Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520616014049/xk5031sup1.cif | |
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520616014049/xk5031sup2.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520616014049/xk5031Isup3.hkl |
B-IncStrDB reference: 12392EA3Waa
CCDC reference: 1502345
K1.50Mg2O7Si2H0.5 | F(000) = 273 |
Mr = 275.45 | Dx = 3.128 Mg m−3 |
a = 5.0535 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 5.0535 (3) Å | Cell parameters from 1268 reflections |
c = 13.2229 (6) Å | θ = 4.7–26.9° |
α = 90° | µ = 1.88 mm−1 |
β = 90° | T = 293 K |
γ = 120° | Plate, colourless |
V = 292.45 (3) Å3 | 0.23 × 0.16 × 0.06 mm |
Z = 2 |
Excalibur EOS detector Agilent Technologies diffractometer | 143 independent reflections |
Radiation source: fine-focus sealed tube | 143 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
1K CCD–based area detector scans | θmax = 27.3°, θmin = 3.1° |
Absorption correction: multi-scan | h = −6→6 |
Tmin = 0.688, Tmax = 1.000 | k = −6→6 |
2759 measured reflections | l = −16→16 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.083 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.45 | w = 1/[σ2(Fo2) + (0.0307P)2 + 0.5285P] where P = (Fo2 + 2Fc2)/3 |
143 reflections | (Δ/σ)max < 0.001 |
21 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.38 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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
K | 0.342 (10) | 0.636 (3) | 0.2500 | 0.026 (5) | 0.2452 (19) |
Mg | 0.3333 | 0.6667 | 0.0000 | 0.0122 (5) | |
Si | 0.0000 | 0.0000 | 0.12314 (9) | 0.0083 (5) | |
O1 | 0.0000 | 0.0000 | 0.2500 | 0.0123 (12) | |
O2 | 0.3099 (4) | 0.0000 | 0.41003 (13) | 0.0100 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K | 0.030 (13) | 0.014 (7) | 0.0067 (8) | −0.009 (5) | 0.000 | 0.000 |
Mg | 0.0142 (7) | 0.0142 (7) | 0.0082 (8) | 0.0071 (3) | 0.000 | 0.000 |
Si | 0.0106 (6) | 0.0106 (6) | 0.0037 (7) | 0.0053 (3) | 0.000 | 0.000 |
O1 | 0.0169 (18) | 0.0169 (18) | 0.003 (2) | 0.0085 (9) | 0.000 | 0.000 |
O2 | 0.0105 (8) | 0.0122 (11) | 0.0078 (9) | 0.0061 (5) | −0.0007 (7) | 0.000 |
K—Ki | 0.31 (7) | Si—O1 | 1.6774 (12) |
K—Kii | 0.31 (7) | Si—Kiii | 3.251 (9) |
K—Kiii | 2.57 (10) | Si—Kxxi | 3.251 (9) |
K—O2iv | 2.68 (3) | Si—Kxxii | 3.251 (9) |
K—O2v | 2.68 (3) | Si—Kxxiii | 3.251 (9) |
