2—O8vi | 127.15 (10) | Si3—O11—Ba1x | 93.51 (15) |
O1ii—Pr2—O8vi | 81.79 (10) | Pr1—O11—Ba1x | 102.09 (11) |
O12vi—Pr2—O8vi | 74.33 (9) | Si3—O11—Ba1iii | 78.98 (12) |
O3—Pr2—O8vi | 116.41 (9) | Pr1—O11—Ba1iii | 129.19 (12) |
O3vi—Pr2—O8vi | 60.67 (9) | Ba1x—O11—Ba1iii | 91.04 (8) |
O2v—Pr2—O8ii | 121.37 (10) | Si2—O12—Pr2vi | 113.71 (14) |
O10—Pr2—O8ii | 68.85 (10) | Si2—O12—Ba2ix | 98.02 (13) |
O1ii—Pr2—O8ii | 60.35 (9) | Pr2vi—O12—Ba2ix | 139.35 (12) |
O12vi—Pr2—O8ii | 119.93 (9) | Si2—O12—Ba2iv | 92.79 (13) |
O3—Pr2—O8ii | 135.57 (9) | Pr2vi—O12—Ba2iv | 96.60 (9) |
O3vi—Pr2—O8ii | 74.72 (9) | Ba2ix—O12—Ba2iv | 106.94 (9) |
O8vi—Pr2—O8ii | 61.44 (11) | Si2—O13—Si3 | 134.88 (19) |
O2v—Pr2—Si4ii | 99.88 (8) | Si2—O13—Ba2vi | 99.84 (13) |
O10—Pr2—Si4ii | 80.03 (8) | Si3—O13—Ba2vi | 109.40 (14) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) −x+2, −y+1, −z+2; (v) x, y+1, z; (vi) −x+1, −y+1, −z+2; (vii) −x+2, −y, −z+1; (viii) −x+2, −y+1, −z+1; (ix) x, y−1, z; (x) x+1, y, z. |
Ba2O13Si4Sm2 | F(000) = 1584 |
Mr = 895.74 | Dx = 5.116 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.9961 (9) Å | Cell parameters from 3082 reflections |
b = 5.2355 (7) Å | θ = 3.2–26.7° |
c = 17.626 (3) Å | µ = 17.12 mm−1 |
β = 104.148 (18)° | T = 298 K |
V = 1162.9 (3) Å3 | Block, yellow |
Z = 4 | 0.22 × 0.15 × 0.15 mm |
Rigaku AFC8S diffractometer | 1174 independent reflections |
Radiation source: fine-focus sealed tube | 1129 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.084 |
ω scans | θmax = 26.5°, θmin = 3.2° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −16→16 |
Tmin = 0.449, Tmax = 1.000 | k = −6→6 |
4506 measured reflections | l = −21→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.049 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.146 | (Δ/σ)max < 0.001 |
S = 1.18 | Δρmax = 2.13 e Å−3 |
1174 reflections | Δρmin = −3.88 e Å−3 |
97 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0062 (4) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Sm1 | 0.88505 (4) | 0.00895 (8) | 0.41518 (3) | 0.0080 (3) | |
Ba1 | 0.66214 (5) | 0.49513 (8) | 0.33290 (4) | 0.0103 (3) | |
Si1 | 0.8820 (2) | −0.4667 (5) | 0.54470 (16) | 0.0081 (6) | |
Si2 | 1.0627 (2) | −0.5441 (5) | 0.68454 (16) | 0.0088 (6) | |
O1 | 0.9819 (4) | −0.6424 (11) | 0.5998 (3) | 0.0109 (12) | |
O2 | 0.7949 (5) | −0.4620 (12) | 0.5968 (4) | 0.0103 (13) | |
O3 | 0.9290 (4) | −0.1748 (11) | 0.5388 (3) | 0.0100 (12) | |
O4 | 0.8430 (5) | −0.5948 (12) | 0.4600 (3) | 0.0124 (13) | |
O5 | 0.5000 | 0.1478 (16) | 0.2500 | 0.0106 (16) | |
O6 | 0.9196 (5) | 0.2427 (12) | 0.3098 (3) | 0.0147 (13) | |
O7 | 0.8354 (5) | −0.2760 (12) | 0.3060 (3) | 0.0123 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.0058 (5) | 0.0109 (5) | 0.0080 (5) | −0.00020 (12) | 0.0030 (3) | −0.00011 (13) |
Ba1 | 0.0090 (5) | 0.0120 (5) | 0.0104 (5) | −0.00173 (14) | 0.0035 (3) | −0.00090 (15) |
Si1 | 0.0068 (11) | 0.0109 (11) | 0.0077 (14) | −0.0014 (8) | 0.0036 (9) | −0.0010 (8) |
Si2 | 0.0073 (12) | 0.0123 (11) | 0.0072 (12) | 0.0002 (9) | 0.0024 (9) | −0.0004 (9) |
O1 | 0.010 (3) | 0.011 (3) | 0.014 (3) | −0.001 (2) | 0.006 (2) | −0.002 (2) |
O2 | 0.008 (3) | 0.017 (3) | 0.007 (3) | −0.001 (2) | 0.004 (2) | −0.001 (2) |
O3 | 0.012 (3) | 0.013 (3) | 0.004 (3) | 0.000 (2) | −0.001 (2) | 0.001 (2) |
O4 | 0.015 (3) | 0.014 (3) | 0.009 (3) | 0.001 (2) | 0.005 (2) | −0.005 (2) |
O5 | 0.014 (4) | 0.012 (4) | 0.007 (4) | 0.000 | 0.006 (3) | 0.000 |
O6 | 0.021 (3) | 0.014 (3) | 0.011 (3) | −0.006 (2) | 0.009 (3) | 0.002 (2) |
O7 | 0.008 (3) | 0.016 (3) | 0.014 (3) | 0.002 (2) | 0.005 (2) | 0.003 (2) |
Sm1—O2i | 2.309 (7) | Si1—Ba1v | 3.418 (3) |
Sm1—O3 | 2.323 (5) | Si1—Ba1i | 3.639 (3) |
Sm1—O4ii | 2.332 (6) | Si2—O6iii | 1.594 (7) |
Sm1—O6 | 2.357 (6) | Si2—O7iv | 1.600 (6) |
Sm1—O7 | 2.395 (6) | Si2—O5i | 1.658 (4) |
Sm1—O3iii | 2.508 (6) | Si2—O1 | 1.683 (6) |
Sm1—O1iv | 2.639 (6) | Si2—Sm1iv | 3.171 (3) |
Sm1—Si2iv | 3.171 (3) | Si2—Sm1iii | 3.462 (3) |
Sm1—Si1 | 3.385 (3) | Si2—Ba1viii | 3.526 (3) |
Sm1—Si2iii | 3.462 (3) | Si2—Ba1iii | 3.672 (3) |
Sm1—Sm1iii | 3.6755 (13) | Si2—Ba1i | 3.711 (3) |
Sm1—Ba1 | 3.8627 (9) | O1—Sm1iv | 2.639 (6) |
Ba1—O7ii | 2.693 (6) | O1—Ba1i | 3.068 (6) |
Ba1—O2v | 2.736 (7) | O2—Sm1i | 2.309 (7) |
Ba1—O6vi | 2.799 (6) | O2—Ba1v | 2.736 (7) |
Ba1—O7vi | 2.837 (6) | O2—Ba1i | 3.049 (7) |
Ba1—O4ii | 2.861 (6) | O3—Sm1iii | 2.508 (6) |
Ba1—O5 | 2.894 (5) | O3—Ba1v | 2.951 (6) |
Ba1—O3v | 2.951 (6) | O4—Sm1ix | 2.332 (6) |
Ba1—O2i | 3.049 (7) | O4—Ba1ix | 2.861 (6) |
Ba1—O1i | 3.068 (6) | O5—Si2vii | 1.658 (4) |
Ba1—Si1v | 3.418 (3) | O5—Si2i | 1.658 (4) |
Ba1—Si2vii | 3.526 (3) | O5—Ba1x | 2.894 (5) |
Ba1—Si1i | 3.639 (3) | O6—Si2iii | 1.594 (7) |
Si1—O4 | 1.602 (6) | O6—Ba1xi | 2.799 (6) |
Si1—O2 | 1.624 (7) | O7—Si2iv | 1.600 (6) |
Si1—O3 | 1.658 (6) | O7—Ba1ix | 2.693 (6) |
Si1—O1 | 1.691 (6) | O7—Ba1xi | 2.837 (6) |
O2i—Sm1—O3 | 93.1 (2) | O6vi—Ba1—Si2vii | 69.74 (13) |
O2i—Sm1—O4ii | 79.0 (2) | O7vi—Ba1—Si2vii | 26.40 (12) |
O3—Sm1—O4ii | 94.3 (2) | O4ii—Ba1—Si2vii | 123.53 (13) |
O2i—Sm1—O6 | 111.5 (2) | O5—Ba1—Si2vii | 27.77 (6) |
O3—Sm1—O6 | 154.7 (2) | O3v—Ba1—Si2vii | 129.68 (12) |
O4ii—Sm1—O6 | 84.8 (2) | O2i—Ba1—Si2vii | 71.69 (14) |
O2i—Sm1—O7 | 78.0 (2) | O1i—Ba1—Si2vii | 74.69 (12) |
O3—Sm1—O7 | 116.9 (2) | Si1v—Ba1—Si2vii | 149.78 (7) |
O4ii—Sm1—O7 | 141.9 (2) | O7ii—Ba1—Si1i | 134.62 (13) |
O6—Sm1—O7 | 75.9 (2) | O2v—Ba1—Si1i | 117.08 (15) |
O2i—Sm1—O3iii | 160.1 (2) | O6vi—Ba1—Si1i | 143.59 (14) |
O3—Sm1—O3iii | 81.0 (2) | O7vi—Ba1—Si1i | 99.67 (13) |
O4ii—Sm1—O3iii | 82.5 (2) | O4ii—Ba1—Si1i | 68.24 (14) |
O6—Sm1—O3iii | 73.78 (19) | O5—Ba1—Si1i | 67.71 (10) |
O7—Sm1—O3iii | 121.61 (19) | O3v—Ba1—Si1i | 68.72 (12) |
O2i—Sm1—O1iv | 125.9 (2) | O2i—Ba1—Si1i | 26.26 (14) |
O3—Sm1—O1iv | 77.03 (19) | O1i—Ba1—Si1i | 27.55 (11) |
O4ii—Sm1—O1iv | 153.43 (19) | Si1v—Ba1—Si1i | 95.72 (7) |
O6—Sm1—O1iv | 92.5 (2) | Si2vii—Ba1—Si1i | 81.27 (6) |
O7—Sm1—O1iv | 61.39 (18) | O4—Si1—O2 | 115.3 (4) |
O3iii—Sm1—O1iv | 71.41 (19) | O4—Si1—O3 | 111.4 (3) |
O2i—Sm1—Si2iv | 102.52 (17) | O2—Si1—O3 | 109.9 (3) |
O3—Sm1—Si2iv | 99.52 (15) | O4—Si1—O1 | 109.4 (3) |
O4ii—Sm1—Si2iv | 165.96 (16) | O2—Si1—O1 | 103.1 (3) |
O6—Sm1—Si2iv | 81.61 (16) | O3—Si1—O1 | 107.1 (3) |
O7—Sm1—Si2iv | 29.41 (14) | O4—Si1—Sm1 | 74.5 (2) |
O3iii—Sm1—Si2iv | 97.17 (14) | O2—Si1—Sm1 | 119.7 (3) |
O1iv—Sm1—Si2iv | 32.03 (13) | O3—Si1—Sm1 | 38.3 (2) |
O2i—Sm1—Si1 | 78.76 (18) | O1—Si1—Sm1 | 130.8 (2) |
O3—Sm1—Si1 | 26.25 (15) | O4—Si1—Ba1v | 145.8 (3) |
O4ii—Sm1—Si1 | 112.58 (16) | O2—Si1—Ba1v | 52.0 (2) |
O6—Sm1—Si1 | 161.66 (16) | O3—Si1—Ba1v | 59.7 (2) |
O7—Sm1—Si1 | 92.19 (15) | O1—Si1—Ba1v | 104.7 (2) |
O3iii—Sm1—Si1 | 101.88 (14) | Sm1—Si1—Ba1v | 85.74 (6) |
O1iv—Sm1—Si1 | 69.40 (13) | O4—Si1—Ba1i | 100.1 (3) |
Si2iv—Sm1—Si1 | 81.29 (7) | O2—Si1—Ba1i | 56.2 (2) |
O2i—Sm1—Si2iii | 111.07 (17) | O3—Si1—Ba1i | 148.4 (2) |
O3—Sm1—Si2iii | 141.07 (15) | O1—Si1—Ba1i | 57.1 (2) |
O4ii—Sm1—Si2iii | 62.81 (16) | Sm1—Si1—Ba1i | 171.34 (10) |
O6—Sm1—Si2iii | 23.20 (15) | Ba1v—Si1—Ba1i | 95.72 (7) |
O7—Sm1—Si2iii | 98.28 (15) | O6iii—Si2—O7iv | 118.2 (3) |
O3iii—Sm1—Si2iii | 65.85 (13) | O6iii—Si2—O5i | 111.6 (4) |
O1iv—Sm1—Si2iii | 108.86 (14) | O7iv—Si2—O5i | 105.7 (3) |
Si2iv—Sm1—Si2iii | 104.16 (8) | O6iii—Si2—O1 | 114.0 (3) |
Si1—Sm1—Si2iii | 166.87 (7) | O7iv—Si2—O1 | 103.5 (3) |
O2i—Sm1—Sm1iii | 132.49 (17) | O5i—Si2—O1 | 102.2 (3) |
O3—Sm1—Sm1iii | 42.38 (14) | O6iii—Si2—Sm1iv | 138.3 (3) |
O4ii—Sm1—Sm1iii | 87.62 (15) | O7iv—Si2—Sm1iv | 47.3 (2) |
O6—Sm1—Sm1iii | 112.37 (15) | O5i—Si2—Sm1iv | 110.0 (3) |
O7—Sm1—Sm1iii | 130.04 (14) | O1—Si2—Sm1iv | 56.3 (2) |
O3iii—Sm1—Sm1iii | 38.62 (12) | O6iii—Si2—Sm1iii | 35.6 (2) |
O1iv—Sm1—Sm1iii | 68.94 (12) | O7iv—Si2—Sm1iii | 105.6 (2) |
Si2iv—Sm1—Sm1iii | 100.94 (5) | O5i—Si2—Sm1iii | 144.0 (3) |
Si1—Sm1—Sm1iii | 64.77 (5) | O1—Si2—Sm1iii | 87.4 (2) |
Si2iii—Sm1—Sm1iii | 102.26 (5) | Sm1iv—Si2—Sm1iii | 104.16 (8) |
O2i—Sm1—Ba1 | 52.11 (17) | O6iii—Si2—Ba1viii | 126.6 (3) |
O3—Sm1—Ba1 | 127.97 (14) | O7iv—Si2—Ba1viii | 52.0 (2) |
O4ii—Sm1—Ba1 | 47.50 (15) | O5i—Si2—Ba1viii | 54.42 (18) |
O6—Sm1—Ba1 | 68.40 (16) | O1—Si2—Ba1viii | 119.3 (2) |
O7—Sm1—Ba1 | 94.52 (14) | Sm1iv—Si2—Ba1viii | 78.92 (6) |
O3iii—Sm1—Ba1 | 117.90 (13) | Sm1iii—Si2—Ba1viii | 146.80 (8) |
O1iv—Sm1—Ba1 | 153.02 (13) | O6iii—Si2—Ba1iii | 78.9 (2) |
Si2iv—Sm1—Ba1 | 122.70 (5) | O7iv—Si2—Ba1iii | 41.6 (2) |
Si1—Sm1—Ba1 | 127.36 (5) | O5i—Si2—Ba1iii | 137.34 (14) |
Si2iii—Sm1—Ba1 | 59.88 (4) | O1—Si2—Ba1iii | 110.8 (2) |
Sm1iii—Sm1—Ba1 | 135.08 (2) | Sm1iv—Si2—Ba1iii | 70.27 (5) |
O7ii—Ba1—O2v | 66.11 (19) | Sm1iii—Si2—Ba1iii | 65.49 (5) |
O7ii—Ba1—O6vi | 77.63 (18) | Ba1viii—Si2—Ba1iii | 85.47 (6) |
O2v—Ba1—O6vi | 89.07 (19) | O6iii—Si2—Ba1i | 137.2 (3) |
O7ii—Ba1—O7vi | 83.37 (13) | O7iv—Si2—Ba1i | 104.4 (2) |
O2v—Ba1—O7vi | 142.54 (19) | O5i—Si2—Ba1i | 48.58 (18) |
O6vi—Ba1—O7vi | 62.47 (17) | O1—Si2—Ba1i | 54.8 (2) |
O7ii—Ba1—O4ii | 69.44 (18) | Sm1iv—Si2—Ba1i | 74.73 (6) |
O2v—Ba1—O4ii | 75.80 (19) | Sm1iii—Si2—Ba1i | 136.15 (8) |
O6vi—Ba1—O4ii | 146.99 (18) | Ba1viii—Si2—Ba1i | 76.92 (6) |
O7vi—Ba1—O4ii | 114.39 (17) | Ba1iii—Si2—Ba1i | 143.20 (8) |
O7ii—Ba1—O5 | 136.69 (13) | Si2—O1—Si1 | 124.6 (4) |
O2v—Ba1—O5 | 146.40 (18) | Si2—O1—Sm1iv | 91.7 (2) |
O6vi—Ba1—O5 | 76.56 (17) | Si1—O1—Sm1iv | 140.2 (3) |
O7vi—Ba1—O5 | 53.86 (12) | Si2—O1—Ba1i | 98.5 (3) |
O4ii—Ba1—O5 | 130.48 (18) | Si1—O1—Ba1i | 95.4 (2) |
O7ii—Ba1—O3v | 120.17 (17) | Sm1iv—O1—Ba1i | 94.45 (18) |
O2v—Ba1—O3v | 56.23 (18) | Si1—O2—Sm1i | 141.0 (4) |
O6vi—Ba1—O3v | 113.93 (16) | Si1—O2—Ba1v | 100.1 (3) |
O7vi—Ba1—O3v | 155.76 (16) | Sm1i—O2—Ba1v | 103.1 (2) |
O4ii—Ba1—O3v | 81.93 (16) | Si1—O2—Ba1i | 97.6 (3) |
O5—Ba1—O3v | 102.00 (12) | Sm1i—O2—Ba1i | 91.2 (2) |
O7ii—Ba1—O2i | 113.61 (18) | Ba1v—O2—Ba1i | 129.6 (2) |
O2v—Ba1—O2i | 129.6 (2) | Si1—O3—Sm1 | 115.5 (3) |
O6vi—Ba1—O2i | 141.33 (18) | Si1—O3—Sm1iii | 129.7 (3) |
O7vi—Ba1—O2i | 81.54 (18) | Sm1—O3—Sm1iii | 99.0 (2) |
O4ii—Ba1—O2i | 59.84 (18) | Si1—O3—Ba1v | 91.3 (2) |
O5—Ba1—O2i | 70.64 (18) | Sm1—O3—Ba1v | 122.3 (2) |
O3v—Ba1—O2i | 92.79 (17) | Sm1iii—O3—Ba1v | 100.23 (18) |
O7ii—Ba1—O1i | 162.10 (17) | Si1—O4—Sm1ix | 129.8 (3) |
O2v—Ba1—O1i | 116.06 (18) | Si1—O4—Ba1ix | 132.3 (3) |
O6vi—Ba1—O1i | 119.54 (17) | Sm1ix—O4—Ba1ix | 95.57 (19) |
O7vi—Ba1—O1i | 99.74 (16) | Si2vii—O5—Si2i | 141.8 (6) |
O4ii—Ba1—O1i | 93.47 (17) | Si2vii—O5—Ba1x | 105.98 (16) |
O5—Ba1—O1i | 51.62 (12) | Si2i—O5—Ba1x | 97.82 (16) |
O3v—Ba1—O1i | 59.88 (16) | Si2vii—O5—Ba1 | 97.82 (16) |
O2i—Ba1—O1i | 50.24 (17) | Si2i—O5—Ba1 | 105.98 (16) |
O7ii—Ba1—Si1v | 93.81 (14) | Ba1x—O5—Ba1 | 102.2 (3) |
O2v—Ba1—Si1v | 27.88 (15) | Si2iii—O6—Sm1 | 121.2 (3) |
O6vi—Ba1—Si1v | 98.48 (13) | Si2iii—O6—Ba1xi | 122.1 (3) |
O7vi—Ba1—Si1v | 160.93 (13) | Sm1—O6—Ba1xi | 111.3 (2) |
O4ii—Ba1—Si1v | 81.80 (13) | Si2iv—O7—Sm1 | 103.3 (3) |
O5—Ba1—Si1v | 123.95 (9) | Si2iv—O7—Ba1ix | 115.2 (3) |
O3v—Ba1—Si1v | 29.01 (12) | Sm1—O7—Ba1ix | 102.0 (2) |
O2i—Ba1—Si1v | 116.56 (14) | Si2iv—O7—Ba1xi | 101.6 (3) |
O1i—Ba1—Si1v | 88.74 (12) | Sm1—O7—Ba1xi | 108.9 (2) |
O7ii—Ba1—Si2vii | 109.76 (14) | Ba1ix—O7—Ba1xi | 124.1 (2) |
O2v—Ba1—Si2vii | 158.67 (15) |
Symmetry codes: (i) −x+3/2, −y−1/2, −z+1; (ii) x, y+1, z; (iii) −x+2, −y, −z+1; (iv) −x+2, −y−1, −z+1; (v) −x+3/2, −y+1/2, −z+1; (vi) −x+3/2, y+1/2, −z+1/2; (vii) x−1/2, −y−1/2, z−1/2; (viii) x+1/2, −y−1/2, z+1/2; (ix) x, y−1, z; (x) −x+1, y, −z+1/2; (xi) −x+3/2, y−1/2, −z+1/2. |
