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The crystal structures of the Ln3Ag1 − δGeS7 (Ln = La–Nd, Sm, Gd–Er, Y; δ = 0.11–0.50, space group P63) compounds were determined by means of X-ray single-crystal diffraction and the similarities among the crystal structures of all Ln3M1 − δTX7 (space group P63; Ln – lanthanide element, M – monovalent element; T – tetravalent element and X – S, Se) compounds deposited in the Inorganic Crystal Structure Database (ICSD) are discussed. Substitutions of each element in Ln3M1 − δTX7 result in a different structural effect. On the basis of the data deposited in the ICSD the large family of the Ln3M1 − δTX7 compounds was divided into three groups depending on the position of the monovalent element in the lattice. This position determines what kind of stereoisomer is present in the structure, either the ++ enantiomer or the +− diastereoisomer. Since the silver ions can occupy a different position and the energy barriers between positions are low the ions can move through the channel. It was shown that this movement is not a stochastic process but a correlated one.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810900144X/bp5017sup1.cif Contains datablocks la, ce, pr, nd, sm, gd, tb, dy, ho, er, y |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017lasup2.hkl Contains datablock la |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017cesup3.hkl Contains datablock ce |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017prsup4.hkl Contains datablock pr |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017ndsup5.hkl Contains datablock nd |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017smsup6.hkl Contains datablock sm |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017gdsup7.hkl Contains datablock gd |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017tbsup8.hkl Contains datablock tb |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017dysup9.hkl Contains datablock dy |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017hosup10.hkl Contains datablock ho |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017ersup11.hkl Contains datablock er |
| Structure factor file (CIF format) https://doi.org/10.1107/S010876810900144X/bp5017ysup12.hkl Contains datablock y |
For all compounds, data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED; data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
Ag0.82GeLa3S7 | Dx = 4.875 Mg m−3 |
Mr = 802.19 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 729 reflections |
Hall symbol: P 6c | θ = 4.2–26.4° |
a = 10.4056 (15) Å | µ = 16.91 mm−1 |
c = 5.8280 (12) Å | T = 295 K |
V = 546.49 (16) Å3 | Prism, dark red |
Z = 2 | 0.09 × 0.04 × 0.03 mm |
F(000) = 707 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 743 independent reflections |
Radiation source: fine-focus sealed tube | 729 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 4.2° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.097, Tmax = 0.599 | l = −7→7 |
5858 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0107P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.011 | (Δ/σ)max = 0.001 |
wR(F2) = 0.022 | Δρmax = 0.37 e Å−3 |
S = 1.04 | Δρmin = −0.44 e Å−3 |
743 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0042 (2) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 334 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.014 (12) |
Crystal data top
Ag0.82GeLa3S7 | Z = 2 |
Mr = 802.19 | Mo Kα radiation |
Hexagonal, P63 | µ = 16.91 mm−1 |
a = 10.4056 (15) Å | T = 295 K |
c = 5.8280 (12) Å | 0.09 × 0.04 × 0.03 mm |
V = 546.49 (16) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 743 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 729 reflections with I > 2σ(I) |
Tmin = 0.097, Tmax = 0.599 | Rint = 0.039 |
5858 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.011 | 1 restraint |
wR(F2) = 0.022 | Δρmax = 0.37 e Å−3 |
S = 1.04 | Δρmin = −0.44 e Å−3 |
743 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 334 Friedel pairs |
43 parameters | Absolute structure parameter: 0.014 (12) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
La | 0.875611 (18) | 0.641442 (18) | 0.24144 (6) | 0.00881 (6) | |
Ag1 | 0.0000 | 0.0000 | 0.18424 (19) | 0.0387 (6) | 0.719 (3) |
Ag2 | 0.0000 | 0.0000 | 0.9766 (13) | 0.018 (2) | 0.102 (3) |
Ge1 | 0.3333 | 0.6667 | 0.32488 (9) | 0.00826 (14) | |
S1 | 0.3333 | 0.6667 | 0.9515 (2) | 0.0114 (3) | |
S2 | 0.90929 (9) | 0.73775 (9) | 0.72749 (15) | 0.01254 (16) | |
S3 | 0.58764 (10) | 0.47816 (10) | 0.97462 (12) | 0.00978 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
La | 0.00902 (10) | 0.00790 (10) | 0.00959 (8) | 0.00429 (8) | −0.00087 (11) | −0.00073 (9) |
Ag1 | 0.0098 (3) | 0.0098 (3) | 0.0966 (17) | 0.00489 (16) | 0.000 | 0.000 |
Ag2 | 0.0101 (18) | 0.0101 (18) | 0.034 (5) | 0.0050 (9) | 0.000 | 0.000 |
Ge1 | 0.0089 (2) | 0.0089 (2) | 0.0070 (2) | 0.00445 (10) | 0.000 | 0.000 |
S1 | 0.0132 (5) | 0.0132 (5) | 0.0078 (7) | 0.0066 (3) | 0.000 | 0.000 |
S2 | 0.0097 (4) | 0.0169 (4) | 0.0111 (3) | 0.0066 (3) | 0.0010 (4) | −0.0007 (4) |
S3 | 0.0102 (5) | 0.0084 (4) | 0.0114 (3) | 0.0051 (4) | 0.0013 (3) | 0.0011 (3) |
Geometric parameters (Å, º) top
La—S3i | 2.9145 (9) | Ag2—S2xvi | 2.811 (4) |
La—S2ii | 2.9399 (9) | Ag2—S2xvii | 2.811 (4) |
La—S2iii | 2.9452 (9) | Ag2—S2xviii | 2.811 (4) |
La—S2 | 2.9665 (11) | Ag2—Ag2viii | 2.9140 (6) |
La—S3iv | 3.0319 (9) | Ag2—Ag2xi | 2.9140 (6) |
La—S3iii | 3.0732 (9) | Ag2—Laxvii | 3.556 (3) |
La—S1v | 3.0878 (7) | Ag2—Laxvi | 3.556 (3) |
La—S2iv | 3.1221 (11) | Ge1—S1iv | 2.1758 (14) |
La—Ag1vi | 3.2981 (5) | Ge1—S3ii | 2.2245 (9) |
La—Ag2v | 3.556 (3) | Ge1—S3xix | 2.2245 (9) |
La—Ag2vii | 3.626 (3) | Ge1—S3v | 2.2245 (9) |
Ag1—Ag2iv | 1.210 (7) | S1—Ge1xv | 2.1758 (14) |
Ag1—Ag2viii | 1.704 (7) | S1—Laxx | 3.0878 (7) |
Ag1—S2ix | 2.4136 (9) | S1—Laxvi | 3.0878 (7) |
Ag1—S2v | 2.4136 (9) | S1—Laxxi | 3.0878 (7) |
Ag1—S2x | 2.4136 (9) | S2—Ag1xvi | 2.4136 (9) |
Ag1—Ag1viii | 2.9140 (6) | S2—Ag2vi | 2.805 (4) |
Ag1—Ag1xi | 2.9140 (6) | S2—Ag2v | 2.811 (4) |
Ag1—Laxii | 3.2981 (5) | S2—Laxxii | 2.9399 (9) |
Ag1—Laxiii | 3.2981 (5) | S2—Laxxi | 2.9452 (9) |
Ag1—Laxiv | 3.2981 (5) | S2—Laxv | 3.1221 (11) |
Ag2—Ag1xv | 1.210 (7) | S3—Ge1xvi | 2.2245 (9) |
Ag2—Ag1xi | 1.704 (7) | S3—Laxxiii | 2.9145 (9) |
Ag2—S2xiii | 2.805 (4) | S3—Laxv | 3.0319 (9) |
Ag2—S2xiv | 2.805 (4) | S3—Laxxi | 3.0732 (9) |
Ag2—S2xii | 2.805 (4) | | |
| | | |
S3i—La—S2ii | 140.33 (3) | Ag1xi—Ag2—S2xiii | 58.84 (13) |
S3i—La—S2iii | 107.53 (2) | Ag1xv—Ag2—S2xiv | 121.16 (13) |
S2ii—La—S2iii | 89.89 (3) | Ag1xi—Ag2—S2xiv | 58.84 (13) |
S3i—La—S2 | 137.75 (2) | S2xiii—Ag2—S2xiv | 95.64 (18) |
S2ii—La—S2 | 79.46 (2) | Ag1xv—Ag2—S2xii | 121.16 (13) |
S2iii—La—S2 | 79.38 (2) | Ag1xi—Ag2—S2xii | 58.84 (13) |
S3i—La—S3iv | 73.14 (3) | S2xiii—Ag2—S2xii | 95.64 (18) |
S2ii—La—S3iv | 71.59 (2) | S2xiv—Ag2—S2xii | 95.64 (18) |
S2iii—La—S3iv | 142.08 (3) | Ag1xv—Ag2—S2xvi | 58.65 (13) |
S2—La—S3iv | 126.57 (2) | Ag1xi—Ag2—S2xvi | 121.35 (13) |
