Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106025900/ck5016sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025900/ck50166-foldsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025900/ck50165-foldsup3.hkl |
For both compounds, data collection: X-AREA (Stoe, 2002); cell refinement: FullProf Suite (Rodriguez-Carvajal); data reduction: X-RED (Stoe, 1996); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS Version 5.1; software used to prepare material for publication: WinGX 1.64.05 (Farrugia, 1999).
AlSiCa | Dx = 2.383 Mg m−3 Dm = 2.383 Mg m−3 Dm measured by not measured |
Mr = 95.15 | Melting point: 0 K |
Hexagonal, P6m2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P -6 2 | Cell parameters from 23 reflections |
a = 4.17720 (4) Å | θ = 10.1–47.2° |
c = 26.3246 (4) Å | µ = 2.76 mm−1 |
V = 397.80 (1) Å3 | T = 298 K |
Z = 6 | Cuboid, metallic dark grey |
F(000) = 282 | 0.18 × 0.16 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 233 reflections with I > 2σ(I) |
rotation method scans | Rint = 0.049 |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | θmax = 27.1°, θmin = 1.6° |
Tmin = 0.557, Tmax = 0.660 | h = −5→5 |
3136 measured reflections | k = −5→5 |
429 independent reflections | l = −33→33 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.013P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.03 | (Δ/σ)max < 0.001 |
wR(F2) = 0.082 | Δρmax = 0.25 e Å−3 |
S = 1.96 | Δρmin = −0.29 e Å−3 |
429 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
31 parameters | Absolute structure parameter: 0.1 (3) |
0 restraints |
AlSiCa | Z = 6 |
Mr = 95.15 | Mo Kα radiation |
Hexagonal, P6m2 | µ = 2.76 mm−1 |
a = 4.17720 (4) Å | T = 298 K |
c = 26.3246 (4) Å | 0.18 × 0.16 × 0.15 × 0 (radius) mm |
V = 397.80 (1) Å3 |
STOE IPDS 2 diffractometer | 429 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 233 reflections with I > 2σ(I) |
Tmin = 0.557, Tmax = 0.660 | Rint = 0.049 |
3136 measured reflections |
R[F2 > 2σ(F2)] = 0.03 | 0 restraints |
wR(F2) = 0.082 | Δρmax = 0.25 e Å−3 |
S = 1.96 | Δρmin = −0.29 e Å−3 |
429 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
31 parameters | Absolute structure parameter: 0.1 (3) |
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 | Occ. (<1) | |
Ca1 | 0 | 0 | 0.08205 (12) | 0.0160 (6) | |
Ca2 | 0 | 0 | 0.24927 (15) | 0.0151 (6) | |
Ca3 | 0 | 0 | 0.41729 (14) | 0.0172 (7) | |
SI1 | 0.3333 | 0.6667 | 0 | 0.038 (2) | 0.5 |
