Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011049/wm6067sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011049/wm6067Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (i-O) = 0.006 Å
- R factor = 0.024
- wR factor = 0.055
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.522 From the CIF: _refine_ls_abs_structure_Flack_su 0.019 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.52 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.01
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: Ce4 O14 Si4 Atom count from _chemical_formula_moiety: REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 28.93 From the CIF: _reflns_number_total 2729 From the CIF: _diffrn_reflns_limit_ max hkl 9. 9. 31. From the CIF: _diffrn_reflns_limit_ min hkl -9. -8. -31. TEST1: Expected hkl limits for theta max Calculated maximum hkl 9. 9. 33. Calculated minimum hkl -9. -9. -33. REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.93 From the CIF: _reflns_number_total 2729 Count of symmetry unique reflns 1545 Completeness (_total/calc) 176.63% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1184 Fraction of Friedel pairs measured 0.766 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker,2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL (Sheldrick, 2003); molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.
Ce4[Si2O7]2 | Dx = 5.215 Mg m−3 |
Mr = 896.84 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P41 | Cell parameters from 2729 reflections |
Hall symbol: P 4w | θ = 3.0–28.9° |
a = 6.7964 (3) Å | µ = 16.14 mm−1 |
c = 24.7282 (14) Å | T = 153 K |
V = 1142.22 (10) Å3 | Block, green |
Z = 4 | 0.10 × 0.04 × 0.04 mm |
F(000) = 1600 |
Bruker SMART 1000 CCD area-detector diffractometer | 2729 independent reflections |
Radiation source: fine-focus sealed tube | 2637 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
ω scans | θmax = 28.9°, θmin = 3.0° |
Absorption correction: numerical face-indexed using SHELXTL (Sheldrick, 2003) | h = −9→9 |
Tmin = 0.482, Tmax = 0.741 | k = −8→9 |
10648 measured reflections | l = −31→31 |
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)] = 0.024 | w = 1/[σ2(Fo2) + (0.028P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.055 | (Δ/σ)max = 0.001 |
S = 1.15 | Δρmax = 2.40 e Å−3 |
2729 reflections | Δρmin = −1.19 e Å−3 |
200 parameters | Absolute structure: Flack (1983), with 1284 Friedel pairs |
1 restraint | Absolute structure parameter: 0.522 (19) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ce1 | 0.11721 (6) | 0.23463 (6) | 0.125617 (17) | 0.00974 (10) | |