K—O2vi | 2.707 (18) | Si—Kxxiv | 3.251 (9) |
K—O2iii | 2.707 (18) | Si—Kii | 3.34 (4) |
K—O1 | 2.785 (11) | Si—Kxxv | 3.34 (4) |
K—Kvii | 2.792 (9) | O1—Sixx | 1.6774 (12) |
K—Kviii | 2.792 (9) | O1—Kxxiii | 2.785 (11) |
K—O2ix | 2.86 (2) | O1—Kxxiv | 2.785 (11) |
K—O2x | 2.86 (2) | O1—Kiii | 2.785 (11) |
Mg—O2xi | 2.1133 (13) | O1—Kxxi | 2.785 (11) |
Mg—O2x | 2.1133 (13) | O1—Kxxii | 2.785 (11) |
Mg—O2vi | 2.1133 (13) | O1—Kxxvi | 2.89 (4) |
Mg—O2xii | 2.1133 (13) | O1—Kxxvii | 2.89 (4) |
Mg—O2xiii | 2.1133 (13) | O1—Kii | 2.89 (4) |
Mg—O2v | 2.1133 (13) | O1—Kxxv | 2.89 (4) |
Mg—Mgxiv | 2.9177 (2) | O2—Sixx | 1.626 (2) |
Mg—Mgxv | 2.9177 (2) | O2—Mgxxviii | 2.1133 (13) |
Mg—Mgxvi | 2.9177 (2) | O2—Mgxxix | 2.1133 (13) |
Mg—Kxvii | 3.311 (2) | O2—Kxxx | 2.68 (3) |
Mg—Ki | 3.311 (2) | O2—Kxxv | 2.68 (3) |
Mg—Kxviii | 3.311 (2) | O2—Kxxi | 2.707 (18) |
Si—O2xix | 1.626 (2) | O2—Kiii | 2.707 (18) |
Si—O2vi | 1.626 (2) | O2—Kxxxi | 2.86 (2) |
Si—O2xx | 1.626 (2) | O2—Kviii | 2.86 (2) |
Ki—K—Kii | 60.00 (4) | O1—Si—Kxxi | 58.94 (10) |
Ki—K—Kiii | 132 (10) | K—Si—Kxxi | 95.78 (13) |
Kii—K—Kiii | 168 (10) | Kiii—Si—Kxxi | 54.8 (18) |
Ki—K—O2iv | 92 (7) | O2xix—Si—Kxxii | 95.9 (9) |
Kii—K—O2iv | 123 (3) | O2vi—Si—Kxxii | 56.2 (6) |
Kiii—K—O2iv | 61.3 (8) | O2xx—Si—Kxxii | 150.6 (9) |
Ki—K—O2v | 92 (7) | O1—Si—Kxxii | 58.94 (10) |
Kii—K—O2v | 123 (3) | K—Si—Kxxii | 54.8 (18) |
Kiii—K—O2v | 61.3 (8) | Kiii—Si—Kxxii | 95.78 (13) |
O2iv—K—O2v | 104.5 (18) | Kxxi—Si—Kxxii | 117.7 (3) |
Ki—K—O2vi | 116 (6) | O2xix—Si—Kxxiii | 56.2 (6) |
Kii—K—O2vi | 81 (9) | O2vi—Si—Kxxiii | 95.9 (9) |
Kiii—K—O2vi | 91.5 (10) | O2xx—Si—Kxxiii | 150.6 (9) |
O2iv—K—O2vi | 150.1 (13) | O1—Si—Kxxiii | 58.94 (10) |
O2v—K—O2vi | 68.4 (2) | K—Si—Kxxiii | 95.78 (13) |
Ki—K—O2iii | 116 (6) | Kiii—Si—Kxxiii | 117.7 (3) |
Kii—K—O2iii | 81 (9) | Kxxi—Si—Kxxiii | 95.78 (13) |
Kiii—K—O2iii | 91.5 (10) | Kxxii—Si—Kxxiii | 46.6 (18) |
O2iv—K—O2iii | 68.4 (2) | O2xix—Si—Kxxiv | 56.2 (6) |
O2v—K—O2iii | 150.1 (13) | O2vi—Si—Kxxiv | 150.6 (9) |
O2vi—K—O2iii | 102.8 (9) | O2xx—Si—Kxxiv | 95.9 (9) |
Ki—K—O1 | 166 (10) | O1—Si—Kxxiv | 58.94 (10) |
Kii—K—O1 | 106 (10) | K—Si—Kxxiv | 117.7 (3) |
Kiii—K—O1 | 62.5 (11) | Kiii—Si—Kxxiv | 95.78 (13) |
O2iv—K—O1 | 96.6 (8) | Kxxi—Si—Kxxiv | 46.6 (18) |
O2v—K—O1 | 96.6 (8) | Kxxii—Si—Kxxiv | 95.78 (13) |