Ba2Eu2O13Si4 | F(000) = 1592 |
Mr = 898.96 | Dx = 5.166 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.9545 (13) Å | Cell parameters from 2928 reflections |
b = 5.2311 (8) Å | θ = 2.4–26.7° |
c = 17.595 (5) Å | µ = 17.92 mm−1 |
β = 104.23 (2)° | T = 298 K |
V = 1155.7 (4) Å3 | Block, colourless |
Z = 4 | 0.18 × 0.16 × 0.13 mm |
Rigaku AFC8S diffractometer | 1196 independent reflections |
Radiation source: fine-focus sealed tube | 1095 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.080 |
ω scans | θmax = 26.5°, θmin = 2.4° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −16→16 |
Tmin = 0.382, Tmax = 1.000 | k = −6→5 |
4857 measured reflections | l = −22→22 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.044 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.119 | (Δ/σ)max < 0.001 |
S = 1.11 | Δρmax = 2.82 e Å−3 |
1196 reflections | Δρmin = −3.04 e Å−3 |
97 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00065 (12) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Eu1 | 0.88547 (3) | 0.00868 (7) | 0.41531 (3) | 0.0099 (3) | |
Ba1 | 0.66220 (4) | 0.49521 (8) | 0.33281 (3) | 0.0121 (3) | |
Si1 | 0.8815 (2) | −0.4671 (5) | 0.54424 (14) | 0.0101 (5) | |
Si2 | 1.06251 (19) | −0.5431 (5) | 0.68445 (14) | 0.0105 (5) | |
O1 | 0.9823 (4) | −0.6417 (11) | 0.6001 (3) | 0.0147 (12) | |
O2 | 0.7948 (5) | −0.4610 (12) | 0.5967 (4) | 0.0142 (12) | |
O3 | 0.9291 (4) | −0.1749 (11) | 0.5387 (3) | 0.0115 (11) | |
O4 | 0.8431 (5) | −0.5980 (12) | 0.4602 (3) | 0.0155 (12) | |
O5 | 0.5000 | 0.1443 (16) | 0.2500 | 0.0118 (16) | |
O6 | 0.9192 (5) | 0.2432 (12) | 0.3107 (4) | 0.0194 (13) | |
O7 | 0.8354 (5) | −0.2766 (12) | 0.3062 (3) | 0.0141 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu1 | 0.0110 (3) | 0.0110 (3) | 0.0086 (4) | −0.00005 (13) | 0.0040 (2) | 0.00017 (12) |
Ba1 | 0.0137 (4) | 0.0122 (4) | 0.0110 (4) | −0.00158 (15) | 0.0043 (3) | −0.00098 (15) |
Si1 | 0.0115 (10) | 0.0109 (10) | 0.0085 (12) | −0.0002 (8) | 0.0034 (9) | 0.0007 (8) |
Si2 | 0.0119 (11) | 0.0116 (10) | 0.0095 (12) | 0.0002 (8) | 0.0054 (9) | 0.0008 (9) |
O1 | 0.016 (3) | 0.011 (3) | 0.016 (3) | −0.001 (2) | 0.004 (2) | −0.002 (2) |
O2 | 0.012 (3) | 0.019 (3) | 0.013 (3) | 0.002 (2) | 0.006 (2) | 0.002 (2) |
O3 | 0.017 (3) | 0.010 (3) | 0.007 (3) | −0.001 (2) | 0.002 (2) | 0.000 (2) |
O4 | 0.019 (3) | 0.015 (3) | 0.014 (3) | 0.002 (2) | 0.007 (2) | −0.004 (2) |
O5 | 0.018 (4) | 0.013 (4) | 0.006 (4) | 0.000 | 0.006 (3) | 0.000 |
O6 | 0.025 (3) | 0.016 (3) | 0.019 (3) | −0.005 (2) | 0.008 (3) | −0.003 (2) |
O7 | 0.015 (3) | 0.017 (3) | 0.010 (3) | 0.001 (2) | 0.003 (2) | 0.002 (2) |
Eu1—O2i | 2.307 (6) | Si1—Eu1viii | 3.567 (2) |
Eu1—O3 | 2.313 (5) | Si1—Ba1i | 3.638 (3) |
Eu1—O4ii | 2.317 (6) | Si2—O6iii | 1.586 (7) |
Eu1—O6 | 2.341 (6) | Si2—O7iv | 1.600 (6) |
Eu1—O7 | 2.392 (6) | Si2—O5i | 1.651 (4) |
Eu1—O3iii | 2.495 (6) | Si2—O1 | 1.670 (6) |
Eu1—O1iv | 2.631 (6) | Si2—Eu1iv | 3.170 (2) |
Eu1—Si2iv | 3.170 (2) | Si2—Eu1iii | 3.454 (2) |
Eu1—Si1 | 3.377 (2) | Si2—Ba1ix | 3.524 (3) |
Eu1—Si2iii | 3.454 (2) | Si2—Ba1iii | 3.661 (2) |
Eu1—Si1ii | 3.567 (2) | Si2—Ba1i | 3.705 (2) |
Eu1—Eu1iii | 3.6533 (14) | O1—Eu1iv | 2.631 (6) |
Ba1—O7ii | 2.683 (6) | O1—Ba1i | 3.066 (6) |
Ba1—O2v | 2.729 (7) | O2—Eu1i | 2.307 (6) |
Ba1—O6vi | 2.804 (6) | O2—Ba1v | 2.729 (7) |
Ba1—O7vi | 2.835 (6) | O2—Ba1i | 3.053 (6) |
Ba1—O4ii | 2.858 (6) | O3—Eu1iii | 2.495 (6) |
Ba1—O5 | 2.898 (5) | O3—Ba1v | 2.951 (5) |
Ba1—O3v | 2.951 (5) | O4—Eu1viii | 2.317 (6) |
Ba1—O2i | 3.053 (6) | O4—Ba1viii | 2.858 (6) |
Ba1—O1i | 3.066 (6) | O5—Si2vii | 1.651 (4) |
Ba1—Si1v | 3.420 (2) | O5—Si2i | 1.651 (4) |
Ba1—Si2vii | 3.524 (3) | O5—Ba1x | 2.899 (5) |
Ba1—Si1i | 3.638 (3) | O6—Si2iii | 1.586 (7) |
Si1—O4 | 1.595 (6) | O6—Ba1xi | 2.804 (6) |
Si1—O2 | 1.619 (6) | O7—Si2iv | 1.600 (6) |
Si1—O3 | 1.660 (6) | O7—Ba1viii | 2.683 (6) |
Si1—O1 | 1.695 (6) | O7—Ba1xi | 2.836 (6) |
Si1—Ba1v | 3.420 (2) | ||
O2i—Eu1—O3 | 92.8 (2) | O5—Ba1—Si2vii | 27.66 (5) |
O2i—Eu1—O4ii | 78.9 (2) | O3v—Ba1—Si2vii | 129.68 (12) |
O3—Eu1—O4ii | 94.2 (2) | O2i—Ba1—Si2vii | 71.56 (13) |
O2i—Eu1—O6 | 111.4 (2) | O1i—Ba1—Si2vii | 74.52 (12) |
O3—Eu1—O6 | 154.9 (2) | Si1v—Ba1—Si2vii | 149.93 (7) |
O4ii—Eu1—O6 | 84.7 (2) | O7ii—Ba1—Si1i | 134.51 (13) |
O2i—Eu1—O7 | 77.9 (2) | O2v—Ba1—Si1i | 116.86 (14) |
O3—Eu1—O7 | 116.7 (2) | O6vi—Ba1—Si1i | 143.88 (15) |
O4ii—Eu1—O7 | 141.9 (2) | O7vi—Ba1—Si1i | 99.70 (13) |
O6—Eu1—O7 | 76.2 (2) | O4ii—Ba1—Si1i | 67.78 (13) |
O2i—Eu1—O3iii | 160.0 (2) | O5—Ba1—Si1i | 67.57 (10) |
O3—Eu1—O3iii | 81.2 (2) | O3v—Ba1—Si1i | 68.65 (12) |
O4ii—Eu1—O3iii | 82.5 (2) | O2i—Ba1—Si1i | 26.19 (12) |
O6—Eu1—O3iii | 73.8 (2) | O1i—Ba1—Si1i | 27.65 (12) |
O7—Eu1—O3iii | 121.81 (19) | Si1v—Ba1—Si1i | 95.61 (6) |
O2i—Eu1—O1iv | 125.6 (2) | Si2vii—Ba1—Si1i | 81.29 (6) |
O3—Eu1—O1iv | 77.23 (19) | O4—Si1—O2 | 115.8 (4) |
O4ii—Eu1—O1iv | 153.8 (2) | O4—Si1—O3 | 112.1 (3) |
O6—Eu1—O1iv | 92.8 (2) | O2—Si1—O3 | 109.6 (3) |
O7—Eu1—O1iv | 61.11 (19) | O4—Si1—O1 | 109.1 (3) |
O3iii—Eu1—O1iv | 71.84 (18) | O2—Si1—O1 | 102.9 (3) |
O2i—Eu1—Si2iv | 102.40 (17) | O3—Si1—O1 | 106.6 (3) |
O3—Eu1—Si2iv | 99.47 (15) | O4—Si1—Eu1 | 75.3 (2) |
O4ii—Eu1—Si2iv | 166.19 (15) | O2—Si1—Eu1 | 119.7 (3) |
O6—Eu1—Si2iv | 82.01 (16) | O3—Si1—Eu1 | 38.2 (2) |
O7—Eu1—Si2iv | 29.40 (14) | O1—Si1—Eu1 | 130.5 (2) |
O3iii—Eu1—Si2iv | 97.39 (14) | O4—Si1—Ba1v | 146.5 (2) |
O1iv—Eu1—Si2iv | 31.77 (13) | O2—Si1—Ba1v | 51.6 (2) |
O2i—Eu1—Si1 | 78.43 (17) | O3—Si1—Ba1v | 59.6 (2) |
O3—Eu1—Si1 | 26.36 (15) | O1—Si1—Ba1v | 104.2 (2) |
O4ii—Eu1—Si1 | 112.44 (15) | Eu1—Si1—Ba1v | 85.70 (6) |
O6—Eu1—Si1 | 162.02 (16) | O4—Si1—Eu1viii | 29.5 (2) |
O7—Eu1—Si1 | 91.92 (15) | O2—Si1—Eu1viii | 119.9 (3) |
O3iii—Eu1—Si1 | 102.20 (14) | O3—Si1—Eu1viii | 127.4 (2) |
O1iv—Eu1—Si1 | 69.47 (14) | O1—Si1—Eu1viii | 79.9 (2) |
Si2iv—Eu1—Si1 | 81.15 (6) | Eu1—Si1—Eu1viii | 97.72 (6) |
O2i—Eu1—Si2iii | 111.15 (17) | Ba1v—Si1—Eu1viii | 170.96 (9) |
O3—Eu1—Si2iii | 141.24 (15) | O4—Si1—Ba1i | 99.6 (3) |
O4ii—Eu1—Si2iii | 63.04 (15) | O2—Si1—Ba1i | 56.3 (2) |
O6—Eu1—Si2iii | 22.90 (16) | O3—Si1—Ba1i | 148.1 (2) |
O7—Eu1—Si2iii | 98.35 (15) | O1—Si1—Ba1i | 57.1 (2) |
O3iii—Eu1—Si2iii | 65.81 (14) | Eu1—Si1—Ba1i | 171.71 (9) |
O1iv—Eu1—Si2iii | 108.95 (14) | Ba1v—Si1—Ba1i | 95.61 (6) |
Si2iv—Eu1—Si2iii | 104.23 (7) | Eu1viii—Si1—Ba1i | 79.81 (5) |
Si1—Eu1—Si2iii | 167.17 (7) | O6iii—Si2—O7iv | 118.0 (4) |
O2i—Eu1—Si1ii | 88.21 (17) | O6iii—Si2—O5i | 111.8 (4) |
O3—Eu1—Si1ii | 76.16 (15) | O7iv—Si2—O5i | 105.9 (3) |
O4ii—Eu1—Si1ii | 19.83 (15) | O6iii—Si2—O1 | 113.9 (3) |
O6—Eu1—Si1ii | 97.58 (16) | O7iv—Si2—O1 | 103.1 (3) |
O7—Eu1—Si1ii | 161.19 (15) | O5i—Si2—O1 | 102.5 (3) |
O3iii—Eu1—Si1ii | 71.88 (14) | O6iii—Si2—Eu1iv | 137.8 (3) |
O1iv—Eu1—Si1ii | 137.56 (13) | O7iv—Si2—Eu1iv | 47.2 (2) |
Si2iv—Eu1—Si1ii | 168.80 (7) | O5i—Si2—Eu1iv | 110.4 (3) |
Si1—Eu1—Si1ii | 97.73 (6) | O1—Si2—Eu1iv | 56.0 (2) |
Si2iii—Eu1—Si1ii | 74.70 (6) | O6iii—Si2—Eu1iii | 35.1 (2) |
O2i—Eu1—Eu1iii | 132.30 (16) | O7iv—Si2—Eu1iii | 105.7 (2) |
O3—Eu1—Eu1iii | 42.45 (14) | O5i—Si2—Eu1iii | 143.6 (3) |
O4ii—Eu1—Eu1iii | 87.54 (15) | O1—Si2—Eu1iii | 87.4 (2) |
O6—Eu1—Eu1iii | 112.54 (16) | Eu1iv—Si2—Eu1iii | 104.23 (7) |
O7—Eu1—Eu1iii | 130.15 (14) | O6iii—Si2—Ba1ix | 127.0 (3) |
O3iii—Eu1—Eu1iii | 38.73 (13) | O7iv—Si2—Ba1ix | 52.0 (2) |
O1iv—Eu1—Eu1iii | 69.34 (13) | O5i—Si2—Ba1ix | 54.59 (19) |
Si2iv—Eu1—Eu1iii | 101.07 (5) | O1—Si2—Ba1ix | 119.0 (2) |
Si1—Eu1—Eu1iii | 64.98 (5) | Eu1iv—Si2—Ba1ix | 78.78 (6) |
Si2iii—Eu1—Eu1iii | 102.35 (5) | Eu1iii—Si2—Ba1ix | 146.91 (8) |
Si1ii—Eu1—Eu1iii | 68.66 (4) | O6iii—Si2—Ba1iii | 78.5 (3) |
O7ii—Ba1—O2v | 66.19 (18) | O7iv—Si2—Ba1iii | 41.5 (2) |
O7ii—Ba1—O6vi | 77.43 (19) | O5i—Si2—Ba1iii | 137.30 (14) |
O2v—Ba1—O6vi | 89.19 (19) | O1—Si2—Ba1iii | 110.7 (2) |
O7ii—Ba1—O7vi | 83.43 (13) | Eu1iv—Si2—Ba1iii | 70.28 (5) |
O2v—Ba1—O7vi | 142.71 (18) | Eu1iii—Si2—Ba1iii | 65.59 (4) |
O6vi—Ba1—O7vi | 62.40 (18) | Ba1ix—Si2—Ba1iii | 85.43 (6) |
O7ii—Ba1—O4ii | 69.69 (17) | O6iii—Si2—Ba1i | 137.7 (3) |
O2v—Ba1—O4ii | 76.09 (18) | O7iv—Si2—Ba1i | 104.2 (2) |
O6vi—Ba1—O4ii | 147.06 (18) | O5i—Si2—Ba1i | 48.85 (18) |
O7vi—Ba1—O4ii | 114.19 (17) | O1—Si2—Ba1i | 54.9 (2) |
O7ii—Ba1—O5 | 136.73 (13) | Eu1iv—Si2—Ba1i | 74.57 (5) |
O2v—Ba1—O5 | 146.68 (17) | Eu1iii—Si2—Ba1i | 136.27 (8) |
O6vi—Ba1—O5 | 76.98 (18) | Ba1ix—Si2—Ba1i | 76.69 (5) |
O7vi—Ba1—O5 | 53.79 (12) | Ba1iii—Si2—Ba1i | 143.00 (7) |
O4ii—Ba1—O5 | 129.75 (18) | Si2—O1—Si1 | 124.8 (4) |
O7ii—Ba1—O3v | 120.13 (17) | Si2—O1—Eu1iv | 92.2 (3) |
O2v—Ba1—O3v | 56.12 (17) | Si1—O1—Eu1iv | 139.6 (3) |
O6vi—Ba1—O3v | 114.19 (16) | Si2—O1—Ba1i | 98.6 (3) |
O7vi—Ba1—O3v | 155.77 (16) | Si1—O1—Ba1i | 95.3 (2) |
O4ii—Ba1—O3v | 81.93 (15) | Eu1iv—O1—Ba1i | 94.26 (18) |
O5—Ba1—O3v | 102.08 (12) | Si1—O2—Eu1i | 140.7 (4) |
O7ii—Ba1—O2i | 113.68 (17) | Si1—O2—Ba1v | 100.6 (3) |
O2v—Ba1—O2i | 129.5 (2) | Eu1i—O2—Ba1v | 103.1 (2) |
O6vi—Ba1—O2i | 141.28 (19) | Si1—O2—Ba1i | 97.5 (3) |
O7vi—Ba1—O2i | 81.49 (17) | Eu1i—O2—Ba1i | 91.0 (2) |
O4ii—Ba1—O2i | 59.52 (18) | Ba1v—O2—Ba1i | 129.5 (2) |
O5—Ba1—O2i | 70.23 (18) | Si1—O3—Eu1 | 115.4 (3) |
O3v—Ba1—O2i | 92.72 (16) | Si1—O3—Eu1iii | 130.0 (3) |
O7ii—Ba1—O1i | 162.10 (17) | Eu1—O3—Eu1iii | 98.8 (2) |
O2v—Ba1—O1i | 116.04 (17) | Si1—O3—Ba1v | 91.4 (2) |
O6vi—Ba1—O1i | 119.71 (18) | Eu1—O3—Ba1v | 122.4 (2) |
O7vi—Ba1—O1i | 99.60 (16) | Eu1iii—O3—Ba1v | 100.11 (18) |
O4ii—Ba1—O1i | 93.21 (17) | Si1—O4—Eu1viii | 130.6 (3) |
O5—Ba1—O1i | 51.38 (12) | Si1—O4—Ba1viii | 131.5 (3) |
O3v—Ba1—O1i | 59.98 (16) | Eu1viii—O4—Ba1viii | 95.8 (2) |
O2i—Ba1—O1i | 50.14 (16) | Si2vii—O5—Si2i | 142.6 (6) |
O7ii—Ba1—Si1v | 93.73 (14) | Si2vii—O5—Ba1 | 97.75 (16) |
O2v—Ba1—Si1v | 27.73 (13) | Si2i—O5—Ba1 | 105.75 (17) |
O6vi—Ba1—Si1v | 98.71 (14) | Si2vii—O5—Ba1x | 105.75 (17) |
O7vi—Ba1—Si1v | 161.09 (13) | Si2i—O5—Ba1x | 97.75 (16) |
O4ii—Ba1—Si1v | 81.88 (12) | Ba1—O5—Ba1x | 101.4 (3) |
O5—Ba1—Si1v | 124.24 (9) | Si2iii—O6—Eu1 | 122.0 (3) |
O3v—Ba1—Si1v | 29.03 (12) | Si2iii—O6—Ba1xi | 121.6 (3) |
O2i—Ba1—Si1v | 116.47 (13) | Eu1—O6—Ba1xi | 111.4 (2) |
O1i—Ba1—Si1v | 88.86 (12) | Si2iv—O7—Eu1 | 103.4 (3) |
O7ii—Ba1—Si2vii | 109.83 (13) | Si2iv—O7—Ba1viii | 115.2 (3) |
O2v—Ba1—Si2vii | 158.87 (14) | Eu1—O7—Ba1viii | 102.2 (2) |
O6vi—Ba1—Si2vii | 69.83 (14) | Si2iv—O7—Ba1xi | 101.6 (3) |
O7vi—Ba1—Si2vii | 26.41 (12) | Eu1—O7—Ba1xi | 108.7 (2) |
O4ii—Ba1—Si2vii | 123.14 (13) | Ba1viii—O7—Ba1xi | 124.1 (2) |
Symmetry codes: (i) −x+3/2, −y−1/2, −z+1; (ii) x, y+1, z; (iii) −x+2, −y, −z+1; (iv) −x+2, −y−1, −z+1; (v) −x+3/2, −y+1/2, −z+1; (vi) −x+3/2, y+1/2, −z+1/2; (vii) x−1/2, −y−1/2, z−1/2; (viii) x, y−1, z; (ix) x+1/2, −y−1/2, z+1/2; (x) −x+1, y, −z+1/2; (xi) −x+3/2, y−1/2, −z+1/2. |
Ba2O13Si4Tb2 | F(000) = 1608 |
Mr = 912.88 | Dx = 5.335 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.8568 (5) Å | Cell parameters from 7901 reflections |
b = 5.2019 (2) Å | θ = 2.5–33.2° |
c = 17.5243 (7) Å | µ = 19.63 mm−1 |
β = 104.1469 (15)° | T = 298 K |
V = 1136.48 (8) Å3 | Block, colourless |
Z = 4 | 0.16 × 0.16 × 0.06 mm |
Bruker Photon 100 diffractometer | 1098 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.035 |
φ and ω scans | θmax = 26.5°, θmin = 2.4° |
Absorption correction: multi-scan SADABS, Bruker | h = −16→16 |
Tmin = 0.839, Tmax = 1.000 | k = −6→6 |
6944 measured reflections | l = −22→22 |
1177 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0119P)2 + 18.0813P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.002 |