Ce2 | 0.16750 (6) | 0.51956 (6) | 0.367822 (16) | 0.00966 (9) | |
Ce3 | 0.33539 (6) | 0.08110 (6) | 0.265631 (17) | 0.00948 (9) | |
Ce4 | 0.69879 (6) | 0.23761 (6) | 0.015776 (17) | 0.01020 (10) | |
Si1 | 0.2332 (3) | 0.1505 (3) | 0.00002 (9) | 0.0085 (4) | |
Si2 | 0.2943 (3) | 0.0053 (3) | 0.39499 (8) | 0.0089 (4) | |
Si3 | 0.3784 (3) | 0.2598 (3) | 0.49333 (9) | 0.0086 (4) | |
Si4 | 0.5945 (3) | 0.3035 (3) | 0.15184 (8) | 0.0081 (4) | |
O1 | 0.0404 (8) | 0.1533 (8) | 0.2183 (2) | 0.0118 (11) | |
O2 | 0.0397 (8) | 0.4561 (8) | 0.5985 (2) | 0.0127 (11) | |
O3 | 0.0553 (8) | 0.2839 (8) | 0.0247 (2) | 0.0092 (11) | |
O4 | 0.1212 (8) | 0.5662 (8) | 0.1910 (2) | 0.0104 (11) | |
O5 | 0.1330 (7) | 0.1502 (8) | 0.3675 (2) | 0.0113 (11) | |
O6 | 0.1865 (8) | 0.2084 (8) | 0.6723 (2) | 0.0109 (11) | |
O7 | 0.2369 (8) | 0.4407 (8) | 0.4736 (2) | 0.0118 (11) | |
O8 | 0.2431 (8) | 0.1254 (8) | 0.5343 (2) | 0.0107 (11) | |
O9 | 0.3276 (8) | 0.4292 (8) | 0.2756 (2) | 0.0089 (11) | |
O10 | 0.3826 (8) | 0.1088 (8) | 0.0507 (2) | 0.0124 (11) | |
O11 | 0.4286 (8) | 0.1389 (8) | 0.1711 (2) | 0.0109 (11) | |
O12 | 0.4805 (8) | 0.4848 (8) | 0.1248 (2) | 0.0125 (11) | |
O13 | 0.7159 (8) | 0.3708 (8) | 0.2080 (2) | 0.0119 (11) | |
O14 | 0.7487 (7) | 0.1845 (8) | 0.1132 (2) | 0.0106 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ce1 | 0.0097 (2) | 0.0101 (2) | 0.0094 (2) | 0.00114 (15) | −0.00046 (15) | 0.00082 (17) |
Ce2 | 0.0095 (2) | 0.0096 (2) | 0.0099 (2) | −0.00032 (16) | 0.00005 (16) | 0.00008 (17) |
Ce3 | 0.0098 (2) | 0.0096 (2) | 0.0090 (2) | 0.00112 (16) | −0.00015 (16) | 0.00028 (16) |
Ce4 | 0.0092 (2) | 0.0110 (2) | 0.0104 (2) | −0.00110 (16) | −0.00047 (17) | 0.00198 (17) |
Si1 | 0.0096 (10) | 0.0071 (10) | 0.0090 (10) | −0.0003 (8) | 0.0000 (7) | −0.0008 (7) |
Si2 | 0.0097 (10) | 0.0100 (10) | 0.0070 (10) | 0.0003 (8) | 0.0009 (8) | 0.0006 (8) |
Si3 | 0.0092 (10) | 0.0083 (10) | 0.0082 (10) | −0.0006 (8) | 0.0004 (8) | −0.0015 (8) |
Si4 | 0.0064 (10) | 0.0085 (10) | 0.0094 (10) | −0.0004 (8) | −0.0005 (8) | −0.0021 (8) |
O1 | 0.019 (3) | 0.005 (3) | 0.011 (3) | −0.001 (2) | −0.002 (2) | 0.001 (2) |
O2 | 0.009 (3) | 0.011 (3) | 0.018 (3) | −0.003 (2) | 0.002 (2) | −0.002 (2) |
O3 | 0.011 (3) | 0.007 (3) | 0.010 (3) | 0.003 (2) | −0.001 (2) | −0.003 (2) |
O4 | 0.011 (3) | 0.007 (2) | 0.013 (3) | −0.003 (2) | −0.002 (2) | 0.002 (2) |
O5 | 0.007 (2) | 0.015 (3) | 0.012 (3) | 0.000 (2) | −0.003 (2) | 0.000 (2) |