O2vi—K—O1 | 57.3 (3) | Kxxiii—Si—Kxxiv | 54.8 (18) |
O2iii—K—O1 | 57.3 (3) | O2xix—Si—Kii | 146.0 (6) |
Ki—K—Kvii | 103 (10) | O2vi—Si—Kii | 52.43 (14) |
Kii—K—Kvii | 43 (10) | O2xx—Si—Kii | 100.8 (6) |
Kiii—K—Kvii | 124.8 (4) | O1—Si—Kii | 59.8 (4) |
O2iv—K—Kvii | 125.9 (8) | K—Si—Kii | 5.3 (14) |
O2v—K—Kvii | 125.9 (8) | Kiii—Si—Kii | 51.8 (5) |
O2vi—K—Kvii | 58.2 (10) | Kxxi—Si—Kii | 100.2 (8) |
O2iii—K—Kvii | 58.2 (10) | Kxxii—Si—Kii | 50.1 (3) |
O1—K—Kvii | 62.3 (11) | Kxxiii—Si—Kii | 92.4 (14) |
Ki—K—Kviii | 127 (10) | Kxxiv—Si—Kii | 118.8 (4) |
Kii—K—Kviii | 173 (10) | O2xix—Si—Kxxv | 146.0 (6) |
Kiii—K—Kviii | 4.8 (4) | O2vi—Si—Kxxv | 100.8 (6) |
O2iv—K—Kviii | 59.3 (8) | O2xx—Si—Kxxv | 52.43 (14) |
O2v—K—Kviii | 59.3 (8) | O1—Si—Kxxv | 59.8 (4) |
O2vi—K—Kviii | 94.5 (11) | K—Si—Kxxv | 51.8 (5) |
O2iii—K—Kviii | 94.5 (11) | Kiii—Si—Kxxv | 5.3 (14) |
O1—K—Kviii | 67.3 (12) | Kxxi—Si—Kxxv | 50.1 (3) |
Kvii—K—Kviii | 129.6 (8) | Kxxii—Si—Kxxv | 100.2 (8) |
Ki—K—O2ix | 51 (4) | Kxxiii—Si—Kxxv | 118.8 (4) |
Kii—K—O2ix | 58 (5) | Kxxiv—Si—Kxxv | 92.4 (14) |
Kiii—K—O2ix | 127.3 (9) | Kii—Si—Kxxv | 57.1 (8) |
O2iv—K—O2ix | 66.12 (14) | Si—O1—Sixx | 180.0 |
O2v—K—O2ix | 139.8 (7) | Si—O1—K | 90.000 (7) |
O2vi—K—O2ix | 138 (2) | Sixx—O1—K | 90.000 (7) |
O2iii—K—O2ix | 65.7 (5) | Si—O1—Kxxiii | 90.000 (7) |
O1—K—O2ix | 122.7 (8) | Sixx—O1—Kxxiii | 90.000 (7) |
Kvii—K—O2ix | 84.0 (10) | K—O1—Kxxiii | 120.000 (2) |
Kviii—K—O2ix | 125.4 (9) | Si—O1—Kxxiv | 90.000 (7) |
Ki—K—O2x | 51 (4) | Sixx—O1—Kxxiv | 90.000 (7) |
Kii—K—O2x | 58 (5) | K—O1—Kxxiv | 175 (2) |
Kiii—K—O2x | 127.3 (9) | Kxxiii—O1—Kxxiv | 65 (2) |
O2iv—K—O2x | 139.8 (7) | Si—O1—Kiii | 90.000 (7) |
O2v—K—O2x | 66.12 (14) | Sixx—O1—Kiii | 90.000 (7) |
O2vi—K—O2x | 65.7 (5) | K—O1—Kiii | 55 (2) |
O2iii—K—O2x | 138 (2) | Kxxiii—O1—Kiii | 175 (2) |
O1—K—O2x | 122.7 (8) | Kxxiv—O1—Kiii | 120.000 (2) |
Kvii—K—O2x | 84.0 (10) | Si—O1—Kxxi | 90.000 (1) |
Kviii—K—O2x | 125.4 (9) | Sixx—O1—Kxxi | 90.000 (1) |
O2ix—K—O2x | 95.4 (10) | K—O1—Kxxi | 120.000 (11) |
O2xi—Mg—O2x | 84.74 (11) | Kxxiii—O1—Kxxi | 120.000 (11) |
O2xi—Mg—O2vi | 92.69 (7) | Kxxiv—O1—Kxxi | 55 (2) |
O2x—Mg—O2vi | 91.41 (6) | Kiii—O1—Kxxi | 65 (2) |
O2xi—Mg—O2xii | 91.41 (6) | Si—O1—Kxxii | 90.000 (1) |
O2x—Mg—O2xii | 92.69 (7) | Sixx—O1—Kxxii | 90.000 (1) |