wR(F2) = 0.049 | Δρmax = 1.08 e Å−3 |
S = 1.19 | Δρmin = −0.94 e Å−3 |
1177 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
97 parameters | Extinction coefficient: 0.00262 (8) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Tb1 | 0.88615 (2) | 0.01050 (4) | 0.41555 (2) | 0.00352 (12) | |
Ba1 | 0.66248 (2) | 0.49457 (5) | 0.33304 (2) | 0.00617 (12) | |
Si1 | 0.88092 (11) | −0.4664 (3) | 0.54303 (8) | 0.0030 (3) | |
Si2 | 1.06229 (11) | −0.5447 (3) | 0.68364 (8) | 0.0035 (3) | |
O1 | 0.9808 (3) | −0.6440 (6) | 0.6000 (2) | 0.0046 (7) | |
O2 | 0.7934 (3) | −0.4569 (7) | 0.5959 (2) | 0.0078 (7) | |
O3 | 0.9292 (3) | −0.1766 (6) | 0.5377 (2) | 0.0054 (7) | |
O4 | 0.8433 (3) | −0.5999 (7) | 0.4588 (2) | 0.0073 (7) | |
O5 | 0.5000 | 0.1432 (9) | 0.2500 | 0.0063 (10) | |
O6 | 0.9190 (3) | 0.2426 (7) | 0.3110 (2) | 0.0080 (7) | |
O7 | 0.8352 (3) | −0.2715 (7) | 0.3069 (2) | 0.0054 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tb1 | 0.00309 (15) | 0.00519 (16) | 0.00301 (16) | −0.00016 (8) | 0.00216 (10) | 0.00009 (8) |
Ba1 | 0.00615 (18) | 0.00703 (18) | 0.00599 (19) | −0.00200 (10) | 0.00274 (13) | −0.00101 (10) |
Si1 | 0.0025 (6) | 0.0047 (6) | 0.0021 (6) | −0.0007 (5) | 0.0014 (5) | −0.0005 (5) |
Si2 | 0.0046 (6) | 0.0036 (6) | 0.0033 (6) | −0.0001 (5) | 0.0026 (5) | 0.0002 (5) |
O1 | 0.0048 (16) | 0.0055 (16) | 0.0033 (16) | −0.0009 (13) | 0.0008 (13) | −0.0004 (14) |
O2 | 0.0056 (17) | 0.0099 (17) | 0.0101 (19) | −0.0040 (13) | 0.0059 (15) | −0.0026 (15) |
O3 | 0.0074 (16) | 0.0043 (16) | 0.0052 (17) | 0.0001 (13) | 0.0026 (13) | 0.0012 (13) |
O4 | 0.0072 (17) | 0.0084 (17) | 0.0064 (17) | 0.0020 (14) | 0.0020 (14) | −0.0018 (14) |
O5 | 0.008 (2) | 0.008 (2) | 0.005 (2) | 0.000 | 0.0055 (19) | 0.000 |
O6 | 0.0137 (18) | 0.0046 (16) | 0.0061 (17) | −0.0030 (13) | 0.0030 (14) | 0.0011 (14) |
O7 | 0.0040 (16) | 0.0072 (17) | 0.0055 (16) | 0.0012 (13) | 0.0024 (13) | −0.0002 (14) |
Tb1—O4i | 2.278 (3) | Si1—Ba1ii | 3.6289 (14) |
Tb1—O2ii | 2.285 (3) | Si2—O6iii | 1.589 (4) |
Tb1—O3 | 2.292 (3) | Si2—O7iv | 1.603 (4) |
Tb1—O6 | 2.318 (4) | Si2—O5ii | 1.647 (2) |
Tb1—O7 | 2.366 (3) | Si2—O1 | 1.662 (3) |
Tb1—O3iii | 2.470 (3) | Si2—Tb1iv | 3.1456 (14) |
Tb1—O1iv | 2.620 (3) | Si2—Tb1iii | 3.4273 (14) |
Tb1—Si2iv | 3.1456 (14) | Si2—Ba1ix | 3.5131 (14) |
Tb1—Si1 | 3.3502 (14) | Si2—Ba1iii | 3.6305 (14) |
Tb1—Si2iii | 3.4273 (14) | Si2—Ba1ii | 3.6742 (14) |
Tb1—Tb1iii | 3.6203 (5) | O1—Tb1iv | 2.620 (3) |
Tb1—Ba1 | 3.8300 (4) | O1—Ba1ii | 3.025 (3) |
Ba1—O7i | 2.668 (3) | O2—Tb1ii | 2.285 (3) |
Ba1—O2v | 2.704 (4) | O2—Ba1v | 2.704 (4) |
Ba1—O6vi | 2.800 (3) | O2—Ba1ii | 3.058 (4) |
Ba1—O7vi | 2.822 (3) | O3—Tb1iii | 2.471 (3) |
Ba1—O4i | 2.828 (3) | O3—Ba1v | 2.954 (3) |
Ba1—O5 | 2.887 (3) | O4—Tb1x | 2.278 (3) |
Ba1—O3v | 2.954 (3) | O4—Ba1x | 2.828 (3) |
Ba1—O1ii | 3.025 (3) | O5—Si2viii | 1.647 (2) |
Ba1—O2ii | 3.058 (4) | O5—Si2ii | 1.647 (2) |
Ba1—O6vii | 3.320 (4) | O5—Ba1xi | 2.887 (3) |
Ba1—Si1v | 3.4125 (14) | O6—Si2iii | 1.589 (4) |
Ba1—Si2viii | 3.5131 (14) | O6—Ba1xii | 2.800 (3) |
Si1—O4 | 1.595 (4) | O6—Ba1xiii | 3.320 (4) |
Si1—O2 | 1.624 (4) | O7—Si2iv | 1.603 (4) |
Si1—O3 | 1.642 (4) | O7—Ba1x | 2.668 (3) |
Si1—O1 | 1.695 (3) | O7—Ba1xii | 2.822 (3) |
Si1—Ba1v | 3.4125 (14) | ||
O4i—Tb1—O2ii | 79.41 (13) | O7vi—Ba1—Si1v | 160.70 (7) |
O4i—Tb1—O3 | 95.17 (12) | O4i—Ba1—Si1v | 81.95 (7) |
O2ii—Tb1—O3 | 92.20 (13) | O5—Ba1—Si1v | 124.43 (5) |
O4i—Tb1—O6 | 84.56 (13) | O3v—Ba1—Si1v | 28.75 (7) |
O2ii—Tb1—O6 | 111.68 (13) | O1ii—Ba1—Si1v | 88.68 (7) |
O3—Tb1—O6 | 155.54 (12) | O2ii—Ba1—Si1v | 116.21 (7) |
O4i—Tb1—O7 | 141.03 (12) | O6vii—Ba1—Si1v | 59.89 (6) |
O2ii—Tb1—O7 | 77.21 (12) | O7i—Ba1—Si2viii | 110.17 (8) |
O3—Tb1—O7 | 116.37 (12) | O2v—Ba1—Si2viii | 158.93 (8) |
O6—Tb1—O7 | 75.81 (12) | O6vi—Ba1—Si2viii | 69.32 (7) |
O4i—Tb1—O3iii | 82.50 (12) | O7vi—Ba1—Si2viii | 26.57 (7) |
O2ii—Tb1—O3iii | 160.08 (12) | O4i—Ba1—Si2viii | 123.16 (7) |
O3—Tb1—O3iii | 81.12 (13) | O5—Ba1—Si2viii | 27.67 (3) |
O6—Tb1—O3iii | 74.58 (12) | O3v—Ba1—Si2viii | 130.00 (7) |
O7—Tb1—O3iii | 122.58 (12) | O1ii—Ba1—Si2viii | 74.95 (7) |
O4i—Tb1—O1iv | 154.07 (11) | O2ii—Ba1—Si2viii | 72.06 (7) |
O2ii—Tb1—O1iv | 124.99 (12) | O6vii—Ba1—Si2viii | 90.49 (6) |
O3—Tb1—O1iv | 76.89 (11) | Si1v—Ba1—Si2viii | 150.02 (3) |
O6—Tb1—O1iv | 92.70 (12) | O4—Si1—O2 | 116.4 (2) |
O7—Tb1—O1iv | 61.59 (11) | O4—Si1—O3 | 112.3 (2) |
O3iii—Tb1—O1iv | 71.95 (11) | O2—Si1—O3 | 109.21 (19) |
O4i—Tb1—Si2iv | 165.90 (9) | O4—Si1—O1 | 108.84 (18) |
O2ii—Tb1—Si2iv | 101.67 (10) | O2—Si1—O1 | 102.20 (19) |
O3—Tb1—Si2iv | 98.82 (9) | O3—Si1—O1 | 106.95 (18) |
O6—Tb1—Si2iv | 81.99 (9) | O4—Si1—Tb1 | 75.89 (14) |
O7—Tb1—Si2iv | 29.76 (8) | O2—Si1—Tb1 | 119.18 (15) |
O3iii—Tb1—Si2iv | 97.91 (8) | O3—Si1—Tb1 | 38.03 (12) |
O1iv—Tb1—Si2iv | 31.88 (7) | O1—Si1—Tb1 | 131.35 (13) |
O4i—Tb1—Si1 | 113.02 (9) | O4—Si1—Ba1v | 147.33 (14) |
O2ii—Tb1—Si1 | 77.51 (10) | O2—Si1—Ba1v | 51.02 (13) |
O3—Tb1—Si1 | 26.18 (9) | O3—Si1—Ba1v | 59.92 (13) |
O6—Tb1—Si1 | 161.84 (9) | O1—Si1—Ba1v | 103.61 (13) |
O7—Tb1—Si1 | 91.76 (9) | Tb1—Si1—Ba1v | 85.69 (3) |
O3iii—Tb1—Si1 | 102.24 (8) | O4—Si1—Ba1ii | 99.67 (14) |
O1iv—Tb1—Si1 | 69.54 (8) | O2—Si1—Ba1ii | 56.78 (14) |
Si2iv—Tb1—Si1 | 80.76 (3) | O3—Si1—Ba1ii | 147.68 (14) |
O4i—Tb1—Si2iii | 62.61 (9) | O1—Si1—Ba1ii | 55.95 (12) |
O2ii—Tb1—Si2iii | 111.77 (10) | Tb1—Si1—Ba1ii | 172.23 (5) |
O3—Tb1—Si2iii | 141.75 (9) | Ba1v—Si1—Ba1ii | 95.20 (3) |
O6—Tb1—Si2iii | 23.28 (9) | O6iii—Si2—O7iv | 118.3 (2) |
O7—Tb1—Si2iii | 98.30 (9) | O6iii—Si2—O5ii | 111.0 (2) |
O3iii—Tb1—Si2iii | 66.13 (8) | O7iv—Si2—O5ii | 105.70 (19) |
O1iv—Tb1—Si2iii | 108.98 (8) | O6iii—Si2—O1 | 114.40 (19) |
Si2iv—Tb1—Si2iii | 104.55 (4) | O7iv—Si2—O1 | 103.36 (19) |
Si1—Tb1—Si2iii | 167.56 (3) | O5ii—Si2—O1 | 102.45 (16) |
O4i—Tb1—Tb1iii | 88.17 (8) | O6iii—Si2—Tb1iv | 138.17 (15) |
O2ii—Tb1—Tb1iii | 131.75 (9) | O7iv—Si2—Tb1iv | 47.08 (13) |
O3—Tb1—Tb1iii | 42.39 (8) | O5ii—Si2—Tb1iv | 110.80 (18) |
O6—Tb1—Tb1iii | 113.26 (9) | O1—Si2—Tb1iv | 56.35 (12) |
O7—Tb1—Tb1iii | 130.44 (8) | O6iii—Si2—Tb1iii | 35.21 (13) |
O3iii—Tb1—Tb1iii | 38.73 (8) | O7iv—Si2—Tb1iii | 106.25 (14) |
O1iv—Tb1—Tb1iii | 69.21 (7) | O5ii—Si2—Tb1iii | 142.96 (18) |
Si2iv—Tb1—Tb1iii | 101.01 (3) | O1—Si2—Tb1iii | 87.88 (13) |
Si1—Tb1—Tb1iii | 64.94 (2) | Tb1iv—Si2—Tb1iii | 104.55 (4) |
Si2iii—Tb1—Tb1iii | 102.78 (2) | O6iii—Si2—Ba1ix | 126.29 (14) |
O4i—Tb1—Ba1 | 47.17 (8) | O7iv—Si2—Ba1ix | 51.93 (13) |
O2ii—Tb1—Ba1 | 52.97 (9) | O5ii—Si2—Ba1ix | 54.51 (11) |
O3—Tb1—Ba1 | 128.27 (9) | O1—Si2—Ba1ix | 119.19 (13) |
O6—Tb1—Ba1 | 67.92 (9) | Tb1iv—Si2—Ba1ix | 79.07 (3) |
O7—Tb1—Ba1 | 93.97 (8) | Tb1iii—Si2—Ba1ix | 146.82 (4) |
O3iii—Tb1—Ba1 | 117.85 (8) | O6iii—Si2—Ba1iii | 78.30 (14) |
O1iv—Tb1—Ba1 | 152.66 (7) | O7iv—Si2—Ba1iii | 42.15 (13) |
Si2iv—Tb1—Ba1 | 122.55 (3) | O5ii—Si2—Ba1iii | 136.97 (8) |
Si1—Tb1—Ba1 | 127.09 (2) | O1—Si2—Ba1iii | 111.60 (13) |
Si2iii—Tb1—Ba1 | 59.73 (2) | Tb1iv—Si2—Ba1iii | 70.71 (3) |
Tb1iii—Tb1—Ba1 | 135.315 (11) | Tb1iii—Si2—Ba1iii | 65.66 (2) |
O7i—Ba1—O2v | 65.40 (11) | Ba1ix—Si2—Ba1iii | 85.46 (3) |
O7i—Ba1—O6vi | 77.22 (10) | O6iii—Si2—Ba1ii | 137.67 (15) |
O2v—Ba1—O6vi | 89.73 (11) | O7iv—Si2—Ba1ii | 103.83 (14) |
O7i—Ba1—O7vi | 83.60 (7) | O5ii—Si2—Ba1ii | 49.40 (11) |
O2v—Ba1—O7vi | 142.26 (11) | O1—Si2—Ba1ii | 54.41 (13) |
O6vi—Ba1—O7vi | 61.57 (10) | Tb1iv—Si2—Ba1ii | 74.53 (3) |
O7i—Ba1—O4i | 69.69 (10) | Tb1iii—Si2—Ba1ii | 136.21 (4) |
O2v—Ba1—O4i | 75.86 (11) | Ba1ix—Si2—Ba1ii | 76.88 (3) |
O6vi—Ba1—O4i | 146.90 (11) | Ba1iii—Si2—Ba1ii | 143.37 (4) |
O7vi—Ba1—O4i | 114.26 (10) | Si2—O1—Si1 | 125.0 (2) |
O7i—Ba1—O5 | 137.07 (7) | Si2—O1—Tb1iv | 91.77 (14) |
O2v—Ba1—O5 | 147.10 (10) | Si1—O1—Tb1iv | 139.06 (18) |
O6vi—Ba1—O5 | 76.83 (10) | Si2—O1—Ba1ii | 99.07 (15) |
O7vi—Ba1—O5 | 53.95 (7) | Si1—O1—Ba1ii | 96.40 (14) |
O4i—Ba1—O5 | 129.68 (10) | Tb1iv—O1—Ba1ii | 94.39 (10) |
O7i—Ba1—O3v | 119.37 (10) | Si1—O2—Tb1ii | 140.6 (2) |
O2v—Ba1—O3v | 55.92 (10) | Si1—O2—Ba1v | 101.15 (16) |
O6vi—Ba1—O3v | 114.34 (10) | Tb1ii—O2—Ba1v | 104.04 (13) |
O7vi—Ba1—O3v | 156.14 (9) | Si1—O2—Ba1ii | 96.84 (16) |
O4i—Ba1—O3v | 82.18 (10) | Tb1ii—O2—Ba1ii | 90.40 (11) |
O5—Ba1—O3v | 102.38 (7) | Ba1v—O2—Ba1ii | 128.97 (13) |
O7i—Ba1—O1ii | 162.30 (10) | Si1—O3—Tb1 | 115.78 (18) |
O2v—Ba1—O1ii | 115.89 (10) | Si1—O3—Tb1iii | 130.42 (18) |
O6vi—Ba1—O1ii | 119.89 (10) | Tb1—O3—Tb1iii | 98.88 (13) |
O7vi—Ba1—O1ii | 100.25 (9) | Si1—O3—Ba1v | 91.33 (15) |
O4i—Ba1—O1ii | 93.17 (10) | Tb1—O3—Ba1v | 121.96 (13) |
O5—Ba1—O1ii | 51.67 (7) | Tb1iii—O3—Ba1v | 99.47 (11) |
O3v—Ba1—O1ii | 60.06 (9) | Si1—O4—Tb1x | 130.6 (2) |
O7i—Ba1—O2ii | 114.06 (10) | Si1—O4—Ba1x | 130.64 (18) |
O2v—Ba1—O2ii | 128.97 (13) | Tb1x—O4—Ba1x | 96.60 (12) |
O6vi—Ba1—O2ii | 141.25 (10) | Si2viii—O5—Si2ii | 143.7 (3) |
O7vi—Ba1—O2ii | 82.24 (10) | Si2viii—O5—Ba1 | 97.82 (9) |
O4i—Ba1—O2ii | 59.23 (10) | Si2ii—O5—Ba1 | 104.95 (10) |
O5—Ba1—O2ii | 70.46 (10) | Si2viii—O5—Ba1xi | 104.95 (10) |
O3v—Ba1—O2ii | 92.87 (9) | Si2ii—O5—Ba1xi | 97.82 (9) |
O1ii—Ba1—O2ii | 50.25 (9) | Ba1—O5—Ba1xi | 101.45 (15) |
O7i—Ba1—O6vii | 127.12 (9) | Si2iii—O6—Tb1 | 121.5 (2) |
O2v—Ba1—O6vii | 78.09 (10) | Si2iii—O6—Ba1xii | 121.80 (18) |
O6vi—Ba1—O6vii | 65.27 (12) | Tb1—O6—Ba1xii | 111.85 (13) |
O7vi—Ba1—O6vii | 107.41 (9) | Si2iii—O6—Ba1xiii | 104.63 (17) |
O4i—Ba1—O6vii | 136.90 (9) | Tb1—O6—Ba1xiii | 93.11 (11) |
O5—Ba1—O6vii | 69.01 (9) | Ba1xii—O6—Ba1xiii | 93.45 (10) |
O3v—Ba1—O6vii | 54.76 (9) | Si2iv—O7—Tb1 | 103.16 (17) |
O1ii—Ba1—O6vii | 68.49 (9) | Si2iv—O7—Ba1x | 114.07 (17) |
O2ii—Ba1—O6vii | 118.60 (9) | Tb1—O7—Ba1x | 102.88 (13) |
O7i—Ba1—Si1v | 93.08 (8) | Si2iv—O7—Ba1xii | 101.50 (16) |
O2v—Ba1—Si1v | 27.83 (8) | Tb1—O7—Ba1xii | 109.60 (13) |
O6vi—Ba1—Si1v | 99.14 (7) | Ba1x—O7—Ba1xii | 123.96 (12) |
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, −y−1/2, −z+1; (iii) −x+2, −y, −z+1; (iv) −x+2, −y−1, −z+1; (v) −x+3/2, −y+1/2, −z+1; (vi) −x+3/2, y+1/2, −z+1/2; (vii) x−1/2, y+1/2, z; (viii) x−1/2, −y−1/2, z−1/2; (ix) x+1/2, −y−1/2, z+1/2; (x) x, y−1, z; (xi) −x+1, y, −z+1/2; (xii) −x+3/2, y−1/2, −z+1/2; (xiii) x+1/2, y−1/2, z. |
Ba2Dy2O13Si4 | F(000) = 1616 |
Mr = 920.04 | Dx = 5.379 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.8478 (9) Å | Cell parameters from 3018 reflections |
b = 5.2020 (6) Å | θ = 2.4–26.7° |
c = 17.525 (3) Å | µ = 20.34 mm−1 |
β = 104.077 (15)° | T = 298 K |
V = 1136.1 (3) Å3 | Block, green |
Z = 4 | 0.26 × 0.19 × 0.18 mm |
Rigaku AFC8S diffractometer | 1190 independent reflections |
Radiation source: fine-focus sealed tube | 1130 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.075 |
ω scans | θmax = 26.7°, θmin = 3.3° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −16→16 |
Tmin = 0.405, Tmax = 1.000 | k = −6→6 |
4778 measured reflections | l = −21→22 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.130 | (Δ/σ)max = 0.001 |
S = 1.16 | Δρmax = 1.90 e Å−3 |
1190 reflections | Δρmin = −4.00 e Å−3 |
97 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0043 (3) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Dy1 | 0.88648 (3) | 0.01023 (7) | 0.41576 (3) | 0.0076 (3) | |
Ba1 | 0.66244 (5) | 0.49475 (8) | 0.33307 (4) | 0.0097 (3) | |
Si1 | 0.8806 (2) | −0.4678 (5) | 0.54261 (16) | 0.0080 (6) | |
Si2 | 1.0623 (2) | −0.5444 (5) | 0.68300 (15) | 0.0088 (5) | |
O1 | 0.9803 (4) | −0.6448 (11) | 0.5994 (3) | 0.0122 (11) | |
O2 | 0.7917 (5) | −0.4577 (12) | 0.5946 (4) | 0.0117 (12) | |