O6 | 0.010 (3) | 0.010 (3) | 0.012 (3) | −0.002 (2) | 0.000 (2) | −0.001 (2) |
O7 | 0.013 (3) | 0.008 (2) | 0.015 (3) | −0.005 (2) | 0.002 (2) | 0.001 (2) |
O8 | 0.011 (3) | 0.011 (3) | 0.010 (3) | −0.001 (2) | −0.001 (2) | 0.003 (2) |
O9 | 0.012 (3) | 0.006 (2) | 0.008 (3) | −0.005 (2) | 0.000 (2) | −0.003 (2) |
O10 | 0.009 (3) | 0.013 (3) | 0.015 (3) | −0.003 (2) | 0.002 (2) | 0.000 (2) |
O11 | 0.012 (3) | 0.012 (3) | 0.009 (3) | −0.002 (2) | 0.000 (2) | −0.005 (2) |
O12 | 0.015 (3) | 0.016 (3) | 0.006 (2) | 0.008 (2) | −0.005 (2) | −0.003 (2) |
O13 | 0.012 (3) | 0.014 (3) | 0.010 (3) | −0.001 (2) | −0.002 (2) | −0.001 (2) |
O14 | 0.008 (3) | 0.017 (3) | 0.007 (3) | −0.001 (2) | 0.001 (2) | −0.003 (2) |
Ce1—O1 | 2.414 (5) | Si1—O3 | 1.630 (5) |
Ce1—O2i | 2.450 (6) | Si1—O10 | 1.638 (6) |
Ce1—O11 | 2.483 (6) | Si1—O13iv | 1.667 (6) |
Ce1—O5ii | 2.517 (5) | Si1—Ce3ii | 3.482 (2) |
Ce1—O14iii | 2.546 (5) | Si2—O6ii | 1.581 (6) |
Ce1—O3 | 2.553 (5) | Si2—O2ii | 1.619 (6) |
Ce1—O10 | 2.723 (5) | Si2—O5 | 1.622 (6) |
Ce1—O4 | 2.774 (5) | Si2—O4v | 1.678 (6) |
Ce1—Si1 | 3.255 (2) | Si2—Ce1v | 3.326 (2) |
Ce1—Si2iv | 3.326 (2) | Si2—Ce4xiv | 3.413 (2) |
Ce1—Si4 | 3.341 (2) | Si2—Ce2xv | 3.477 (2) |
Ce1—Ce2ii | 3.8710 (6) | Si3—O9v | 1.599 (6) |
Ce2—O12v | 2.384 (6) | Si3—O7 | 1.636 (6) |
Ce2—O6iv | 2.426 (5) | Si3—O4v | 1.644 (6) |
Ce2—O5 | 2.521 (6) | Si3—O8 | 1.645 (6) |
Ce2—O11vi | 2.541 (5) | Si3—Ce3vi | 3.213 (2) |
Ce2—O9 | 2.601 (5) | Si3—Ce2v | 3.217 (2) |
Ce2—O8iv | 2.637 (5) | Si3—Ce4xiv | 3.466 (2) |
Ce2—O10vi | 2.673 (5) | Si4—O12 | 1.602 (6) |
Ce2—O7 | 2.711 (6) | Si4—O14 | 1.632 (6) |
Ce2—O14vi | 2.857 (5) | Si4—O11 | 1.658 (6) |
Ce2—Si3iv | 3.217 (2) | Si4—O13 | 1.679 (6) |
Ce2—Si4vi | 3.348 (2) | Si4—Ce2ii | 3.348 (2) |
Ce2—Si2vii | 3.477 (2) | O1—Si1vi | 1.611 (6) |
Ce3—O2ii | 2.356 (6) | O2—Si2vi | 1.619 (6) |
Ce3—O1 | 2.373 (6) | O2—Ce3vi | 2.356 (6) |
Ce3—O9 | 2.379 (5) | O2—Ce1xvi | 2.450 (6) |
Ce3—O11 | 2.453 (5) | O3—Ce4iii | 2.453 (5) |
Ce3—O7ii | 2.503 (5) | O3—Ce3iv | 2.603 (5) |
Ce3—O3v | 2.603 (5) | O4—Si3iv | 1.644 (6) |
Ce3—O8ii | 2.666 (6) | O4—Si2iv | 1.678 (6) |
Ce3—O5 | 2.909 (6) | O5—Ce1vi | 2.517 (5) |
Ce3—Si3ii | 3.213 (2) | O6—Si2vi | 1.581 (6) |
Ce3—Si2 | 3.252 (2) | O6—Ce4xvii | 2.420 (5) |
Ce3—Si1vi | 3.482 (2) | O6—Ce2v | 2.426 (5) |
Ce3—Ce4viii | 3.8953 (6) | O7—Ce4xviii | 2.461 (5) |
Ce4—O6ix | 2.420 (5) | O7—Ce3vi | 2.503 (5) |
Ce4—O3x | 2.453 (5) | O8—Ce4xiv | 2.540 (6) |