S3i—La—S3iii | 73.508 (19) | S2xiii—Ag2—S2xvi | 179.8 (3) |
S2ii—La—S3iii | 145.66 (3) | S2xiv—Ag2—S2xvi | 84.483 (14) |
S2iii—La—S3iii | 68.66 (2) | S2xii—Ag2—S2xvi | 84.483 (14) |
S2—La—S3iii | 70.65 (2) | Ag1xv—Ag2—S2xvii | 58.65 (13) |
S3iv—La—S3iii | 140.85 (2) | Ag1xi—Ag2—S2xvii | 121.35 (13) |
S3i—La—S1v | 70.13 (2) | S2xiii—Ag2—S2xvii | 84.483 (14) |
S2ii—La—S1v | 112.021 (18) | S2xiv—Ag2—S2xvii | 84.483 (14) |
S2iii—La—S1v | 148.62 (2) | S2xii—Ag2—S2xvii | 179.8 (3) |
S2—La—S1v | 82.82 (3) | S2xvi—Ag2—S2xvii | 95.39 (18) |
S3iv—La—S1v | 68.65 (2) | Ag1xv—Ag2—S2xviii | 58.65 (13) |
S3iii—La—S1v | 81.15 (2) | Ag1xi—Ag2—S2xviii | 121.35 (13) |
S3i—La—S2iv | 72.98 (2) | S2xiii—Ag2—S2xviii | 84.483 (14) |
S2ii—La—S2iv | 76.97 (2) | S2xiv—Ag2—S2xviii | 179.8 (3) |
S2iii—La—S2iv | 76.90 (2) | S2xii—Ag2—S2xviii | 84.483 (14) |
S2—La—S2iv | 146.34 (3) | S2xvi—Ag2—S2xviii | 95.39 (18) |
S3iv—La—S2iv | 66.96 (2) | S2xvii—Ag2—S2xviii | 95.39 (18) |
S3iii—La—S2iv | 120.71 (2) | Ag1xv—Ag2—Ag2viii | 180.000 (4) |
S1v—La—S2iv | 128.42 (3) | Ag1xi—Ag2—Ag2viii | 0.000 (1) |
S3i—La—Ag1vi | 136.06 (3) | S2xiii—Ag2—Ag2viii | 58.84 (13) |
S2ii—La—Ag1vi | 45.071 (16) | S2xiv—Ag2—Ag2viii | 58.84 (13) |
S2iii—La—Ag1vi | 45.044 (16) | S2xii—Ag2—Ag2viii | 58.84 (13) |
S2—La—Ag1vi | 78.53 (3) | S2xvi—Ag2—Ag2viii | 121.35 (13) |
S3iv—La—Ag1vi | 107.52 (2) | S2xvii—Ag2—Ag2viii | 121.35 (13) |
S3iii—La—Ag1vi | 110.62 (2) | S2xviii—Ag2—Ag2viii | 121.35 (13) |
S1v—La—Ag1vi | 152.74 (2) | Ag1xv—Ag2—Ag2xi | 0.000 (1) |
S2iv—La—Ag1vi | 67.81 (3) | Ag1xi—Ag2—Ag2xi | 180.000 (3) |
S3i—La—Ag2v | 157.44 (6) | S2xiii—Ag2—Ag2xi | 121.16 (13) |
S2ii—La—Ag2v | 50.08 (5) | S2xiv—Ag2—Ag2xi | 121.16 (13) |
S2iii—La—Ag2v | 50.05 (5) | S2xii—Ag2—Ag2xi | 121.16 (13) |
S2—La—Ag2v | 50.06 (11) | S2xvi—Ag2—Ag2xi | 58.65 (13) |
S3iv—La—Ag2v | 121.66 (5) | S2xvii—Ag2—Ag2xi | 58.65 (13) |
S3iii—La—Ag2v | 96.59 (6) | S2xviii—Ag2—Ag2xi | 58.65 (13) |
S1v—La—Ag2v | 129.39 (11) | Ag2viii—Ag2—Ag2xi | 180.000 (3) |
S2iv—La—Ag2v | 96.28 (12) | Ag1xv—Ag2—Laxvii | 112.67 (11) |
Ag1vi—La—Ag2v | 28.47 (11) | Ag1xi—Ag2—Laxvii | 67.33 (11) |
S3i—La—Ag2vii | 118.48 (10) | S2xiii—Ag2—Laxvii | 53.60 (6) |
S2ii—La—Ag2vii | 49.34 (4) | S2xiv—Ag2—Laxvii | 53.49 (6) |
S2iii—La—Ag2vii | 49.32 (4) | S2xii—Ag2—Laxvii | 126.2 (2) |
S2—La—Ag2vii | 97.92 (11) | S2xvi—Ag2—Laxvii | 126.42 (3) |
S3iv—La—Ag2vii | 95.89 (7) | S2xvii—Ag2—Laxvii | 54.02 (3) |
S3iii—La—Ag2vii | 117.90 (4) | S2xviii—Ag2—Laxvii | 126.53 (3) |
S1v—La—Ag2vii | 160.202 (7) | Ag2viii—Ag2—Laxvii | 67.33 (11) |
S2iv—La—Ag2vii | 48.42 (11) | Ag2xi—Ag2—Laxvii | 112.67 (11) |
Ag1vi—La—Ag2vii | 19.39 (10) | Ag1xv—Ag2—Laxvi | 112.67 (11) |
Ag2v—La—Ag2vii | 47.861 (12) | Ag1xi—Ag2—Laxvi | 67.33 (11) |
Ag2iv—Ag1—Ag2viii | 180.000 (1) | S2xiii—Ag2—Laxvi | 126.2 (2) |
Ag2iv—Ag1—S2ix | 95.99 (3) | S2xiv—Ag2—Laxvi | 53.60 (6) |
Ag2viii—Ag1—S2ix | 84.01 (3) | S2xii—Ag2—Laxvi | 53.49 (6) |
Ag2iv—Ag1—S2v | 95.99 (3) | S2xvi—Ag2—Laxvi | 54.02 (3) |
Ag2viii—Ag1—S2v | 84.01 (3) | S2xvii—Ag2—Laxvi | 126.53 (3) |
S2ix—Ag1—S2v | 118.924 (11) | S2xviii—Ag2—Laxvi | 126.42 (3) |
Ag2iv—Ag1—S2x | 95.99 (3) | Ag2viii—Ag2—Laxvi | 67.33 (11) |
Ag2viii—Ag1—S2x | 84.01 (3) | Ag2xi—Ag2—Laxvi | 112.67 (11) |
S2ix—Ag1—S2x | 118.924 (11) | Laxvii—Ag2—Laxvi | 106.09 (13) |
S2v—Ag1—S2x | 118.924 (11) | S1iv—Ge1—S3ii | 113.10 (2) |
Ag2iv—Ag1—Ag1viii | 0.0 | S1iv—Ge1—S3xix | 113.10 (2) |
Ag2viii—Ag1—Ag1viii | 180.000 (1) | S3ii—Ge1—S3xix | 105.61 (3) |
S2ix—Ag1—Ag1viii | 95.99 (3) | S1iv—Ge1—S3v | 113.10 (2) |
S2v—Ag1—Ag1viii | 95.99 (3) | S3ii—Ge1—S3v | 105.61 (3) |
S2x—Ag1—Ag1viii | 95.99 (3) | S3xix—Ge1—S3v | 105.61 (3) |
Ag2iv—Ag1—Ag1xi | 180.0 | Ge1xv—S1—Laxx | 113.36 (2) |
Ag2viii—Ag1—Ag1xi | 0.000 (1) | Ge1xv—S1—Laxvi | 113.36 (2) |
S2ix—Ag1—Ag1xi | 84.01 (3) | Laxx—S1—Laxvi | 105.31 (3) |
S2v—Ag1—Ag1xi | 84.01 (3) | Ge1xv—S1—Laxxi | 113.36 (2) |
S2x—Ag1—Ag1xi | 84.01 (3) | Laxx—S1—Laxxi | 105.31 (3) |
Ag1viii—Ag1—Ag1xi | 180.0 | Laxvi—S1—Laxxi | 105.31 (3) |
Ag2iv—Ag1—Laxii | 95.80 (2) | Ag2vi—S2—Ag2v | 62.51 (2) |
Ag2viii—Ag1—Laxii | 84.20 (2) | Ag1xvi—S2—Laxxii | 75.34 (2) |
S2ix—Ag1—Laxii | 168.21 (5) | Ag2vi—S2—Laxxii | 76.44 (3) |
S2v—Ag1—Laxii | 59.715 (19) | Ag2v—S2—Laxxii | 78.15 (3) |
S2x—Ag1—Laxii | 59.586 (19) | Ag1xvi—S2—Laxxi | 75.24 (2) |
Ag1viii—Ag1—Laxii | 95.80 (2) | Ag2vi—S2—Laxxi | 76.35 (3) |
Ag1xi—Ag1—Laxii | 84.20 (2) | Ag2v—S2—Laxxi | 78.06 (3) |
Ag2iv—Ag1—Laxiii | 95.80 (2) | Laxxii—S2—Laxxi | 149.90 (3) |
Ag2viii—Ag1—Laxiii | 84.20 (2) | Ag1xvi—S2—La | 101.28 (4) |
S2ix—Ag1—Laxiii | 59.586 (19) | Ag2vi—S2—La | 138.44 (13) |
S2v—Ag1—Laxiii | 168.21 (5) | Ag2v—S2—La | 75.92 (13) |
S2x—Ag1—Laxiii | 59.715 (19) | Laxxii—S2—La | 95.97 (3) |
Ag1viii—Ag1—Laxiii | 95.80 (2) | Laxxi—S2—La | 95.86 (3) |
Ag1xi—Ag1—Laxiii | 84.20 (2) | Ag1xvi—S2—Laxv | 112.38 (4) |
Laxii—Ag1—Laxiii | 118.992 (7) | Ag2vi—S2—Laxv | 75.22 (14) |
Ag2iv—Ag1—Laxiv | 95.80 (2) | Ag2v—S2—Laxv | 137.74 (14) |
Ag2viii—Ag1—Laxiv | 84.20 (2) | Laxxii—S2—Laxv | 92.71 (2) |
S2ix—Ag1—Laxiv | 59.715 (19) | Laxxi—S2—Laxv | 92.61 (2) |
S2v—Ag1—Laxiv | 59.586 (19) | La—S2—Laxv | 146.34 (3) |
S2x—Ag1—Laxiv | 168.21 (5) | Ge1xvi—S3—Laxxiii | 92.15 (3) |
Ag1viii—Ag1—Laxiv | 95.80 (2) | Ge1xvi—S3—Laxv | 89.10 (3) |
Ag1xi—Ag1—Laxiv | 84.20 (2) | Laxxiii—S3—Laxv | 111.30 (3) |
Laxii—Ag1—Laxiv | 118.992 (7) | Ge1xvi—S3—Laxxi | 122.50 (3) |
Laxiii—Ag1—Laxiv | 118.992 (7) | Laxxiii—S3—Laxxi | 139.09 (3) |
Ag1xv—Ag2—Ag1xi | 180.000 (1) | Laxv—S3—Laxxi | 91.91 (2) |
Ag1xv—Ag2—S2xiii | 121.16 (13) | | |
Symmetry codes: (i) −x+y+1, −x+1, z−1; (ii) y, −x+y+1, z−1/2; (iii) x−y+1, x, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) −x, −y, z−1/2; (ix) y−1, −x+y, z−1/2; (x) x−y, x−1, z−1/2; (xi) −x, −y, z+1/2; (xii) −y+1, x−y, z; (xiii) x−1, y−1, z; (xiv) −x+y, −x+1, z; (xv) x, y, z+1; (xvi) −x+1, −y+1, z+1/2; (xvii) y−1, −x+y, z+1/2; (xviii) x−y, x−1, z+1/2; (xix) x−y, x, z−1/2; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) −y+1, x−y, z+1. |
Crystal data top
Ag0.88Ce3GeS7 | Dx = 4.939 Mg m−3 |
Mr = 812.30 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 704 reflections |
Hall symbol: P 6c | θ = 4.2–26.4° |
a = 10.3902 (15) Å | µ = 17.79 mm−1 |
c = 5.8425 (12) Å | T = 295 K |
V = 546.23 (16) Å3 | Prism, dark red |
Z = 2 | 0.09 × 0.08 × 0.06 mm |
F(000) = 719 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 726 independent reflections |
Radiation source: fine-focus sealed tube | 704 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 4.2° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.097, Tmax = 0.599 | l = −7→6 |
6515 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0294P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.021 | (Δ/σ)max = 0.001 |
wR(F2) = 0.046 | Δρmax = 1.01 e Å−3 |
S = 1.06 | Δρmin = −0.70 e Å−3 |
726 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0122 (6) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 319 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.04 (2) |
Crystal data top
Ag0.88Ce3GeS7 | Z = 2 |
Mr = 812.30 | Mo Kα radiation |