O2vi—Mg—O2xii | 174.44 (10) | K—O1—Kxxii | 65 (2) |
O2xi—Mg—O2xiii | 91.41 (6) | Kxxiii—O1—Kxxii | 55 (2) |
O2x—Mg—O2xiii | 174.44 (10) | Kxxiv—O1—Kxxii | 120.000 (14) |
O2vi—Mg—O2xiii | 84.74 (11) | Kiii—O1—Kxxii | 120.000 (13) |
O2xii—Mg—O2xiii | 91.41 (6) | Kxxi—O1—Kxxii | 175 (2) |
O2xi—Mg—O2v | 174.44 (10) | Si—O1—Kxxvi | 90.000 (7) |
O2x—Mg—O2v | 91.41 (6) | Sixx—O1—Kxxvi | 90.000 (7) |
O2vi—Mg—O2v | 91.41 (6) | K—O1—Kxxvi | 126.0 (17) |
O2xii—Mg—O2v | 84.74 (11) | Kxxiii—O1—Kxxvi | 6.0 (17) |
O2xiii—Mg—O2v | 92.69 (7) | Kxxiv—O1—Kxxvi | 59.0 (5) |
O2xi—Mg—Mgxiv | 87.22 (5) | Kiii—O1—Kxxvi | 179.0 (5) |
O2x—Mg—Mgxiv | 46.35 (3) | Kxxi—O1—Kxxvi | 114.0 (17) |
O2vi—Mg—Mgxiv | 137.63 (5) | Kxxii—O1—Kxxvi | 61.0 (5) |
O2xii—Mg—Mgxiv | 46.35 (3) | Si—O1—Kxxvii | 90.000 (7) |
O2xiii—Mg—Mgxiv | 137.63 (5) | Sixx—O1—Kxxvii | 90.000 (7) |
O2v—Mg—Mgxiv | 87.22 (5) | K—O1—Kxxvii | 179.0 (5) |
O2xi—Mg—Mgxv | 46.35 (3) | Kxxiii—O1—Kxxvii | 59.0 (5) |
O2x—Mg—Mgxv | 87.22 (5) | Kxxiv—O1—Kxxvii | 6.0 (17) |
O2vi—Mg—Mgxv | 46.35 (3) | Kiii—O1—Kxxvii | 126.0 (17) |
O2xii—Mg—Mgxv | 137.63 (5) | Kxxi—O1—Kxxvii | 61.0 (5) |
O2xiii—Mg—Mgxv | 87.22 (5) | Kxxii—O1—Kxxvii | 114.0 (17) |
O2v—Mg—Mgxv | 137.63 (5) | Kxxvi—O1—Kxxvii | 52.9 (13) |
Mgxiv—Mg—Mgxv | 120.0 | Si—O1—Kii | 90.000 (14) |
O2xi—Mg—Mgxvi | 137.63 (5) | Sixx—O1—Kii | 90.000 (14) |
O2x—Mg—Mgxvi | 137.63 (5) | K—O1—Kii | 6.0 (17) |
O2vi—Mg—Mgxvi | 87.22 (5) | Kxxiii—O1—Kii | 114.0 (17) |
O2xii—Mg—Mgxvi | 87.22 (5) | Kxxiv—O1—Kii | 179.0 (5) |
O2xiii—Mg—Mgxvi | 46.35 (3) | Kiii—O1—Kii | 61.0 (5) |
O2v—Mg—Mgxvi | 46.35 (3) | Kxxi—O1—Kii | 126.0 (17) |
Mgxiv—Mg—Mgxvi | 120.0 | Kxxii—O1—Kii | 59.0 (5) |
Mgxv—Mg—Mgxvi | 120.0 | Kxxvi—O1—Kii | 120.000 (4) |
O2xi—Mg—Kxvii | 53.8 (9) | Kxxvii—O1—Kii | 172.9 (13) |
O2x—Mg—Kxvii | 125.0 (5) | Si—O1—Kxxv | 90.000 (14) |
O2vi—Mg—Kxvii | 121.2 (5) | Sixx—O1—Kxxv | 90.000 (14) |
O2xii—Mg—Kxvii | 58.9 (6) | K—O1—Kxxv | 61.0 (5) |
O2xiii—Mg—Kxvii | 54.6 (4) | Kxxiii—O1—Kxxv | 179.0 (5) |
O2v—Mg—Kxvii | 126.5 (9) | Kxxiv—O1—Kxxv | 114.0 (17) |
Mgxiv—Mg—Kxvii | 92.34 (19) | Kiii—O1—Kxxv | 6.0 (17) |
Mgxv—Mg—Kxvii | 87.0 (8) | Kxxi—O1—Kxxv | 59.0 (5) |
Mgxvi—Mg—Kxvii | 90.7 (8) | Kxxii—O1—Kxxv | 126.0 (17) |
O2xi—Mg—Ki | 125.0 (5) | Kxxvi—O1—Kxxv | 172.9 (13) |