Ce4—O14 | 2.459 (6) | O8—Ce2v | 2.637 (5) |
Ce4—O7xi | 2.461 (5) | O8—Ce3vi | 2.666 (6) |
Ce4—O10 | 2.476 (5) | O9—Si3iv | 1.599 (6) |
Ce4—O8xii | 2.540 (6) | O10—Ce2ii | 2.673 (5) |
Ce4—O13iv | 2.667 (5) | O11—Ce2ii | 2.541 (5) |
Ce4—Si1 | 3.243 (2) | O12—Ce2iv | 2.384 (6) |
Ce4—Si2xii | 3.413 (2) | O13—Si1v | 1.667 (6) |
Ce4—Si3xii | 3.466 (2) | O13—Ce4v | 2.667 (5) |
Ce4—Si4 | 3.467 (2) | O14—Ce1x | 2.546 (5) |
Ce4—Ce3xiii | 3.8953 (6) | O14—Ce2ii | 2.857 (5) |
Si1—O1ii | 1.611 (6) | ||
O1—Ce1—O2i | 111.20 (19) | O3x—Ce4—O10 | 150.58 (18) |
O1—Ce1—O11 | 72.20 (19) | O14—Ce4—O10 | 74.08 (17) |
O2i—Ce1—O11 | 136.00 (17) | O7xi—Ce4—O10 | 128.02 (18) |
O1—Ce1—O5ii | 82.38 (18) | O6ix—Ce4—O8xii | 89.55 (17) |
O2i—Ce1—O5ii | 150.32 (18) | O3x—Ce4—O8xii | 87.42 (17) |
O11—Ce1—O5ii | 72.54 (17) | O14—Ce4—O8xii | 70.10 (17) |
O1—Ce1—O14iii | 82.61 (19) | O7xi—Ce4—O8xii | 155.70 (19) |
O2i—Ce1—O14iii | 69.74 (17) | O10—Ce4—O8xii | 74.26 (18) |
O11—Ce1—O14iii | 149.08 (19) | O6ix—Ce4—O13iv | 73.95 (18) |
O5ii—Ce1—O14iii | 86.86 (17) | O3x—Ce4—O13iv | 149.17 (17) |
O1—Ce1—O3 | 157.26 (18) | O14—Ce4—O13iv | 131.10 (17) |
O2i—Ce1—O3 | 63.16 (18) | O7xi—Ce4—O13iv | 79.41 (17) |
O11—Ce1—O3 | 128.15 (17) | O10—Ce4—O13iv | 60.22 (17) |
O5ii—Ce1—O3 | 93.87 (17) | O8xii—Ce4—O13iv | 109.97 (17) |
O14iii—Ce1—O3 | 74.77 (17) | O6ix—Ce4—Si1 | 96.52 (14) |
O1—Ce1—O10 | 135.79 (18) | O3x—Ce4—Si1 | 176.37 (13) |
O2i—Ce1—O10 | 111.83 (17) | O14—Ce4—Si1 | 103.03 (12) |
O11—Ce1—O10 | 70.20 (17) | O7xi—Ce4—Si1 | 106.53 (13) |
O5ii—Ce1—O10 | 64.86 (17) | O10—Ce4—Si1 | 29.60 (13) |
O14iii—Ce1—O10 | 121.84 (17) | O8xii—Ce4—Si1 | 89.76 (13) |
O3—Ce1—O10 | 59.05 (17) | O13iv—Ce4—Si1 | 30.85 (12) |
O1—Ce1—O4 | 68.58 (16) | O6ix—Ce4—Si2xii | 24.71 (14) |
O2i—Ce1—O4 | 57.77 (18) | O3x—Ce4—Si2xii | 97.30 (12) |
O11—Ce1—O4 | 86.58 (16) | O14—Ce4—Si2xii | 141.66 (13) |
O5ii—Ce1—O4 | 148.43 (18) | O7xi—Ce4—Si2xii | 93.23 (14) |
O14iii—Ce1—O4 | 100.88 (16) | O10—Ce4—Si2xii | 98.43 (13) |
O3—Ce1—O4 | 117.70 (16) | O8xii—Ce4—Si2xii | 71.67 (12) |
O10—Ce1—O4 | 130.17 (15) | O13iv—Ce4—Si2xii | 66.43 (12) |
O1—Ce1—Si1 | 156.61 (13) | Si1—Ce4—Si2xii | 79.63 (5) |
O2i—Ce1—Si1 | 89.74 (14) | O6ix—Ce4—Si3xii | 75.33 (14) |
O11—Ce1—Si1 | 100.36 (13) | O3x—Ce4—Si3xii | 106.80 (12) |
O5ii—Ce1—Si1 | 74.23 (13) | O14—Ce4—Si3xii | 91.99 (13) |
O14iii—Ce1—Si1 | 95.71 (13) | O7xi—Ce4—Si3xii | 145.63 (14) |
O3—Ce1—Si1 | 29.57 (12) | O10—Ce4—Si3xii | 65.15 (13) |
O10—Ce1—Si1 | 30.17 (12) | O8xii—Ce4—Si3xii | 26.49 (13) |