O3 | 0.9292 (4) | −0.1771 (11) | 0.5366 (3) | 0.0099 (11) | |
O4 | 0.8427 (4) | −0.6012 (12) | 0.4583 (3) | 0.0117 (11) | |
O5 | 0.5000 | 0.1406 (16) | 0.2500 | 0.0121 (16) | |
O6 | 0.9182 (4) | 0.2440 (12) | 0.3123 (3) | 0.0149 (12) | |
O7 | 0.8353 (4) | −0.2698 (11) | 0.3078 (3) | 0.0119 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Dy1 | 0.0057 (4) | 0.0124 (4) | 0.0059 (4) | −0.00007 (10) | 0.0039 (2) | 0.00022 (11) |
Ba1 | 0.0080 (4) | 0.0139 (4) | 0.0084 (5) | −0.00187 (13) | 0.0043 (3) | −0.00091 (14) |
Si1 | 0.0061 (10) | 0.0122 (11) | 0.0070 (13) | −0.0011 (7) | 0.0040 (9) | −0.0003 (8) |
Si2 | 0.0072 (11) | 0.0132 (10) | 0.0068 (12) | −0.0003 (8) | 0.0032 (9) | 0.0004 (9) |
O1 | 0.011 (2) | 0.013 (3) | 0.012 (3) | 0.001 (2) | 0.003 (2) | 0.000 (2) |
O2 | 0.006 (3) | 0.019 (3) | 0.012 (3) | 0.000 (2) | 0.007 (2) | −0.003 (2) |
O3 | 0.009 (2) | 0.013 (3) | 0.008 (3) | 0.001 (2) | 0.002 (2) | −0.001 (2) |
O4 | 0.011 (2) | 0.015 (3) | 0.009 (3) | 0.001 (2) | 0.003 (2) | 0.001 (2) |
O5 | 0.012 (3) | 0.017 (4) | 0.010 (4) | 0.000 | 0.006 (3) | 0.000 |
O6 | 0.015 (3) | 0.019 (3) | 0.012 (3) | −0.004 (2) | 0.006 (2) | −0.003 (2) |
O7 | 0.007 (2) | 0.018 (3) | 0.013 (3) | 0.002 (2) | 0.006 (2) | −0.002 (2) |
Dy1—O2i | 2.268 (6) | Si1—Ba1vi | 3.420 (3) |
Dy1—O4ii | 2.272 (6) | Si1—Ba1i | 3.627 (3) |
Dy1—O3 | 2.274 (5) | Si2—O6iii | 1.581 (6) |
Dy1—O6 | 2.300 (6) | Si2—O7iv | 1.609 (6) |
Dy1—O7 | 2.351 (6) | Si2—O5i | 1.651 (4) |
Dy1—O3iii | 2.468 (5) | Si2—O1 | 1.667 (6) |
Dy1—O1iv | 2.615 (5) | Si2—Dy1iv | 3.139 (3) |
Dy1—Si2iv | 3.139 (3) | Si2—Ba1ix | 3.523 (3) |
Dy1—Si1 | 3.349 (3) | Si2—Ba1iii | 3.624 (2) |
Dy1—Dy1iii | 3.6121 (11) | Si2—Ba1i | 3.676 (3) |
Dy1—Ba1 | 3.8352 (8) | O1—Dy1iv | 2.615 (5) |
Dy1—Ba1v | 3.9430 (7) | O1—Ba1i | 3.022 (6) |
Ba1—O7ii | 2.666 (5) | O2—Dy1i | 2.268 (6) |
Ba1—O2vi | 2.718 (7) | O2—Ba1vi | 2.718 (7) |
Ba1—O4ii | 2.821 (5) | O2—Ba1i | 3.065 (7) |
Ba1—O6vii | 2.821 (6) | O3—Dy1iii | 2.469 (5) |
Ba1—O7vii | 2.833 (6) | O3—Ba1vi | 2.968 (5) |
Ba1—O5 | 2.897 (5) | O4—Dy1v | 2.272 (6) |
Ba1—O3vi | 2.968 (5) | O4—Ba1v | 2.821 (5) |
Ba1—O1i | 3.022 (6) | O5—Si2viii | 1.651 (4) |
Ba1—O2i | 3.065 (7) | O5—Si2i | 1.651 (4) |
Ba1—Si1vi | 3.420 (3) | O5—Ba1x | 2.897 (5) |
Ba1—Si2viii | 3.524 (3) | O6—Si2iii | 1.581 (6) |
Ba1—Si2iii | 3.624 (3) | O6—Ba1xi | 2.821 (6) |
Si1—O4 | 1.597 (6) | O7—Si2iv | 1.609 (6) |
Si1—O2 | 1.627 (7) | O7—Ba1v | 2.666 (5) |
Si1—O3 | 1.650 (6) | O7—Ba1xi | 2.833 (6) |
Si1—O1 | 1.690 (6) | ||
O2i—Dy1—O4ii | 78.9 (2) | O1i—Ba1—Si1vi | 88.65 (12) |
O2i—Dy1—O3 | 91.9 (2) | O2i—Ba1—Si1vi | 115.93 (14) |
O4ii—Dy1—O3 | 95.6 (2) | O7ii—Ba1—Si2viii | 110.45 (13) |
O2i—Dy1—O6 | 111.7 (2) | O2vi—Ba1—Si2viii | 159.30 (16) |
O4ii—Dy1—O6 | 83.9 (2) | O4ii—Ba1—Si2viii | 123.01 (13) |
O3—Dy1—O6 | 155.74 (19) | O6vii—Ba1—Si2viii | 69.17 (13) |
O2i—Dy1—O7 | 77.4 (2) | O7vii—Ba1—Si2viii | 26.59 (11) |
O4ii—Dy1—O7 | 140.6 (2) | O5—Ba1—Si2viii | 27.67 (5) |
O3—Dy1—O7 | 116.2 (2) | O3vi—Ba1—Si2viii | 130.20 (11) |
O6—Dy1—O7 | 76.2 (2) | O1i—Ba1—Si2viii | 75.27 (12) |
O2i—Dy1—O3iii | 159.3 (2) | O2i—Ba1—Si2viii | 72.61 (14) |
O4ii—Dy1—O3iii | 82.52 (18) | Si1vi—Ba1—Si2viii | 150.20 (7) |
O3—Dy1—O3iii | 80.9 (2) | O7ii—Ba1—Si2iii | 23.99 (13) |
O6—Dy1—O3iii | 75.02 (19) | O2vi—Ba1—Si2iii | 82.41 (14) |
O7—Dy1—O3iii | 123.19 (18) | O4ii—Ba1—Si2iii | 56.03 (12) |
O2i—Dy1—O1iv | 125.2 (2) | O6vii—Ba1—Si2iii | 92.75 (12) |
O4ii—Dy1—O1iv | 154.24 (18) | O7vii—Ba1—Si2iii | 75.51 (11) |
O3—Dy1—O1iv | 76.53 (18) | O5—Ba1—Si2iii | 127.12 (8) |
O6—Dy1—O1iv | 93.35 (19) | O3vi—Ba1—Si2iii | 127.90 (11) |
O7—Dy1—O1iv | 61.95 (18) | O1i—Ba1—Si2iii | 140.33 (11) |
O3iii—Dy1—O1iv | 72.07 (18) | O2i—Ba1—Si2iii | 90.21 (12) |
O2i—Dy1—Si2iv | 101.85 (17) | Si1vi—Ba1—Si2iii | 108.08 (6) |
O4ii—Dy1—Si2iv | 165.83 (15) | Si2viii—Ba1—Si2iii | 100.10 (6) |
O3—Dy1—Si2iv | 98.46 (15) | O4—Si1—O2 | 115.8 (3) |
O6—Dy1—Si2iv | 82.67 (15) | O4—Si1—O3 | 112.0 (3) |
O7—Dy1—Si2iv | 29.92 (13) | O2—Si1—O3 | 109.5 (3) |
O3iii—Dy1—Si2iv | 98.36 (13) | O4—Si1—O1 | 108.9 (3) |
O1iv—Dy1—Si2iv | 32.07 (13) | O2—Si1—O1 | 102.9 (3) |
O2i—Dy1—Si1 | 77.21 (18) | O3—Si1—O1 | 107.0 (3) |
O4ii—Dy1—Si1 | 113.28 (15) | O4—Si1—Dy1 | 76.1 (2) |
O3—Dy1—Si1 | 26.21 (15) | O2—Si1—Dy1 | 118.7 (3) |
O6—Dy1—Si1 | 162.31 (15) | O3—Si1—Dy1 | 37.5 (2) |
O7—Dy1—Si1 | 91.54 (15) | O1—Si1—Dy1 | 131.2 (2) |
O3iii—Dy1—Si1 | 102.20 (14) | O4—Si1—Ba1vi | 147.3 (2) |
O1iv—Dy1—Si1 | 69.41 (13) | O2—Si1—Ba1vi | 51.3 (2) |
Si2iv—Dy1—Si1 | 80.46 (7) | O3—Si1—Ba1vi | 60.2 (2) |
O2i—Dy1—Dy1iii | 131.35 (18) | O1—Si1—Ba1vi | 103.5 (2) |
O4ii—Dy1—Dy1iii | 88.45 (14) | Dy1—Si1—Ba1vi | 85.51 (6) |
O3—Dy1—Dy1iii | 42.43 (13) | O4—Si1—Ba1i | 99.8 (2) |
O6—Dy1—Dy1iii | 113.41 (14) | O2—Si1—Ba1i | 57.1 (2) |
O7—Dy1—Dy1iii | 130.67 (13) | O3—Si1—Ba1i | 147.9 (2) |
O3iii—Dy1—Dy1iii | 38.43 (13) | O1—Si1—Ba1i | 55.9 (2) |
O1iv—Dy1—Dy1iii | 69.08 (12) | Dy1—Si1—Ba1i | 172.51 (9) |
Si2iv—Dy1—Dy1iii | 101.07 (5) | Ba1vi—Si1—Ba1i | 95.12 (7) |
Si1—Dy1—Dy1iii | 65.14 (5) | O6iii—Si2—O7iv | 118.2 (3) |
O2i—Dy1—Ba1 | 53.05 (17) | O6iii—Si2—O5i | 111.1 (4) |
O4ii—Dy1—Ba1 | 46.88 (14) | O7iv—Si2—O5i | 105.8 (3) |
O3—Dy1—Ba1 | 128.51 (13) | O6iii—Si2—O1 | 114.4 (3) |
O6—Dy1—Ba1 | 67.38 (14) | O7iv—Si2—O1 | 103.1 (3) |
O7—Dy1—Ba1 | 93.77 (13) | O5i—Si2—O1 | 102.6 (3) |
O3iii—Dy1—Ba1 | 117.82 (13) | O6iii—Si2—Dy1iv | 137.7 (2) |
O1iv—Dy1—Ba1 | 152.78 (13) | O7iv—Si2—Dy1iv | 46.8 (2) |
Si2iv—Dy1—Ba1 | 122.52 (5) | O5i—Si2—Dy1iv | 111.2 (3) |
Si1—Dy1—Ba1 | 127.08 (5) | O1—Si2—Dy1iv | 56.4 (2) |
Dy1iii—Dy1—Ba1 | 135.31 (2) | O6iii—Si2—Ba1ix | 126.4 (2) |
O2i—Dy1—Ba1v | 41.95 (17) | O7iv—Si2—Ba1ix | 52.0 (2) |
O4ii—Dy1—Ba1v | 120.59 (13) | O5i—Si2—Ba1ix | 54.54 (19) |
O3—Dy1—Ba1v | 92.31 (14) | O1—Si2—Ba1ix | 119.1 (2) |
O6—Dy1—Ba1v | 108.85 (14) | Dy1iv—Si2—Ba1ix | 79.09 (6) |
O7—Dy1—Ba1v | 41.11 (13) | O6iii—Si2—Ba1iii | 77.8 (2) |
O3iii—Dy1—Ba1v | 156.60 (13) | O7iv—Si2—Ba1iii | 42.3 (2) |
O1iv—Dy1—Ba1v | 84.59 (12) | O5i—Si2—Ba1iii | 136.69 (14) |
Si2iv—Dy1—Ba1v | 60.30 (5) | O1—Si2—Ba1iii | 112.0 (2) |
Si1—Dy1—Ba1v | 66.84 (5) | Dy1iv—Si2—Ba1iii | 70.91 (5) |
Dy1iii—Dy1—Ba1v | 130.74 (2) | Ba1ix—Si2—Ba1iii | 85.37 (6) |
Ba1—Dy1—Ba1v | 83.936 (18) | O6iii—Si2—Ba1i | 138.2 (2) |
O7ii—Ba1—O2vi | 64.86 (18) | O7iv—Si2—Ba1i | 103.5 (2) |
O7ii—Ba1—O4ii | 69.58 (17) | O5i—Si2—Ba1i | 49.73 (19) |
O2vi—Ba1—O4ii | 75.53 (19) | O1—Si2—Ba1i | 54.3 (2) |
O7ii—Ba1—O6vii | 77.10 (17) | Dy1iv—Si2—Ba1i | 74.44 (5) |
O2vi—Ba1—O6vii | 90.24 (19) | Ba1ix—Si2—Ba1i | 76.75 (5) |
O4ii—Ba1—O6vii | 146.67 (16) | Ba1iii—Si2—Ba1i | 143.38 (8) |
O7ii—Ba1—O7vii | 83.85 (12) | Si2—O1—Si1 | 125.0 (4) |
O2vi—Ba1—O7vii | 142.14 (19) | Si2—O1—Dy1iv | 91.6 (2) |
O4ii—Ba1—O7vii | 114.31 (16) | Si1—O1—Dy1iv | 139.2 (3) |
O6vii—Ba1—O7vii | 61.03 (17) | Si2—O1—Ba1i | 99.1 (3) |
O7ii—Ba1—O5 | 137.42 (13) | Si1—O1—Ba1i | 96.5 (2) |
O2vi—Ba1—O5 | 147.76 (17) | Dy1iv—O1—Ba1i | 94.38 (17) |
O4ii—Ba1—O5 | 129.29 (17) | Si1—O2—Dy1i | 141.6 (4) |
O6vii—Ba1—O5 | 77.12 (16) | Si1—O2—Ba1vi | 100.8 (3) |
O7vii—Ba1—O5 | 53.98 (11) | Dy1i—O2—Ba1vi | 104.2 (2) |
O7ii—Ba1—O3vi | 118.91 (16) | Si1—O2—Ba1i | 96.4 (3) |
O2vi—Ba1—O3vi | 55.95 (18) | Dy1i—O2—Ba1i | 90.7 (2) |
O4ii—Ba1—O3vi | 82.08 (15) | Ba1vi—O2—Ba1i | 128.1 (3) |
O6vii—Ba1—O3vi | 114.87 (15) | Si1—O3—Dy1 | 116.3 (3) |
O7vii—Ba1—O3vi | 156.33 (14) | Si1—O3—Dy1iii | 130.4 (3) |
O5—Ba1—O3vi | 102.57 (11) | Dy1—O3—Dy1iii | 99.1 (2) |
O7ii—Ba1—O1i | 162.01 (16) | Si1—O3—Ba1vi | 91.0 (2) |
O2vi—Ba1—O1i | 115.76 (18) | Dy1—O3—Ba1vi | 121.9 (2) |
O4ii—Ba1—O1i | 92.87 (16) | Dy1iii—O3—Ba1vi | 98.92 (17) |
O6vii—Ba1—O1i | 120.40 (16) | Si1—O4—Dy1v | 130.3 (3) |
O7vii—Ba1—O1i | 100.64 (16) | Si1—O4—Ba1v | 130.6 (3) |
O5—Ba1—O1i | 51.84 (12) | Dy1v—O4—Ba1v | 97.11 (19) |
O3vi—Ba1—O1i | 59.93 (16) | Si2viii—O5—Si2i | 144.7 (6) |
O7ii—Ba1—O2i | 113.77 (17) | Si2viii—O5—Ba1x | 104.48 (17) |
O2vi—Ba1—O2i | 128.1 (3) | Si2i—O5—Ba1x | 97.79 (17) |
O4ii—Ba1—O2i | 58.54 (17) | Si2viii—O5—Ba1 | 97.79 (17) |
O6vii—Ba1—O2i | 141.59 (18) | Si2i—O5—Ba1 | 104.48 (17) |
O7vii—Ba1—O2i | 82.87 (17) | Ba1x—O5—Ba1 | 101.0 (3) |
O5—Ba1—O2i | 70.78 (18) | Si2iii—O6—Dy1 | 122.5 (3) |
O3vi—Ba1—O2i | 92.62 (17) | Si2iii—O6—Ba1xi | 121.3 (3) |
O1i—Ba1—O2i | 50.44 (15) | Dy1—O6—Ba1xi | 111.9 (2) |
O7ii—Ba1—Si1vi | 92.61 (13) | Si2iv—O7—Dy1 | 103.3 (3) |
O2vi—Ba1—Si1vi | 27.86 (14) | Si2iv—O7—Ba1v | 113.7 (3) |
O4ii—Ba1—Si1vi | 82.01 (12) | Dy1—O7—Ba1v | 103.4 (2) |
O6vii—Ba1—Si1vi | 99.43 (13) | Si2iv—O7—Ba1xi | 101.4 (3) |
O7vii—Ba1—Si1vi | 160.45 (13) | Dy1—O7—Ba1xi | 109.9 (2) |
O5—Ba1—Si1vi | 124.71 (9) | Ba1v—O7—Ba1xi | 123.6 (2) |
O3vi—Ba1—Si1vi | 28.84 (12) |
Symmetry codes: (i) −x+3/2, −y−1/2, −z+1; (ii) x, y+1, z; (iii) −x+2, −y, −z+1; (iv) −x+2, −y−1, −z+1; (v) x, y−1, z; (vi) −x+3/2, −y+1/2, −z+1; (vii) −x+3/2, y+1/2, −z+1/2; (viii) x−1/2, −y−1/2, z−1/2; (ix) x+1/2, −y−1/2, z+1/2; (x) −x+1, y, −z+1/2; (xi) −x+3/2, y−1/2, −z+1/2. |
Ba2Ho2O13Si4 | F(000) = 1624 |
Mr = 924.90 | Dx = 5.432 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.8127 (7) Å | Cell parameters from 2892 reflections |
b = 5.1934 (5) Å | θ = 2.4–26.7° |
c = 17.514 (3) Å | µ = 21.21 mm−1 |
β = 103.971 (12)° | T = 298 K |
V = 1130.9 (2) Å3 | Block, pink |
Z = 4 | 0.27 × 0.25 × 0.22 mm |
Rigaku AFC8S diffractometer | 1182 independent reflections |
Radiation source: fine-focus sealed tube | 1104 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.050 |
ω scans | θmax = 26.7°, θmin = 2.4° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −16→14 |
Tmin = 0.523, Tmax = 1.000 | k = −6→6 |
4762 measured reflections | l = −21→22 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.103 | (Δ/σ)max = 0.001 |
S = 1.13 | Δρmax = 2.12 e Å−3 |
1182 reflections | Δρmin = −3.12 e Å−3 |
97 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0081 (3) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ho1 | 0.88679 (3) | 0.01047 (6) | 0.41597 (2) | 0.0078 (2) | |
Ba1 | 0.66256 (4) | 0.49473 (7) | 0.33300 (3) | 0.0100 (2) | |
Si1 | 0.8803 (2) | −0.4681 (4) | 0.54234 (14) | 0.0085 (5) | |
Si2 | 1.06245 (18) | −0.5449 (4) | 0.68267 (13) | 0.0089 (5) | |
O1 | 0.9795 (4) | −0.6463 (9) | 0.5988 (3) | 0.0116 (10) | |
O2 | 0.7911 (5) | −0.4564 (11) | 0.5940 (3) | 0.0122 (11) | |
O3 | 0.9295 (4) | −0.1774 (9) | 0.5368 (3) | 0.0107 (10) | |
O4 | 0.8428 (4) | −0.6024 (10) | 0.4583 (3) | 0.0123 (10) | |
O5 | 0.5000 | 0.1411 (13) | 0.2500 | 0.0117 (14) | |
O6 | 0.9187 (4) | 0.2425 (10) | 0.3125 (3) | 0.0159 (11) | |
O7 | 0.8355 (4) | −0.2686 (10) | 0.3082 (3) | 0.0141 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ho1 | 0.0100 (3) | 0.0085 (3) | 0.0060 (3) | −0.00013 (9) | 0.0043 (2) | 0.00006 (9) |
Ba1 | 0.0124 (4) | 0.0104 (3) | 0.0084 (4) | −0.00184 (12) | 0.0046 (3) | −0.00093 (12) |
Si1 | 0.0103 (10) | 0.0082 (9) | 0.0080 (12) | −0.0001 (7) | 0.0042 (8) | −0.0005 (7) |
Si2 | 0.0124 (10) | 0.0082 (9) | 0.0079 (10) | 0.0002 (8) | 0.0057 (8) | −0.0001 (7) |
O1 | 0.017 (3) | 0.008 (2) | 0.010 (2) | 0.0010 (19) | 0.004 (2) | −0.0002 (18) |
O2 | 0.012 (3) | 0.016 (2) | 0.011 (3) | 0.001 (2) | 0.007 (2) | −0.002 (2) |
O3 | 0.014 (2) | 0.008 (2) | 0.009 (2) | −0.0023 (19) | 0.0018 (19) | 0.0012 (18) |
O4 | 0.015 (2) | 0.012 (3) | 0.010 (2) | 0.002 (2) | 0.004 (2) | −0.0023 (19) |
O5 | 0.023 (4) | 0.009 (3) | 0.007 (3) | 0.000 | 0.010 (3) | 0.000 |
O6 | 0.023 (3) | 0.014 (3) | 0.013 (3) | −0.004 (2) | 0.009 (2) | −0.002 (2) |
O7 | 0.014 (2) | 0.014 (2) | 0.016 (3) | 0.0022 (19) | 0.006 (2) | 0.001 (2) |