O2x—Mg—Ki | 53.8 (9) | Kxxvii—O1—Kxxv | 120.000 (3) |
O2vi—Mg—Ki | 58.9 (6) | Kii—O1—Kxxv | 67.1 (13) |
O2xii—Mg—Ki | 121.2 (5) | Sixx—O2—Mgxxviii | 126.12 (7) |
O2xiii—Mg—Ki | 126.5 (9) | Sixx—O2—Mgxxix | 126.12 (7) |
O2v—Mg—Ki | 54.6 (4) | Mgxxviii—O2—Mgxxix | 87.31 (7) |
Mgxiv—Mg—Ki | 87.0 (8) | Sixx—O2—Kxxx | 98.8 (5) |
Mgxv—Mg—Ki | 92.34 (19) | Mgxxviii—O2—Kxxx | 127.2 (3) |
Mgxvi—Mg—Ki | 90.7 (8) | Mgxxix—O2—Kxxx | 86.6 (9) |
Kxvii—Mg—Ki | 178.7 (16) | Sixx—O2—Kxxv | 98.8 (5) |
O2xi—Mg—Kxviii | 54.6 (4) | Mgxxviii—O2—Kxxv | 86.6 (9) |
O2x—Mg—Kxviii | 121.2 (5) | Mgxxix—O2—Kxxv | 127.2 (3) |
O2vi—Mg—Kxviii | 126.5 (9) | Kxxx—O2—Kxxv | 57.4 (16) |
O2xii—Mg—Kxviii | 53.8 (9) | Sixx—O2—Kxxi | 93.9 (6) |
O2xiii—Mg—Kxviii | 58.9 (6) | Mgxxviii—O2—Kxxi | 133.6 (10) |
O2v—Mg—Kxviii | 125.0 (5) | Mgxxix—O2—Kxxi | 85.8 (4) |
Mgxiv—Mg—Kxviii | 87.0 (8) | Kxxx—O2—Kxxi | 6.7 (13) |
Mgxv—Mg—Kxviii | 90.7 (8) | Kxxv—O2—Kxxi | 62.5 (2) |
Mgxvi—Mg—Kxviii | 92.34 (19) | Sixx—O2—Kiii | 93.9 (6) |
Kxvii—Mg—Kxviii | 5.5 (11) | Mgxxviii—O2—Kiii | 85.8 (4) |
Ki—Mg—Kxviii | 174.0 (17) | Mgxxix—O2—Kiii | 133.6 (10) |
O2xix—Si—O2vi | 113.01 (6) | Kxxx—O2—Kiii | 62.5 (2) |
O2xix—Si—O2xx | 113.01 (6) | Kxxv—O2—Kiii | 6.7 (13) |
O2vi—Si—O2xx | 113.01 (6) | Kxxi—O2—Kiii | 67.1 (18) |
O2xix—Si—O1 | 105.65 (7) | Sixx—O2—Kxxxi | 99.5 (10) |
O2vi—Si—O1 | 105.65 (7) | Mgxxviii—O2—Kxxxi | 129.0 (9) |
O2xx—Si—O1 | 105.65 (7) | Mgxxix—O2—Kxxxi | 81.9 (5) |
O2xix—Si—K | 150.6 (9) | Kxxx—O2—Kxxxi | 5.3 (9) |
O2vi—Si—K | 56.2 (6) | Kxxv—O2—Kxxxi | 62.6 (10) |
O2xx—Si—K | 95.9 (9) | Kxxi—O2—Kxxxi | 5.6 (14) |
O1—Si—K | 58.94 (10) | Kiii—O2—Kxxxi | 67.7 (8) |
O2xix—Si—Kiii | 150.6 (9) | Sixx—O2—Kviii | 99.5 (10) |
O2vi—Si—Kiii | 95.9 (9) | Mgxxviii—O2—Kviii | 81.9 (5) |
O2xx—Si—Kiii | 56.2 (6) | Mgxxix—O2—Kviii | 129.0 (9) |
O1—Si—Kiii | 58.94 (10) | Kxxx—O2—Kviii | 62.6 (10) |
K—Si—Kiii | 46.6 (18) | Kxxv—O2—Kviii | 5.3 (9) |
O2xix—Si—Kxxi | 95.9 (9) | Kxxi—O2—Kviii | 67.7 (9) |
O2vi—Si—Kxxi | 150.6 (9) | Kiii—O2—Kviii | 5.6 (14) |
O2xx—Si—Kxxi | 56.2 (6) | Kxxxi—O2—Kviii | 67.7 (6) |