SI2 | 0.6667 | 0.3333 | 0 | 0.0147 (14) | 0.5 |
SI3 | 0.3333 | 0.6667 | 0.1605 (2) | 0.0217 (12) | 0.5 |
SI4 | 0.6667 | 0.3333 | 0.17111 (19) | 0.0145 (12) | 0.5 |
SI5 | 0.3333 | 0.6667 | 0.32802 (15) | 0.0128 (10) | 0.5 |
SI6 | 0.6667 | 0.3333 | 0.3412 (2) | 0.0219 (11) | 0.5 |
SI7 | 0.3333 | 0.6667 | 0.5 | 0.0084 (11) | 0.5 |
SI8 | 0.6667 | 0.3333 | 0.5 | 0.039 (3) | 0.5 |
AL1 | 0.3333 | 0.6667 | 0 | 0.038 (2) | 0.5 |
AL2 | 0.6667 | 0.3333 | 0 | 0.0147 (14) | 0.5 |
AL3 | 0.3333 | 0.6667 | 0.1605 (2) | 0.0217 (12) | 0.5 |
AL4 | 0.6667 | 0.3333 | 0.17111 (19) | 0.0145 (12) | 0.5 |
AL5 | 0.3333 | 0.6667 | 0.32802 (15) | 0.0128 (10) | 0.5 |
AL6 | 0.6667 | 0.3333 | 0.3412 (2) | 0.0219 (11) | 0.5 |
AL7 | 0.3333 | 0.6667 | 0.5 | 0.0084 (11) | 0.5 |
AL8 | 0.6667 | 0.3333 | 0.5 | 0.039 (3) | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ca1 | 0.0189 (9) | 0.0189 (9) | 0.0104 (11) | 0.0094 (5) | 0 | 0 |
Ca2 | 0.0158 (8) | 0.0158 (8) | 0.0139 (10) | 0.0079 (4) | 0 | 0 |
Ca3 | 0.0156 (9) | 0.0156 (9) | 0.0202 (14) | 0.0078 (5) | 0 | 0 |
SI1 | 0.0141 (19) | 0.0141 (19) | 0.086 (7) | 0.0071 (10) | 0 | 0 |
SI2 | 0.0130 (18) | 0.0130 (18) | 0.018 (3) | 0.0065 (9) | 0 | 0 |
SI3 | 0.0168 (14) | 0.0168 (14) | 0.032 (3) | 0.0084 (7) | 0 | 0 |
SI4 | 0.0073 (12) | 0.0073 (12) | 0.029 (3) | 0.0036 (6) | 0 | 0 |
SI5 | 0.0115 (13) | 0.0115 (13) | 0.015 (2) | 0.0057 (7) | 0 | 0 |
SI6 | 0.0127 (12) | 0.0127 (12) | 0.040 (3) | 0.0063 (6) | 0 | 0 |
SI7 | 0.0048 (15) | 0.0048 (15) | 0.015 (3) | 0.0024 (7) | 0 | 0 |
SI8 | 0.0088 (18) | 0.0088 (18) | 0.101 (8) | 0.0044 (9) | 0 | 0 |
AL1 | 0.0141 (19) | 0.0141 (19) | 0.086 (7) | 0.0071 (10) | 0 | 0 |
AL2 | 0.0130 (18) | 0.0130 (18) | 0.018 (3) | 0.0065 (9) | 0 | 0 |
AL3 | 0.0168 (14) | 0.0168 (14) | 0.032 (3) | 0.0084 (7) | 0 | 0 |
AL4 | 0.0073 (12) | 0.0073 (12) | 0.029 (3) | 0.0036 (6) | 0 | 0 |
AL5 | 0.0115 (13) | 0.0115 (13) | 0.015 (2) | 0.0057 (7) | 0 | 0 |
AL6 | 0.0127 (12) | 0.0127 (12) | 0.040 (3) | 0.0063 (6) | 0 | 0 |
AL7 | 0.0048 (15) | 0.0048 (15) | 0.015 (3) | 0.0024 (7) | 0 | 0 |
AL8 | 0.0088 (18) | 0.0088 (18) | 0.101 (8) | 0.0044 (9) | 0 | 0 |
Ca1—SI3 | 3.175 (4) | Ca3—Ca3iii | 4.1772 |
Ca1—AL3i | 3.175 (4) | Ca3—Ca3viii | 4.355 (7) |
Ca1—SI3i | 3.175 (4) | SI1—AL2v | 2.4117 |
Ca1—AL3ii | 3.175 (4) | SI1—AL2iii | 2.4117 |
Ca1—SI3ii | 3.175 (4) | SI1—SI2v | 2.4117 |
Ca1—AL2ii | 3.238 (2) | SI1—SI2iii | 2.4117 |
Ca1—AL1ii | 3.238 (2) | SI1—SI2 | 2.4117 |
