Table 1. Crystal data, data collection and structure refinement for fibre_T and fibre_C.
Computer programs: SHELXL2014/7 (Sheldrick, 2015 ▸).Geometry. All ESDs [except the ESD in the dihedral angle between two least-squares (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 F 2 against all reflections. The weighted R-factor wR and goodness of fit S are based on F 2, conventional R-factors R are based on F, with F set to zero for negative F 2. The threshold expression of F 2 > 2σ(F 2) is only used for calculating R factors, e.g. R[F 2 > 2σ(F 2)], and is not relevant to the choice of reflections for refinement. R factors based on F 2 are statistically about twice as large as those based on F, and R factors based on all data will be even larger.
| fibre_T | fibre_C | |
|---|---|---|
| Crystal data | ||
| Chemical formula | Ca0.18Fe5.40Mg1.25Al0.17Si8O23.92F0.08H1.92 | Ca0.17Fe5.30Mg1.31Al0.22Si8O24H2 |
| M r | 954.66 | 951.39 |
| Crystal system, space group | Monoclinic, C2/m | Monoclinic, C2/m |
| Temperature (K) | 293 | 293 |
| a, b, c (Å) | 9.5440 (2), 18.2455 (4), 5.32660 (12) | 9.5343 (2), 18.2210 (4), 5.3202 (2) |
| β (°) | 101.883 (2) | 101.846 (3) |
| V (Å3) | 907.67 (3) | 904.57 (4) |
| Z | 2 | 2 |
| Radiation type, wavelength (Å) | Synchrotron, λ = 0.30909 | Synchrotron, λ = 0.30911 |
| Photon flux (s−1) | 1.88 × 106 | 1.88 × 106 |
| μ (mm−1) | 0.5 | 0.5 |
| Crystal size (mm) | 0.001 × 0.001 × 0.001 | 0.001 × 0.001 × 0.001 |
| Data collection | ||
| Diffractometer | ID11 nanoscope | ID11 nanoscope |
| Absorption correction | Multi-scan SCALE3 ABSPACK; Oxford Diffraction (2006 ▸) | Multi-scan SCALE3 ABSPACK; Oxford Diffraction (2006 ▸) |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 7498, 1089, 986 | 6629, 1090, 1044 |
| R int | 0.030 | 0.047 |
| (sin θ/λ)max (Å−1) | 0.666 | 0.666 |
| Refinement | ||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.045, 0.159, 1.30 | 0.054, 0.135, 1.23 |
| No. of reflections | 1089 | 1090 |
| No. of parameters | 107 | 105 |
| No. of restraints | 5 | 4 |
| Hydrogen atom treatment | Only hydrogen atom coordinates refined w = 1/[σ2(F o 2) + (0.0581P)2 + 17.3651P] where P = (F o 2 + 2F c 2)/3 | Only hydrogen atom coordinates refined w = 1/[σ2(F o 2) + (0.0301P)2 + 27.1117P] where P = (F o 2 + 2F c 2)/3 |
| Δρmax, Δρmin (e Å−3) | 1.27, −0.95 | 1.12, −1.20 |