Hexagonal, P63 | µ = 17.79 mm−1 |
a = 10.3902 (15) Å | T = 295 K |
c = 5.8425 (12) Å | 0.09 × 0.08 × 0.06 mm |
V = 546.23 (16) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 726 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 704 reflections with I > 2σ(I) |
Tmin = 0.097, Tmax = 0.599 | Rint = 0.043 |
6515 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.021 | 1 restraint |
wR(F2) = 0.046 | Δρmax = 1.01 e Å−3 |
S = 1.06 | Δρmin = −0.70 e Å−3 |
726 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 319 Friedel pairs |
43 parameters | Absolute structure parameter: −0.04 (2) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ce | 0.87483 (3) | 0.64142 (3) | 0.23920 (14) | 0.01007 (13) | |
Ag1 | 0.0000 | 0.0000 | 0.1694 (6) | 0.0391 (16) | 0.783 (9) |
Ag2 | 0.0000 | 0.0000 | 0.965 (4) | 0.026 (7) | 0.098 (9) |
Ge1 | 0.3333 | 0.6667 | 0.3228 (2) | 0.0100 (3) | |
S1 | 0.3333 | 0.6667 | 0.9480 (5) | 0.0116 (6) | |
S2 | 0.90743 (17) | 0.73512 (17) | 0.7237 (4) | 0.0135 (3) | |
S3 | 0.5867 (2) | 0.47870 (19) | 0.9745 (3) | 0.0108 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ce | 0.00999 (19) | 0.00870 (19) | 0.0116 (2) | 0.00471 (14) | −0.0008 (2) | −0.0009 (2) |
Ag1 | 0.0109 (6) | 0.0109 (6) | 0.096 (5) | 0.0054 (3) | 0.000 | 0.000 |
Ag2 | 0.020 (4) | 0.020 (4) | 0.04 (2) | 0.010 (2) | 0.000 | 0.000 |
Ge1 | 0.0102 (4) | 0.0102 (4) | 0.0096 (6) | 0.00509 (19) | 0.000 | 0.000 |
S1 | 0.0127 (9) | 0.0127 (9) | 0.0094 (16) | 0.0063 (5) | 0.000 | 0.000 |
S2 | 0.0112 (7) | 0.0171 (7) | 0.0126 (8) | 0.0074 (6) | 0.0003 (8) | −0.0016 (9) |
S3 | 0.0113 (8) | 0.0099 (8) | 0.0115 (8) | 0.0055 (7) | 0.0014 (7) | 0.0004 (6) |
Geometric parameters (Å, º) top
Ce—S3i | 2.9091 (18) | Ag2—S2xvi | 2.854 (13) |
Ce—S2ii | 2.9425 (16) | Ag2—S2xvii | 2.854 (13) |
Ce—S2iii | 2.9446 (16) | Ag2—S2xviii | 2.854 (13) |
Ce—S2 | 2.957 (2) | Ag2—Ag2xi | 2.9212 (6) |
Ce—S3iv | 3.0251 (18) | Ag2—Ag2viii | 2.9212 (6) |
Ce—S3ii | 3.0758 (18) | Ag2—Cexviii | 3.530 (9) |
Ce—S1v | 3.0805 (13) | Ag2—Cexvi | 3.530 (9) |
Ce—S2iv | 3.131 (2) | Ge1—S1iv | 2.190 (3) |
Ce—Ag1vi | 3.3005 (7) | Ge1—S3iii | 2.2391 (19) |
Ce—Ag2v | 3.530 (9) | Ge1—S3xix | 2.2391 (19) |
Ce—Ag2vii | 3.647 (11) | Ge1—S3v | 2.2391 (19) |
Ag1—Ag2iv | 1.20 (2) | S1—Ge1xv | 2.190 (3) |
Ag1—Ag2viii | 1.73 (2) | S1—Cexx | 3.0805 (13) |
Ag1—S2v | 2.4399 (16) | S1—Cexvi | 3.0805 (13) |
Ag1—S2ix | 2.4399 (16) | S1—Cexxi | 3.0805 (13) |
Ag1—S2x | 2.4399 (16) | S2—Ag1xvi | 2.4399 (16) |
Ag1—Ag1viii | 2.9212 (6) | S2—Ag2vi | 2.799 (12) |
Ag1—Ag1xi | 2.9213 (6) | S2—Ag2v | 2.854 (13) |
Ag1—Cexii | 3.3005 (7) | S2—Cexxi | 2.9425 (16) |
Ag1—Cexiii | 3.3005 (7) | S2—Cexxii | 2.9446 (16) |
Ag1—Cexiv | 3.3005 (7) | S2—Cexv | 3.131 (2) |
Ag2—Ag1xv | 1.20 (2) | S3—Ge1xvi | 2.2391 (19) |
Ag2—Ag1xi | 1.73 (2) | S3—Cexxiii | 2.9091 (18) |
Ag2—S2xiii | 2.799 (12) | S3—Cexv | 3.0251 (18) |
Ag2—S2xii | 2.799 (12) | S3—Cexxi | 3.0758 (18) |
Ag2—S2xiv | 2.799 (12) | | |
| | | |
S3i—Ce—S2ii | 106.58 (5) | Ag1xi—Ag2—S2xiii | 59.8 (4) |
S3i—Ce—S2iii | 140.39 (6) | Ag1xv—Ag2—S2xii | 120.2 (4) |
S2ii—Ce—S2iii | 90.76 (6) | Ag1xi—Ag2—S2xii | 59.8 (4) |
S3i—Ce—S2 | 137.17 (5) | S2xiii—Ag2—S2xii | 96.9 (6) |
S2ii—Ce—S2 | 80.01 (5) | Ag1xv—Ag2—S2xiv | 120.2 (4) |
S2iii—Ce—S2 | 79.98 (5) | Ag1xi—Ag2—S2xiv | 59.8 (4) |
S3i—Ce—S3iv | 73.73 (7) | S2xiii—Ag2—S2xiv | 96.9 (6) |
S2ii—Ce—S3iv | 142.23 (6) | S2xii—Ag2—S2xiv | 96.9 (6) |
S2iii—Ce—S3iv | 71.11 (5) | Ag1xv—Ag2—S2xvi | 58.0 (4) |
S2—Ce—S3iv | 126.28 (5) | Ag1xi—Ag2—S2xvi | 122.0 (4) |
S3i—Ce—S3ii | 73.27 (3) | S2xiii—Ag2—S2xvi | 178.2 (8) |
S2ii—Ce—S3ii | 68.46 (5) | S2xii—Ag2—S2xvi | 84.28 (3) |
S2iii—Ce—S3ii | 145.89 (5) | S2xiv—Ag2—S2xvi | 84.28 (3) |
S2—Ce—S3ii | 70.23 (5) | Ag1xv—Ag2—S2xvii | 58.0 (4) |
S3iv—Ce—S3ii | 140.90 (5) | Ag1xi—Ag2—S2xvii | 122.0 (4) |
S3i—Ce—S1v | 70.19 (5) | S2xiii—Ag2—S2xvii | 84.28 (3) |
S2ii—Ce—S1v | 148.24 (5) | S2xii—Ag2—S2xvii | 84.28 (3) |
S2iii—Ce—S1v | 111.99 (4) | S2xiv—Ag2—S2xvii | 178.2 (8) |
S2—Ce—S1v | 82.44 (6) | S2xvi—Ag2—S2xvii | 94.5 (6) |
S3iv—Ce—S1v | 68.73 (5) | Ag1xv—Ag2—S2xviii | 58.0 (4) |
S3ii—Ce—S1v | 80.76 (4) | Ag1xi—Ag2—S2xviii | 122.0 (4) |
S3i—Ce—S2iv | 72.60 (5) | S2xiii—Ag2—S2xviii | 84.28 (3) |
S2ii—Ce—S2iv | 77.22 (5) | S2xii—Ag2—S2xviii | 178.2 (8) |
S2iii—Ce—S2iv | 77.19 (5) | S2xiv—Ag2—S2xviii | 84.28 (3) |
S2—Ce—S2iv | 147.31 (6) | S2xvi—Ag2—S2xviii | 94.5 (6) |
S3iv—Ce—S2iv | 66.74 (4) | S2xvii—Ag2—S2xviii | 94.5 (6) |
S3ii—Ce—S2iv | 120.98 (5) | Ag1xv—Ag2—Ag2xi | 0.000 (4) |
S1v—Ce—S2iv | 127.92 (6) | Ag1xi—Ag2—Ag2xi | 180.000 (9) |
S3i—Ce—Ag1vi | 134.75 (7) | S2xiii—Ag2—Ag2xi | 120.2 (4) |
S2ii—Ce—Ag1vi | 45.56 (3) | S2xii—Ag2—Ag2xi | 120.2 (4) |
S2iii—Ce—Ag1vi | 45.55 (3) | S2xiv—Ag2—Ag2xi | 120.2 (4) |
S2—Ce—Ag1vi | 80.27 (7) | S2xvi—Ag2—Ag2xi | 58.0 (4) |
S3iv—Ce—Ag1vi | 106.80 (5) | S2xvii—Ag2—Ag2xi | 58.0 (4) |
S3ii—Ce—Ag1vi | 111.20 (5) | S2xviii—Ag2—Ag2xi | 58.0 (4) |
S1v—Ce—Ag1vi | 153.84 (5) | Ag1xv—Ag2—Ag2viii | 180.000 (12) |
S2iv—Ce—Ag1vi | 67.04 (7) | Ag1xi—Ag2—Ag2viii | 0.000 (2) |
S3i—Ce—Ag2v | 156.6 (2) | S2xiii—Ag2—Ag2viii | 59.8 (4) |
S2ii—Ce—Ag2v | 50.24 (14) | S2xii—Ag2—Ag2viii | 59.8 (4) |
S2iii—Ce—Ag2v | 50.23 (14) | S2xiv—Ag2—Ag2viii | 59.8 (4) |
S2—Ce—Ag2v | 51.3 (4) | S2xvi—Ag2—Ag2viii | 122.0 (4) |
S3iv—Ce—Ag2v | 121.33 (15) | S2xvii—Ag2—Ag2viii | 122.0 (4) |
S3ii—Ce—Ag2v | 96.9 (2) | S2xviii—Ag2—Ag2viii | 122.0 (4) |
S1v—Ce—Ag2v | 130.2 (3) | Ag2xi—Ag2—Ag2viii | 180.000 (11) |
S2iv—Ce—Ag2v | 96.0 (4) | Ag1xv—Ag2—Cexviii | 111.9 (4) |
Ag1vi—Ce—Ag2v | 29.0 (3) | Ag1xi—Ag2—Cexviii | 68.1 (4) |
S3i—Ce—Ag2vii | 117.6 (3) | S2xiii—Ag2—Cexviii | 53.92 (19) |
S2ii—Ce—Ag2vii | 49.93 (13) | S2xii—Ag2—Cexviii | 127.9 (8) |
S2iii—Ce—Ag2vii | 49.92 (13) | S2xiv—Ag2—Cexviii | 53.96 (19) |
S2—Ce—Ag2vii | 99.3 (3) | S2xvi—Ag2—Cexviii | 126.26 (12) |
S3iv—Ce—Ag2vii | 95.4 (2) | S2xvii—Ag2—Cexviii | 126.22 (12) |
S3ii—Ce—Ag2vii | 118.29 (11) | S2xviii—Ag2—Cexviii | 53.94 (6) |
S1v—Ce—Ag2vii | 160.43 (3) | Ag2xi—Ag2—Cexviii | 111.9 (4) |
S2iv—Ce—Ag2vii | 48.0 (3) | Ag2viii—Ag2—Cexviii | 68.1 (4) |
Ag1vi—Ce—Ag2vii | 19.0 (3) | Ag1xv—Ag2—Cexvi | 111.9 (4) |
Ag2v—Ce—Ag2vii | 48.00 (3) | Ag1xi—Ag2—Cexvi | 68.1 (4) |
Ag2iv—Ag1—Ag2viii | 180.000 (3) | S2xiii—Ag2—Cexvi | 127.9 (8) |
Ag2iv—Ag1—S2v | 97.47 (9) | S2xii—Ag2—Cexvi | 53.96 (19) |
Ag2viii—Ag1—S2v | 82.53 (9) | S2xiv—Ag2—Cexvi | 53.92 (19) |
Ag2iv—Ag1—S2ix | 97.47 (9) | S2xvi—Ag2—Cexvi | 53.94 (6) |
Ag2viii—Ag1—S2ix | 82.53 (9) | S2xvii—Ag2—Cexvi | 126.26 (12) |
S2v—Ag1—S2ix | 118.34 (4) | S2xviii—Ag2—Cexvi | 126.22 (12) |
Ag2iv—Ag1—S2x | 97.47 (9) | Ag2xi—Ag2—Cexvi | 111.9 (4) |
Ag2viii—Ag1—S2x | 82.53 (9) | Ag2viii—Ag2—Cexvi | 68.1 (4) |
S2v—Ag1—S2x | 118.34 (4) | Cexviii—Ag2—Cexvi | 106.9 (4) |
S2ix—Ag1—S2x | 118.34 (4) | S1iv—Ge1—S3iii | 113.33 (5) |
Ag2iv—Ag1—Ag1viii | 0.0 | S1iv—Ge1—S3xix | 113.33 (5) |
Ag2viii—Ag1—Ag1viii | 180.000 (3) | S3iii—Ge1—S3xix | 105.35 (6) |
S2v—Ag1—Ag1viii | 97.47 (9) | S1iv—Ge1—S3v | 113.33 (5) |
S2ix—Ag1—Ag1viii | 97.47 (9) | S3iii—Ge1—S3v | 105.35 (6) |
S2x—Ag1—Ag1viii | 97.47 (9) | S3xix—Ge1—S3v | 105.35 (6) |