Ca1—SI2ii | 3.238 (2) | SI1—Ca1iv | 3.238 (2) |
Ca1—SI1ii | 3.238 (2) | SI1—Ca1v | 3.238 (2) |
Ca1—AL2iii | 3.238 (2) | SI1—Ca1vii | 3.238 (2) |
Ca1—AL1i | 3.238 (2) | SI1—Ca1ix | 3.238 (2) |
Ca1—SI2iii | 3.238 (2) | SI1—Ca1x | 3.238 (2) |
Ca1—SI1i | 3.238 (2) | SI1—SI3 | 4.224 (5) |
Ca1—SI2 | 3.238 (2) | SI2—AL1vi | 2.4117 |
Ca1—SI1 | 3.238 (2) | SI2—AL1i | 2.4117 |
Ca1—SI4 | 3.363 (5) | SI2—SI1vi | 2.4117 |
Ca1—AL4iii | 3.363 (5) | SI2—SI1i | 2.4117 |
Ca1—SI4iii | 3.363 (5) | SI2—Ca1iv | 3.238 (2) |
Ca1—AL4ii | 3.363 (5) | SI2—Ca1vi | 3.238 (2) |
Ca1—SI4ii | 3.363 (5) | SI2—Ca1vii | 3.238 (2) |
Ca1—Ca1ii | 4.1772 | SI2—Ca1xi | 3.238 (2) |
Ca1—Ca1iv | 4.1772 | SI2—Ca1x | 3.238 (2) |
Ca1—Ca1v | 4.1772 | SI2—SI4 | 4.504 (5) |
Ca1—Ca1iii | 4.1772 | SI3—AL4v | 2.4279 (7) |
Ca1—Ca1i | 4.1772 | SI3—SI4v | 2.4279 (7) |
Ca1—Ca1vi | 4.1772 | SI3—AL4iii | 2.4279 (6) |
Ca1—Ca1vii | 4.320 (7) | SI3—SI4iii | 2.4279 (6) |
Ca1—Ca2 | 4.402 (5) | SI3—SI4 | 2.4279 (7) |
Ca2—AL4ii | 3.170 (4) | SI3—Ca1v | 3.175 (4) |
Ca2—SI4ii | 3.170 (4) | SI3—Ca1iv | 3.175 (4) |
Ca2—AL4iii | 3.170 (4) | SI3—Ca2iv | 3.359 (5) |
Ca2—SI4iii | 3.170 (4) | SI3—Ca2v | 3.359 (5) |
Ca2—SI4 | 3.170 (4) | SI3—SI5 | 4.411 (5) |
Ca2—SI5 | 3.180 (4) | SI4—AL3i | 2.4279 (6) |
Ca2—AL5i | 3.180 (4) | SI4—SI3i | 2.4279 (6) |
Ca2—SI5i | 3.180 (4) | SI4—AL3vi | 2.4279 (7) |
Ca2—AL5ii | 3.180 (4) | SI4—SI3vi | 2.4279 (7) |
Ca2—SI5ii | 3.180 (4) | SI4—Ca2iv | 3.170 (4) |
Ca2—AL3ii | 3.359 (5) | SI4—Ca2vi | 3.170 (4) |
Ca2—SI3ii | 3.359 (5) | SI4—Ca1vi | 3.363 (5) |
Ca2—AL3i | 3.359 (5) | SI4—Ca1iv | 3.363 (5) |
Ca2—SI3i | 3.359 (5) | SI4—SI6 | 4.479 (8) |
Ca2—SI3 | 3.359 (5) | SI5—AL6v | 2.4367 (9) |
Ca2—SI6 | 3.417 (5) | SI5—SI6v | 2.4367 (9) |
Ca2—AL6iii | 3.417 (5) | SI5—AL6iii | 2.4367 (9) |
Ca2—SI6iii | 3.417 (5) | SI5—SI6iii | 2.4367 (9) |
Ca2—AL6ii | 3.417 (5) | SI5—SI6 | 2.4367 (9) |
Ca2—SI6ii | 3.417 (5) | SI5—Ca2v | 3.180 (4) |
Ca2—Ca2iv | 4.1772 | SI5—Ca2iv | 3.180 (4) |
Ca2—Ca2ii | 4.1772 | SI5—Ca3iv | 3.367 (4) |
Ca2—Ca2i | 4.1772 | SI5—Ca3v | 3.367 (4) |
Ca2—Ca2iii | 4.1772 | SI5—SI7 | 4.527 (4) |
Ca2—Ca2vi | 4.1772 | SI6—AL5i | 2.4367 (9) |
Ca2—Ca2v | 4.1772 | SI6—SI5i | 2.4367 (9) |
Ca2—Ca3 | 4.423 (5) | SI6—AL5vi | 2.4367 (9) |
Ca3—AL6ii | 3.134 (5) | SI6—SI5vi | 2.4367 (9) |
Ca3—SI6ii | 3.134 (5) | SI6—Ca3iv | 3.134 (5) |
Ca3—AL6iii | 3.134 (5) | SI6—Ca3vi | 3.134 (5) |
Ca3—SI6iii | 3.134 (5) | SI6—Ca2vi | 3.417 (5) |