O4—Ce1—Si1 | 134.16 (12) | O13iv—Ce4—Si3xii | 84.45 (12) |
O1—Ce1—Si2iv | 91.96 (13) | Si1—Ce4—Si3xii | 69.81 (5) |
O2i—Ce1—Si2iv | 27.62 (13) | Si2xii—Ce4—Si3xii | 52.42 (5) |
O11—Ce1—Si2iv | 112.45 (13) | O6ix—Ce4—Si4 | 176.55 (14) |
O5ii—Ce1—Si2iv | 171.01 (13) | O3x—Ce4—Si4 | 95.63 (13) |
O14iii—Ce1—Si2iv | 85.48 (13) | O14—Ce4—Si4 | 25.40 (13) |
O3—Ce1—Si2iv | 88.67 (12) | O7xi—Ce4—Si4 | 109.44 (14) |
O10—Ce1—Si2iv | 123.49 (12) | O10—Ce4—Si4 | 61.93 (13) |
O4—Ce1—Si2iv | 30.24 (12) | O8xii—Ce4—Si4 | 88.99 (12) |
Si1—Ce1—Si2iv | 111.23 (5) | O13iv—Ce4—Si4 | 109.49 (12) |
O1—Ce1—Si4 | 93.31 (14) | Si1—Ce4—Si4 | 86.60 (5) |
O2i—Ce1—Si4 | 110.82 (13) | Si2xii—Ce4—Si4 | 156.12 (5) |
O11—Ce1—Si4 | 28.52 (13) | Si3xii—Ce4—Si4 | 104.50 (5) |
O5ii—Ce1—Si4 | 93.89 (13) | O6ix—Ce4—Ce3xiii | 86.10 (13) |
O14iii—Ce1—Si4 | 175.72 (13) | O3x—Ce4—Ce3xiii | 41.04 (12) |
O3—Ce1—Si4 | 109.35 (12) | O14—Ce4—Ce3xiii | 91.04 (12) |
O10—Ce1—Si4 | 62.14 (12) | O7xi—Ce4—Ce3xiii | 38.69 (13) |
O4—Ce1—Si4 | 76.33 (11) | O10—Ce4—Ce3xiii | 147.41 (13) |
Si1—Ce1—Si4 | 88.54 (6) | O8xii—Ce4—Ce3xiii | 128.33 (12) |
Si2iv—Ce1—Si4 | 93.40 (5) | O13iv—Ce4—Ce3xiii | 117.96 (12) |
O1—Ce1—Ce2ii | 92.20 (14) | Si1—Ce4—Ce3xiii | 141.89 (4) |
O2i—Ce1—Ce2ii | 154.09 (13) | Si2xii—Ce4—Ce3xiii | 110.51 (4) |
O11—Ce1—Ce2ii | 40.15 (12) | Si3xii—Ce4—Ce3xiii | 145.85 (4) |
O5ii—Ce1—Ce2ii | 39.84 (12) | Si4—Ce4—Ce3xiii | 92.35 (4) |
O14iii—Ce1—Ce2ii | 126.47 (12) | O1ii—Si1—O3 | 112.4 (3) |
O3—Ce1—Ce2ii | 99.23 (11) | O1ii—Si1—O10 | 116.3 (3) |
O10—Ce1—Ce2ii | 43.65 (12) | O3—Si1—O10 | 105.6 (3) |
O4—Ce1—Ce2ii | 126.56 (11) | O1ii—Si1—O13iv | 108.9 (3) |
Si1—Ce1—Ce2ii | 69.96 (4) | O3—Si1—O13iv | 110.2 (3) |
Si2iv—Ce1—Ce2ii | 148.05 (4) | O10—Si1—O13iv | 102.9 (3) |
Si4—Ce1—Ce2ii | 54.73 (4) | O1ii—Si1—Ce4 | 122.3 (2) |
O12v—Ce2—O6iv | 86.43 (18) | O3—Si1—Ce4 | 125.3 (2) |
O12v—Ce2—O5 | 88.93 (17) | O10—Si1—Ce4 | 48.3 (2) |
O6iv—Ce2—O5 | 146.31 (18) | O13iv—Si1—Ce4 | 55.1 (2) |
O12v—Ce2—O11vi | 138.36 (18) | O1ii—Si1—Ce1 | 121.7 (2) |
O6iv—Ce2—O11vi | 90.34 (18) | O3—Si1—Ce1 | 50.6 (2) |
O5—Ce2—O11vi | 71.52 (17) | O10—Si1—Ce1 | 56.6 (2) |
O12v—Ce2—O9 | 67.85 (17) | O13iv—Si1—Ce1 | 129.4 (2) |
O6iv—Ce2—O9 | 129.34 (18) | Ce4—Si1—Ce1 | 95.14 (6) |
O5—Ce2—O9 | 78.55 (17) | O3—Si1—Ce3ii | 105.4 (2) |
O11vi—Ce2—O9 | 137.77 (17) | O10—Si1—Ce3ii | 86.3 (2) |
O12v—Ce2—O8iv | 103.47 (18) | O13iv—Si1—Ce3ii | 138.8 (2) |
O6iv—Ce2—O8iv | 86.80 (18) | Ce4—Si1—Ce3ii | 116.72 (6) |
O5—Ce2—O8iv | 126.64 (18) | Ce1—Si1—Ce3ii | 89.37 (5) |