Ho1—O4i | 2.260 (5) | Si1—Ba1vi | 3.419 (2) |
Ho1—O2ii | 2.262 (6) | Si1—Ba1ii | 3.623 (2) |
Ho1—O3 | 2.274 (5) | Si2—O6iii | 1.588 (6) |
Ho1—O6 | 2.295 (5) | Si2—O7iv | 1.604 (5) |
Ho1—O7 | 2.345 (5) | Si2—O5ii | 1.654 (3) |
Ho1—O3iii | 2.457 (5) | Si2—O1 | 1.677 (5) |
Ho1—O1iv | 2.606 (5) | Si2—Ho1iv | 3.130 (2) |
Ho1—Si2iv | 3.130 (2) | Si2—Ba1x | 3.522 (2) |
Ho1—Si1 | 3.342 (2) | Si2—Ba1iii | 3.609 (2) |
Ho1—Ho1iii | 3.6011 (9) | Si2—Ba1ii | 3.669 (2) |
Ho1—Ba1 | 3.8308 (7) | O1—Ho1iv | 2.606 (5) |
Ho1—Ba1v | 3.9401 (6) | O1—Ba1ii | 3.011 (5) |
Ba1—O7i | 2.659 (5) | O2—Ho1ii | 2.261 (6) |
Ba1—O2vi | 2.715 (6) | O2—Ba1vi | 2.715 (6) |
Ba1—O6vii | 2.819 (5) | O2—Ba1ii | 3.072 (6) |
Ba1—O4i | 2.821 (5) | O3—Ho1iii | 2.457 (5) |
Ba1—O7vii | 2.831 (5) | O3—Ba1vi | 2.965 (5) |
Ba1—O5 | 2.892 (4) | O4—Ho1v | 2.260 (5) |
Ba1—O3vi | 2.965 (5) | O4—Ba1v | 2.821 (5) |
Ba1—O1ii | 3.011 (5) | O5—Si2ix | 1.654 (3) |
Ba1—O2ii | 3.072 (6) | O5—Si2ii | 1.654 (3) |
Ba1—O6viii | 3.317 (6) | O5—Ba1xi | 2.892 (4) |
Ba1—Si1vi | 3.419 (2) | O6—Si2iii | 1.588 (5) |
Ba1—Si2ix | 3.522 (2) | O6—Ba1xii | 2.819 (5) |
Si1—O4 | 1.595 (5) | O6—Ba1xiii | 3.317 (6) |
Si1—O2 | 1.620 (6) | O7—Si2iv | 1.604 (5) |
Si1—O3 | 1.648 (5) | O7—Ba1v | 2.660 (5) |
Si1—O1 | 1.686 (5) | O7—Ba1xii | 2.831 (5) |
O4i—Ho1—O2ii | 79.01 (19) | O2ii—Ba1—O6viii | 118.71 (14) |
O4i—Ho1—O3 | 95.74 (18) | O7i—Ba1—Si1vi | 92.32 (12) |
O2ii—Ho1—O3 | 91.72 (19) | O2vi—Ba1—Si1vi | 27.70 (13) |
O4i—Ho1—O6 | 84.13 (19) | O6vii—Ba1—Si1vi | 99.65 (11) |
O2ii—Ho1—O6 | 111.9 (2) | O4i—Ba1—Si1vi | 81.92 (11) |
O3—Ho1—O6 | 155.77 (18) | O7vii—Ba1—Si1vi | 160.34 (11) |
O4i—Ho1—O7 | 140.36 (18) | O5—Ba1—Si1vi | 124.79 (8) |
O2ii—Ho1—O7 | 77.28 (19) | O3vi—Ba1—Si1vi | 28.81 (10) |
O3—Ho1—O7 | 116.21 (17) | O1ii—Ba1—Si1vi | 88.46 (10) |
O6—Ho1—O7 | 75.96 (18) | O2ii—Ba1—Si1vi | 115.66 (12) |
O4i—Ho1—O3iii | 82.52 (17) | O6viii—Ba1—Si1vi | 59.88 (10) |
O2ii—Ho1—O3iii | 159.34 (19) | O7i—Ba1—Si2ix | 110.60 (12) |
O3—Ho1—O3iii | 80.92 (18) | O2vi—Ba1—Si2ix | 159.51 (13) |
O6—Ho1—O3iii | 75.03 (17) | O6vii—Ba1—Si2ix | 68.84 (11) |
O7—Ho1—O3iii | 123.29 (18) | O4i—Ba1—Si2ix | 123.01 (11) |
O4i—Ho1—O1iv | 154.11 (17) | O7vii—Ba1—Si2ix | 26.51 (11) |
O2ii—Ho1—O1iv | 125.23 (18) | O5—Ba1—Si2ix | 27.73 (5) |
O3—Ho1—O1iv | 76.37 (17) | O3vi—Ba1—Si2ix | 130.28 (10) |
O6—Ho1—O1iv | 93.21 (17) | O1ii—Ba1—Si2ix | 75.65 (10) |
O7—Ho1—O1iv | 62.29 (16) | O2ii—Ba1—Si2ix | 72.93 (12) |
O3iii—Ho1—O1iv | 71.96 (16) | O6viii—Ba1—Si2ix | 90.73 (10) |
O4i—Ho1—Si2iv | 165.78 (14) | Si1vi—Ba1—Si2ix | 150.31 (6) |
O2ii—Ho1—Si2iv | 101.63 (15) | O4—Si1—O2 | 115.9 (3) |
O3—Ho1—Si2iv | 98.43 (13) | O4—Si1—O3 | 112.3 (3) |
O6—Ho1—Si2iv | 82.48 (13) | O2—Si1—O3 | 109.3 (3) |
O7—Ho1—Si2iv | 29.92 (13) | O4—Si1—O1 | 108.5 (3) |
O3iii—Ho1—Si2iv | 98.55 (12) | O2—Si1—O1 | 103.1 (3) |
O1iv—Ho1—Si2iv | 32.39 (12) | O3—Si1—O1 | 107.0 (3) |
O4i—Ho1—Si1 | 113.35 (14) | O4—Si1—Ho1 | 76.3 (2) |
O2ii—Ho1—Si1 | 76.86 (15) | O2—Si1—Ho1 | 118.4 (2) |
O3—Ho1—Si1 | 26.30 (13) | O3—Si1—Ho1 | 37.69 (18) |
O6—Ho1—Si1 | 162.08 (14) | O1—Si1—Ho1 | 131.3 (2) |
O7—Ho1—Si1 | 91.52 (13) | O4—Si1—Ba1vi | 147.7 (2) |
O3iii—Ho1—Si1 | 102.39 (12) | O2—Si1—Ba1vi | 51.2 (2) |
O1iv—Ho1—Si1 | 69.40 (12) | O3—Si1—Ba1vi | 60.13 (18) |
Si2iv—Ho1—Si1 | 80.38 (6) | O1—Si1—Ba1vi | 103.59 (19) |
O4i—Ho1—Ho1iii | 88.53 (13) | Ho1—Si1—Ba1vi | 85.51 (5) |
O2ii—Ho1—Ho1iii | 131.10 (15) | O4—Si1—Ba1ii | 99.8 (2) |
O3—Ho1—Ho1iii | 42.35 (12) | O2—Si1—Ba1ii | 57.5 (2) |
O6—Ho1—Ho1iii | 113.54 (14) | O3—Si1—Ba1ii | 147.5 (2) |
O7—Ho1—Ho1iii | 130.80 (12) | O1—Si1—Ba1ii | 55.59 (18) |
O3iii—Ho1—Ho1iii | 38.57 (11) | Ho1—Si1—Ba1ii | 172.75 (8) |
O1iv—Ho1—Ho1iii | 68.89 (11) | Ba1vi—Si1—Ba1ii | 94.99 (6) |
Si2iv—Ho1—Ho1iii | 101.19 (4) | O6iii—Si2—O7iv | 118.8 (3) |
Si1—Ho1—Ho1iii | 65.19 (4) | O6iii—Si2—O5ii | 110.7 (3) |
O4i—Ho1—Ba1 | 46.92 (13) | O7iv—Si2—O5ii | 105.6 (3) |
O2ii—Ho1—Ba1 | 53.31 (15) | O6iii—Si2—O1 | 114.4 (3) |
O3—Ho1—Ba1 | 128.67 (13) | O7iv—Si2—O1 | 103.1 (3) |
O6—Ho1—Ba1 | 67.41 (14) | O5ii—Si2—O1 | 102.5 (2) |
O7—Ho1—Ba1 | 93.53 (12) | O6iii—Si2—Ho1iv | 138.1 (2) |
O3iii—Ho1—Ba1 | 117.76 (11) | O7iv—Si2—Ho1iv | 46.8 (2) |
O1iv—Ho1—Ba1 | 152.82 (11) | O5ii—Si2—Ho1iv | 111.2 (2) |
Si2iv—Ho1—Ba1 | 122.31 (4) | O1—Si2—Ho1iv | 56.36 (18) |
Si1—Ho1—Ba1 | 127.08 (4) | O6iii—Si2—Ba1x | 126.3 (2) |
Ho1iii—Ho1—Ba1 | 135.423 (17) | O7iv—Si2—Ba1x | 52.0 (2) |
O4i—Ho1—Ba1v | 120.55 (13) | O5ii—Si2—Ba1x | 54.42 (16) |
O2ii—Ho1—Ba1v | 41.88 (14) | O1—Si2—Ba1x | 119.1 (2) |
O3—Ho1—Ba1v | 92.39 (12) | Ho1iv—Si2—Ba1x | 79.25 (5) |
O6—Ho1—Ba1v | 108.60 (13) | O6iii—Si2—Ba1iii | 78.1 (2) |
O7—Ho1—Ba1v | 40.98 (13) | O7iv—Si2—Ba1iii | 42.6 (2) |
O3iii—Ho1—Ba1v | 156.65 (12) | O5ii—Si2—Ba1iii | 136.49 (12) |
O1iv—Ho1—Ba1v | 84.75 (11) | O1—Si2—Ba1iii | 112.3 (2) |
Si2iv—Ho1—Ba1v | 60.10 (4) | Ho1iv—Si2—Ba1iii | 71.15 (4) |
Si1—Ho1—Ba1v | 66.81 (4) | Ba1x—Si2—Ba1iii | 85.34 (5) |
Ho1iii—Ho1—Ba1v | 130.749 (17) | O6iii—Si2—Ba1ii | 137.7 (2) |
Ba1—Ho1—Ba1v | 83.862 (15) | O7iv—Si2—Ba1ii | 103.3 (2) |
O7i—Ba1—O2vi | 64.72 (17) | O5ii—Si2—Ba1ii | 49.79 (15) |
O7i—Ba1—O6vii | 77.41 (16) | O1—Si2—Ba1ii | 54.14 (19) |
O2vi—Ba1—O6vii | 90.78 (17) | Ho1iv—Si2—Ba1ii | 74.40 (5) |
O7i—Ba1—O4i | 69.61 (16) | Ba1x—Si2—Ba1ii | 76.78 (5) |
O2vi—Ba1—O4i | 75.33 (16) | Ba1iii—Si2—Ba1ii | 143.53 (7) |
O6vii—Ba1—O4i | 147.02 (16) | Si2—O1—Si1 | 124.7 (3) |
O7i—Ba1—O7vii | 84.09 (12) | Si2—O1—Ho1iv | 91.3 (2) |
O2vi—Ba1—O7vii | 142.29 (17) | Si1—O1—Ho1iv | 139.6 (3) |
O6vii—Ba1—O7vii | 60.70 (15) | Si2—O1—Ba1ii | 99.0 (2) |
O4i—Ba1—O7vii | 114.49 (15) | Si1—O1—Ba1ii | 96.9 (2) |
O7i—Ba1—O5 | 137.62 (12) | Ho1iv—O1—Ba1ii | 94.47 (15) |
O2vi—Ba1—O5 | 147.85 (16) | Si1—O2—Ho1ii | 141.8 (3) |
O6vii—Ba1—O5 | 76.80 (14) | Si1—O2—Ba1vi | 101.1 (3) |
O4i—Ba1—O5 | 129.24 (15) | Ho1ii—O2—Ba1vi | 104.3 (2) |
O7vii—Ba1—O5 | 53.94 (11) | Si1—O2—Ba1ii | 96.1 (2) |
O7i—Ba1—O3vi | 118.66 (15) | Ho1ii—O2—Ba1ii | 90.51 (18) |
O2vi—Ba1—O3vi | 55.75 (16) | Ba1vi—O2—Ba1ii | 127.5 (2) |
O6vii—Ba1—O3vi | 114.84 (14) | Si1—O3—Ho1 | 116.0 (3) |
O4i—Ba1—O3vi | 82.08 (14) | Si1—O3—Ho1iii | 130.8 (3) |
O7vii—Ba1—O3vi | 156.27 (14) | Ho1—O3—Ho1iii | 99.08 (18) |
O5—Ba1—O3vi | 102.58 (10) | Si1—O3—Ba1vi | 91.1 (2) |
O7i—Ba1—O1ii | 161.78 (15) | Ho1—O3—Ba1vi | 121.82 (19) |
O2vi—Ba1—O1ii | 115.35 (16) | Ho1iii—O3—Ba1vi | 98.90 (16) |
O6vii—Ba1—O1ii | 120.41 (15) | Si1—O4—Ho1v | 130.4 (3) |
O4i—Ba1—O1ii | 92.51 (14) | Si1—O4—Ba1v | 130.3 (3) |
O7vii—Ba1—O1ii | 100.95 (14) | Ho1v—O4—Ba1v | 97.26 (17) |
O5—Ba1—O1ii | 52.18 (10) | Si2ix—O5—Si2ii | 144.8 (5) |
O3vi—Ba1—O1ii | 59.75 (13) | Si2ix—O5—Ba1xi | 104.31 (14) |
O7i—Ba1—O2ii | 113.82 (16) | Si2ii—O5—Ba1xi | 97.85 (14) |
O2vi—Ba1—O2ii | 127.5 (2) | Si2ix—O5—Ba1 | 97.85 (14) |
O6vii—Ba1—O2ii | 141.60 (16) | Si2ii—O5—Ba1 | 104.31 (14) |
O4i—Ba1—O2ii | 58.25 (15) | Ba1xi—O5—Ba1 | 101.1 (2) |
O7vii—Ba1—O2ii | 83.25 (15) | Si2iii—O6—Ho1 | 122.1 (3) |
O5—Ba1—O2ii | 71.01 (15) | Si2iii—O6—Ba1xii | 121.2 (3) |
O3vi—Ba1—O2ii | 92.50 (14) | Ho1—O6—Ba1xii | 112.1 (2) |
O1ii—Ba1—O2ii | 50.38 (14) | Si2iii—O6—Ba1xiii | 104.5 (3) |
O7i—Ba1—O6viii | 127.08 (14) | Ho1—O6—Ba1xiii | 93.07 (17) |
O2vi—Ba1—O6viii | 78.55 (15) | Ba1xii—O6—Ba1xiii | 93.08 (14) |
O6vii—Ba1—O6viii | 65.93 (17) | Si2iv—O7—Ho1 | 103.3 (3) |
O4i—Ba1—O6viii | 136.62 (14) | Si2iv—O7—Ba1v | 113.3 (3) |
O7vii—Ba1—O6viii | 107.43 (14) | Ho1—O7—Ba1v | 103.70 (19) |
O5—Ba1—O6viii | 69.31 (13) | Si2iv—O7—Ba1xii | 101.5 (2) |
O3vi—Ba1—O6viii | 54.56 (13) | Ho1—O7—Ba1xii | 110.16 (19) |
O1ii—Ba1—O6viii | 68.44 (13) | Ba1v—O7—Ba1xii | 123.33 (19) |
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, −y−1/2, −z+1; (iii) −x+2, −y, −z+1; (iv) −x+2, −y−1, −z+1; (v) x, y−1, z; (vi) −x+3/2, −y+1/2, −z+1; (vii) −x+3/2, y+1/2, −z+1/2; (viii) x−1/2, y+1/2, z; (ix) x−1/2, −y−1/2, z−1/2; (x) x+1/2, −y−1/2, z+1/2; (xi) −x+1, y, −z+1/2; (xii) −x+3/2, y−1/2, −z+1/2; (xiii) x+1/2, y−1/2, z. |
Ba2Er2F2O12Si4 | Z = 1 |
Mr = 951.56 | F(000) = 418 |
Triclinic, P1 | Dx = 4.873 Mg m−3 |
a = 5.476 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.166 (6) Å | Cell parameters from 1898 reflections |
c = 8.958 (8) Å | θ = 2.5–26.7° |
α = 108.138 (18)° | µ = 19.25 mm−1 |
β = 102.03 (2)° | T = 298 K |
γ = 92.742 (19)° | Block, pink |
V = 324.3 (4) Å3 | 0.15 × 0.14 × 0.12 mm |
Rigaku AFC8S diffractometer | 1168 independent reflections |
Radiation source: fine-focus sealed tube | 1114 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.035 |
ω scans | θmax = 25.2°, θmin = 3.0° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −6→6 |
Tmin = 0.469, Tmax = 1.000 | k = −8→8 |
2675 measured reflections | l = −10→10 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.094 | (Δ/σ)max < 0.001 |
S = 1.15 | Δρmax = 2.35 e Å−3 |
1168 reflections | Δρmin = −3.30 e Å−3 |
101 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0104 (12) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.76057 (10) | 0.25712 (8) | 0.04472 (6) | 0.0144 (2) | |
Er1 | 0.16296 (7) | 0.14956 (6) | 0.70128 (4) | 0.0115 (2) | |
Si1 | 0.3837 (5) | 0.1771 (4) | 0.3689 (3) | 0.0111 (5) | |
Si2 | 0.6772 (4) | 0.4417 (4) | 0.7105 (3) | 0.0103 (5) | |
O1 | 0.6111 (12) | 0.3101 (10) | 0.5199 (7) | 0.0155 (14) | |
O2 | 0.1672 (12) | 0.0900 (10) | 0.4380 (8) | 0.0162 (14) | |
O3 | 0.2546 (12) | 0.3274 (9) | 0.2769 (8) | 0.0143 (13) | |
O4 | 0.5019 (12) | 0.0134 (9) | 0.2479 (8) | 0.0155 (13) | |
O5 | 0.4479 (12) | 0.4178 (10) | 0.7926 (8) | 0.0155 (14) | |
O6 | 0.9269 (12) | 0.3812 (9) | 0.8052 (8) | 0.0143 (14) | |
F1 | 0.1524 (13) | 0.0975 (9) | 0.9272 (7) | 0.0263 (14) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.0151 (4) | 0.0125 (4) | 0.0135 (4) | 0.0016 (2) | 0.0017 (2) | 0.0024 (2) |
Er1 | 0.0111 (3) | 0.0112 (3) | 0.0107 (3) | 0.00044 (18) | 0.00130 (18) | 0.0026 (2) |
Si1 | 0.0118 (12) | 0.0109 (12) | 0.0096 (12) | −0.0001 (9) | 0.0022 (9) | 0.0024 (9) |
Si2 | 0.0091 (11) | 0.0108 (12) | 0.0107 (12) | 0.0004 (9) | 0.0015 (9) | 0.0037 (9) |
O1 | 0.015 (3) | 0.020 (3) | 0.007 (3) | −0.001 (3) | 0.001 (2) | −0.001 (3) |
O2 | 0.018 (3) | 0.013 (3) | 0.017 (3) | −0.001 (3) | 0.005 (3) | 0.003 (3) |
O3 | 0.021 (3) | 0.008 (3) | 0.011 (3) | 0.000 (2) | −0.002 (3) | 0.005 (3) |
O4 | 0.015 (3) | 0.012 (3) | 0.013 (3) | 0.003 (3) | −0.002 (2) | 0.000 (3) |
O5 | 0.015 (3) | 0.015 (3) | 0.021 (4) | 0.002 (3) | 0.012 (3) | 0.007 (3) |
O6 | 0.014 (3) | 0.010 (3) | 0.013 (3) | 0.001 (2) | −0.001 (2) | −0.002 (3) |
F1 | 0.041 (4) | 0.027 (3) | 0.022 (3) | 0.015 (3) | 0.016 (3) | 0.016 (3) |
Ba1—F1i | 2.685 (6) | Si1—O4 | 1.594 (7) |
Ba1—F1ii | 2.729 (6) | Si1—O2 | 1.629 (7) |
Ba1—O5iii | 2.773 (7) | Si1—O1 | 1.634 (6) |
Ba1—O4iv | 2.774 (6) | Si1—O3 | 1.650 (7) |
Ba1—O6v | 2.811 (7) | Si2—O6 | 1.606 (7) |
Ba1—O6vi | 2.855 (7) | Si2—O5 | 1.609 (7) |
Ba1—O3vii | 2.961 (7) | Si2—O1 | 1.626 (6) |
Ba1—O5vi | 3.091 (7) | Si2—O3iii | 1.643 (7) |
Ba1—F1vi | 3.306 (7) | Si2—Ba1v | 3.542 (3) |
Ba1—Si2v | 3.542 (3) | Si2—Ba1x | 3.588 (3) |
Ba1—Si2vi | 3.588 (3) | O2—Er1ix | 2.280 (7) |
Ba1—Er1vi | 3.854 (2) | O3—Si2iii | 1.643 (7) |
Er1—F1 | 2.181 (6) | O3—Ba1viii | 2.961 (7) |
Er1—O5 | 2.236 (7) | O4—Er1i | 2.264 (7) |
Er1—O6viii | 2.244 (6) | O4—Ba1iv | 2.774 (6) |
Er1—O4i | 2.264 (7) | O5—Ba1iii | 2.773 (7) |
Er1—O2 | 2.268 (7) | O5—Ba1x | 3.091 (7) |
Er1—O2ix | 2.280 (7) | O6—Er1vii | 2.244 (6) |
Er1—Si2 | 3.398 (3) | O6—Ba1v | 2.811 (7) |
Er1—Er1ix | 3.595 (3) | O6—Ba1x | 2.855 (7) |
Er1—Ba1x | 3.854 (2) | F1—Ba1i | 2.685 (6) |