Ca3—SI6 | 3.134 (5) | SI6—Ca2iv | 3.417 (5) |
Ca3—SI8 | 3.249 (2) | SI6—SI8 | 4.179 (6) |
Ca3—SI7 | 3.249 (2) | SI7—AL8v | 2.4117 |
Ca3—AL8iii | 3.249 (2) | SI7—AL8iii | 2.4117 |
Ca3—AL7i | 3.249 (2) | SI7—SI8v | 2.4117 |
Ca3—SI8iii | 3.249 (2) | SI7—SI8iii | 2.4117 |
Ca3—SI7i | 3.249 (2) | SI7—SI8 | 2.4117 |
Ca3—AL8ii | 3.249 (2) | SI7—Ca3xii | 3.249 (2) |
Ca3—AL7ii | 3.249 (2) | SI7—Ca3xiii | 3.249 (2) |
Ca3—SI8ii | 3.249 (2) | SI7—Ca3v | 3.249 (2) |
Ca3—SI7ii | 3.249 (2) | SI7—Ca3viii | 3.249 (2) |
Ca3—AL5ii | 3.367 (4) | SI7—Ca3iv | 3.249 (2) |
Ca3—SI5ii | 3.367 (4) | SI8—AL7vi | 2.4117 |
Ca3—AL5i | 3.367 (4) | SI8—AL7i | 2.4117 |
Ca3—SI5i | 3.367 (4) | SI8—SI7vi | 2.4117 |
Ca3—SI5 | 3.367 (4) | SI8—SI7i | 2.4117 |
Ca3—Ca3iv | 4.1772 | SI8—Ca3xii | 3.249 (2) |
Ca3—Ca3ii | 4.1772 | SI8—Ca3xiv | 3.249 (2) |
Ca3—Ca3i | 4.1772 | SI8—Ca3vi | 3.249 (2) |
Ca3—Ca3vi | 4.1772 | SI8—Ca3viii | 3.249 (2) |
Ca3—Ca3v | 4.1772 | SI8—Ca3iv | 3.249 (2) |
Symmetry codes: (i) x, y−1, z; (ii) x−1, y−1, z; (iii) x−1, y, z; (iv) x+1, y+1, z; (v) x, y+1, z; (vi) x+1, y, z; (vii) x, y, −z; (viii) x, y, −z+1; (ix) x, y+1, −z; (x) x+1, y+1, −z; (xi) x+1, y, −z; (xii) x+1, y+1, −z+1; (xiii) x, y+1, −z+1; (xiv) x+1, y, −z+1. |
AlSiCa | Dx = 2.383 Mg m−3 Dm = 2.383 Mg m−3 Dm measured by not measured |
Mr = 95.15 | Melting point: 0 K |
Hexagonal, P6m2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P -6 2 | Cell parameters from 23 reflections |
a = 4.17720 (4) Å | θ = 10.1–47.2° |
c = 21.9372 (3) Å | µ = 2.76 mm−1 |
V = 331.50 (1) Å3 | T = 298 K |
Z = 5 | Cuboid, metallic dark grey |
F(000) = 235 | 0.21 × 0.20 × 0.18 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 340 reflections with I > 2σ(I) |
rotation method scans | Rint = 0.058 |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | θmax = 29.2°, θmin = 1.9° |
Tmin = 0.531, Tmax = 0.607 | h = −5→5 |
4754 measured reflections | k = −5→5 |
422 independent reflections | l = −30→30 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.023P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.035 | (Δ/σ)max < 0.001 |
wR(F2) = 0.086 | Δρmax = 0.46 e Å−3 |
S = 1.99 | Δρmin = −0.41 e Å−3 |
422 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
26 parameters | Absolute structure parameter: 0.5 (4) |
0 restraints |
AlSiCa | Z = 5 |
Mr = 95.15 | Mo Kα radiation |
Hexagonal, P6m2 | µ = 2.76 mm−1 |
a = 4.17720 (4) Å | T = 298 K |
c = 21.9372 (3) Å | 0.21 × 0.20 × 0.18 × 0 (radius) mm |
