Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520618012271/lo5031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520618012271/lo5031Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520618012271/lo5031sup3.pdf |
CCDC reference: 1864463
Data collection: Wojdyla, J. A.; Kaminski, J. W.; Panepucci, E.; Ebner, S.; Wang, X.; Gabadinho, J. & Wang, M. DA+ data acquisition and analysis software at the Swiss Light Source macromolecular crystallography beamlines Journal of Synchroton Radiation, 2018, 25 doi:10.1107/S1600577517014503; cell refinement: CrysAlis PRO 1.171.38.43 (Rigaku OD, 2015); data reduction: XDS Version 2016-11-01 Kabsch, W. Integration, scaling, space-group assignment and post refinement Acta Crystallographica, 2010, D66, 133-144; program(s) used to solve structure: SIR2004, Burla et al. 2005; program(s) used to refine structure: Jana2006 Version: 6/5/2017; molecular graphics: Vesta 3.
C0.919Ba2Ca17.621F3.462Na0.379O39.7P2.96Si6 | F(000) = 2854 |
Mr = 1961.8 | Dx = 3.353 Mg m−3 |
Trigonal, R3m | Cell parameters from 2944 reflections |
Hall symbol: -R 3;-2 | θ = 2.8–32.0° |
a = 7.12550 (11) Å | µ = 4.70 mm−1 |
c = 66.2902 (13) Å | T = 293 K |
V = 2914.81 (8) Å3 | Prism, black |
Z = 3 | 0.06 × 0.03 × 0.03 mm |
PRIGo diffractometer | 1291 independent reflections |
Radiation source: SLS super-bending magnet 2.9T, X06DA | 1145 reflections with I > 3σ(I) |
Bartels Monochromator with dual channel cut crystals (DCCM) in (±∓) geometry monochromator | Rint = 0.049 |
Detector resolution: 5.81 pixels mm-1 | θmax = 32.0°, θmin = 0.9° |
φ scans | h = −8→9 |
Absorption correction: empirical (using intensity measurements) XDS Version 2016-11-01 Kabsch, W. Integration, scaling, space-group assignment and post refinement Acta Crystallographica, 2010, D66, 133-144 | k = −10→6 |
l = −84→96 | |
5677 measured reflections |
Refinement on F2 | 0 restraints |
R[F2 > 2σ(F2)] = 0.082 | 0 constraints |
wR(F2) = 0.184 | Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0004I2) |
S = 3.60 | (Δ/σ)max = 0.049 |
1291 reflections | Δρmax = 12.08 e Å−3 |
85 parameters | Δρmin = −2.45 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ba1 | 0 | 0 | 0.270337 (10) | 0.0140 (3) | |
Ca1 | 0.49749 (8) | 0.99499 (16) | 0.23253 (2) | 0.0066 (4) | |