Er1—Ba1xi | 4.053 (3) | F1—Ba1xi | 2.729 (6) |
Er1—Ba1iii | 4.103 (3) | F1—Ba1x | 3.306 (7) |
Er1—Ba1i | 4.206 (3) | ||
F1i—Ba1—F1ii | 64.1 (2) | F1—Er1—Ba1x | 58.91 (19) |
F1i—Ba1—O5iii | 136.53 (19) | O5—Er1—Ba1x | 53.31 (18) |
F1ii—Ba1—O5iii | 150.25 (19) | O6viii—Er1—Ba1x | 102.81 (16) |
F1i—Ba1—O4iv | 75.5 (2) | O4i—Er1—Ba1x | 45.26 (16) |
F1ii—Ba1—O4iv | 80.1 (2) | O2—Er1—Ba1x | 123.90 (17) |
O5iii—Ba1—O4iv | 121.8 (2) | O2ix—Er1—Ba1x | 140.57 (17) |
F1i—Ba1—O6v | 128.0 (2) | Si2—Er1—Ba1x | 58.91 (6) |
F1ii—Ba1—O6v | 88.3 (2) | Er1ix—Er1—Ba1x | 147.34 (3) |
O5iii—Ba1—O6v | 62.1 (2) | F1—Er1—Ba1xi | 39.01 (17) |
O4iv—Ba1—O6v | 145.3 (2) | O5—Er1—Ba1xi | 102.47 (17) |
F1i—Ba1—O6vi | 120.37 (19) | O6viii—Er1—Ba1xi | 42.97 (18) |
F1ii—Ba1—O6vi | 60.46 (18) | O4i—Er1—Ba1xi | 113.73 (18) |
O5iii—Ba1—O6vi | 103.02 (19) | O2—Er1—Ba1xi | 148.13 (17) |
O4iv—Ba1—O6vi | 75.2 (2) | O2ix—Er1—Ba1xi | 82.30 (17) |
O6v—Ba1—O6vi | 70.6 (2) | Si2—Er1—Ba1xi | 125.57 (5) |
F1i—Ba1—O3vii | 74.63 (19) | Er1ix—Er1—Ba1xi | 116.80 (6) |
F1ii—Ba1—O3vii | 62.7 (2) | Ba1x—Er1—Ba1xi | 87.62 (7) |
O5iii—Ba1—O3vii | 98.55 (19) | F1—Er1—Ba1iii | 87.11 (17) |
O4iv—Ba1—O3vii | 139.69 (18) | O5—Er1—Ba1iii | 39.55 (17) |
O6v—Ba1—O3vii | 53.38 (18) | O6viii—Er1—Ba1iii | 40.64 (17) |
O6vi—Ba1—O3vii | 97.57 (19) | O4i—Er1—Ba1iii | 116.85 (16) |
F1i—Ba1—O5vi | 137.36 (18) | O2—Er1—Ba1iii | 112.43 (17) |
F1ii—Ba1—O5vi | 108.08 (18) | O2ix—Er1—Ba1iii | 135.35 (17) |
O5iii—Ba1—O5vi | 71.7 (2) | Si2—Er1—Ba1iii | 61.20 (6) |
O4iv—Ba1—O5vi | 61.93 (19) | Er1ix—Er1—Ba1iii | 133.79 (2) |
O6v—Ba1—O5vi | 91.58 (19) | Ba1x—Er1—Ba1iii | 73.36 (3) |
O6vi—Ba1—O5vi | 52.35 (18) | Ba1xi—Er1—Ba1iii | 69.05 (3) |
O3vii—Ba1—O5vi | 142.21 (18) | F1—Er1—Ba1i | 33.85 (16) |
F1i—Ba1—F1vi | 88.63 (18) | O5—Er1—Ba1i | 117.47 (18) |
F1ii—Ba1—F1vi | 130.0 (2) | O6viii—Er1—Ba1i | 110.30 (18) |
O5iii—Ba1—F1vi | 77.69 (18) | O4i—Er1—Ba1i | 52.35 (18) |
O4iv—Ba1—F1vi | 51.79 (18) | O2—Er1—Ba1i | 127.02 (18) |
O6v—Ba1—F1vi | 138.27 (18) | O2ix—Er1—Ba1i | 76.50 (18) |
O6vi—Ba1—F1vi | 110.87 (16) | Si2—Er1—Ba1i | 119.93 (5) |
O3vii—Ba1—F1vi | 151.48 (16) | Er1ix—Er1—Ba1i | 103.40 (6) |
O5vi—Ba1—F1vi | 63.98 (16) | Ba1x—Er1—Ba1i | 64.46 (4) |
F1i—Ba1—Si2v | 101.86 (16) | Ba1xi—Er1—Ba1i | 67.48 (4) |
F1ii—Ba1—Si2v | 72.17 (15) | Ba1iii—Er1—Ba1i | 119.16 (6) |
O5iii—Ba1—Si2v | 81.21 (15) | O4—Si1—O2 | 114.8 (4) |
O4iv—Ba1—Si2v | 149.88 (15) | O4—Si1—O1 | 108.4 (4) |
O6v—Ba1—Si2v | 26.19 (13) | O2—Si1—O1 | 109.5 (4) |
O6vi—Ba1—Si2v | 80.96 (14) | O4—Si1—O3 | 109.7 (4) |
O3vii—Ba1—Si2v | 27.44 (13) | O2—Si1—O3 | 107.0 (4) |
O5vi—Ba1—Si2v | 115.82 (14) | O1—Si1—O3 | 107.2 (4) |
F1vi—Ba1—Si2v | 157.65 (11) | O6—Si2—O5 | 109.9 (4) |
F1i—Ba1—Si2vi | 132.96 (13) | O6—Si2—O1 | 110.4 (3) |
F1ii—Ba1—Si2vi | 83.53 (13) | O5—Si2—O1 | 111.6 (4) |
O5iii—Ba1—Si2vi | 87.93 (16) | O6—Si2—O3iii | 106.1 (4) |
O4iv—Ba1—Si2vi | 65.58 (16) | O5—Si2—O3iii | 111.5 (4) |
O6v—Ba1—Si2vi | 80.72 (15) | O1—Si2—O3iii | 107.2 (4) |
O6vi—Ba1—Si2vi | 25.80 (13) | O6—Si2—Er1 | 110.1 (3) |
O3vii—Ba1—Si2vi | 120.91 (14) | O5—Si2—Er1 | 33.3 (2) |
O5vi—Ba1—Si2vi | 26.56 (12) | O1—Si2—Er1 | 81.4 (2) |
F1vi—Ba1—Si2vi | 87.42 (11) | O3iii—Si2—Er1 | 136.9 (3) |
Si2v—Ba1—Si2vi | 99.17 (7) | O6—Si2—Ba1v | 50.6 (2) |
F1i—Ba1—Er1vi | 104.84 (15) | O5—Si2—Ba1v | 118.8 (3) |
F1ii—Ba1—Er1vi | 110.55 (14) | O1—Si2—Ba1v | 129.5 (3) |
O5iii—Ba1—Er1vi | 86.67 (15) | O3iii—Si2—Ba1v | 56.2 (2) |
O4iv—Ba1—Er1vi | 35.43 (14) | Er1—Si2—Ba1v | 145.70 (8) |
O6v—Ba1—Er1vi | 126.52 (14) | O6—Si2—Ba1x | 50.7 (3) |
O6vi—Ba1—Er1vi | 76.52 (14) | O5—Si2—Ba1x | 59.2 (3) |
O3vii—Ba1—Er1vi | 172.93 (13) | O1—Si2—Ba1x | 126.5 (3) |
O5vi—Ba1—Er1vi | 35.45 (13) | O3iii—Si2—Ba1x | 125.6 (2) |
F1vi—Ba1—Er1vi | 34.40 (10) | Er1—Si2—Ba1x | 66.90 (5) |
Si2v—Ba1—Er1vi | 151.26 (5) | Ba1v—Si2—Ba1x | 80.83 (7) |
Si2vi—Ba1—Er1vi | 54.20 (5) | Si2—O1—Si1 | 143.6 (4) |
F1—Er1—O5 | 100.4 (3) | Si1—O2—Er1 | 126.7 (4) |
F1—Er1—O6viii | 78.9 (2) | Si1—O2—Er1ix | 128.4 (4) |
O5—Er1—O6viii | 80.0 (2) | Er1—O2—Er1ix | 104.4 (3) |
F1—Er1—O4i | 74.7 (2) | Si2iii—O3—Si1 | 135.4 (4) |
O5—Er1—O4i | 84.6 (2) | Si2iii—O3—Ba1viii | 96.4 (3) |
O6viii—Er1—O4i | 146.5 (2) | Si1—O3—Ba1viii | 128.0 (3) |
F1—Er1—O2 | 160.4 (2) | Si1—O4—Er1i | 130.2 (4) |
O5—Er1—O2 | 94.5 (2) | Si1—O4—Ba1iv | 125.7 (3) |
O6viii—Er1—O2 | 116.4 (2) | Er1i—O4—Ba1iv | 99.3 (2) |
O4i—Er1—O2 | 94.4 (2) | Si2—O5—Er1 | 123.4 (4) |
F1—Er1—O2ix | 91.5 (3) | Si2—O5—Ba1iii | 121.6 (3) |
O5—Er1—O2ix | 166.0 (3) | Er1—O5—Ba1iii | 109.6 (2) |
O6viii—Er1—O2ix | 95.4 (2) | Si2—O5—Ba1x | 94.2 (3) |
O4i—Er1—O2ix | 105.6 (2) | Er1—O5—Ba1x | 91.2 (2) |
O2—Er1—O2ix | 75.6 (3) | Ba1iii—O5—Ba1x | 108.3 (2) |
F1—Er1—Si2 | 115.72 (19) | Si2—O6—Er1vii | 127.3 (3) |
O5—Er1—Si2 | 23.28 (17) | Si2—O6—Ba1v | 103.3 (3) |
O6viii—Er1—Si2 | 100.23 (18) | Er1vii—O6—Ba1v | 108.0 (2) |
O4i—Er1—Si2 | 73.64 (19) | Si2—O6—Ba1x | 103.5 (3) |
O2—Er1—Si2 | 75.24 (17) | Er1vii—O6—Ba1x | 104.6 (2) |
O2ix—Er1—Si2 | 150.64 (18) | Ba1v—O6—Ba1x | 109.4 (2) |
F1—Er1—Er1ix | 127.69 (19) | Er1—F1—Ba1i | 119.3 (2) |
O5—Er1—Er1ix | 131.72 (17) | Er1—F1—Ba1xi | 110.8 (2) |
O6viii—Er1—Er1ix | 109.85 (16) | Ba1i—F1—Ba1xi | 115.9 (2) |
O4i—Er1—Er1ix | 102.66 (16) | Er1—F1—Ba1x | 86.7 (2) |
O2—Er1—Er1ix | 37.90 (17) | Ba1i—F1—Ba1x | 91.37 (18) |
O2ix—Er1—Er1ix | 37.66 (17) | Ba1xi—F1—Ba1x | 130.0 (2) |
Si2—Er1—Er1ix | 113.09 (6) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z; (v) −x+2, −y+1, −z+1; (vi) x, y, z−1; (vii) x+1, y, z; (viii) x−1, y, z; (ix) −x, −y, −z+1; (x) x, y, z+1; (xi) x−1, y, z+1. |
Ba2F2O12Si4Tm2 | Z = 1 |
Mr = 954.90 | F(000) = 420 |
Triclinic, P1 | Dx = 4.932 Mg m−3 |
a = 5.4609 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.1258 (5) Å | Cell parameters from 7901 reflections |
c = 8.9379 (7) Å | θ = 2.5–33.2° |
α = 107.809 (2)° | µ = 20.17 mm−1 |
β = 101.987 (2)° | T = 300 K |
γ = 92.866 (2)° | Block, green |
V = 321.50 (4) Å3 | 0.13 × 0.12 × 0.10 mm |
Bruker Photon 100 diffractometer | 2210 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.038 |
φ and ω scans | θmax = 33.2°, θmin = 2.5° |
Absorption correction: multi-scan SADABS, Bruker | h = −8→8 |
Tmin = 0.839, Tmax = 1.000 | k = −7→10 |
8263 measured reflections | l = −13→13 |
2236 independent reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.022 | w = 1/[σ2(Fo2) + (0.0266P)2 + 1.9341P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.063 | (Δ/σ)max = 0.001 |
S = 1.14 | Δρmax = 1.93 e Å−3 |
2236 reflections | Δρmin = −2.82 e Å−3 |
101 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.102 (2) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.75906 (4) | 0.25721 (4) | 0.04489 (3) | 0.00685 (9) | |
Tm1 | 0.16255 (3) | 0.14925 (2) | 0.70100 (2) | 0.00334 (8) | |
Si1 | 0.3842 (2) | 0.17744 (16) | 0.36902 (13) | 0.00286 (19) | |
Si2 | 0.6775 (2) | 0.44118 (16) | 0.71041 (13) | 0.00305 (19) | |
O1 | 0.6123 (6) | 0.3108 (5) | 0.5186 (4) | 0.0081 (5) | |
O2 | 0.1671 (6) | 0.0890 (5) | 0.4375 (4) | 0.0072 (5) | |
O3 | 0.2540 (6) | 0.3258 (5) | 0.2753 (4) | 0.0071 (5) | |
O4 | 0.5054 (6) | 0.0152 (5) | 0.2486 (4) | 0.0085 (6) | |
O5 | 0.4456 (6) | 0.4175 (5) | 0.7914 (4) | 0.0087 (6) | |
O6 | 0.9295 (6) | 0.3796 (5) | 0.8033 (4) | 0.0062 (5) | |
F1 | 0.1516 (6) | 0.0981 (5) | 0.9274 (4) | 0.0173 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00833 (12) | 0.00515 (13) | 0.00576 (13) | 0.00107 (9) | 0.00147 (9) | −0.00003 (9) |
Tm1 | 0.00333 (10) | 0.00337 (11) | 0.00275 (11) | −0.00008 (6) | 0.00119 (6) | −0.00006 (7) |
Si1 | 0.0032 (4) | 0.0026 (4) | 0.0022 (4) | 0.0001 (3) | 0.0008 (3) | 0.0000 (4) |
Si2 | 0.0023 (4) | 0.0025 (5) | 0.0036 (4) | 0.0000 (3) | 0.0002 (3) | 0.0002 (4) |
O1 | 0.0086 (12) | 0.0079 (14) | 0.0048 (13) | −0.0017 (10) | −0.0001 (10) | −0.0007 (11) |
O2 | 0.0082 (12) | 0.0077 (14) | 0.0055 (13) | −0.0034 (10) | 0.0029 (10) | 0.0018 (11) |
O3 | 0.0103 (13) | 0.0021 (12) | 0.0070 (13) | −0.0020 (10) | −0.0028 (10) | 0.0023 (10) |
O4 | 0.0083 (12) | 0.0087 (14) | 0.0058 (13) | 0.0055 (11) | 0.0020 (10) | −0.0025 (11) |
O5 | 0.0053 (12) | 0.0078 (14) | 0.0128 (15) | −0.0014 (10) | 0.0070 (11) | 0.0002 (12) |
O6 | 0.0049 (12) | 0.0059 (13) | 0.0070 (13) | 0.0026 (10) | −0.0001 (10) | 0.0015 (10) |
F1 | 0.0287 (16) | 0.0204 (15) | 0.0140 (14) | 0.0163 (13) | 0.0157 (12) | 0.0126 (12) |
Ba1—F1i | 2.677 (3) | Si1—O4 | 1.595 (3) |
Ba1—F1ii | 2.726 (3) | Si1—O2 | 1.625 (3) |
Ba1—O5iii | 2.762 (3) | Si1—O1 | 1.630 (3) |
Ba1—O4iv | 2.787 (3) | Si1—O3 | 1.642 (3) |
Ba1—O6v | 2.808 (3) | Si2—O6 | 1.608 (3) |
Ba1—O6vi | 2.863 (3) | Si2—O5 | 1.609 (3) |
Ba1—O3vii | 2.954 (3) | Si2—O1 | 1.633 (3) |
Ba1—O5vi | 3.088 (4) | Si2—O3iii | 1.644 (3) |
Ba1—F1vi | 3.293 (4) | Si2—Ba1v | 3.5410 (11) |
Ba1—O4 | 3.307 (3) | Si2—Ba1x | 3.5716 (12) |
Ba1—Si2v | 3.5410 (11) | O2—Tm1ix | 2.267 (3) |
Ba1—Si2vi | 3.5717 (12) | O3—Si2iii | 1.644 (3) |
Tm1—F1 | 2.175 (3) | O3—Ba1viii | 2.954 (3) |
Tm1—O6viii | 2.219 (3) | O4—Tm1i | 2.250 (3) |
Tm1—O5 | 2.222 (3) | O4—Ba1iv | 2.787 (3) |
Tm1—O4i | 2.250 (3) | O5—Ba1iii | 2.762 (3) |
Tm1—O2 | 2.267 (3) | O5—Ba1x | 3.088 (4) |
Tm1—O2ix | 2.267 (3) | O6—Tm1vii | 2.219 (3) |
Tm1—Si2 | 3.3840 (11) | O6—Ba1v | 2.808 (3) |
Tm1—Tm1ix | 3.5895 (4) | O6—Ba1x | 2.863 (3) |
Tm1—Ba1x | 3.8463 (4) | F1—Ba1i | 2.677 (3) |
Tm1—Ba1xi | 4.0534 (4) | F1—Ba1xi | 2.726 (3) |
Tm1—Ba1iii | 4.0950 (4) | F1—Ba1x | 3.293 (4) |
Tm1—Ba1i | 4.1803 (4) | ||
F1i—Ba1—F1ii | 63.77 (11) | O6viii—Tm1—Ba1x | 102.55 (8) |
F1i—Ba1—O5iii | 136.73 (9) | O5—Tm1—Ba1x | 53.38 (9) |
F1ii—Ba1—O5iii | 149.93 (10) | O4i—Tm1—Ba1x | 45.69 (8) |
F1i—Ba1—O4iv | 75.39 (10) | O2—Tm1—Ba1x | 124.07 (8) |
F1ii—Ba1—O4iv | 80.10 (10) | O2ix—Tm1—Ba1x | 140.79 (8) |
O5iii—Ba1—O4iv | 122.25 (9) | Si2—Tm1—Ba1x | 58.79 (2) |
F1i—Ba1—O6v | 127.78 (10) | Tm1ix—Tm1—Ba1x | 147.464 (8) |
F1ii—Ba1—O6v | 88.69 (10) | F1—Tm1—Ba1xi | 38.87 (8) |
O5iii—Ba1—O6v | 61.43 (9) | O6viii—Tm1—Ba1xi | 42.99 (8) |
O4iv—Ba1—O6v | 145.79 (10) | O5—Tm1—Ba1xi | 102.21 (8) |
F1i—Ba1—O6vi | 119.38 (9) | O4i—Tm1—Ba1xi | 113.72 (8) |
F1ii—Ba1—O6vi | 59.79 (9) | O2—Tm1—Ba1xi | 148.19 (8) |
O5iii—Ba1—O6vi | 103.76 (9) | O2ix—Tm1—Ba1xi | 82.45 (8) |
O4iv—Ba1—O6vi | 75.05 (9) | Si2—Tm1—Ba1xi | 125.41 (2) |
O6v—Ba1—O6vi | 71.40 (10) | Tm1ix—Tm1—Ba1xi | 116.978 (9) |
F1i—Ba1—O3vii | 74.37 (10) | Ba1x—Tm1—Ba1xi | 87.422 (9) |
F1ii—Ba1—O3vii | 62.46 (10) | F1—Tm1—Ba1iii | 86.57 (9) |
O5iii—Ba1—O3vii | 98.34 (9) | O6viii—Tm1—Ba1iii | 40.55 (8) |
O4iv—Ba1—O3vii | 139.41 (9) | O5—Tm1—Ba1iii | 39.31 (8) |
O6v—Ba1—O3vii | 53.42 (9) | O4i—Tm1—Ba1iii | 116.98 (8) |
O6vi—Ba1—O3vii | 97.18 (9) | O2—Tm1—Ba1iii | 112.87 (8) |
F1i—Ba1—O5vi | 137.10 (10) | O2ix—Tm1—Ba1iii | 135.37 (8) |
F1ii—Ba1—O5vi | 107.91 (8) | Si2—Tm1—Ba1iii | 61.246 (19) |
O5iii—Ba1—O5vi | 72.27 (11) | Tm1ix—Tm1—Ba1iii | 134.016 (8) |
O4iv—Ba1—O5vi | 61.75 (9) | Ba1x—Tm1—Ba1iii | 73.006 (7) |
O6v—Ba1—O5vi | 92.00 (9) | Ba1xi—Tm1—Ba1iii | 68.822 (7) |
O6vi—Ba1—O5vi | 52.79 (8) | F1—Tm1—Ba1i | 34.20 (8) |
O3vii—Ba1—O5vi | 142.36 (8) | O6viii—Tm1—Ba1i | 110.53 (8) |
F1i—Ba1—F1vi | 89.02 (9) | O5—Tm1—Ba1i | 117.36 (9) |
F1ii—Ba1—F1vi | 130.03 (12) | O4i—Tm1—Ba1i | 51.93 (9) |
O5iii—Ba1—F1vi | 78.06 (8) | O2—Tm1—Ba1i | 126.77 (8) |
O4iv—Ba1—F1vi | 51.71 (8) | O2ix—Tm1—Ba1i | 76.88 (8) |
O6v—Ba1—F1vi | 137.98 (8) | Si2—Tm1—Ba1i | 119.53 (2) |
O6vi—Ba1—F1vi | 110.93 (8) | Tm1ix—Tm1—Ba1i | 103.568 (9) |
O3vii—Ba1—F1vi | 151.76 (8) | Ba1x—Tm1—Ba1i | 64.267 (7) |
O5vi—Ba1—F1vi | 63.73 (8) | Ba1xi—Tm1—Ba1i | 67.705 (7) |