V = 331.50 (1) Å3 |
STOE IPDS 2 diffractometer | 422 independent reflections |
Absorption correction: empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | 340 reflections with I > 2σ(I) |
Tmin = 0.531, Tmax = 0.607 | Rint = 0.058 |
4754 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.086 | Δρmax = 0.46 e Å−3 |
S = 1.99 | Δρmin = −0.41 e Å−3 |
422 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
26 parameters | Absolute structure parameter: 0.5 (4) |
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 | Occ. (<1) | |
Ca1 | 0 | 0 | 0 | 0.0202 (6) | |
Ca2 | 0 | 0 | 0.19941 (8) | 0.0160 (4) | |
Ca3 | 0 | 0 | 0.40126 (5) | 0.0165 (5) | |
Si1 | 0.3333 | 0.6667 | 0.08767 (12) | 0.0210 (5) | 0.5 |
Si2 | 0.6667 | 0.3333 | 0.10556 (8) | 0.0120 (6) | 0.5 |
Si3 | 0.3333 | 0.6667 | 0.29191 (9) | 0.0122 (5) | 0.5 |
Si4 | 0.6667 | 0.3333 | 0.30909 (12) | 0.0241 (7) | 0.5 |
Si5 | 0.3333 | 0.6667 | 0.5 | 0.0136 (6) | 0.5 |
Si6 | 0.6667 | 0.3333 | 0.5 | 0.0472 (14) | 0.5 |
Al1 | 0.3333 | 0.6667 | 0.08767 (12) | 0.0210 (5) | 0.5 |
Al2 | 0.6667 | 0.3333 | 0.10556 (8) | 0.0120 (6) | 0.5 |
Al3 | 0.3333 | 0.6667 | 0.29191 (9) | 0.0122 (5) | 0.5 |
Al4 | 0.6667 | 0.3333 | 0.30909 (12) | 0.0241 (7) | 0.5 |
Al5 | 0.3333 | 0.6667 | 0.5 | 0.0136 (6) | 0.5 |
Al6 | 0.6667 | 0.3333 | 0.5 | 0.0472 (14) | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ca1 | 0.0203 (10) | 0.0203 (10) | 0.0202 (10) | 0.0101 (5) | 0 | 0 |
Ca2 | 0.0155 (5) | 0.0155 (5) | 0.0169 (5) | 0.0078 (3) | 0 | 0 |
Ca3 | 0.0189 (7) | 0.0189 (7) | 0.0116 (6) | 0.0095 (3) | 0 | 0 |
Si1 | 0.0137 (8) | 0.0137 (8) | 0.0356 (9) | 0.0068 (4) | 0 | 0 |
Si2 | 0.0097 (8) | 0.0097 (8) | 0.0167 (7) | 0.0048 (4) | 0 | 0 |
Si3 | 0.0088 (7) | 0.0088 (7) | 0.0189 (7) | 0.0044 (3) | 0 | 0 |
Si4 | 0.0150 (10) | 0.0150 (10) | 0.0422 (10) | 0.0075 (5) | 0 | 0 |
Si5 | 0.0088 (9) | 0.0088 (9) | 0.0231 (12) | 0.0044 (4) | 0 | 0 |
Si6 | 0.0137 (14) | 0.0137 (14) | 0.114 (4) | 0.0068 (7) | 0 | 0 |
Al1 | 0.0137 (8) | 0.0137 (8) | 0.0356 (9) | 0.0068 (4) | 0 | 0 |
Al2 | 0.0097 (8) | 0.0097 (8) | 0.0167 (7) | 0.0048 (4) | 0 | 0 |
Al3 | 0.0088 (7) | 0.0088 (7) | 0.0189 (7) | 0.0044 (3) | 0 | 0 |
Al4 | 0.0150 (10) | 0.0150 (10) | 0.0422 (10) | 0.0075 (5) | 0 | 0 |
Al5 | 0.0088 (9) | 0.0088 (9) | 0.0231 (12) | 0.0044 (4) | 0 | 0 |
Al6 | 0.0137 (14) | 0.0137 (14) | 0.114 (4) | 0.0068 (7) | 0 | 0 |
Ca1—Si1 | 3.0846 (17) | Ca3—Al5v | 3.2416 (8) |