Ca2 | 0.98845 (19) | 0.49422 (9) | 0.30918 (2) | 0.0086 (4) | |
Ca3 | 0.48954 (9) | 0.97909 (18) | 0.146883 (19) | 0.0058 (4) | 0.937 (12) |
Na3 | 0.48954 (9) | 0.97909 (18) | 0.146883 (19) | 0.0058 (4) | 0.063 (12) |
T1 | 0.666667 | 0.333333 | 0.19130 (4) | 0.0022 (5) | |
T2 | 0.333333 | 0.666667 | 0.34596 (4) | 0.0015 (5)* | |
T3 | 0 | 0 | 0.21838 (4) | 0.0022 (5) | |
T4 | 0.666667 | 0.333333 | 0.26572 (5) | 0.0063 (8) | 0.940 (12) |
T5p | 0.333333 | 0.666667 | 0.27450 (7) | 0.0071 (13)* | 0.54 (2) |
T5c | 0.333333 | 0.666667 | 0.27450 (7) | 0.0071 (13)* | 0.46 (2) |
O1 | 0.2223 (4) | 0.7777 (4) | 0.28273 (8) | 0.017 (2) | 0.865 (14) |
O2 | 0.333333 | 0.666667 | 0.25243 (12) | 0.012 (2) | |
O3 | 0.4578 (4) | 0.9155 (7) | 0.35310 (8) | 0.0193 (16) | |
O4 | 0.666667 | 0.333333 | 0.28903 (12) | 0.0103 (19) | |
O5 | 0.5421 (3) | 0.0842 (7) | 0.18354 (7) | 0.0101 (8)* | |
O6 | 0.333333 | 0.666667 | 0.32173 (13) | 0.018 (2) | |
O7 | 0.666667 | 0.333333 | 0.21597 (11) | 0.0088 (19) | |
O8 | 0.7482 (6) | 0.8741 (3) | 0.22475 (7) | 0.0111 (14) | |
O9 | 0.7834 (3) | 0.2166 (3) | 0.25706 (6) | 0.0114 (14) | |
O10 | 0 | 0 | 0.19203 (11) | 0.0031* | |
O11 | 0.333333 | 0.666667 | 0.166667 | 0.002 (2)* | 0.53 (16) |
F1 | 0.333333 | 0.666667 | 0.166667 | 0.002 (2)* | 0.47 (16) |
F2 | 0.666667 | 0.333333 | 0.333333 | 0.013 (2) | |
F3 | 0.333333 | 0.666667 | 0.12406 (10) | 0.0082 (18) | 0.993 (19) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.0142 (3) | 0.0142 (3) | 0.0135 (4) | 0.00711 (16) | 0 | 0 |
Ca1 | 0.0017 (5) | 0.0015 (6) | 0.0164 (7) | 0.0008 (3) | −0.0007 (2) | −0.0014 (4) |
Ca2 | 0.0033 (6) | 0.0028 (5) | 0.0201 (8) | 0.0016 (3) | −0.0010 (4) | −0.0005 (2) |
Ca3 | 0.0023 (5) | 0.0034 (6) | 0.0119 (7) | 0.0017 (3) | 0.0006 (2) | 0.0012 (4) |
Na3 | 0.0023 (5) | 0.0034 (6) | 0.0119 (7) | 0.0017 (3) | 0.0006 (2) | 0.0012 (4) |
T1 | 0.0003 (5) | 0.0003 (5) | 0.0058 (9) | 0.0002 (3) | 0 | 0 |
T3 | 0.0003 (5) | 0.0003 (5) | 0.0058 (9) | 0.0002 (3) | 0 | 0 |
T4 | 0.0069 (10) | 0.0069 (10) | 0.0051 (14) | 0.0035 (5) | 0 | 0 |
O1 | 0.022 (2) | 0.022 (2) | 0.010 (3) | 0.013 (2) | −0.0006 (10) | 0.0006 (10) |
O2 | 0.014 (2) | 0.014 (2) | 0.008 (4) | 0.0072 (12) | 0 | 0 |
O3 | 0.0065 (15) | 0.0035 (19) | 0.047 (3) | 0.0017 (10) | −0.0052 (10) | −0.010 (2) |