Ag2iv—Ag1—Ag1xi | 180.0 | Ge1xv—S1—Cexx | 113.33 (5) |
Ag2viii—Ag1—Ag1xi | 0.000 (3) | Ge1xv—S1—Cexvi | 113.33 (5) |
S2v—Ag1—Ag1xi | 82.53 (9) | Cexx—S1—Cexvi | 105.35 (6) |
S2ix—Ag1—Ag1xi | 82.53 (9) | Ge1xv—S1—Cexxi | 113.33 (5) |
S2x—Ag1—Ag1xi | 82.53 (9) | Cexx—S1—Cexxi | 105.35 (6) |
Ag1viii—Ag1—Ag1xi | 180.0 | Cexvi—S1—Cexxi | 105.35 (6) |
Ag2iv—Ag1—Cexii | 97.09 (6) | Ag2vi—S2—Ag2v | 62.23 (4) |
Ag2viii—Ag1—Cexii | 82.91 (6) | Ag1xvi—S2—Cexxi | 74.99 (4) |
S2v—Ag1—Cexii | 59.44 (4) | Ag2vi—S2—Cexxi | 75.84 (7) |
S2ix—Ag1—Cexii | 165.44 (14) | Ag2v—S2—Cexxi | 77.96 (9) |
S2x—Ag1—Cexii | 59.49 (4) | Ag1xvi—S2—Cexxii | 74.95 (4) |
Ag1viii—Ag1—Cexii | 97.09 (6) | Ag2vi—S2—Cexxii | 75.80 (7) |
Ag1xi—Ag1—Cexii | 82.91 (6) | Ag2v—S2—Cexxii | 77.93 (9) |
Ag2iv—Ag1—Cexiii | 97.09 (6) | Cexxi—S2—Cexxii | 148.99 (6) |
Ag2viii—Ag1—Cexiii | 82.91 (6) | Ag1xvi—S2—Ce | 99.36 (10) |
S2v—Ag1—Cexiii | 165.44 (14) | Ag2vi—S2—Ce | 137.0 (4) |
S2ix—Ag1—Cexiii | 59.49 (4) | Ag2v—S2—Ce | 74.8 (4) |
S2x—Ag1—Cexiii | 59.44 (4) | Cexxi—S2—Ce | 96.12 (6) |
Ag1viii—Ag1—Cexiii | 97.09 (6) | Cexxii—S2—Ce | 96.08 (5) |
Ag1xi—Ag1—Cexiii | 82.91 (6) | Ag1xvi—S2—Cexv | 113.33 (10) |
Cexii—Ag1—Cexiii | 118.50 (3) | Ag2vi—S2—Cexv | 75.7 (4) |
Ag2iv—Ag1—Cexiv | 97.09 (6) | Ag2v—S2—Cexv | 137.9 (4) |
Ag2viii—Ag1—Cexiv | 82.91 (6) | Cexxi—S2—Cexv | 92.49 (5) |
S2v—Ag1—Cexiv | 59.49 (4) | Cexxii—S2—Cexv | 92.45 (5) |
S2ix—Ag1—Cexiv | 59.44 (4) | Ce—S2—Cexv | 147.31 (6) |
S2x—Ag1—Cexiv | 165.44 (14) | Ge1xvi—S3—Cexxiii | 91.96 (6) |
Ag1viii—Ag1—Cexiv | 97.09 (6) | Ge1xvi—S3—Cexv | 88.97 (6) |
Ag1xi—Ag1—Cexiv | 82.91 (6) | Cexxiii—S3—Cexv | 111.29 (6) |
Cexii—Ag1—Cexiv | 118.50 (3) | Ge1xvi—S3—Cexxi | 121.90 (7) |
Cexiii—Ag1—Cexiv | 118.50 (3) | Cexxiii—S3—Cexxi | 139.74 (7) |
Ag1xv—Ag2—Ag1xi | 180.000 (3) | Cexv—S3—Cexxi | 92.00 (5) |
Ag1xv—Ag2—S2xiii | 120.2 (4) | | |
Symmetry codes: (i) −x+y+1, −x+1, z−1; (ii) x−y+1, x, z−1/2; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) −x, −y, z−1/2; (ix) y−1, −x+y, z−1/2; (x) x−y, x−1, z−1/2; (xi) −x, −y, z+1/2; (xii) −y+1, x−y, z; (xiii) x−1, y−1, z; (xiv) −x+y, −x+1, z; (xv) x, y, z+1; (xvi) −x+1, −y+1, z+1/2; (xvii) x−y, x−1, z+1/2; (xviii) y−1, −x+y, z+1/2; (xix) x−y, x, z−1/2; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) −y+1, x−y, z+1. |
Crystal data top
Ag0.89GePr3S7 | Dx = 5.176 Mg m−3 |
Mr = 815.74 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 585 reflections |
Hall symbol: P 6c | θ = 4.0–25.0° |
a = 10.2290 (14) Å | µ = 19.50 mm−1 |
c = 5.7760 (11) Å | T = 295 K |
V = 523.39 (14) Å3 | Prism, dark red |
Z = 2 | 0.10 × 0.09 × 0.07 mm |
F(000) = 726 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 602 independent reflections |
Radiation source: fine-focus sealed tube | 585 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.059 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 25.0°, θmin = 4.0° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→11 |
Tmin = 0.163, Tmax = 0.272 | l = −6→6 |
5174 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0287P)2 + 1.032P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max < 0.001 |
wR(F2) = 0.051 | Δρmax = 1.22 e Å−3 |
S = 1.09 | Δρmin = −0.73 e Å−3 |
602 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0145 (7) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.05 (3) |
Crystal data top
Ag0.89GePr3S7 | Z = 2 |
Mr = 815.74 | Mo Kα radiation |
Hexagonal, P63 | µ = 19.50 mm−1 |
a = 10.2290 (14) Å | T = 295 K |
c = 5.7760 (11) Å | 0.10 × 0.09 × 0.07 mm |
V = 523.39 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 602 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 585 reflections with I > 2σ(I) |
Tmin = 0.163, Tmax = 0.272 | Rint = 0.059 |
5174 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.025 | 1 restraint |
wR(F2) = 0.051 | Δρmax = 1.22 e Å−3 |
S = 1.09 | Δρmin = −0.73 e Å−3 |
602 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs |
43 parameters | Absolute structure parameter: 0.05 (3) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pr | 0.87391 (5) | 0.64129 (5) | 0.23910 (18) | 0.01118 (19) | |
Ag1 | 0.0000 | 0.0000 | 0.1692 (9) | 0.027 (4) | 0.49 (5) |
Ag2 | 0.0000 | 0.0000 | 1.094 (18) | 0.165 (10) | 0.41 (5) |
Ge1 | 0.3333 | 0.6667 | 0.3227 (3) | 0.0104 (4) | |
S1 | 0.3333 | 0.6667 | 0.9467 (7) | 0.0131 (10) | |
S2 | 0.9060 (2) | 0.7345 (3) | 0.7230 (5) | 0.0152 (5) | |
S3 | 0.5856 (3) | 0.4788 (3) | 0.9755 (4) | 0.0123 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr | 0.0115 (3) | 0.0105 (3) | 0.0116 (3) | 0.0055 (2) | −0.0010 (3) | −0.0008 (3) |
Ag1 | 0.011 (2) | 0.011 (2) | 0.059 (9) | 0.0054 (10) | 0.000 | 0.000 |
Ag2 | 0.019 (3) | 0.019 (3) | 0.46 (3) | 0.0097 (16) | 0.000 | 0.000 |
Ge1 | 0.0121 (6) | 0.0121 (6) | 0.0071 (9) | 0.0060 (3) | 0.000 | 0.000 |
S1 | 0.0147 (14) | 0.0147 (14) | 0.010 (3) | 0.0073 (7) | 0.000 | 0.000 |
S2 | 0.0112 (11) | 0.0187 (11) | 0.0149 (12) | 0.0068 (9) | −0.0001 (11) | −0.0018 (14) |
S3 | 0.0137 (12) | 0.0113 (12) | 0.0122 (13) | 0.0063 (11) | 0.0006 (10) | −0.0001 (10) |
Geometric parameters (Å, º) top
Pr—S3i | 2.863 (2) | Ag2—Ag2xi | 2.8880 (6) |
Pr—S2ii | 2.893 (2) | Ag2—Ag2x | 2.8880 (6) |
Pr—S2iii | 2.905 (2) | Ag2—Ag1xix | 3.32 (11) |
Pr—S2 | 2.918 (3) | Ag2—Prxx | 3.33 (3) |
Pr—S3iv | 2.980 (2) | Ag2—Prxxi | 3.33 (3) |
Pr—S1v | 3.0293 (18) | Ag2—Prxxii | 3.33 (3) |
Pr—S3ii | 3.037 (3) | Ge1—S1iv | 2.172 (4) |
Pr—S2iv | 3.097 (3) | Ge1—S3xxiii | 2.217 (3) |
Pr—Ag1vi | 3.2492 (9) | Ge1—S3iii | 2.217 (3) |
Pr—Ag2vii | 3.33 (3) | Ge1—S3v | 2.217 (3) |
Ag1—S2viii | 2.405 (2) | S1—Ge1xxiv | 2.172 (4) |
Ag1—S2v | 2.405 (2) | S1—Prxxv | 3.0293 (18) |
Ag1—S2ix | 2.405 (2) | S1—Prxvi | 3.0293 (18) |
Ag1—Ag2x | 2.45 (11) | S1—Prxxvi | 3.0293 (18) |
Ag1—Ag1xi | 2.8880 (5) | S2—Ag1xvi | 2.405 (2) |
Ag1—Ag1x | 2.8880 (5) | S2—Ag2v | 2.50 (3) |
Ag1—Prxii | 3.2492 (9) | S2—Prxxvi | 2.893 (2) |
Ag1—Prxiii | 3.2492 (9) | S2—Prxxvii | 2.905 (2) |
Ag1—Prxiv | 3.2492 (9) | S2—Prxxiv | 3.097 (3) |
Ag1—Ag2xv | 3.32 (11) | S3—Ge1xvi | 2.217 (3) |
Ag2—Ag1xi | 2.45 (11) | S3—Prxx | 2.863 (2) |
Ag2—S2xvi | 2.50 (3) | S3—Prxxiv | 2.980 (2) |
Ag2—S2xvii | 2.50 (3) | S3—Prxxvi | 3.037 (3) |
Ag2—S2xviii | 2.50 (3) | | |
| | | |
S3i—Pr—S2ii | 105.95 (7) | Ag2x—Ag1—Ag2xv | 180.000 (15) |
S3i—Pr—S2iii | 140.58 (8) | Ag1xi—Ag1—Ag2xv | 180.000 (5) |
S2ii—Pr—S2iii | 90.90 (9) | Ag1x—Ag1—Ag2xv | 0.0 |
S3i—Pr—S2 | 137.04 (7) | Prxii—Ag1—Ag2xv | 97.13 (10) |
S2ii—Pr—S2 | 80.27 (7) | Prxiii—Ag1—Ag2xv | 97.13 (10) |
S2iii—Pr—S2 | 80.07 (7) | Prxiv—Ag1—Ag2xv | 97.13 (10) |
S3i—Pr—S3iv | 74.12 (10) | Ag1xi—Ag2—S2xvi | 107 (2) |
S2ii—Pr—S3iv | 142.26 (8) | Ag1xi—Ag2—S2xvii | 107 (2) |
S2iii—Pr—S3iv | 71.10 (7) | S2xvi—Ag2—S2xvii | 112 (2) |
S2—Pr—S3iv | 126.16 (7) | Ag1xi—Ag2—S2xviii | 107 (2) |
S3i—Pr—S1v | 70.35 (7) | S2xvi—Ag2—S2xviii | 112 (2) |
S2ii—Pr—S1v | 148.00 (7) | S2xvii—Ag2—S2xviii | 112 (2) |
S2iii—Pr—S1v | 112.28 (5) | Ag1xi—Ag2—Ag2xi | 180.00 (3) |
S2—Pr—S1v | 82.33 (9) | S2xvi—Ag2—Ag2xi | 73 (2) |
S3iv—Pr—S1v | 68.85 (7) | S2xvii—Ag2—Ag2xi | 73 (2) |