Ca1—Al1i | 3.0846 (17) | Ca3—Si6v | 3.2416 (8) |
Ca1—Si1i | 3.0846 (17) | Ca3—Si5v | 3.2416 (8) |
Ca1—Al1ii | 3.0846 (17) | Ca3—Al3v | 3.4016 (15) |
Ca1—Al1iii | 3.0846 (17) | Ca3—Si3v | 3.4016 (15) |
Ca1—Si1ii | 3.0846 (17) | Ca3—Al3iii | 3.4016 (15) |
Ca1—Si1iii | 3.0846 (17) | Ca3—Si3iii | 3.4016 (15) |
Ca1—Al1iv | 3.0846 (17) | Ca3—Si3 | 3.4016 (15) |
Ca1—Al1v | 3.0846 (17) | Ca3—Ca3viii | 4.1772 |
Ca1—Si1iv | 3.0846 (17) | Ca3—Ca3v | 4.1772 |
Ca1—Si1v | 3.0846 (17) | Ca3—Ca3iii | 4.1772 |
Ca1—Si2 | 3.3435 (12) | Ca3—Ca3ix | 4.1772 |
Ca1—Al2i | 3.3435 (12) | Ca3—Ca3x | 4.1772 |
Ca1—Si2i | 3.3435 (12) | Ca3—Ca3vii | 4.1772 |
Ca1—Al2vi | 3.3435 (12) | Ca3—Ca3xi | 4.332 (2) |
Ca1—Al2vii | 3.3435 (12) | Si1—Al2x | 2.4434 (4) |
Ca1—Si2vi | 3.3435 (12) | Si1—Si2x | 2.4434 (4) |
Ca1—Si2vii | 3.3435 (12) | Si1—Al2vii | 2.4434 (4) |
Ca1—Al2iv | 3.3435 (12) | Si1—Si2vii | 2.4434 (4) |
Ca1—Si2v | 3.3435 (12) | Si1—Si2 | 2.4434 (4) |
Ca1—Si2iv | 3.3435 (12) | Si1—Ca1x | 3.0846 (17) |
Ca1—Al2v | 3.3435 (12) | Si1—Ca1viii | 3.0846 (17) |
Ca1—Ca1viii | 4.1772 | Si1—Ca2viii | 3.439 (3) |
Ca1—Ca1v | 4.1772 | Si1—Ca2x | 3.439 (3) |
Ca1—Ca1iii | 4.1772 | Si2—Al1iii | 2.4434 (4) |
Ca1—Ca1ix | 4.1772 | Si2—Si1iii | 2.4434 (4) |
Ca1—Ca1vii | 4.1772 | Si2—Al1ix | 2.4434 (4) |
Ca1—Ca1x | 4.1772 | Si2—Si1ix | 2.4434 (4) |
Ca1—Ca2iv | 4.3746 (18) | Si2—Ca2viii | 3.1710 (14) |
Ca1—Ca2 | 4.3746 (18) | Si2—Ca2ix | 3.1710 (14) |
Ca2—Si3 | 3.1518 (15) | Si2—Ca1ix | 3.3435 (12) |
Ca2—Al3iii | 3.1518 (15) | Si2—Ca1viii | 3.3435 (12) |
Ca2—Si3iii | 3.1518 (15) | Si3—Al4x | 2.4410 (3) |
Ca2—Al3v | 3.1518 (15) | Si3—Si4x | 2.4410 (3) |
Ca2—Si3v | 3.1518 (15) | Si3—Al4vii | 2.4410 (3) |
Ca2—Al2v | 3.1710 (14) | Si3—Si4vii | 2.4410 (3) |
Ca2—Si2v | 3.1710 (14) | Si3—Si4 | 2.4410 (3) |
Ca2—Al2vii | 3.1710 (14) | Si3—Ca2x | 3.1518 (15) |
Ca2—Si2vii | 3.1710 (14) | Si3—Ca2viii | 3.1518 (15) |
Ca2—Si2 | 3.1710 (14) | Si3—Ca3viii | 3.4016 (15) |
Ca2—Si4 | 3.407 (2) | Si3—Ca3x | 3.4016 (15) |
Ca2—Al4vii | 3.407 (2) | Si4—Al3iii | 2.4410 (3) |
Ca2—Si4vii | 3.407 (2) | Si4—Si3iii | 2.4410 (3) |
Ca2—Al4v | 3.407 (2) | Si4—Al3ix | 2.4410 (3) |
Ca2—Si4v | 3.407 (2) | Si4—Si3ix | 2.4410 (3) |
Ca2—Si1v | 3.439 (3) | Si4—Ca3viii | 3.1472 (18) |
Ca2—Al1v | 3.439 (3) | Si4—Ca3ix | 3.1472 (18) |
Ca2—Al1iii | 3.439 (3) | Si4—Ca2ix | 3.407 (2) |
Ca2—Si1iii | 3.439 (3) | Si4—Ca2viii | 3.407 (2) |
Ca2—Si1 | 3.439 (3) | Si5—Al6x | 2.4117 |
Ca2—Ca2v | 4.1772 | Si5—Al6vii | 2.4117 |