O4 | 0.013 (2) | 0.013 (2) | 0.005 (4) | 0.0066 (11) | 0 | 0 |
O6 | 0.021 (3) | 0.021 (3) | 0.012 (4) | 0.0104 (14) | 0 | 0 |
O7 | 0.009 (2) | 0.009 (2) | 0.008 (4) | 0.0046 (11) | 0 | 0 |
O8 | 0.0023 (18) | 0.0063 (14) | 0.023 (3) | 0.0011 (9) | 0.0020 (16) | 0.0010 (8) |
O9 | 0.0129 (15) | 0.0129 (15) | 0.012 (2) | 0.0092 (18) | −0.0013 (8) | 0.0013 (8) |
F2 | 0.016 (3) | 0.016 (3) | 0.007 (4) | 0.0079 (14) | 0 | 0 |
F3 | 0.008 (2) | 0.008 (2) | 0.009 (3) | 0.0038 (10) | 0 | 0 |
Ba1—T2i | 3.339 (3) | T1—O5xii | 1.621 (5) |
Ba1—T3 | 3.444 (3) | T1—O7 | 1.636 (8) |
Ba1—O1ii | 2.864 (4) | T1—O10xxii | 3.314 (8) |
Ba1—O1iii | 2.864 (4) | T2—O3 | 1.607 (5) |
Ba1—O1iv | 2.864 (4) | T2—O3iii | 1.607 (5) |
Ba1—O3i | 3.251 (5) | T2—O3ix | 1.607 (5) |
Ba1—O3v | 3.251 (5) | T2—O6 | 1.606 (9) |
Ba1—O3vi | 3.251 (6) | T3—O8vii | 1.610 (4) |
Ba1—O8vii | 3.398 (5) | T3—O8viii | 1.610 (5) |
Ba1—O8viii | 3.398 (5) | T3—O8ix | 1.610 (4) |
Ba1—O8ix | 3.398 (5) | T3—O10 | 1.747 (7) |
Ba1—O9x | 2.815 (3) | T4—O4 | 1.545 (8) |
Ba1—O9xi | 2.815 (3) | T4—O7 | 3.298 (8) |
Ba1—O9xii | 2.815 (3) | T4—O9 | 1.551 (3) |
Ca1—T1xiii | 3.439 (3) | T4—O9viii | 1.551 (3) |
Ca1—T4xiii | 3.033 (2) | T4—O9xii | 1.551 (3) |
Ca1—T5p | 3.442 (4) | T5p—T5c | 0 |
Ca1—T5c | 3.442 (4) | T5p—O1 | 1.475 (4) |
Ca1—O2 | 2.418 (4) | T5p—O1iii | 1.475 (4) |
Ca1—O5xiii | 3.294 (5) | T5p—O1ix | 1.475 (4) |
Ca1—O7xiii | 2.359 (4) | T5p—O2 | 1.463 (9) |
Ca1—O8 | 2.395 (5) | T5p—O6 | 3.130 (10) |
Ca1—O8iii | 2.395 (3) | T5c—O1 | 1.475 (4) |
Ca1—O9xiii | 2.464 (3) | T5c—O1iii | 1.475 (4) |
Ca1—O9xiv | 2.464 (4) | T5c—O1ix | 1.475 (4) |
Ca1—F3xv | 2.546 (4) | T5c—O2 | 1.463 (9) |
Ca2—Ca2viii | 3.4393 (17) | T5c—O6 | 3.130 (10) |
Ca2—Ca2xii | 3.4393 (12) | O1—O1iii | 2.373 (6) |
Ca2—T2xvi | 3.236 (2) | O1—O1ix | 2.373 (6) |
Ca2—T4 | 3.499 (3) | O1—O2 | 2.431 (8) |
Ca2—T5pxvi | 3.133 (3) | O1—O3xxiv | 3.139 (6) |
Ca2—T5cxvi | 3.133 (3) | O1—O3xxv | 3.139 (7) |
Ca2—O1xvi | 2.563 (4) | O1—O6 | 2.926 (9) |
Ca2—O1xvii | 2.563 (5) | O1—O9xxvi | 3.199 (5) |
Ca2—O3xvii | 2.971 (6) | O1—O9xiv | 3.199 (5) |
Ca2—O3xviii | 2.357 (7) | O2—O8 | 3.150 (6) |
Ca2—O3xix | 2.357 (6) | O2—O8iii | 3.150 (7) |
Ca2—O4 | 2.393 (4) | O2—O8ix | 3.150 (6) |
Ca2—O6xvi | 2.285 (3) | O2—F3xv | 2.861 (10) |
Ca2—F2 | 2.5507 (12) | O3—O3iii | 2.660 (5) |