O11vi—Ce2—O8iv | 117.79 (17) | O6ii—Si2—O2ii | 113.5 (3) |
O9—Ce2—O8iv | 60.17 (17) | O6ii—Si2—O5 | 115.5 (3) |
O12v—Ce2—O10vi | 134.65 (17) | O2ii—Si2—O5 | 106.1 (3) |
O6iv—Ce2—O10vi | 135.40 (18) | O6ii—Si2—O4v | 107.8 (3) |
O5—Ce2—O10vi | 65.56 (16) | O2ii—Si2—O4v | 100.7 (3) |
O11vi—Ce2—O10vi | 70.20 (18) | O5—Si2—O4v | 112.4 (3) |
O9—Ce2—O10vi | 70.58 (16) | O6ii—Si2—Ce3 | 125.7 (2) |
O8iv—Ce2—O10vi | 69.54 (17) | O5—Si2—Ce3 | 63.3 (2) |
O12v—Ce2—O7 | 74.64 (17) | O4v—Si2—Ce3 | 123.0 (2) |
O6iv—Ce2—O7 | 66.84 (17) | O6ii—Si2—Ce1v | 127.3 (2) |
O5—Ce2—O7 | 79.75 (17) | O5—Si2—Ce1v | 116.8 (2) |
O11vi—Ce2—O7 | 66.06 (17) | O4v—Si2—Ce1v | 56.4 (2) |
O9—Ce2—O7 | 136.61 (18) | Ce3—Si2—Ce1v | 74.89 (5) |
O8iv—Ce2—O7 | 153.61 (16) | O2ii—Si2—Ce4xiv | 121.3 (2) |
O10vi—Ce2—O7 | 130.70 (16) | O5—Si2—Ce4xiv | 132.0 (2) |
O12v—Ce2—O14vi | 153.34 (17) | O4v—Si2—Ce4xiv | 68.0 (2) |
O6iv—Ce2—O14vi | 70.69 (16) | Ce3—Si2—Ce4xiv | 159.43 (7) |
O5—Ce2—O14vi | 117.70 (16) | Ce1v—Si2—Ce4xiv | 102.91 (6) |
O11vi—Ce2—O14vi | 57.80 (16) | O2ii—Si2—Ce2xv | 81.5 (2) |
O9—Ce2—O14vi | 116.35 (16) | O5—Si2—Ce2xv | 109.2 (2) |
O8iv—Ce2—O14vi | 62.88 (16) | O4v—Si2—Ce2xv | 135.8 (2) |
O10vi—Ce2—O14vi | 64.95 (16) | Ce3—Si2—Ce2xv | 88.95 (5) |
O7—Ce2—O14vi | 106.99 (17) | Ce1v—Si2—Ce2xv | 115.33 (6) |
O12v—Ce2—Si3iv | 84.29 (13) | Ce4xiv—Si2—Ce2xv | 73.34 (4) |
O6iv—Ce2—Si3iv | 109.39 (14) | O9v—Si3—O7 | 114.4 (3) |
O5—Ce2—Si3iv | 103.30 (14) | O9v—Si3—O4v | 111.7 (3) |
O11vi—Ce2—Si3iv | 135.11 (13) | O7—Si3—O4v | 109.3 (3) |
O9—Ce2—Si3iv | 29.55 (13) | O9v—Si3—O8 | 108.1 (3) |
O8iv—Ce2—Si3iv | 30.63 (12) | O7—Si3—O8 | 105.8 (3) |
O10vi—Ce2—Si3iv | 67.56 (12) | O4v—Si3—O8 | 107.1 (3) |
O7—Ce2—Si3iv | 158.71 (12) | O9v—Si3—Ce3vi | 131.5 (2) |
O14vi—Ce2—Si3iv | 90.42 (12) | O7—Si3—Ce3vi | 50.16 (19) |
O12v—Ce2—Si4vi | 161.09 (13) | O4v—Si3—Ce3vi | 116.7 (2) |
O6iv—Ce2—Si4vi | 81.06 (14) | O8—Si3—Ce3vi | 55.9 (2) |
O5—Ce2—Si4vi | 93.63 (12) | O9v—Si3—Ce2v | 53.4 (2) |
O11vi—Ce2—Si4vi | 28.75 (13) | O7—Si3—Ce2v | 124.0 (2) |
O9—Ce2—Si4vi | 131.01 (12) | O4v—Si3—Ce2v | 126.3 (2) |
O8iv—Ce2—Si4vi | 90.00 (12) | O8—Si3—Ce2v | 54.78 (19) |
O10vi—Ce2—Si4vi | 62.43 (12) | Ce3vi—Si3—Ce2v | 94.38 (6) |
O7—Ce2—Si4vi | 87.37 (12) | O9v—Si3—Ce4xiv | 109.0 (2) |
O14vi—Ce2—Si4vi | 29.15 (11) | O7—Si3—Ce4xiv | 133.8 (2) |
Si3iv—Ce2—Si4vi | 113.20 (5) | O4v—Si3—Ce4xiv | 66.5 (2) |
O12v—Ce2—Si2vii | 81.15 (14) | Ce3vi—Si3—Ce4xiv | 88.93 (5) |
O6iv—Ce2—Si2vii | 23.44 (13) | Ce2v—Si3—Ce4xiv | 71.89 (4) |