S3i—Pr—S3ii | 73.06 (5) | S2xviii—Ag2—Ag2xi | 73 (2) |
S2ii—Pr—S3ii | 68.47 (7) | Ag1xi—Ag2—Ag2x | 0.000 (3) |
S2iii—Pr—S3ii | 145.87 (8) | S2xvi—Ag2—Ag2x | 107 (2) |
S2—Pr—S3ii | 70.11 (7) | S2xvii—Ag2—Ag2x | 107 (2) |
S3iv—Pr—S3ii | 140.86 (7) | S2xviii—Ag2—Ag2x | 107 (2) |
S1v—Pr—S3ii | 80.42 (6) | Ag2xi—Ag2—Ag2x | 180.00 (5) |
S3i—Pr—S2iv | 72.42 (7) | Ag1xi—Ag2—Ag1xix | 180.000 (2) |
S2ii—Pr—S2iv | 77.34 (7) | S2xvi—Ag2—Ag1xix | 73 (2) |
S2iii—Pr—S2iv | 77.16 (7) | S2xvii—Ag2—Ag1xix | 73 (2) |
S2—Pr—S2iv | 147.58 (9) | S2xviii—Ag2—Ag1xix | 73 (2) |
S3iv—Pr—S2iv | 66.61 (6) | Ag2xi—Ag2—Ag1xix | 0.00 (2) |
S1v—Pr—S2iv | 127.77 (9) | Ag2x—Ag2—Ag1xix | 180.000 (8) |
S3ii—Pr—S2iv | 121.21 (7) | Ag1xi—Ag2—Prxx | 104.6 (18) |
S3i—Pr—Ag1vi | 134.41 (10) | S2xvi—Ag2—Prxx | 57.4 (6) |
S2ii—Pr—Ag1vi | 45.65 (5) | S2xvii—Ag2—Prxx | 148 (4) |
S2iii—Pr—Ag1vi | 45.59 (5) | S2xviii—Ag2—Prxx | 57.7 (6) |
S2—Pr—Ag1vi | 80.43 (10) | Ag2xi—Ag2—Prxx | 75.4 (17) |
S3iv—Pr—Ag1vi | 106.85 (8) | Ag2x—Ag2—Prxx | 104.6 (18) |
S1v—Pr—Ag1vi | 154.12 (8) | Ag1xix—Ag2—Prxx | 75.4 (18) |
S3ii—Pr—Ag1vi | 111.23 (6) | Ag1xi—Ag2—Prxxi | 104.6 (18) |
S2iv—Pr—Ag1vi | 67.15 (10) | S2xvi—Ag2—Prxxi | 57.7 (6) |
S3i—Pr—Ag2vii | 127.8 (16) | S2xvii—Ag2—Prxxi | 57.4 (6) |
S2ii—Pr—Ag2vii | 46.7 (4) | S2xviii—Ag2—Prxxi | 148 (4) |
S2iii—Pr—Ag2vii | 46.6 (4) | Ag2xi—Ag2—Prxxi | 75.4 (18) |
S2—Pr—Ag2vii | 87.9 (18) | Ag2x—Ag2—Prxxi | 104.6 (18) |
S3iv—Pr—Ag2vii | 102.5 (11) | Ag1xix—Ag2—Prxxi | 75.4 (18) |
S1v—Pr—Ag2vii | 158.3 (8) | Prxx—Ag2—Prxxi | 113.9 (14) |
S3ii—Pr—Ag2vii | 114.3 (7) | Ag1xi—Ag2—Prxxii | 104.6 (18) |
S2iv—Pr—Ag2vii | 59.7 (18) | S2xvi—Ag2—Prxxii | 148 (4) |
Ag1vi—Pr—Ag2vii | 7.4 (18) | S2xvii—Ag2—Prxxii | 57.7 (6) |
S2viii—Ag1—S2v | 118.36 (6) | S2xviii—Ag2—Prxxii | 57.4 (6) |
S2viii—Ag1—S2ix | 118.36 (6) | Ag2xi—Ag2—Prxxii | 75.4 (18) |
S2v—Ag1—S2ix | 118.36 (6) | Ag2x—Ag2—Prxxii | 104.6 (18) |
S2viii—Ag1—Ag2x | 82.58 (14) | Ag1xix—Ag2—Prxxii | 75.4 (18) |
S2v—Ag1—Ag2x | 82.58 (13) | Prxx—Ag2—Prxxii | 113.9 (14) |
S2ix—Ag1—Ag2x | 82.58 (13) | Prxxi—Ag2—Prxxii | 113.9 (14) |
S2viii—Ag1—Ag1xi | 82.58 (13) | S1iv—Ge1—S3xxiii | 113.47 (7) |
S2v—Ag1—Ag1xi | 82.58 (13) | S1iv—Ge1—S3iii | 113.47 (7) |
S2ix—Ag1—Ag1xi | 82.58 (13) | S3xxiii—Ge1—S3iii | 105.19 (8) |
Ag2x—Ag1—Ag1xi | 0.000 (10) | S1iv—Ge1—S3v | 113.47 (7) |
S2viii—Ag1—Ag1x | 97.42 (13) | S3xxiii—Ge1—S3v | 105.19 (8) |
S2v—Ag1—Ag1x | 97.42 (13) | S3iii—Ge1—S3v | 105.19 (8) |
S2ix—Ag1—Ag1x | 97.42 (13) | Ge1xxiv—S1—Prxxv | 113.32 (8) |
Ag2x—Ag1—Ag1x | 180.000 (10) | Ge1xxiv—S1—Prxvi | 113.32 (8) |
Ag1xi—Ag1—Ag1x | 180.000 (1) | Prxxv—S1—Prxvi | 105.37 (9) |
S2viii—Ag1—Prxii | 165.4 (2) | Ge1xxiv—S1—Prxxvi | 113.32 (8) |
S2v—Ag1—Prxii | 59.32 (5) | Prxxv—S1—Prxxvi | 105.37 (9) |
S2ix—Ag1—Prxii | 59.62 (5) | Prxvi—S1—Prxxvi | 105.37 (9) |
Ag2x—Ag1—Prxii | 82.87 (10) | Ag1xvi—S2—Prxxvi | 75.03 (6) |
Ag1xi—Ag1—Prxii | 82.87 (10) | Ag2v—S2—Prxxvi | 75.9 (3) |
Ag1x—Ag1—Prxii | 97.13 (10) | Ag1xvi—S2—Prxxvii | 74.79 (6) |
S2viii—Ag1—Prxiii | 59.62 (5) | Ag2v—S2—Prxxvii | 75.7 (3) |
S2v—Ag1—Prxiii | 165.4 (2) | Prxxvi—S2—Prxxvii | 148.83 (9) |
S2ix—Ag1—Prxiii | 59.32 (5) | Ag1xvi—S2—Pr | 99.29 (15) |
Ag2x—Ag1—Prxiii | 82.87 (10) | Ag2v—S2—Pr | 89 (2) |
Ag1xi—Ag1—Prxiii | 82.87 (10) | Prxxvi—S2—Pr | 96.30 (8) |
Ag1x—Ag1—Prxiii | 97.13 (10) | Prxxvii—S2—Pr | 96.03 (8) |
Prxii—Ag1—Prxiii | 118.48 (4) | Ag1xvi—S2—Prxxiv | 113.13 (15) |
S2viii—Ag1—Prxiv | 59.32 (5) | Ag2v—S2—Prxxiv | 123 (2) |
S2v—Ag1—Prxiv | 59.62 (5) | Prxxvi—S2—Prxxiv | 92.49 (8) |
S2ix—Ag1—Prxiv | 165.4 (2) | Prxxvii—S2—Prxxiv | 92.25 (8) |
Ag2x—Ag1—Prxiv | 82.87 (10) | Pr—S2—Prxxiv | 147.58 (9) |
Ag1xi—Ag1—Prxiv | 82.87 (10) | Ge1xvi—S3—Prxx | 91.85 (9) |
Ag1x—Ag1—Prxiv | 97.13 (10) | Ge1xvi—S3—Prxxiv | 88.84 (8) |
Prxii—Ag1—Prxiv | 118.48 (4) | Prxx—S3—Prxxiv | 111.09 (8) |
Prxiii—Ag1—Prxiv | 118.48 (4) | Ge1xvi—S3—Prxxvi | 121.46 (10) |
S2viii—Ag1—Ag2xv | 97.42 (13) | Prxx—S3—Prxxvi | 140.32 (9) |
S2v—Ag1—Ag2xv | 97.42 (14) | Prxxiv—S3—Prxxvi | 92.01 (7) |
S2ix—Ag1—Ag2xv | 97.42 (13) | | |
Symmetry codes: (i) −x+y+1, −x+1, z−1; (ii) x−y+1, x, z−1/2; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) y−1, −x+y, z−1/2; (ix) x−y, x−1, z−1/2; (x) −x, −y, z−1/2; (xi) −x, −y, z+1/2; (xii) −y+1, x−y, z; (xiii) x−1, y−1, z; (xiv) −x+y, −x+1, z; (xv) −x, −y, z−3/2; (xvi) −x+1, −y+1, z+1/2; (xvii) y−1, −x+y, z+1/2; (xviii) x−y, x−1, z+1/2; (xix) −x, −y, z+3/2; (xx) −y+1, x−y, z+1; (xxi) −x+y, −x+1, z+1; (xxii) x−1, y−1, z+1; (xxiii) x−y, x, z−1/2; (xxiv) x, y, z+1; (xxv) x−y, x, z+1/2; (xxvi) y, −x+y+1, z+1/2; (xxvii) x−y+1, x, z+1/2. |
Crystal data top
Ag0.84GeNd3S7 | Dx = 5.245 Mg m−3 |
Mr = 819.80 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 700 reflections |
Hall symbol: P 6c | θ = 4.2–26.4° |
a = 10.1930 (14) Å | µ = 20.49 mm−1 |
c = 5.7693 (12) Å | T = 295 K |
V = 519.11 (15) Å3 | Prism, dark red |
Z = 2 | 0.11 × 0.09 × 0.08 mm |
F(000) = 726 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 713 independent reflections |
Radiation source: fine-focus sealed tube | 700 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 4.2° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.093, Tmax = 0.261 | l = −7→7 |
5463 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0193P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.016 | (Δ/σ)max = 0.001 |
wR(F2) = 0.035 | Δρmax = 0.72 e Å−3 |
S = 1.08 | Δρmin = −0.75 e Å−3 |
713 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0335 (7) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 320 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.027 (19) |
Crystal data top
Ag0.84GeNd3S7 | Z = 2 |
Mr = 819.80 | Mo Kα radiation |
Hexagonal, P63 | µ = 20.49 mm−1 |
a = 10.1930 (14) Å | T = 295 K |
c = 5.7693 (12) Å | 0.11 × 0.09 × 0.08 mm |
V = 519.11 (15) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 713 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 700 reflections with I > 2σ(I) |
Tmin = 0.093, Tmax = 0.261 | Rint = 0.038 |
5463 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.016 | 1 restraint |
wR(F2) = 0.035 | Δρmax = 0.72 e Å−3 |
S = 1.08 | Δρmin = −0.75 e Å−3 |
713 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 320 Friedel pairs |
43 parameters | Absolute structure parameter: −0.027 (19) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Nd | 0.87317 (3) | 0.64140 (3) | 0.24353 (16) | 0.01001 (11) | |
Ag1 | 0.0000 | 0.0000 | 0.159 (2) | 0.053 (4) | 0.69 (2) |
Ag2 | 0.0000 | 0.0000 | 0.971 (7) | 0.029 (9) | 0.15 (2) |
Ge1 | 0.3333 | 0.6667 | 0.3272 (2) | 0.0087 (2) | |
S1 | 0.3333 | 0.6667 | 0.9504 (4) | 0.0110 (5) | |
S2 | 0.90545 (14) | 0.73476 (15) | 0.7252 (3) | 0.0140 (3) | |
S3 | 0.58466 (16) | 0.47936 (16) | 0.9818 (3) | 0.0103 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd | 0.00997 (15) | 0.00902 (15) | 0.01111 (16) | 0.00481 (11) | −0.00099 (18) | −0.00074 (16) |
Ag1 | 0.0114 (6) | 0.0114 (6) | 0.136 (11) | 0.0057 (3) | 0.000 | 0.000 |
Ag2 | 0.013 (2) | 0.013 (2) | 0.06 (3) | 0.0063 (12) | 0.000 | 0.000 |