Ca3—Ca3iii | 3.3392 (12) | O3—O3ix | 2.660 (7) |
Ca3—Ca3ix | 3.3392 (16) | O3—O4xxvii | 3.048 (6) |
Ca3—Ca3xv | 3.2552 (18) | O3—O6 | 2.585 (9) |
Ca3—Ca3xx | 3.2552 (15) | O3—F2xiii | 2.892 (5) |
Ca3—Na3 | 0 | O4—O9 | 2.563 (7) |
Ca3—Na3iii | 3.3392 (12) | O4—O9viii | 2.563 (7) |
Ca3—Na3ix | 3.3392 (16) | O4—O9xii | 2.563 (7) |
Ca3—Na3xv | 3.2552 (18) | O4—F2 | 2.937 (8) |
Ca3—Na3xx | 3.2552 (15) | O5—O5viii | 2.663 (5) |
Ca3—T3xxi | 3.043 (2) | O5—O5xii | 2.663 (6) |
Ca3—O5xiii | 2.515 (5) | O5—O5xxviii | 3.412 (7) |
Ca3—O5xxii | 2.329 (5) | O5—O5xx | 3.412 (5) |
Ca3—O5xxiii | 2.329 (3) | O5—O7 | 2.643 (7) |
Ca3—O8xv | 2.616 (5) | O5—O10xxii | 3.194 (7) |
Ca3—O10xxi | 2.2170 (16) | O5—O11ii | 2.809 (4) |
Ca3—O11 | 2.3317 (12) | O5—F1ii | 2.809 (4) |
Ca3—F1 | 2.3317 (12) | O5—F3xxix | 3.090 (6) |
Ca3—F3 | 2.451 (4) | O7—O9 | 3.081 (8) |
Na3—Na3iii | 3.3392 (12) | O7—O9viii | 3.081 (8) |
Na3—Na3ix | 3.3392 (16) | O7—O9xii | 3.081 (8) |
Na3—Na3xv | 3.2552 (18) | O8—O8xvii | 2.691 (6) |
Na3—Na3xx | 3.2552 (15) | O8—O8xiv | 2.691 (4) |
Na3—T3xxi | 3.043 (2) | O8—O9xiii | 3.162 (5) |
Na3—O5xiii | 2.515 (5) | O8—O9viii | 3.162 (6) |
Na3—O5xxii | 2.329 (5) | O8—O10xxx | 2.668 (7) |
Na3—O5xxiii | 2.329 (3) | O8—F3xv | 2.758 (5) |
Na3—O8xv | 2.616 (5) | O9—O9viii | 2.495 (5) |
Na3—O10xxi | 2.2170 (16) | O9—O9xii | 2.495 (5) |
Na3—O11 | 2.3317 (12) | O11—F1 | 0 |
Na3—F1 | 2.3317 (12) | O11—F3 | 2.825 (6) |
Na3—F3 | 2.451 (4) | O11—F3xv | 2.825 (6) |
T1—O5 | 1.621 (4) | F1—F3 | 2.825 (6) |
T1—O5viii | 1.621 (4) | F1—F3xv | 2.825 (6) |
Symmetry codes: (i) y−2/3, x−1/3, −z+2/3; (ii) x, y−1, z; (iii) −y+1, x−y+1, z; (iv) −x+y−1, −x, z; (v) x−y+1/3, −y+2/3, −z+2/3; (vi) −x+1/3, −x+y−1/3, −z+2/3; (vii) x−1, y−1, z; (viii) −y+1, x−y, z; (ix) −x+y, −x+1, z; (x) x−1, y, z; (xi) −y, x−y−1, z; (xii) −x+y+1, −x+1, z; (xiii) x, y+1, z; (xiv) −x+y+1, −x+2, z; (xv) y−1/3, x+1/3, −z+1/3; (xvi) x+1, y, z; (xvii) −y+2, x−y+1, z; (xviii) x−y+4/3, −y+5/3, −z+2/3; (xix) −x+4/3, −x+y−1/3, −z+2/3; (xx) −x+2/3, −x+y+1/3, −z+1/3; (xxi) y+2/3, x+4/3, −z+1/3; (xxii) y+2/3, x+1/3, −z+1/3; (xxiii) −x+2/3, −x+y+4/3, −z+1/3; (xxiv) y−2/3, x+2/3, −z+2/3; (xxv) x−y+1/3, −y+5/3, −z+2/3; (xxvi) −y, x−y, z; (xxvii) y+1/3, x+2/3, −z+2/3; (xxviii) y+2/3, x−2/3, −z+1/3; (xxix) y−1/3, x−2/3, −z+1/3; (xxx) x+1, y+1, z. |