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, −z+1/2; (iii) y, x, z; (iv) −x+1, −x+y+1, z; (v) −x+1, −x+y+1, −z+1/2; (vi) y, x, −z+1/2; (vii) x−y, −y+1, −z+1/2; (viii) x−y+1, −y+1, −z+1/2; (ix) x, y+1, z; (x) x, y+1, −z+1/2; (xi) −y, −x+1, z−1/2; (xii) −x+1, −y+1, z−1/2; (xiii) x, x−y, z−1/2; (xiv) −x+1, −y+2, −z; (xv) −x, −y+1, −z; (xvi) −x+1, −y+1, −z; (xvii) −x+y, y, z−1/2; (xviii) x, x−y+1, −z; (xix) −x, −x+y, −z+1/2; (xx) x, y, −z+1/2; (xxi) −x+y, −x, −z+1/2; (xxii) −x, −x+y, z; (xxiii) −y, x−y, z; (xxiv) x−y, −y, −z+1/2; (xxv) −x+1, −x+y, z; (xxvi) x−1, y−1, z; (xxvii) y−1, x−1, z; (xxviii) −x+1, −y+1, z+1/2; (xxix) x, y−1, −z+1/2; (xxx) −y+1, x−y, z; (xxxi) x, y−1, z. |
H0K1.5Mg2O7Si2 | Z = 4 |
Mr = 275.4 | F(000) = 546 |
Orthorhombic, Cmcm(0β0)s00† | Dx = 3.108 Mg m−3 |
q = 0.750000b* | Mo Kα radiation, λ = 0.71069 Å |
a = 8.7623 (10) Å | µ = 1.87 mm−1 |
b = 5.0703 (7) Å | T = 293 K |
c = 13.2505 (11) Å | Plate, colourless |
V = 588.69 (12) Å3 | 0.24 × 0.18 × 0.06 mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, x3+1/2, −x4; (3) −x1, x2, −x3+1/2, x4+1/2; (4) x1, −x2, −x3, −x4+1/2; (5) −x1, −x2, −x3, −x4; (6) x1, x2, −x3+1/2, x4; (7) x1, −x2, x3+1/2, −x4+1/2; (8) −x1, x2, x3, x4+1/2; (9) x1+1/2, x2+1/2, x3, x4; (10) −x1+1/2, −x2+1/2, x3+1/2, −x4; (11) −x1+1/2, x2+1/2, −x3+1/2, x4+1/2; (12) x1+1/2, −x2+1/2, −x3, −x4+1/2; (13) −x1+1/2, −x2+1/2, −x3, −x4; (14) x1+1/2, x2+1/2, −x3+1/2, x4; (15) x1+1/2, −x2+1/2, x3+1/2, −x4+1/2; (16) −x1+1/2, x2+1/2, x3, x4+1/2. |
Xcalibur diffractometer | 2500 reflections with I > 3σ(I) |
Radiation source: X-ray tube | h = −11→11 |
Graphite monochromator | k = −7→7 |
19703 measured reflections | l = −17→16 |
6596 independent reflections |
Refinement on F | 0 restraints |
R[F2 > 2σ(F2)] = 0.069 | 0 constraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.59 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
6596 reflections | (Δ/σ)max = 0.028 |
98 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Si1 | 0 | −0.0047 (2) | −0.12332 (5) | 0.0042 (4) | |
K1 | 0.16177 (9) | 0.48790 (16) | −0.25 | 0.0104 (2) | 0.75 |
Mg1 | 0.1650 (2) | 0.5 | 0 | 0.0063 (4) | |
O1 | 0 | −0.0068 (7) | −0.25 | 0.0060 (6)* | |
O2 | −0.1559 (2) | 0.1517 (5) | −0.40896 (13) | 0.0059 (4)* | |
O3 | 0 | −0.3092 (5) | −0.41202 (18) | 0.0061 (7)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si1 | 0.0069 (8) | 0.0051 (9) | 0.0007 (5) | 0 | 0 | 0.0008 (4) |
K1 | 0.0124 (4) | 0.0137 (5) | 0.0051 (4) | −0.0011 (3) | 0 | 0 |
Mg1 | 0.0073 (8) | 0.0063 (8) | 0.0053 (6) | 0 | 0 | −0.0009 (5) |