Ge1 | 0.0094 (3) | 0.0094 (3) | 0.0072 (5) | 0.00472 (16) | 0.000 | 0.000 |
S1 | 0.0135 (8) | 0.0135 (8) | 0.0061 (13) | 0.0067 (4) | 0.000 | 0.000 |
S2 | 0.0111 (6) | 0.0188 (6) | 0.0125 (7) | 0.0078 (5) | −0.0005 (7) | −0.0023 (8) |
S3 | 0.0119 (7) | 0.0094 (6) | 0.0102 (7) | 0.0058 (6) | 0.0010 (6) | 0.0006 (6) |
Geometric parameters (Å, º) top
Nd—S3i | 2.8538 (14) | Ag2—S2xvi | 2.79 (2) |
Nd—S2ii | 2.8792 (13) | Ag2—S2xvii | 2.79 (2) |
Nd—S2iii | 2.8935 (13) | Ag2—S2xviii | 2.79 (2) |
Nd—S2 | 2.9025 (19) | Ag2—Ag2viii | 2.8846 (6) |
Nd—S3iv | 2.9664 (15) | Ag2—Ag2xi | 2.8846 (6) |
Nd—S1v | 3.0174 (11) | Ag2—Ndxviii | 3.467 (15) |
Nd—S3ii | 3.0316 (15) | Ag2—Ndxvi | 3.467 (15) |
Nd—S2iv | 3.1051 (19) | Ge1—S1iv | 2.174 (3) |
Nd—Ag1vi | 3.247 (2) | Ge1—S3iii | 2.2256 (16) |
Nd—Ag2v | 3.467 (15) | Ge1—S3xix | 2.2256 (16) |
Nd—Ag2vii | 3.576 (17) | Ge1—S3v | 2.2256 (16) |
Ag1—Ag2iv | 1.09 (3) | S1—Ge1xv | 2.174 (3) |
Ag1—Ag2viii | 1.80 (3) | S1—Ndxx | 3.0174 (11) |
Ag1—S2v | 2.404 (2) | S1—Ndxvi | 3.0174 (11) |
Ag1—S2ix | 2.404 (2) | S1—Ndxxi | 3.0174 (11) |
Ag1—S2x | 2.404 (2) | S2—Ag1xvi | 2.404 (2) |
Ag1—Ag1viii | 2.8846 (6) | S2—Ag2vi | 2.76 (2) |
Ag1—Ag1xi | 2.8846 (6) | S2—Ag2v | 2.79 (2) |
Ag1—Ndxii | 3.247 (2) | S2—Ndxxi | 2.8792 (13) |
Ag1—Ndxiii | 3.247 (2) | S2—Ndxxii | 2.8935 (13) |
Ag1—Ndxiv | 3.247 (2) | S2—Ndxv | 3.1051 (19) |
Ag2—Ag1xv | 1.09 (3) | S3—Ge1xvi | 2.2256 (16) |
Ag2—Ag1xi | 1.80 (3) | S3—Ndxxiii | 2.8538 (14) |
Ag2—S2xiii | 2.76 (2) | S3—Ndxv | 2.9664 (15) |
Ag2—S2xiv | 2.76 (2) | S3—Ndxxi | 3.0316 (15) |
Ag2—S2xii | 2.76 (2) | | |
| | | |
S3i—Nd—S2ii | 105.37 (4) | Ag1xi—Ag2—S2xiii | 59.2 (7) |
S3i—Nd—S2iii | 140.80 (5) | Ag1xv—Ag2—S2xiv | 120.8 (7) |
S2ii—Nd—S2iii | 90.81 (5) | Ag1xi—Ag2—S2xiv | 59.2 (7) |
S3i—Nd—S2 | 136.85 (4) | S2xiii—Ag2—S2xiv | 96.1 (9) |
S2ii—Nd—S2 | 80.49 (4) | Ag1xv—Ag2—S2xii | 120.8 (7) |
S2iii—Nd—S2 | 80.26 (4) | Ag1xi—Ag2—S2xii | 59.2 (7) |
S3i—Nd—S3iv | 74.70 (6) | S2xiii—Ag2—S2xii | 96.1 (9) |
S2ii—Nd—S3iv | 142.13 (5) | S2xiv—Ag2—S2xii | 96.1 (9) |
S2iii—Nd—S3iv | 70.99 (4) | Ag1xv—Ag2—S2xvi | 58.2 (7) |
S2—Nd—S3iv | 126.04 (4) | Ag1xi—Ag2—S2xvi | 121.8 (7) |
S3i—Nd—S1v | 70.38 (4) | S2xiii—Ag2—S2xvi | 179.0 (14) |
S2ii—Nd—S1v | 147.99 (4) | S2xiv—Ag2—S2xvi | 84.52 (3) |
S2iii—Nd—S1v | 112.70 (3) | S2xii—Ag2—S2xvi | 84.52 (3) |
S2—Nd—S1v | 82.43 (5) | Ag1xv—Ag2—S2xvii | 58.2 (7) |
S3iv—Nd—S1v | 68.92 (4) | Ag1xi—Ag2—S2xvii | 121.8 (7) |
S3i—Nd—S3ii | 72.75 (3) | S2xiii—Ag2—S2xvii | 84.52 (3) |
S2ii—Nd—S3ii | 68.73 (4) | S2xiv—Ag2—S2xvii | 179.0 (14) |
S2iii—Nd—S3ii | 145.91 (5) | S2xii—Ag2—S2xvii | 84.52 (3) |
S2—Nd—S3ii | 69.95 (4) | S2xvi—Ag2—S2xvii | 94.8 (9) |
S3iv—Nd—S3ii | 140.86 (4) | Ag1xv—Ag2—S2xviii | 58.2 (7) |
S1v—Nd—S3ii | 80.04 (3) | Ag1xi—Ag2—S2xviii | 121.8 (7) |
S3i—Nd—S2iv | 72.46 (4) | S2xiii—Ag2—S2xviii | 84.52 (3) |
S2ii—Nd—S2iv | 77.15 (4) | S2xiv—Ag2—S2xviii | 84.52 (3) |
S2iii—Nd—S2iv | 76.94 (4) | S2xii—Ag2—S2xviii | 179.0 (14) |
S2—Nd—S2iv | 147.60 (5) | S2xvi—Ag2—S2xviii | 94.8 (9) |
S3iv—Nd—S2iv | 66.67 (4) | S2xvii—Ag2—S2xviii | 94.8 (9) |
S1v—Nd—S2iv | 127.71 (5) | Ag1xv—Ag2—Ag2viii | 180.00 (2) |
S3ii—Nd—S2iv | 121.46 (4) | Ag1xi—Ag2—Ag2viii | 0.000 (1) |
S3i—Nd—Ag1vi | 132.9 (2) | S2xiii—Ag2—Ag2viii | 59.2 (7) |
S2ii—Nd—Ag1vi | 45.72 (3) | S2xiv—Ag2—Ag2viii | 59.2 (7) |
S2iii—Nd—Ag1vi | 45.64 (3) | S2xii—Ag2—Ag2viii | 59.2 (7) |
S2—Nd—Ag1vi | 81.9 (2) | S2xvi—Ag2—Ag2viii | 121.8 (7) |
S3iv—Nd—Ag1vi | 106.03 (13) | S2xvii—Ag2—Ag2viii | 121.8 (7) |
S1v—Nd—Ag1vi | 155.33 (14) | S2xviii—Ag2—Ag2viii | 121.8 (7) |
S3ii—Nd—Ag1vi | 111.93 (10) | Ag1xv—Ag2—Ag2xi | 0.000 (4) |
S2iv—Nd—Ag1vi | 65.7 (2) | Ag1xi—Ag2—Ag2xi | 180.000 (15) |
S3i—Nd—Ag2v | 155.8 (3) | S2xiii—Ag2—Ag2xi | 120.8 (7) |
S2ii—Nd—Ag2v | 50.6 (2) | S2xiv—Ag2—Ag2xi | 120.8 (7) |
S2iii—Nd—Ag2v | 50.5 (2) | S2xii—Ag2—Ag2xi | 120.8 (7) |
S2—Nd—Ag2v | 51.0 (6) | S2xvi—Ag2—Ag2xi | 58.2 (7) |
S3iv—Nd—Ag2v | 121.5 (2) | S2xvii—Ag2—Ag2xi | 58.2 (7) |
S1v—Nd—Ag2v | 130.2 (5) | S2xviii—Ag2—Ag2xi | 58.2 (7) |
S3ii—Nd—Ag2v | 96.6 (3) | Ag2viii—Ag2—Ag2xi | 180.000 (13) |
S2iv—Nd—Ag2v | 96.6 (6) | Ag1xv—Ag2—Ndxviii | 112.2 (6) |
Ag1vi—Nd—Ag2v | 30.8 (4) | Ag1xi—Ag2—Ndxviii | 67.8 (6) |
S3i—Nd—Ag2vii | 117.2 (5) | S2xiii—Ag2—Ndxviii | 53.6 (3) |
S2ii—Nd—Ag2vii | 49.8 (2) | S2xiv—Ag2—Ndxviii | 53.9 (3) |
S2iii—Nd—Ag2vii | 49.8 (2) | S2xii—Ag2—Ndxviii | 127.0 (13) |
S2—Nd—Ag2vii | 99.4 (6) | S2xvi—Ag2—Ndxviii | 126.48 (18) |
S3iv—Nd—Ag2vii | 95.5 (3) | S2xvii—Ag2—Ndxviii | 126.18 (18) |
S1v—Nd—Ag2vii | 160.99 (5) | S2xviii—Ag2—Ndxviii | 53.96 (9) |
S3ii—Nd—Ag2vii | 118.49 (18) | Ag2viii—Ag2—Ndxviii | 67.8 (6) |
S2iv—Nd—Ag2vii | 48.2 (6) | Ag2xi—Ag2—Ndxviii | 112.2 (6) |
Ag1vi—Nd—Ag2vii | 17.5 (3) | Ag1xv—Ag2—Ndxvi | 112.2 (6) |
Ag2v—Nd—Ag2vii | 48.32 (4) | Ag1xi—Ag2—Ndxvi | 67.8 (6) |
Ag2iv—Ag1—Ag2viii | 180.000 (4) | S2xiii—Ag2—Ndxvi | 127.0 (13) |
Ag2iv—Ag1—S2v | 99.1 (3) | S2xiv—Ag2—Ndxvi | 53.6 (3) |
Ag2viii—Ag1—S2v | 80.9 (3) | S2xii—Ag2—Ndxvi | 53.9 (3) |
Ag2iv—Ag1—S2ix | 99.1 (3) | S2xvi—Ag2—Ndxvi | 53.96 (9) |
Ag2viii—Ag1—S2ix | 80.9 (3) | S2xvii—Ag2—Ndxvi | 126.48 (18) |
S2v—Ag1—S2ix | 117.52 (16) | S2xviii—Ag2—Ndxvi | 126.18 (18) |
Ag2iv—Ag1—S2x | 99.1 (3) | Ag2viii—Ag2—Ndxvi | 67.8 (6) |
Ag2viii—Ag1—S2x | 80.9 (3) | Ag2xi—Ag2—Ndxvi | 112.2 (6) |
S2v—Ag1—S2x | 117.52 (16) | Ndxviii—Ag2—Ndxvi | 106.6 (6) |
S2ix—Ag1—S2x | 117.52 (16) | S1iv—Ge1—S3iii | 113.61 (4) |
Ag2iv—Ag1—Ag1viii | 0.000 (1) | S1iv—Ge1—S3xix | 113.61 (4) |
Ag2viii—Ag1—Ag1viii | 180.000 (5) | S3iii—Ge1—S3xix | 105.03 (5) |
S2v—Ag1—Ag1viii | 99.1 (3) | S1iv—Ge1—S3v | 113.61 (4) |
S2ix—Ag1—Ag1viii | 99.1 (3) | S3iii—Ge1—S3v | 105.03 (5) |
S2x—Ag1—Ag1viii | 99.1 (3) | S3xix—Ge1—S3v | 105.03 (5) |
Ag2iv—Ag1—Ag1xi | 180.000 (1) | Ge1xv—S1—Ndxx | 113.29 (4) |
Ag2viii—Ag1—Ag1xi | 0.000 (4) | Ge1xv—S1—Ndxvi | 113.29 (4) |
S2v—Ag1—Ag1xi | 80.9 (3) | Ndxx—S1—Ndxvi | 105.39 (5) |
S2ix—Ag1—Ag1xi | 80.9 (3) | Ge1xv—S1—Ndxxi | 113.29 (4) |
S2x—Ag1—Ag1xi | 80.9 (3) | Ndxx—S1—Ndxxi | 105.39 (5) |
Ag1viii—Ag1—Ag1xi | 180.000 (1) | Ndxvi—S1—Ndxxi | 105.39 (5) |
Ag2iv—Ag1—Ndxii | 98.6 (2) | Ag2vi—S2—Ag2v | 62.57 (3) |
Ag2viii—Ag1—Ndxii | 81.4 (2) | Ag1xvi—S2—Ndxxi | 75.25 (5) |
S2v—Ag1—Ndxii | 59.03 (5) | Ag2vi—S2—Ndxxi | 75.80 (9) |
S2ix—Ag1—Ndxii | 162.2 (5) | Ag2v—S2—Ndxxi | 78.17 (13) |
S2x—Ag1—Ndxii | 59.39 (5) | Ag1xvi—S2—Ndxxii | 74.97 (4) |
Ag1viii—Ag1—Ndxii | 98.6 (2) | Ag2vi—S2—Ndxxii | 75.57 (9) |
Ag1xi—Ag1—Ndxii | 81.4 (2) | Ag2v—S2—Ndxxii | 77.93 (13) |
Ag2iv—Ag1—Ndxiii | 98.6 (2) | Ndxxi—S2—Ndxxii | 148.84 (5) |
Ag2viii—Ag1—Ndxiii | 81.4 (2) | Ag1xvi—S2—Nd | 97.6 (3) |
S2v—Ag1—Ndxiii | 162.2 (5) | Ag2vi—S2—Nd | 137.6 (7) |
S2ix—Ag1—Ndxiii | 59.39 (5) | Ag2v—S2—Nd | 75.0 (7) |
S2x—Ag1—Ndxiii | 59.03 (5) | Ndxxi—S2—Nd | 96.58 (5) |
Ag1viii—Ag1—Ndxiii | 98.6 (2) | Ndxxii—S2—Nd | 96.26 (5) |
Ag1xi—Ag1—Ndxiii | 81.4 (2) | Ag1xvi—S2—Ndxv | 114.8 (3) |
Ndxii—Ag1—Ndxiii | 117.79 (11) | Ag2vi—S2—Ndxv | 74.8 (7) |
Ag2iv—Ag1—Ndxiv | 98.6 (2) | Ag2v—S2—Ndxv | 137.4 (7) |
Ag2viii—Ag1—Ndxiv | 81.4 (2) | Ndxxi—S2—Ndxv | 92.23 (4) |