F1i—Ba1—O4 | 52.14 (8) | Ba1iii—Tm1—Ba1i | 118.876 (9) |
F1ii—Ba1—O4 | 115.30 (8) | O4—Si1—O2 | 115.18 (18) |
O5iii—Ba1—O4 | 86.21 (9) | O4—Si1—O1 | 107.74 (17) |
O4iv—Ba1—O4 | 91.24 (9) | O2—Si1—O1 | 110.13 (17) |
O6v—Ba1—O4 | 122.58 (8) | O4—Si1—O3 | 109.15 (18) |
O6vi—Ba1—O4 | 165.90 (8) | O2—Si1—O3 | 106.83 (17) |
O3vii—Ba1—O4 | 91.09 (8) | O1—Si1—O3 | 107.59 (17) |
O5vi—Ba1—O4 | 123.44 (8) | O6—Si2—O5 | 111.12 (18) |
F1vi—Ba1—O4 | 60.84 (7) | O6—Si2—O1 | 109.87 (17) |
F1i—Ba1—Si2v | 101.63 (8) | O5—Si2—O1 | 111.79 (17) |
F1ii—Ba1—Si2v | 72.19 (8) | O6—Si2—O3iii | 105.78 (17) |
O5iii—Ba1—Si2v | 80.78 (7) | O5—Si2—O3iii | 110.74 (18) |
O4iv—Ba1—Si2v | 149.97 (7) | O1—Si2—O3iii | 107.31 (17) |
O6v—Ba1—Si2v | 26.23 (6) | O6—Si2—Tm1 | 110.66 (12) |
O6vi—Ba1—Si2v | 81.06 (6) | O5—Si2—Tm1 | 33.29 (12) |
O3vii—Ba1—Si2v | 27.46 (6) | O1—Si2—Tm1 | 81.80 (12) |
O5vi—Ba1—Si2v | 116.09 (6) | O3iii—Si2—Tm1 | 136.58 (12) |
F1vi—Ba1—Si2v | 157.65 (6) | O6—Si2—Ba1v | 50.52 (12) |
O4—Ba1—Si2v | 110.75 (6) | O5—Si2—Ba1v | 119.01 (13) |
F1i—Ba1—Si2vi | 132.44 (7) | O1—Si2—Ba1v | 129.19 (12) |
F1ii—Ba1—Si2vi | 83.23 (6) | O3iii—Si2—Ba1v | 55.96 (11) |
O5iii—Ba1—Si2vi | 88.48 (7) | Tm1—Si2—Ba1v | 145.77 (4) |
O4iv—Ba1—Si2vi | 65.48 (7) | O6—Si2—Ba1x | 51.51 (12) |
O6v—Ba1—Si2vi | 81.23 (7) | O5—Si2—Ba1x | 59.63 (13) |
O6vi—Ba1—Si2vi | 26.08 (6) | O1—Si2—Ba1x | 127.19 (13) |
O3vii—Ba1—Si2vi | 120.76 (6) | O3iii—Si2—Ba1x | 124.80 (12) |
O5vi—Ba1—Si2vi | 26.72 (6) | Tm1—Si2—Ba1x | 67.08 (2) |
F1vi—Ba1—Si2vi | 87.33 (5) | Ba1v—Si2—Ba1x | 80.70 (2) |
O4—Ba1—Si2vi | 148.14 (6) | Si1—O1—Si2 | 142.9 (2) |
Si2v—Ba1—Si2vi | 99.30 (2) | Si1—O2—Tm1 | 126.33 (17) |
F1—Tm1—O6viii | 78.75 (11) | Si1—O2—Tm1ix | 128.48 (17) |
F1—Tm1—O5 | 100.16 (13) | Tm1—O2—Tm1ix | 104.70 (12) |
O6viii—Tm1—O5 | 79.67 (12) | Si1—O3—Si2iii | 134.4 (2) |
F1—Tm1—O4i | 74.85 (12) | Si1—O3—Ba1viii | 128.55 (16) |
O6viii—Tm1—O4i | 146.58 (11) | Si2iii—O3—Ba1viii | 96.58 (13) |
O5—Tm1—O4i | 85.16 (12) | Si1—O4—Tm1i | 130.52 (18) |
F1—Tm1—O2 | 160.52 (12) | Si1—O4—Ba1iv | 125.22 (16) |
O6viii—Tm1—O2 | 116.50 (12) | Tm1i—O4—Ba1iv | 99.02 (11) |
O5—Tm1—O2 | 94.78 (11) | Si1—O4—Ba1 | 105.27 (16) |
O4i—Tm1—O2 | 94.18 (12) | Tm1i—O4—Ba1 | 95.69 (10) |
F1—Tm1—O2ix | 91.90 (13) | Ba1iv—O4—Ba1 | 88.76 (9) |
O6viii—Tm1—O2ix | 95.45 (12) | Si2—O5—Tm1 | 123.28 (18) |
O5—Tm1—O2ix | 165.76 (13) | Si2—O5—Ba1iii | 121.71 (17) |
O4i—Tm1—O2ix | 105.46 (12) | Tm1—O5—Ba1iii | 110.04 (11) |
O2—Tm1—O2ix | 75.30 (12) | Si2—O5—Ba1x | 93.65 (14) |
F1—Tm1—Si2 | 115.40 (10) | Tm1—O5—Ba1x | 91.35 (11) |
O6viii—Tm1—Si2 | 100.13 (8) | Ba1iii—O5—Ba1x | 107.73 (11) |
O5—Tm1—Si2 | 23.43 (8) | Si2—O6—Tm1vii | 127.85 (18) |
O4i—Tm1—Si2 | 73.79 (9) | Si2—O6—Ba1v | 103.26 (15) |
O2—Tm1—Si2 | 75.50 (8) | Tm1vii—O6—Ba1v | 108.53 (11) |
O2ix—Tm1—Si2 | 150.64 (8) | Si2—O6—Ba1x | 102.41 (14) |
F1—Tm1—Tm1ix | 128.04 (10) | Tm1vii—O6—Ba1x | 105.10 (12) |
O6viii—Tm1—Tm1ix | 109.98 (8) | Ba1v—O6—Ba1x | 108.60 (10) |
O5—Tm1—Tm1ix | 131.66 (9) | Tm1—F1—Ba1i | 118.61 (12) |
O4i—Tm1—Tm1ix | 102.38 (8) | Tm1—F1—Ba1xi | 111.07 (12) |
O2—Tm1—Tm1ix | 37.65 (8) | Ba1i—F1—Ba1xi | 116.23 (11) |
O2ix—Tm1—Tm1ix | 37.65 (8) | Tm1—F1—Ba1x | 86.88 (10) |
Si2—Tm1—Tm1ix | 113.10 (2) | Ba1i—F1—Ba1x | 90.98 (9) |
F1—Tm1—Ba1x | 58.73 (10) | Ba1xi—F1—Ba1x | 130.03 (12) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z; (v) −x+2, −y+1, −z+1; (vi) x, y, z−1; (vii) x+1, y, z; (viii) x−1, y, z; (ix) −x, −y, −z+1; (x) x, y, z+1; (xi) x−1, y, z+1. |
Ba2F2O12Si4Yb2 | Z = 1 |
Mr = 963.12 | F(000) = 422 |
Triclinic, P1 | Dx = 5.003 Mg m−3 |
a = 5.4461 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.1212 (3) Å | Cell parameters from 9791 reflections |
c = 8.9128 (4) Å | θ = 2.5–26.5° |
α = 107.7984 (14)° | µ = 21.03 mm−1 |
β = 101.8656 (14)° | T = 300 K |
γ = 92.9455 (14)° | Block, colourless |
V = 319.66 (3) Å3 | 0.11 × 0.06 × 0.06 mm |
Bruker Photon 100 diffractometer | 1308 reflections with I > 2σ(I) |
Radiation source: Ius | Rint = 0.023 |
φ and ω scans | θmax = 26.5°, θmin = 2.5° |
Absorption correction: multi-scan SADABS, Bruker | h = −6→6 |
Tmin = 0.839, Tmax = 1.000 | k = −8→8 |
8268 measured reflections | l = −11→11 |
1316 independent reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.014 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.3644P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.058 | (Δ/σ)max = 0.002 |
S = 1.14 | Δρmax = 1.36 e Å−3 |
1316 reflections | Δρmin = −0.91 e Å−3 |
101 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0157 (8) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.75833 (5) | 0.25733 (4) | 0.04525 (3) | 0.00949 (13) | |
Yb1 | 0.16280 (3) | 0.14859 (3) | 0.70082 (2) | 0.00604 (12) | |
Si1 | 0.3840 (2) | 0.17724 (18) | 0.36874 (14) | 0.0055 (2) | |
Si2 | 0.6777 (2) | 0.44045 (18) | 0.70994 (14) | 0.0059 (3) | |
O1 | 0.6134 (6) | 0.3116 (5) | 0.5185 (4) | 0.0107 (7) | |
O2 | 0.1666 (6) | 0.0892 (5) | 0.4379 (4) | 0.0098 (7) | |
O3 | 0.2543 (6) | 0.3256 (5) | 0.2741 (4) | 0.0103 (7) | |
O4 | 0.5059 (6) | 0.0142 (5) | 0.2486 (4) | 0.0116 (7) | |
O5 | 0.4457 (6) | 0.4165 (5) | 0.7918 (4) | 0.0108 (7) | |
O6 | 0.9300 (6) | 0.3783 (5) | 0.8018 (4) | 0.0091 (7) | |
F1 | 0.1513 (6) | 0.0991 (5) | 0.9267 (4) | 0.0186 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.01117 (19) | 0.00726 (18) | 0.00835 (19) | 0.00124 (12) | 0.00118 (13) | 0.00080 (13) |
Yb1 | 0.00635 (16) | 0.00565 (16) | 0.00522 (16) | 0.00008 (9) | 0.00086 (9) | 0.00090 (10) |
Si1 | 0.0059 (6) | 0.0050 (6) | 0.0047 (6) | 0.0002 (4) | 0.0005 (4) | 0.0007 (5) |
Si2 | 0.0043 (6) | 0.0058 (6) | 0.0067 (6) | 0.0001 (4) | 0.0004 (5) | 0.0015 (5) |
O1 | 0.0076 (15) | 0.0111 (17) | 0.0089 (16) | −0.0015 (12) | −0.0022 (13) | 0.0000 (13) |
O2 | 0.0118 (16) | 0.0098 (16) | 0.0086 (16) | −0.0009 (12) | 0.0040 (13) | 0.0035 (13) |
O3 | 0.0119 (16) | 0.0055 (15) | 0.0104 (16) | −0.0015 (12) | −0.0031 (13) | 0.0023 (12) |
O4 | 0.0120 (16) | 0.0106 (16) | 0.0096 (16) | 0.0035 (13) | 0.0015 (13) | −0.0003 (13) |
O5 | 0.0073 (16) | 0.0105 (17) | 0.0127 (17) | −0.0031 (12) | 0.0045 (13) | 0.0002 (14) |
O6 | 0.0077 (16) | 0.0080 (16) | 0.0109 (16) | 0.0034 (12) | 0.0014 (13) | 0.0023 (13) |
F1 | 0.0282 (17) | 0.0210 (15) | 0.0161 (15) | 0.0141 (13) | 0.0131 (13) | 0.0124 (12) |
Ba1—F1i | 2.686 (3) | Si1—O2 | 1.623 (3) |
Ba1—F1ii | 2.723 (3) | Si1—O1 | 1.633 (3) |
Ba1—O5iii | 2.758 (3) | Si1—O3 | 1.644 (3) |
Ba1—O4iv | 2.782 (3) | Si1—Yb1i | 3.4926 (12) |
Ba1—O6v | 2.811 (3) | Si1—Yb1ix | 3.5053 (13) |
Ba1—O6vi | 2.867 (3) | Si2—O6 | 1.605 (3) |
Ba1—O3vii | 2.948 (3) | Si2—O5 | 1.610 (3) |
Ba1—O5vi | 3.077 (3) | Si2—O1 | 1.625 (3) |
Ba1—F1vi | 3.281 (3) | Si2—O3iii | 1.644 (3) |
Ba1—O4 | 3.297 (4) | Si2—Yb1vii | 3.4430 (12) |
Ba1—Si2v | 3.5383 (12) | Si2—Ba1v | 3.5383 (12) |
Ba1—Si2vi | 3.5674 (12) | Si2—Ba1x | 3.5674 (12) |
Yb1—F1 | 2.160 (3) | O2—Yb1ix | 2.260 (3) |
Yb1—O6viii | 2.208 (3) | O3—Si2iii | 1.644 (3) |
Yb1—O5 | 2.216 (3) | O3—Ba1viii | 2.948 (3) |
Yb1—O4i | 2.236 (3) | O4—Yb1i | 2.236 (3) |
Yb1—O2 | 2.255 (3) | O4—Ba1iv | 2.782 (3) |
Yb1—O2ix | 2.260 (3) | O5—Ba1iii | 2.758 (3) |
Yb1—Si2 | 3.3756 (12) | O5—Ba1x | 3.077 (3) |
Yb1—Si2viii | 3.4430 (12) | O6—Yb1vii | 2.208 (3) |
Yb1—Si1 | 3.4733 (12) | O6—Ba1v | 2.811 (3) |
Yb1—Si1i | 3.4927 (12) | O6—Ba1x | 2.867 (3) |
Yb1—Si1ix | 3.5053 (13) | F1—Ba1i | 2.686 (3) |
Yb1—Yb1ix | 3.5791 (4) | F1—Ba1xi | 2.723 (3) |
Si1—O4 | 1.596 (3) | F1—Ba1x | 3.281 (3) |
F1i—Ba1—F1ii | 63.88 (11) | O2—Yb1—Si1i | 75.35 (9) |
F1i—Ba1—O5iii | 137.07 (9) | O2ix—Yb1—Si1i | 93.86 (9) |
F1ii—Ba1—O5iii | 149.63 (10) | Si2—Yb1—Si1i | 75.82 (3) |
F1i—Ba1—O4iv | 75.58 (10) | Si2viii—Yb1—Si1i | 171.67 (3) |
F1ii—Ba1—O4iv | 80.06 (10) | Si1—Yb1—Si1i | 70.51 (3) |
O5iii—Ba1—O4iv | 122.17 (10) | F1—Yb1—Si1ix | 72.47 (9) |
F1i—Ba1—O6v | 127.73 (9) | O6viii—Yb1—Si1ix | 83.63 (9) |
F1ii—Ba1—O6v | 88.82 (9) | O5—Yb1—Si1ix | 162.62 (9) |
O5iii—Ba1—O6v | 61.07 (10) | O4i—Yb1—Si1ix | 107.21 (9) |
O4iv—Ba1—O6v | 145.80 (10) | O2—Yb1—Si1ix | 96.27 (9) |
F1i—Ba1—O6vi | 119.12 (9) | O2ix—Yb1—Si1ix | 21.33 (8) |
F1ii—Ba1—O6vi | 59.43 (9) | Si2—Yb1—Si1ix | 171.84 (3) |
O5iii—Ba1—O6vi | 103.68 (9) | Si2viii—Yb1—Si1ix | 74.81 (3) |
O4iv—Ba1—O6vi | 74.76 (10) | Si1—Yb1—Si1ix | 118.29 (2) |
O6v—Ba1—O6vi | 71.76 (11) | Si1i—Yb1—Si1ix | 102.20 (3) |
F1i—Ba1—O3vii | 74.27 (10) | F1—Yb1—Yb1ix | 128.24 (9) |
F1ii—Ba1—O3vii | 62.31 (10) | O6viii—Yb1—Yb1ix | 109.65 (9) |
O5iii—Ba1—O3vii | 98.56 (9) | O5—Yb1—Yb1ix | 131.83 (9) |
O4iv—Ba1—O3vii | 139.27 (9) | O4i—Yb1—Yb1ix | 102.66 (9) |
O6v—Ba1—O3vii | 53.46 (9) | O2—Yb1—Yb1ix | 37.62 (8) |
O6vi—Ba1—O3vii | 96.98 (10) | O2ix—Yb1—Yb1ix | 37.52 (8) |
F1i—Ba1—O5vi | 137.10 (9) | Si2—Yb1—Yb1ix | 113.14 (2) |
F1ii—Ba1—O5vi | 107.68 (9) | Si2viii—Yb1—Yb1ix | 88.56 (2) |
O5iii—Ba1—O5vi | 72.12 (10) | Si1—Yb1—Yb1ix | 59.59 (2) |
O4iv—Ba1—O5vi | 61.56 (9) | Si1i—Yb1—Yb1ix | 83.29 (2) |
O6v—Ba1—O5vi | 92.08 (9) | Si1ix—Yb1—Yb1ix | 58.71 (2) |
O6vi—Ba1—O5vi | 52.84 (9) | O4—Si1—O2 | 115.08 (19) |
O3vii—Ba1—O5vi | 142.27 (9) | O4—Si1—O1 | 107.61 (18) |
F1i—Ba1—F1vi | 89.28 (8) | O2—Si1—O1 | 110.22 (18) |
F1ii—Ba1—F1vi | 129.95 (11) | O4—Si1—O3 | 109.25 (19) |
O5iii—Ba1—F1vi | 78.21 (8) | O2—Si1—O3 | 107.02 (19) |
O4iv—Ba1—F1vi | 51.58 (9) | O1—Si1—O3 | 107.41 (18) |
O6v—Ba1—F1vi | 137.78 (9) | O4—Si1—Yb1 | 128.92 (14) |
O6vi—Ba1—F1vi | 110.60 (8) | O2—Si1—Yb1 | 31.52 (12) |
O3vii—Ba1—F1vi | 152.27 (8) | O1—Si1—Yb1 | 78.72 (12) |
O5vi—Ba1—F1vi | 63.45 (8) | O3—Si1—Yb1 | 116.97 (14) |
F1i—Ba1—O4 | 51.91 (9) | O4—Si1—Yb1i | 29.07 (12) |
F1ii—Ba1—O4 | 115.22 (8) | O2—Si1—Yb1i | 111.26 (13) |
O5iii—Ba1—O4 | 86.79 (9) | O1—Si1—Yb1i | 83.22 (12) |
O4iv—Ba1—O4 | 91.28 (9) | O3—Si1—Yb1i | 133.47 (14) |
O6v—Ba1—O4 | 122.53 (9) | Yb1—Si1—Yb1i | 109.49 (3) |
O6vi—Ba1—O4 | 165.54 (9) | O4—Si1—Yb1ix | 92.75 (13) |
O3vii—Ba1—O4 | 91.19 (9) | O2—Si1—Yb1ix | 30.42 (12) |
O5vi—Ba1—O4 | 123.61 (8) | O1—Si1—Yb1ix | 139.72 (13) |
F1vi—Ba1—O4 | 61.24 (8) | O3—Si1—Yb1ix | 97.50 (13) |
F1i—Ba1—Si2v | 101.60 (7) | Yb1—Si1—Yb1ix | 61.71 (2) |
F1ii—Ba1—Si2v | 72.25 (7) | Yb1i—Si1—Yb1ix | 102.20 (3) |
O5iii—Ba1—Si2v | 80.64 (7) | O6—Si2—O5 | 111.15 (18) |
O4iv—Ba1—Si2v | 149.95 (7) | O6—Si2—O1 | 109.63 (18) |
O6v—Ba1—Si2v | 26.22 (7) | O5—Si2—O1 | 112.10 (18) |
O6vi—Ba1—Si2v | 81.17 (7) | O6—Si2—O3iii | 105.88 (18) |
O3vii—Ba1—Si2v | 27.49 (7) | O5—Si2—O3iii | 110.32 (19) |
O5vi—Ba1—Si2v | 116.09 (6) | O1—Si2—O3iii | 107.51 (18) |
F1vi—Ba1—Si2v | 157.71 (6) | O6—Si2—Yb1 | 110.68 (13) |
O4—Ba1—Si2v | 110.75 (6) | O5—Si2—Yb1 | 33.38 (12) |
F1i—Ba1—Si2vi | 132.36 (7) | O1—Si2—Yb1 | 82.02 (12) |
F1ii—Ba1—Si2vi | 82.96 (6) | O3iii—Si2—Yb1 | 136.30 (13) |
O5iii—Ba1—Si2vi | 88.29 (7) | O6—Si2—Yb1vii | 30.17 (12) |
O4iv—Ba1—Si2vi | 65.29 (7) | O5—Si2—Yb1vii | 124.18 (14) |
O6v—Ba1—Si2vi | 81.38 (7) | O1—Si2—Yb1vii | 79.48 (12) |
O6vi—Ba1—Si2vi | 26.10 (7) | O3iii—Si2—Yb1vii | 117.60 (13) |
O3vii—Ba1—Si2vi | 120.55 (7) | Yb1—Si2—Yb1vii | 106.01 (3) |
O5vi—Ba1—Si2vi | 26.75 (6) | O6—Si2—Ba1v | 50.72 (12) |
F1vi—Ba1—Si2vi | 87.06 (5) | O5—Si2—Ba1v | 118.86 (13) |
O4—Ba1—Si2vi | 148.26 (6) | O1—Si2—Ba1v | 129.03 (13) |
Si2v—Ba1—Si2vi | 99.30 (3) | O3iii—Si2—Ba1v | 55.83 (12) |
F1—Yb1—O6viii | 78.83 (12) | Yb1—Si2—Ba1v | 145.78 (4) |
F1—Yb1—O5 | 99.82 (13) | Yb1vii—Si2—Ba1v | 71.80 (2) |
O6viii—Yb1—O5 | 79.54 (13) | O6—Si2—Ba1x | 51.78 (12) |
F1—Yb1—O4i | 74.96 (12) | O5—Si2—Ba1x | 59.39 (13) |
O6viii—Yb1—O4i | 146.70 (12) | O1—Si2—Ba1x | 127.55 (13) |