O5—Ce2—Si2vii | 165.65 (13) | O12—Si4—O14 | 116.6 (3) |
O11vi—Ce2—Si2vii | 109.51 (13) | O12—Si4—O11 | 108.0 (3) |
O9—Ce2—Si2vii | 106.85 (12) | O14—Si4—O11 | 105.7 (3) |
O8iv—Ce2—Si2vii | 66.27 (13) | O12—Si4—O13 | 111.9 (3) |
O10vi—Ce2—Si2vii | 128.65 (12) | O14—Si4—O13 | 107.7 (3) |
O7—Ce2—Si2vii | 87.60 (12) | O11—Si4—O13 | 106.3 (3) |
O14vi—Ce2—Si2vii | 72.41 (12) | O12—Si4—Ce1 | 63.7 (2) |
Si3iv—Ce2—Si2vii | 86.10 (5) | O14—Si4—Ce1 | 116.1 (2) |
Si4vi—Ce2—Si2vii | 92.52 (5) | O11—Si4—Ce1 | 45.7 (2) |
O2ii—Ce3—O1 | 142.72 (19) | O13—Si4—Ce1 | 132.5 (2) |
O2ii—Ce3—O9 | 105.33 (18) | O12—Si4—Ce2ii | 123.9 (2) |
O1—Ce3—O9 | 80.01 (18) | O14—Si4—Ce2ii | 58.5 (2) |
O2ii—Ce3—O11 | 142.66 (19) | O11—Si4—Ce2ii | 47.47 (19) |
O1—Ce3—O11 | 73.43 (19) | O13—Si4—Ce2ii | 122.9 (2) |
O9—Ce3—O11 | 86.83 (18) | Ce1—Si4—Ce2ii | 70.71 (4) |
O2ii—Ce3—O7ii | 87.76 (18) | O12—Si4—Ce4 | 78.1 (2) |
O1—Ce3—O7ii | 102.43 (18) | O11—Si4—Ce4 | 109.3 (2) |
O9—Ce3—O7ii | 155.22 (19) | O13—Si4—Ce4 | 137.5 (2) |
O11—Ce3—O7ii | 70.66 (18) | Ce1—Si4—Ce4 | 89.55 (5) |
O2ii—Ce3—O3v | 63.60 (17) | Ce2ii—Si4—Ce4 | 70.36 (4) |
O1—Ce3—O3v | 153.66 (18) | Si1vi—O1—Ce3 | 120.6 (3) |
O9—Ce3—O3v | 94.60 (17) | Si1vi—O1—Ce1 | 124.0 (3) |
O11—Ce3—O3v | 80.57 (17) | Ce3—O1—Ce1 | 109.5 (2) |
O7ii—Ce3—O3v | 72.14 (17) | Si2vi—O2—Ce3vi | 108.4 (3) |
O2ii—Ce3—O8ii | 75.40 (18) | Si2vi—O2—Ce1xvi | 107.8 (3) |
O1—Ce3—O8ii | 78.69 (17) | Ce3vi—O2—Ce1xvi | 112.6 (2) |
O9—Ce3—O8ii | 142.40 (17) | Si1—O3—Ce4iii | 128.9 (3) |
O11—Ce3—O8ii | 115.81 (17) | Si1—O3—Ce1 | 99.8 (2) |
O7ii—Ce3—O8ii | 60.73 (18) | Ce4iii—O3—Ce1 | 103.53 (19) |
O3v—Ce3—O8ii | 117.50 (16) | Si1—O3—Ce3iv | 118.1 (3) |
O2ii—Ce3—O5 | 57.79 (17) | Ce4iii—O3—Ce3iv | 100.74 (18) |
O1—Ce3—O5 | 89.70 (17) | Ce1—O3—Ce3iv | 101.74 (18) |
O9—Ce3—O5 | 74.91 (16) | Si3iv—O4—Si2iv | 132.3 (4) |
O11—Ce3—O5 | 157.15 (17) | Si3iv—O4—Ce1 | 130.6 (3) |
O7ii—Ce3—O5 | 129.37 (17) | Si2iv—O4—Ce1 | 93.4 (2) |
O3v—Ce3—O5 | 113.96 (16) | Si2—O5—Ce1vi | 125.7 (3) |
O8ii—Ce3—O5 | 74.37 (16) | Si2—O5—Ce2 | 122.7 (3) |
O2ii—Ce3—Si3ii | 82.32 (14) | Ce1vi—O5—Ce2 | 100.41 (18) |
O1—Ce3—Si3ii | 88.93 (13) | Si2—O5—Ce3 | 86.9 (2) |
O9—Ce3—Si3ii | 168.76 (13) | Ce1vi—O5—Ce3 | 121.6 (2) |
O11—Ce3—Si3ii | 91.92 (13) | Ce2—O5—Ce3 | 96.84 (18) |
O7ii—Ce3—Si3ii | 30.12 (13) | Si2vi—O6—Ce4xvii | 115.5 (3) |
O3v—Ce3—Si3ii | 96.21 (12) | Si2vi—O6—Ce2v | 118.9 (3) |
O8ii—Ce3—Si3ii | 30.73 (12) | Ce4xvii—O6—Ce2v | 116.3 (2) |
O5—Ce3—Si3ii | 103.30 (12) | Si3—O7—Ce4xviii | 115.9 (3) |