S2v—Ag1—Ndxiv | 59.39 (5) | Ndxxii—S2—Ndxv | 91.96 (4) |
S2ix—Ag1—Ndxiv | 59.03 (5) | Nd—S2—Ndxv | 147.60 (5) |
S2x—Ag1—Ndxiv | 162.2 (5) | Ge1xvi—S3—Ndxxiii | 91.59 (5) |
Ag1viii—Ag1—Ndxiv | 98.6 (2) | Ge1xvi—S3—Ndxv | 88.68 (5) |
Ag1xi—Ag1—Ndxiv | 81.4 (2) | Ndxxiii—S3—Ndxv | 111.12 (5) |
Ndxii—Ag1—Ndxiv | 117.79 (11) | Ge1xvi—S3—Ndxxi | 120.99 (6) |
Ndxiii—Ag1—Ndxiv | 117.79 (11) | Ndxxiii—S3—Ndxxi | 140.93 (6) |
Ag1xv—Ag2—Ag1xi | 180.000 (12) | Ndxv—S3—Ndxxi | 92.03 (4) |
Ag1xv—Ag2—S2xiii | 120.8 (7) | | |
Symmetry codes: (i) −x+y+1, −x+1, z−1; (ii) x−y+1, x, z−1/2; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) −x, −y, z−1/2; (ix) y−1, −x+y, z−1/2; (x) x−y, x−1, z−1/2; (xi) −x, −y, z+1/2; (xii) −y+1, x−y, z; (xiii) x−1, y−1, z; (xiv) −x+y, −x+1, z; (xv) x, y, z+1; (xvi) −x+1, −y+1, z+1/2; (xvii) x−y, x−1, z+1/2; (xviii) y−1, −x+y, z+1/2; (xix) x−y, x, z−1/2; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) −y+1, x−y, z+1. |
Crystal data top
Ag0.74GeS7Sm3 | Dx = 5.420 Mg m−3 |
Mr = 827.34 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 601 reflections |
Hall symbol: P 6c | θ = 4.2–25.3° |
a = 10.0809 (14) Å | µ = 22.80 mm−1 |
c = 5.7604 (12) Å | T = 295 K |
V = 506.97 (15) Å3 | Prism, dark red |
Z = 2 | 0.13 × 0.11 × 0.09 mm |
F(000) = 729 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 604 independent reflections |
Radiation source: fine-focus sealed tube | 601 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 25.3°, θmin = 4.2° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −11→12 |
Tmin = 0.029, Tmax = 0.242 | l = −6→6 |
4935 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0181P)2 + 0.5015P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.014 | (Δ/σ)max = 0.001 |
wR(F2) = 0.034 | Δρmax = 0.70 e Å−3 |
S = 1.17 | Δρmin = −0.51 e Å−3 |
604 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0097 (4) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 270 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.029 (18) |
Crystal data top
Ag0.74GeS7Sm3 | Z = 2 |
Mr = 827.34 | Mo Kα radiation |
Hexagonal, P63 | µ = 22.80 mm−1 |
a = 10.0809 (14) Å | T = 295 K |
c = 5.7604 (12) Å | 0.13 × 0.11 × 0.09 mm |
V = 506.97 (15) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 604 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 601 reflections with I > 2σ(I) |
Tmin = 0.029, Tmax = 0.242 | Rint = 0.046 |
4935 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.014 | 1 restraint |
wR(F2) = 0.034 | Δρmax = 0.70 e Å−3 |
S = 1.17 | Δρmin = −0.51 e Å−3 |
604 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 270 Friedel pairs |
43 parameters | Absolute structure parameter: −0.029 (18) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sm | 0.87145 (3) | 0.64163 (2) | 0.24346 (12) | 0.00914 (12) | |
Ag1 | 0.0000 | 0.0000 | 0.137 (3) | 0.075 (5) | 0.548 (18) |
Ag2 | 0.0000 | 0.0000 | 0.967 (3) | 0.020 (4) | 0.187 (18) |
Ge1 | 0.3333 | 0.6667 | 0.32606 (16) | 0.0069 (2) | |
S1 | 0.3333 | 0.6667 | 0.9482 (4) | 0.0092 (5) | |
S2 | 0.90414 (13) | 0.73662 (14) | 0.7212 (2) | 0.0140 (3) | |
S3 | 0.58278 (15) | 0.47996 (14) | 0.9828 (2) | 0.0091 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sm | 0.00824 (15) | 0.00721 (14) | 0.01210 (17) | 0.00397 (10) | −0.00139 (13) | −0.00070 (13) |
Ag1 | 0.0095 (7) | 0.0095 (7) | 0.205 (15) | 0.0048 (4) | 0.000 | 0.000 |
Ag2 | 0.0091 (17) | 0.0091 (17) | 0.043 (11) | 0.0046 (9) | 0.000 | 0.000 |
Ge1 | 0.0076 (3) | 0.0076 (3) | 0.0055 (5) | 0.00380 (14) | 0.000 | 0.000 |
S1 | 0.0105 (7) | 0.0105 (7) | 0.0066 (12) | 0.0053 (3) | 0.000 | 0.000 |
S2 | 0.0098 (5) | 0.0202 (6) | 0.0129 (6) | 0.0082 (5) | 0.0005 (5) | −0.0028 (6) |
S3 | 0.0113 (6) | 0.0083 (6) | 0.0093 (6) | 0.0062 (5) | 0.0012 (5) | 0.0006 (5) |
Geometric parameters (Å, º) top
Sm—S3i | 2.8332 (13) | Ag2—S2xvi | 2.751 (9) |
Sm—S2ii | 2.8336 (12) | Ag2—S2xvii | 2.751 (9) |
Sm—S2iii | 2.8602 (12) | Ag2—S2xviii | 2.751 (9) |
Sm—S2 | 2.8780 (17) | Ag2—Ag2viii | 2.8802 (6) |
Sm—S3iv | 2.9389 (14) | Ag2—Ag2xi | 2.8802 (6) |
Sm—S1v | 2.9825 (10) | Ag2—Smxviii | 3.421 (6) |
Sm—S3ii | 3.0127 (13) | Ag2—Smxvi | 3.421 (6) |
Sm—S2iv | 3.1243 (17) | Ge1—S1iv | 2.177 (2) |
Sm—Ag1vi | 3.229 (3) | Ge1—S3iii | 2.2281 (14) |
Sm—Ag2v | 3.421 (6) | Ge1—S3xix | 2.2281 (14) |
Sm—Ag2vii | 3.548 (8) | Ge1—S3v | 2.2281 (14) |
Ag1—Ag2iv | 0.981 (7) | S1—Ge1xv | 2.177 (2) |
Ag1—Ag2viii | 1.899 (7) | S1—Smxx | 2.9825 (10) |
Ag1—S2v | 2.378 (4) | S1—Smxvi | 2.9825 (10) |
Ag1—S2ix | 2.378 (4) | S1—Smxxi | 2.9825 (10) |
Ag1—S2x | 2.378 (4) | S2—Ag1xvi | 2.378 (4) |
Ag1—Ag1viii | 2.8802 (6) | S2—Ag2vi | 2.724 (9) |
Ag1—Ag1xi | 2.8802 (6) | S2—Ag2v | 2.751 (9) |
Ag1—Smxii | 3.229 (3) | S2—Smxxi | 2.8336 (12) |
Ag1—Smxiii | 3.229 (3) | S2—Smxxii | 2.8602 (12) |
Ag1—Smxiv | 3.229 (3) | S2—Smxv | 3.1243 (17) |
Ag2—Ag1xv | 0.981 (7) | S3—Ge1xvi | 2.2281 (14) |
Ag2—Ag1xi | 1.899 (7) | S3—Smxxiii | 2.8332 (13) |
Ag2—S2xiii | 2.724 (9) | S3—Smxv | 2.9389 (14) |
Ag2—S2xiv | 2.724 (9) | S3—Smxxi | 3.0127 (13) |
Ag2—S2xii | 2.724 (9) | | |
| | | |
S3i—Sm—S2ii | 104.33 (4) | Ag1xi—Ag2—S2xiii | 58.7 (3) |
S3i—Sm—S2iii | 141.02 (5) | Ag1xv—Ag2—S2xiv | 121.3 (3) |
S2ii—Sm—S2iii | 90.15 (5) | Ag1xi—Ag2—S2xiv | 58.7 (3) |
S3i—Sm—S2 | 137.02 (4) | S2xiii—Ag2—S2xiv | 95.5 (4) |
S2ii—Sm—S2 | 80.83 (4) | Ag1xv—Ag2—S2xii | 121.3 (3) |
S2iii—Sm—S2 | 80.38 (4) | Ag1xi—Ag2—S2xii | 58.7 (3) |
S3i—Sm—S3iv | 75.34 (5) | S2xiii—Ag2—S2xii | 95.5 (4) |
S2ii—Sm—S3iv | 141.56 (4) | S2xiv—Ag2—S2xii | 95.5 (4) |
S2iii—Sm—S3iv | 71.24 (4) | Ag1xv—Ag2—S2xvi | 57.8 (3) |
S2—Sm—S3iv | 126.16 (4) | Ag1xi—Ag2—S2xvi | 122.2 (3) |
S3i—Sm—S1v | 70.70 (4) | S2xiii—Ag2—S2xvi | 179.1 (6) |
S2ii—Sm—S1v | 148.01 (4) | S2xiv—Ag2—S2xvi | 85.13 (2) |
S2iii—Sm—S1v | 113.86 (3) | S2xii—Ag2—S2xvi | 85.13 (2) |
S2—Sm—S1v | 82.71 (5) | Ag1xv—Ag2—S2xvii | 57.8 (3) |
S3iv—Sm—S1v | 69.31 (4) | Ag1xi—Ag2—S2xvii | 122.2 (3) |
S3i—Sm—S3ii | 72.32 (3) | S2xiii—Ag2—S2xvii | 85.13 (2) |
S2ii—Sm—S3ii | 69.33 (3) | S2xiv—Ag2—S2xvii | 179.1 (6) |
S2iii—Sm—S3ii | 145.90 (4) | S2xii—Ag2—S2xvii | 85.13 (2) |
S2—Sm—S3ii | 69.94 (4) | S2xvi—Ag2—S2xvii | 94.2 (4) |
S3iv—Sm—S3ii | 140.72 (3) | Ag1xv—Ag2—S2xviii | 57.8 (3) |
S1v—Sm—S3ii | 79.31 (3) | Ag1xi—Ag2—S2xviii | 122.2 (3) |
S3i—Sm—S2iv | 72.34 (4) | S2xiii—Ag2—S2xviii | 85.13 (2) |
S2ii—Sm—S2iv | 76.69 (4) | S2xiv—Ag2—S2xviii | 85.13 (2) |
S2iii—Sm—S2iv | 76.31 (4) | S2xii—Ag2—S2xviii | 179.1 (6) |
S2—Sm—S2iv | 147.33 (5) | S2xvi—Ag2—S2xviii | 94.2 (4) |
S3iv—Sm—S2iv | 66.51 (4) | S2xvii—Ag2—S2xviii | 94.2 (4) |
S1v—Sm—S2iv | 127.74 (5) | Ag1xv—Ag2—Ag2viii | 180.000 (16) |
S3ii—Sm—S2iv | 121.84 (3) | Ag1xi—Ag2—Ag2viii | 0.000 (1) |
S3i—Sm—Ag1vi | 130.3 (3) | S2xiii—Ag2—Ag2viii | 58.7 (3) |
S2ii—Sm—Ag1vi | 45.60 (4) | S2xiv—Ag2—Ag2viii | 58.7 (3) |
S2iii—Sm—Ag1vi | 45.47 (4) | S2xii—Ag2—Ag2viii | 58.7 (3) |
S2—Sm—Ag1vi | 83.9 (3) | S2xvi—Ag2—Ag2viii | 122.2 (3) |
S3iv—Sm—Ag1vi | 104.81 (18) | S2xvii—Ag2—Ag2viii | 122.2 (3) |
S1v—Sm—Ag1vi | 157.29 (18) | S2xviii—Ag2—Ag2viii | 122.2 (3) |
S3ii—Sm—Ag1vi | 112.96 (14) | Ag1xv—Ag2—Ag2xi | 0.000 (4) |