Ca2—Ca2viii | 4.1772 | Si5—Si6x | 2.4117 |
Ca2—Ca2x | 4.1772 | Si5—Si6vii | 2.4117 |
Ca2—Ca2vii | 4.1772 | Si5—Si6 | 2.4117 |
Ca2—Ca2iii | 4.1772 | Si5—Ca3xii | 3.2416 (8) |
Ca2—Ca2ix | 4.1772 | Si5—Ca3xiii | 3.2416 (8) |
Ca2—Ca3 | 4.4280 (18) | Si5—Ca3x | 3.2416 (8) |
Ca3—Al4v | 3.1472 (18) | Si5—Ca3xi | 3.2416 (8) |
Ca3—Si4v | 3.1472 (18) | Si5—Ca3viii | 3.2416 (8) |
Ca3—Al4vii | 3.1472 (18) | Si6—Al5ix | 2.4117 |
Ca3—Si4vii | 3.1472 (18) | Si6—Al5iii | 2.4117 |
Ca3—Si4 | 3.1472 (18) | Si6—Si5ix | 2.4117 |
Ca3—Si6 | 3.2416 (8) | Si6—Si5iii | 2.4117 |
Ca3—Si5 | 3.2416 (8) | Si6—Ca3xii | 3.2416 (8) |
Ca3—Al6vii | 3.2416 (8) | Si6—Ca3xiv | 3.2416 (8) |
Ca3—Al5iii | 3.2416 (8) | Si6—Ca3ix | 3.2416 (8) |
Ca3—Si6vii | 3.2416 (8) | Si6—Ca3xi | 3.2416 (8) |
Ca3—Si5iii | 3.2416 (8) | Si6—Ca3viii | 3.2416 (8) |
Ca3—Al6v | 3.2416 (8) |
Symmetry codes: (i) x−1, y−1, −z; (ii) x, y−1, −z; (iii) x, y−1, z; (iv) x, y, −z; (v) x−1, y−1, z; (vi) x−1, y, −z; (vii) x−1, y, z; (viii) x+1, y+1, z; (ix) x+1, y, z; (x) x, y+1, z; (xi) x, y, −z+1; (xii) x+1, y+1, −z+1; (xiii) x, y+1, −z+1; (xiv) x+1, y, −z+1. |
Experimental details
(6-fold_superstructure_298K) | (5-fold_superstructure_298K) | |
Crystal data | ||
Chemical formula | AlSiCa | AlSiCa |
Mr | 95.15 | 95.15 |
Crystal system, space group | Hexagonal, P6m2 | Hexagonal, P6m2 |
Temperature (K) | 298 | 298 |
a, c (Å) | 4.17720 (4), 26.3246 (4) | 4.17720 (4), 21.9372 (3) |
V (Å3) | 397.80 (1) | 331.50 (1) |
Z | 6 | 5 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 2.76 | 2.76 |
Crystal size (mm) | 0.18 × 0.16 × 0.15 × 0 (radius) | 0.21 × 0.20 × 0.18 × 0 (radius) |
Data collection | ||
Diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) | Empirical (using intensity measurements) X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.557, 0.660 | 0.531, 0.607 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3136, 429, 233 | 4754, 422, 340 |
Rint | 0.049 | 0.058 |
(sin θ/λ)max (Å−1) | 0.641 | 0.686 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.03, 0.082, 1.96 | 0.035, 0.086, 1.99 |
No. of reflections | 429 | 422 |
No. of parameters | 31 | 26 |
Δρmax, Δρmin (e Å−3) | 0.25, −0.29 | 0.46, −0.41 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.1 (3) | 0.5 (4) |
Computer programs: X-AREA (Stoe, 2002), FullProf Suite (Rodriguez-Carvajal), X-RED (Stoe, 1996), SHELXL97 (Sheldrick, 1997), ATOMS Version 5.1, WinGX 1.64.05 (Farrugia, 1999).