O2ii—Ce3—Si2 | 28.20 (14) | Si3—O7—Ce3vi | 99.7 (2) |
O1—Ce3—Si2 | 116.46 (14) | Ce4xviii—O7—Ce3vi | 103.4 (2) |
O9—Ce3—Si2 | 93.10 (13) | Si3—O7—Ce2 | 122.6 (3) |
O11—Ce3—Si2 | 169.96 (13) | Ce4xviii—O7—Ce2 | 105.31 (19) |
O7ii—Ce3—Si2 | 107.23 (14) | Ce3vi—O7—Ce2 | 107.9 (2) |
O3v—Ce3—Si2 | 89.43 (12) | Si3—O8—Ce4xiv | 110.0 (3) |
O8ii—Ce3—Si2 | 69.70 (12) | Si3—O8—Ce2v | 94.6 (2) |
O5—Ce3—Si2 | 29.87 (11) | Ce4xiv—O8—Ce2v | 98.72 (18) |
Si3ii—Ce3—Si2 | 90.07 (5) | Si3—O8—Ce3vi | 93.3 (2) |
O2ii—Ce3—Si1vi | 122.02 (14) | Ce4xiv—O8—Ce3vi | 128.1 (2) |
O1—Ce3—Si1vi | 23.46 (14) | Ce2v—O8—Ce3vi | 125.7 (2) |
O9—Ce3—Si1vi | 72.25 (13) | Si3iv—O9—Ce3 | 140.2 (3) |
O11—Ce3—Si1vi | 95.26 (13) | Si3iv—O9—Ce2 | 97.1 (2) |
O7ii—Ce3—Si1vi | 118.79 (13) | Ce3—O9—Ce2 | 109.54 (19) |
O3v—Ce3—Si1vi | 166.49 (12) | Si1—O10—Ce4 | 102.1 (3) |
O8ii—Ce3—Si1vi | 75.92 (12) | Si1—O10—Ce2ii | 144.3 (3) |
O5—Ce3—Si1vi | 66.40 (11) | Ce4—O10—Ce2ii | 99.37 (18) |
Si3ii—Ce3—Si1vi | 96.77 (5) | Si1—O10—Ce1 | 93.2 (2) |
Si2—Ce3—Si1vi | 94.28 (5) | Ce4—O10—Ce1 | 134.5 (2) |
O2ii—Ce3—Ce4viii | 60.48 (13) | Ce2ii—O10—Ce1 | 91.68 (17) |
O1—Ce3—Ce4viii | 140.16 (13) | Si4—O11—Ce3 | 123.9 (3) |
O9—Ce3—Ce4viii | 132.82 (13) | Si4—O11—Ce1 | 105.8 (3) |
O11—Ce3—Ce4viii | 85.14 (13) | Ce3—O11—Ce1 | 104.7 (2) |
O7ii—Ce3—Ce4viii | 37.93 (12) | Si4—O11—Ce2ii | 103.8 (3) |
O3v—Ce3—Ce4viii | 38.22 (12) | Ce3—O11—Ce2ii | 115.2 (2) |
O8ii—Ce3—Ce4viii | 81.22 (12) | Ce1—O11—Ce2ii | 100.78 (18) |
O5—Ce3—Ce4viii | 117.33 (10) | Si4—O12—Ce2iv | 137.7 (3) |
Si3ii—Ce3—Ce4viii | 58.05 (4) | Si1v—O13—Si4 | 129.1 (3) |
Si2—Ce3—Ce4viii | 87.56 (4) | Si1v—O13—Ce4v | 94.0 (2) |
Si1vi—Ce3—Ce4viii | 154.79 (4) | Si4—O13—Ce4v | 136.8 (3) |
O6ix—Ce4—O3x | 81.19 (18) | Si4—O14—Ce4 | 114.4 (3) |
O6ix—Ce4—O14 | 151.42 (17) | Si4—O14—Ce1x | 119.6 (3) |
O3x—Ce4—O14 | 78.14 (17) | Ce4—O14—Ce1x | 103.55 (19) |
O6ix—Ce4—O7xi | 71.13 (19) | Si4—O14—Ce2ii | 92.4 (2) |
O3x—Ce4—O7xi | 75.46 (18) | Ce4—O14—Ce2ii | 94.99 (17) |
O14—Ce4—O7xi | 121.39 (18) | Ce1x—O14—Ce2ii | 130.0 (2) |
O6ix—Ce4—O10 | 120.60 (19) |
Symmetry codes: (i) −x, −y+1, z−1/2; (ii) y, −x, z−1/4; (iii) x−1, y, z; (iv) y, −x+1, z−1/4; (v) −y+1, x, z+1/4; (vi) −y, x, z+1/4; (vii) x, y+1, z; (viii) −y+1, x−1, z+1/4; (ix) −y+1, x, z−3/4; (x) x+1, y, z; (xi) −x+1, −y+1, z−1/2; (xii) −x+1, −y, z−1/2; (xiii) y+1, −x+1, z−1/4; (xiv) −x+1, −y, z+1/2; (xv) x, y−1, z; (xvi) −x, −y+1, z+1/2; (xvii) y, −x+1, z+3/4; (xviii) −x+1, −y+1, z+1/2. |