O5—Yb1—O4i | 85.03 (12) | O3iii—Si2—Ba1x | 124.29 (13) |
F1—Yb1—O2 | 160.87 (12) | Yb1—Si2—Ba1x | 67.07 (2) |
O6viii—Yb1—O2 | 116.01 (12) | Yb1vii—Si2—Ba1x | 70.50 (2) |
O5—Yb1—O2 | 94.98 (12) | Ba1v—Si2—Ba1x | 80.70 (3) |
O4i—Yb1—O2 | 94.47 (12) | Si2—O1—Si1 | 142.6 (2) |
F1—Yb1—O2ix | 92.15 (12) | Si1—O2—Yb1 | 126.37 (18) |
O6viii—Yb1—O2ix | 95.45 (13) | Si1—O2—Yb1ix | 128.25 (18) |
O5—Yb1—O2ix | 165.79 (12) | Yb1—O2—Yb1ix | 104.86 (13) |
O4i—Yb1—O2ix | 105.62 (12) | Si1—O3—Si2iii | 134.3 (2) |
O2—Yb1—O2ix | 75.14 (13) | Si1—O3—Ba1viii | 128.44 (17) |
F1—Yb1—Si2 | 115.31 (9) | Si2iii—O3—Ba1viii | 96.68 (14) |
O6viii—Yb1—Si2 | 99.99 (9) | Si1—O4—Yb1i | 130.64 (19) |
O5—Yb1—Si2 | 23.55 (9) | Si1—O4—Ba1iv | 125.09 (17) |
O4i—Yb1—Si2 | 73.74 (9) | Yb1i—O4—Ba1iv | 99.25 (11) |
O2—Yb1—Si2 | 75.57 (9) | Si1—O4—Ba1 | 104.74 (15) |
O2ix—Yb1—Si2 | 150.55 (8) | Yb1i—O4—Ba1 | 95.91 (11) |
F1—Yb1—Si2viii | 94.79 (8) | Ba1iv—O4—Ba1 | 88.72 (9) |
O6viii—Yb1—Si2viii | 21.43 (9) | Si2—O5—Yb1 | 123.07 (18) |
O5—Yb1—Si2viii | 90.69 (9) | Si2—O5—Ba1iii | 121.38 (17) |
O4i—Yb1—Si2viii | 167.99 (9) | Yb1—O5—Ba1iii | 110.34 (12) |
O2—Yb1—Si2viii | 97.09 (9) | Si2—O5—Ba1x | 93.86 (15) |
O2ix—Yb1—Si2viii | 80.63 (9) | Yb1—O5—Ba1x | 91.50 (11) |
Si2—Yb1—Si2viii | 106.01 (3) | Ba1iii—O5—Ba1x | 107.88 (10) |
F1—Yb1—Si1 | 160.35 (8) | Si2—O6—Yb1vii | 128.40 (19) |
O6viii—Yb1—Si1 | 117.29 (9) | Si2—O6—Ba1v | 103.06 (15) |
O5—Yb1—Si1 | 73.98 (9) | Yb1vii—O6—Ba1v | 108.72 (12) |
O4i—Yb1—Si1 | 85.83 (9) | Si2—O6—Ba1x | 102.12 (15) |
O2—Yb1—Si1 | 22.11 (9) | Yb1vii—O6—Ba1x | 105.04 (12) |
O2ix—Yb1—Si1 | 97.05 (8) | Ba1v—O6—Ba1x | 108.24 (11) |
Si2—Yb1—Si1 | 53.55 (3) | Yb1—F1—Ba1i | 118.37 (12) |
Si2viii—Yb1—Si1 | 103.80 (3) | Yb1—F1—Ba1xi | 111.42 (12) |
F1—Yb1—Si1i | 91.64 (8) | Ba1i—F1—Ba1xi | 116.12 (11) |
O6viii—Yb1—Si1i | 166.90 (9) | Yb1—F1—Ba1x | 87.19 (10) |
O5—Yb1—Si1i | 93.43 (9) | Ba1i—F1—Ba1x | 90.72 (8) |
O4i—Yb1—Si1i | 20.29 (9) | Ba1xi—F1—Ba1x | 129.95 (11) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z; (v) −x+2, −y+1, −z+1; (vi) x, y, z−1; (vii) x+1, y, z; (viii) x−1, y, z; (ix) −x, −y, −z+1; (x) x, y, z+1; (xi) x−1, y, z+1. |
Ba2F2Lu2O12Si4 | Z = 1 |
Mr = 966.98 | F(000) = 424 |
Triclinic, P1 | Dx = 5.026 Mg m−3 |
a = 5.451 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.1227 (18) Å | Cell parameters from 1958 reflections |
c = 8.8937 (18) Å | θ = 2.5–26.0° |
α = 107.73 (3)° | µ = 21.86 mm−1 |
β = 101.81 (4)° | T = 298 K |
γ = 93.01 (4)° | Block, colourless |
V = 319.5 (2) Å3 | 0.15 × 0.14 × 0.13 mm |
Rigaku AFC8S diffractometer | 1148 independent reflections |
Radiation source: fine-focus sealed tube | 1116 reflections with I > 2σ(I) |
Detector resolution: 14.6199 pixels mm-1 | Rint = 0.040 |
ω scans | θmax = 25.2°, θmin = 3.0° |
Absorption correction: multi-scan REQAB, CrystalClear | h = −6→5 |
Tmin = 0.273, Tmax = 1.000 | k = −8→8 |
2710 measured reflections | l = −10→10 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | w = 1/[σ2(Fo2) + (0.079P)2 + 31.2028P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.099 | (Δ/σ)max < 0.001 |
S = 1.07 | Δρmax = 2.60 e Å−3 |
1148 reflections | Δρmin = −3.57 e Å−3 |
101 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0255 (18) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.75782 (9) | 0.25769 (7) | 0.04574 (6) | 0.0126 (3) | |
Lu1 | 0.16320 (6) | 0.14784 (5) | 0.70058 (4) | 0.0093 (3) | |
Si1 | 0.3845 (4) | 0.1775 (3) | 0.3683 (3) | 0.0095 (5) | |
Si2 | 0.6784 (4) | 0.4400 (3) | 0.7097 (3) | 0.0083 (5) | |
O1 | 0.6132 (11) | 0.3133 (9) | 0.5173 (7) | 0.0130 (13) | |
O2 | 0.1667 (11) | 0.0888 (9) | 0.4377 (7) | 0.0136 (13) | |
O3 | 0.2516 (11) | 0.3256 (9) | 0.2738 (8) | 0.0128 (12) | |
O4 | 0.5075 (11) | 0.0155 (9) | 0.2497 (8) | 0.0139 (13) | |
O5 | 0.4478 (11) | 0.4140 (9) | 0.7927 (7) | 0.0116 (13) | |
O6 | 0.9312 (11) | 0.3772 (10) | 0.8017 (8) | 0.0129 (13) | |
F1 | 0.1464 (11) | 0.0975 (9) | 0.9233 (7) | 0.0215 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.0133 (4) | 0.0126 (4) | 0.0121 (4) | 0.0024 (2) | 0.0027 (2) | 0.0044 (3) |
Lu1 | 0.0087 (3) | 0.0109 (3) | 0.0091 (3) | 0.00125 (18) | 0.00240 (19) | 0.0044 (2) |
Si1 | 0.0109 (11) | 0.0112 (11) | 0.0068 (11) | 0.0010 (8) | 0.0021 (9) | 0.0032 (9) |
Si2 | 0.0051 (10) | 0.0137 (12) | 0.0086 (11) | 0.0023 (8) | 0.0030 (9) | 0.0061 (9) |
O1 | 0.009 (3) | 0.017 (3) | 0.009 (3) | −0.002 (2) | −0.003 (2) | 0.003 (3) |
O2 | 0.016 (3) | 0.014 (3) | 0.011 (3) | −0.002 (2) | 0.007 (2) | 0.002 (3) |
O3 | 0.012 (3) | 0.012 (3) | 0.014 (3) | 0.001 (2) | −0.005 (2) | 0.009 (2) |
O4 | 0.014 (3) | 0.014 (3) | 0.011 (3) | 0.000 (2) | 0.000 (2) | 0.003 (2) |
O5 | 0.010 (3) | 0.012 (3) | 0.013 (3) | −0.001 (2) | 0.005 (2) | 0.004 (3) |
O6 | 0.011 (3) | 0.016 (3) | 0.013 (3) | 0.004 (2) | 0.001 (2) | 0.008 (3) |
F1 | 0.032 (3) | 0.024 (3) | 0.022 (3) | 0.018 (2) | 0.017 (2) | 0.017 (2) |
Ba1—F1i | 2.693 (6) | Si1—O4 | 1.588 (6) |
Ba1—F1ii | 2.723 (6) | Si1—O2 | 1.627 (6) |
Ba1—O5iii | 2.771 (6) | Si1—O1 | 1.631 (6) |
Ba1—O4iv | 2.796 (6) | Si1—O3 | 1.648 (7) |
Ba1—O6v | 2.815 (6) | Si2—O6 | 1.611 (7) |
Ba1—O6vi | 2.865 (6) | Si2—O5 | 1.612 (6) |
Ba1—O3vii | 2.936 (6) | Si2—O1 | 1.626 (6) |
Ba1—O5vi | 3.054 (7) | Si2—O3iii | 1.648 (7) |
Ba1—O4 | 3.286 (6) | Si2—Ba1v | 3.539 (3) |
Ba1—F1vi | 3.309 (6) | Si2—Ba1x | 3.564 (3) |
Ba1—Si2v | 3.539 (3) | O2—Lu1ix | 2.258 (6) |
Ba1—Si2vi | 3.564 (3) | O3—Si2iii | 1.648 (7) |
Lu1—F1 | 2.137 (6) | O3—Ba1viii | 2.936 (6) |
Lu1—O6viii | 2.206 (6) | O4—Lu1i | 2.232 (7) |
Lu1—O5 | 2.213 (6) | O4—Ba1iv | 2.796 (6) |
Lu1—O4i | 2.232 (7) | O5—Ba1iii | 2.771 (6) |
Lu1—O2 | 2.250 (6) | O5—Ba1x | 3.054 (7) |
Lu1—O2ix | 2.258 (6) | O6—Lu1vii | 2.206 (6) |
Lu1—Si2 | 3.378 (3) | O6—Ba1v | 2.815 (6) |
Lu1—Lu1ix | 3.572 (2) | O6—Ba1x | 2.865 (6) |
Lu1—Ba1x | 3.839 (2) | F1—Ba1i | 2.693 (6) |
Lu1—Ba1xi | 4.0512 (17) | F1—Ba1xi | 2.723 (6) |
Lu1—Ba1iii | 4.0983 (17) | F1—Ba1x | 3.309 (6) |
Lu1—Ba1i | 4.1620 (13) | ||
F1i—Ba1—F1ii | 63.6 (2) | O6viii—Lu1—Ba1x | 102.48 (16) |
F1i—Ba1—O5iii | 137.47 (18) | O5—Lu1—Ba1x | 52.65 (17) |
F1ii—Ba1—O5iii | 149.96 (17) | O4i—Lu1—Ba1x | 46.00 (15) |
F1i—Ba1—O4iv | 76.10 (18) | O2—Lu1—Ba1x | 124.43 (16) |
F1ii—Ba1—O4iv | 79.36 (18) | O2ix—Lu1—Ba1x | 141.08 (18) |
O5iii—Ba1—O4iv | 121.93 (18) | Si2—Lu1—Ba1x | 58.76 (5) |
F1i—Ba1—O6v | 127.17 (18) | Lu1ix—Lu1—Ba1x | 148.00 (3) |
F1ii—Ba1—O6v | 89.38 (18) | F1—Lu1—Ba1xi | 38.41 (15) |
O5iii—Ba1—O6v | 60.97 (18) | O6viii—Lu1—Ba1xi | 43.01 (17) |
O4iv—Ba1—O6v | 145.79 (19) | O5—Lu1—Ba1xi | 101.88 (16) |
F1i—Ba1—O6vi | 118.82 (18) | O4i—Lu1—Ba1xi | 113.97 (17) |
F1ii—Ba1—O6vi | 58.86 (18) | O2—Lu1—Ba1xi | 147.83 (16) |
O5iii—Ba1—O6vi | 103.52 (18) | O2ix—Lu1—Ba1xi | 82.46 (16) |
O4iv—Ba1—O6vi | 74.79 (18) | Si2—Lu1—Ba1xi | 125.23 (5) |
O6v—Ba1—O6vi | 71.8 (2) | Lu1ix—Lu1—Ba1xi | 116.76 (4) |
F1i—Ba1—O3vii | 73.56 (19) | Ba1x—Lu1—Ba1xi | 87.34 (3) |
F1ii—Ba1—O3vii | 62.97 (18) | F1—Lu1—Ba1iii | 86.72 (16) |
O5iii—Ba1—O3vii | 98.88 (18) | O6viii—Lu1—Ba1iii | 40.55 (16) |
O4iv—Ba1—O3vii | 139.19 (18) | O5—Lu1—Ba1iii | 39.40 (16) |
O6v—Ba1—O3vii | 53.61 (18) | O4i—Lu1—Ba1iii | 117.11 (15) |
O6vi—Ba1—O3vii | 96.80 (18) | O2—Lu1—Ba1iii | 112.57 (17) |
F1i—Ba1—O5vi | 137.50 (17) | O2ix—Lu1—Ba1iii | 135.18 (17) |
F1ii—Ba1—O5vi | 107.05 (17) | Si2—Lu1—Ba1iii | 61.10 (6) |
O5iii—Ba1—O5vi | 71.87 (19) | Lu1ix—Lu1—Ba1iii | 133.65 (3) |
O4iv—Ba1—O5vi | 61.42 (18) | Ba1x—Lu1—Ba1iii | 72.88 (5) |
O6v—Ba1—O5vi | 92.13 (18) | Ba1xi—Lu1—Ba1iii | 68.76 (4) |
O6vi—Ba1—O5vi | 53.05 (16) | F1—Lu1—Ba1i | 34.64 (15) |
O3vii—Ba1—O5vi | 142.40 (17) | O6viii—Lu1—Ba1i | 111.00 (17) |
F1i—Ba1—O4 | 52.06 (16) | O5—Lu1—Ba1i | 116.70 (17) |
F1ii—Ba1—O4 | 115.27 (17) | O4i—Lu1—Ba1i | 51.74 (16) |
O5iii—Ba1—O4 | 87.18 (17) | O2—Lu1—Ba1i | 126.81 (17) |
O4iv—Ba1—O4 | 91.30 (17) | O2ix—Lu1—Ba1i | 77.08 (18) |
O6v—Ba1—O4 | 122.52 (16) | Si2—Lu1—Ba1i | 119.40 (5) |
O6vi—Ba1—O4 | 165.50 (16) | Lu1ix—Lu1—Ba1i | 103.66 (3) |
O3vii—Ba1—O4 | 91.08 (17) | Ba1x—Lu1—Ba1i | 64.29 (4) |
O5vi—Ba1—O4 | 123.70 (15) | Ba1xi—Lu1—Ba1i | 68.15 (3) |
F1i—Ba1—F1vi | 90.02 (16) | Ba1iii—Lu1—Ba1i | 119.15 (2) |
F1ii—Ba1—F1vi | 129.0 (2) | O4—Si1—O2 | 115.1 (3) |
O5iii—Ba1—F1vi | 78.36 (16) | O4—Si1—O1 | 107.4 (3) |
O4iv—Ba1—F1vi | 51.18 (16) | O2—Si1—O1 | 110.6 (3) |
O6v—Ba1—F1vi | 137.78 (17) | O4—Si1—O3 | 110.0 (4) |
O6vi—Ba1—F1vi | 110.33 (16) | O2—Si1—O3 | 106.4 (4) |
O3vii—Ba1—F1vi | 152.69 (16) | O1—Si1—O3 | 107.2 (3) |
O5vi—Ba1—F1vi | 63.05 (14) | O6—Si2—O5 | 110.6 (3) |
O4—Ba1—F1vi | 61.74 (14) | O6—Si2—O1 | 110.0 (3) |
F1i—Ba1—Si2v | 100.92 (14) | O5—Si2—O1 | 112.2 (3) |
F1ii—Ba1—Si2v | 72.86 (14) | O6—Si2—O3iii | 105.6 (3) |
O5iii—Ba1—Si2v | 80.78 (13) | O5—Si2—O3iii | 111.0 (3) |
O4iv—Ba1—Si2v | 149.93 (13) | O1—Si2—O3iii | 107.1 (3) |
O6v—Ba1—Si2v | 26.34 (14) | O6—Si2—Lu1 | 110.7 (2) |
O6vi—Ba1—Si2v | 81.06 (13) | O5—Si2—Lu1 | 33.2 (2) |
O3vii—Ba1—Si2v | 27.53 (13) | O1—Si2—Lu1 | 82.2 (2) |
O5vi—Ba1—Si2v | 116.21 (12) | O3iii—Si2—Lu1 | 136.6 (2) |
O4—Ba1—Si2v | 110.69 (11) | O6—Si2—Ba1v | 50.9 (2) |
F1vi—Ba1—Si2v | 158.08 (10) | O5—Si2—Ba1v | 118.8 (2) |
F1i—Ba1—Si2vi | 132.58 (12) | O1—Si2—Ba1v | 128.9 (2) |
F1ii—Ba1—Si2vi | 82.44 (13) | O3iii—Si2—Ba1v | 55.4 (2) |
O5iii—Ba1—Si2vi | 87.92 (14) | Lu1—Si2—Ba1v | 145.89 (8) |
O4iv—Ba1—Si2vi | 65.35 (14) | O6—Si2—Ba1x | 51.9 (2) |
O6v—Ba1—Si2vi | 81.29 (14) | O5—Si2—Ba1x | 58.7 (2) |
O6vi—Ba1—Si2vi | 26.25 (12) | O1—Si2—Ba1x | 128.2 (3) |
O3vii—Ba1—Si2vi | 120.48 (13) | O3iii—Si2—Ba1x | 124.0 (2) |
O5vi—Ba1—Si2vi | 26.80 (11) | Lu1—Si2—Ba1x | 67.09 (6) |
O4—Ba1—Si2vi | 148.43 (11) | Ba1v—Si2—Ba1x | 80.77 (6) |
F1vi—Ba1—Si2vi | 86.73 (11) | Si2—O1—Si1 | 142.5 (4) |
Si2v—Ba1—Si2vi | 99.23 (6) | Si1—O2—Lu1 | 126.3 (3) |
F1—Lu1—O6viii | 78.5 (2) | Si1—O2—Lu1ix | 128.4 (3) |
F1—Lu1—O5 | 100.1 (2) | Lu1—O2—Lu1ix | 104.8 (2) |
O6viii—Lu1—O5 | 79.8 (2) | Si1—O3—Si2iii | 133.6 (4) |
F1—Lu1—O4i | 75.6 (2) | Si1—O3—Ba1viii | 128.9 (3) |
O6viii—Lu1—O4i | 146.9 (2) | Si2iii—O3—Ba1viii | 97.0 (3) |
O5—Lu1—O4i | 84.8 (2) | Si1—O4—Lu1i | 131.2 (4) |
F1—Lu1—O2 | 160.7 (2) | Si1—O4—Ba1iv | 124.7 (3) |
O6viii—Lu1—O2 | 116.0 (2) | Lu1i—O4—Ba1iv | 99.0 (2) |
O5—Lu1—O2 | 95.3 (2) | Si1—O4—Ba1 | 104.7 (3) |
O4i—Lu1—O2 | 94.4 (2) | Lu1i—O4—Ba1 | 96.0 (2) |
F1—Lu1—O2ix | 91.4 (2) | Ba1iv—O4—Ba1 | 88.70 (17) |
O6viii—Lu1—O2ix | 95.3 (2) | Si2—O5—Lu1 | 123.3 (3) |
O5—Lu1—O2ix | 166.2 (2) | Si2—O5—Ba1iii | 120.6 (3) |
O4i—Lu1—O2ix | 105.6 (2) | Lu1—O5—Ba1iii | 110.1 (2) |
O2—Lu1—O2ix | 75.2 (2) | Si2—O5—Ba1x | 94.5 (3) |
F1—Lu1—Si2 | 115.99 (17) | Lu1—O5—Ba1x | 92.2 (2) |
O6viii—Lu1—Si2 | 99.96 (17) | Ba1iii—O5—Ba1x | 108.13 (19) |
O5—Lu1—Si2 | 23.49 (16) | Si2—O6—Lu1vii | 128.5 (4) |
O4i—Lu1—Si2 | 73.86 (16) | Si2—O6—Ba1v | 102.8 (3) |
O2—Lu1—Si2 | 75.64 (16) | Lu1vii—O6—Ba1v | 108.8 (2) |
O2ix—Lu1—Si2 | 150.70 (16) | Si2—O6—Ba1x | 101.9 (3) |
F1—Lu1—Lu1ix | 127.62 (17) | Lu1vii—O6—Ba1x | 105.3 (2) |
O6viii—Lu1—Lu1ix | 109.51 (16) | Ba1v—O6—Ba1x | 108.2 (2) |
O5—Lu1—Lu1ix | 132.20 (16) | Lu1—F1—Ba1i | 118.6 (2) |
O4i—Lu1—Lu1ix | 102.61 (16) | Lu1—F1—Ba1xi | 112.4 (2) |
O2—Lu1—Lu1ix | 37.68 (15) | Ba1i—F1—Ba1xi | 116.4 (2) |
O2ix—Lu1—Lu1ix | 37.53 (16) | Lu1—F1—Ba1x | 86.84 (18) |
Si2—Lu1—Lu1ix | 113.27 (6) | Ba1i—F1—Ba1x | 89.98 (16) |
F1—Lu1—Ba1x | 59.40 (16) | Ba1xi—F1—Ba1x | 129.0 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z; (v) −x+2, −y+1, −z+1; (vi) x, y, z−1; (vii) x+1, y, z; (viii) x−1, y, z; (ix) −x, −y, −z+1; (x) x, y, z+1; (xi) x−1, y, z+1. |
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