S2iv—Sm—Ag1vi | 63.4 (3) | Ag1xi—Ag2—Ag2xi | 180.000 (8) |
S3i—Sm—Ag2v | 154.81 (13) | S2xiii—Ag2—Ag2xi | 121.3 (3) |
S2ii—Sm—Ag2v | 50.57 (10) | S2xiv—Ag2—Ag2xi | 121.3 (3) |
S2iii—Sm—Ag2v | 50.43 (10) | S2xii—Ag2—Ag2xi | 121.3 (3) |
S2—Sm—Ag2v | 50.9 (3) | S2xvi—Ag2—Ag2xi | 57.8 (3) |
S3iv—Sm—Ag2v | 121.66 (11) | S2xvii—Ag2—Ag2xi | 57.8 (3) |
S1v—Sm—Ag2v | 130.6 (2) | S2xviii—Ag2—Ag2xi | 57.8 (3) |
S3ii—Sm—Ag2v | 96.56 (15) | Ag2viii—Ag2—Ag2xi | 180.000 (5) |
S2iv—Sm—Ag2v | 96.4 (3) | Ag1xv—Ag2—Smxviii | 112.1 (3) |
Ag1vi—Sm—Ag2v | 33.03 (12) | Ag1xi—Ag2—Smxviii | 67.9 (3) |
S3i—Sm—Ag2vii | 116.2 (2) | S2xiii—Ag2—Smxviii | 53.47 (13) |
S2ii—Sm—Ag2vii | 49.52 (9) | S2xiv—Ag2—Smxviii | 54.05 (14) |
S2iii—Sm—Ag2vii | 49.42 (9) | S2xii—Ag2—Smxviii | 126.6 (6) |
S2—Sm—Ag2vii | 99.7 (2) | S2xvi—Ag2—Smxviii | 126.61 (9) |
S3iv—Sm—Ag2vii | 95.24 (15) | S2xvii—Ag2—Smxviii | 126.04 (9) |
S1v—Sm—Ag2vii | 161.57 (3) | S2xviii—Ag2—Smxviii | 54.29 (4) |
S3ii—Sm—Ag2vii | 118.78 (8) | Ag2viii—Ag2—Smxviii | 67.9 (3) |
S2iv—Sm—Ag2vii | 47.7 (2) | Ag2xi—Ag2—Smxviii | 112.1 (3) |
Ag1vi—Sm—Ag2vii | 15.75 (13) | Ag1xv—Ag2—Smxvi | 112.1 (3) |
Ag2v—Sm—Ag2vii | 48.78 (2) | Ag1xi—Ag2—Smxvi | 67.9 (3) |
Ag2iv—Ag1—Ag2viii | 180.000 (2) | S2xiii—Ag2—Smxvi | 126.6 (6) |
Ag2iv—Ag1—S2v | 101.8 (4) | S2xiv—Ag2—Smxvi | 53.47 (13) |
Ag2viii—Ag1—S2v | 78.2 (4) | S2xii—Ag2—Smxvi | 54.05 (14) |
Ag2iv—Ag1—S2ix | 101.8 (4) | S2xvi—Ag2—Smxvi | 54.29 (4) |
Ag2viii—Ag1—S2ix | 78.2 (4) | S2xvii—Ag2—Smxvi | 126.61 (9) |
S2v—Ag1—S2ix | 116.0 (3) | S2xviii—Ag2—Smxvi | 126.04 (9) |
Ag2iv—Ag1—S2x | 101.8 (4) | Ag2viii—Ag2—Smxvi | 67.9 (3) |
Ag2viii—Ag1—S2x | 78.2 (4) | Ag2xi—Ag2—Smxvi | 112.1 (3) |
S2v—Ag1—S2x | 116.0 (3) | Smxviii—Ag2—Smxvi | 106.7 (3) |
S2ix—Ag1—S2x | 116.0 (3) | S1iv—Ge1—S3iii | 113.90 (4) |
Ag2iv—Ag1—Ag1viii | 0.000 (1) | S1iv—Ge1—S3xix | 113.90 (4) |
Ag2viii—Ag1—Ag1viii | 180.000 (2) | S3iii—Ge1—S3xix | 104.71 (5) |
S2v—Ag1—Ag1viii | 101.8 (4) | S1iv—Ge1—S3v | 113.90 (4) |
S2ix—Ag1—Ag1viii | 101.8 (4) | S3iii—Ge1—S3v | 104.71 (5) |
S2x—Ag1—Ag1viii | 101.8 (4) | S3xix—Ge1—S3v | 104.71 (5) |
Ag2iv—Ag1—Ag1xi | 180.000 (1) | Ge1xv—S1—Smxx | 113.29 (4) |
Ag2viii—Ag1—Ag1xi | 0.000 (1) | Ge1xv—S1—Smxvi | 113.29 (4) |
S2v—Ag1—Ag1xi | 78.2 (4) | Smxx—S1—Smxvi | 105.40 (5) |
S2ix—Ag1—Ag1xi | 78.2 (4) | Ge1xv—S1—Smxxi | 113.29 (4) |
S2x—Ag1—Ag1xi | 78.2 (4) | Smxx—S1—Smxxi | 105.40 (5) |
Ag1viii—Ag1—Ag1xi | 180.000 (2) | Smxvi—S1—Smxxi | 105.40 (5) |
Ag2iv—Ag1—Smxii | 100.9 (3) | Ag2vi—S2—Ag2v | 63.49 (3) |
Ag2viii—Ag1—Smxii | 79.1 (3) | Ag1xvi—S2—Smxxi | 76.01 (6) |
S2v—Ag1—Smxii | 58.38 (8) | Ag2vi—S2—Smxxi | 75.96 (5) |
S2ix—Ag1—Smxii | 59.04 (8) | Ag2v—S2—Smxxi | 78.89 (7) |
S2x—Ag1—Smxii | 157.3 (7) | Ag1xvi—S2—Smxxii | 75.49 (6) |
Ag1viii—Ag1—Smxii | 100.9 (3) | Ag2vi—S2—Smxxii | 75.52 (5) |
Ag1xi—Ag1—Smxii | 79.1 (3) | Ag2v—S2—Smxxii | 78.43 (7) |
Ag2iv—Ag1—Smxiii | 100.9 (3) | Smxxi—S2—Smxxii | 149.30 (5) |
Ag2viii—Ag1—Smxiii | 79.1 (3) | Ag1xvi—S2—Sm | 95.3 (4) |
S2v—Ag1—Smxiii | 157.3 (7) | Ag2vi—S2—Sm | 138.3 (3) |
S2ix—Ag1—Smxiii | 58.38 (8) | Ag2v—S2—Sm | 74.8 (3) |
S2x—Ag1—Smxiii | 59.04 (8) | Smxxi—S2—Sm | 97.16 (4) |
Ag1viii—Ag1—Smxiii | 100.9 (3) | Smxxii—S2—Sm | 96.56 (4) |
Ag1xi—Ag1—Smxiii | 79.1 (3) | Ag1xvi—S2—Smxv | 117.4 (4) |
Smxii—Ag1—Smxiii | 116.48 (19) | Ag2vi—S2—Smxv | 74.4 (3) |
Ag2iv—Ag1—Smxiv | 100.9 (3) | Ag2v—S2—Smxv | 137.8 (3) |
Ag2viii—Ag1—Smxiv | 79.1 (3) | Smxxi—S2—Smxv | 91.80 (4) |
S2v—Ag1—Smxiv | 59.04 (8) | Smxxii—S2—Smxv | 91.29 (4) |
S2ix—Ag1—Smxiv | 157.3 (7) | Sm—S2—Smxv | 147.33 (5) |
S2x—Ag1—Smxiv | 58.38 (8) | Ge1xvi—S3—Smxxiii | 91.34 (4) |
Ag1viii—Ag1—Smxiv | 100.9 (3) | Ge1xvi—S3—Smxv | 88.62 (4) |
Ag1xi—Ag1—Smxiv | 79.1 (3) | Smxxiii—S3—Smxv | 110.57 (5) |
Smxii—Ag1—Smxiv | 116.48 (19) | Ge1xvi—S3—Smxxi | 120.21 (6) |
Smxiii—Ag1—Smxiv | 116.48 (19) | Smxxiii—S3—Smxxi | 142.07 (5) |
Ag1xv—Ag2—Ag1xi | 180.000 (18) | Smxv—S3—Smxxi | 92.04 (4) |
Ag1xv—Ag2—S2xiii | 121.3 (3) | | |
Symmetry codes: (i) −x+y+1, −x+1, z−1; (ii) x−y+1, x, z−1/2; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) −x, −y, z−1/2; (ix) x−y, x−1, z−1/2; (x) y−1, −x+y, z−1/2; (xi) −x, −y, z+1/2; (xii) −y+1, x−y, z; (xiii) x−1, y−1, z; (xiv) −x+y, −x+1, z; (xv) x, y, z+1; (xvi) −x+1, −y+1, z+1/2; (xvii) x−y, x−1, z+1/2; (xviii) y−1, −x+y, z+1/2; (xix) x−y, x, z−1/2; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) −y+1, x−y, z+1. |
Crystal data top
Ag0.63Gd3GeS7 | Dx = 5.602 Mg m−3 |
Mr = 836.18 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 657 reflections |
Hall symbol: P 6c | θ = 4.3–26.2° |
a = 9.9637 (14) Å | µ = 25.41 mm−1 |
c = 5.7660 (12) Å | T = 295 K |
V = 495.73 (14) Å3 | Prism, dark red |
Z = 2 | 0.13 × 0.12 × 0.10 mm |
F(000) = 731 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 658 independent reflections |
Radiation source: fine-focus sealed tube | 657 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.2°, θmin = 4.3° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→9 |
Tmin = 0.024, Tmax = 0.192 | l = −7→7 |
5095 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0143P)2 + 0.2664P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.013 | (Δ/σ)max = 0.001 |
wR(F2) = 0.029 | Δρmax = 0.58 e Å−3 |
S = 1.12 | Δρmin = −0.81 e Å−3 |
658 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 0.0047 (3) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 296 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.006 (15) |
Crystal data top
Ag0.63Gd3GeS7 | Z = 2 |
Mr = 836.18 | Mo Kα radiation |
Hexagonal, P63 | µ = 25.41 mm−1 |
a = 9.9637 (14) Å | T = 295 K |
c = 5.7660 (12) Å | 0.13 × 0.12 × 0.10 mm |
V = 495.73 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 658 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 657 reflections with I > 2σ(I) |
Tmin = 0.024, Tmax = 0.192 | Rint = 0.044 |
5095 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.013 | 1 restraint |
wR(F2) = 0.029 | Δρmax = 0.58 e Å−3 |
S = 1.12 | Δρmin = −0.81 e Å−3 |
658 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 296 Friedel pairs |
43 parameters | Absolute structure parameter: 0.006 (15) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Gd | 0.86849 (2) | 0.64152 (2) | 0.24476 (11) | 0.01184 (9) | |
Ag1 | 0.0000 | 0.0000 | 0.085 (4) | 0.093 (5) | 0.50 (2) |
Ag2 | 0.0000 | 0.0000 | 0.9545 (16) | 0.014 (4) | 0.12 (2) |
Ge1 | 0.3333 | 0.6667 | 0.32630 (13) | 0.00836 (18) | |
S1 | 0.3333 | 0.6667 | 0.9488 (3) | 0.0104 (4) | |
S2 | 0.90148 (13) | 0.73723 (14) | 0.7161 (2) | 0.0172 (3) | |
S3 | 0.58053 (14) | 0.47996 (13) | 0.9842 (2) | 0.0106 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Gd | 0.00971 (12) | 0.00902 (11) | 0.01695 (12) | 0.00480 (8) | −0.00176 (12) | −0.00048 (12) |
Ag1 | 0.0102 (9) | 0.0102 (9) | 0.258 (16) | 0.0051 (4) | 0.000 | 0.000 |
Ag2 | 0.011 (3) | 0.011 (3) | 0.020 (12) | 0.0055 (13) | 0.000 | 0.000 |
Ge1 | 0.0092 (2) | 0.0092 (2) | 0.0068 (3) | 0.00458 (12) | 0.000 | 0.000 |
S1 | 0.0117 (6) | 0.0117 (6) | 0.0077 (9) | 0.0058 (3) | 0.000 | 0.000 |
S2 | 0.0114 (5) | 0.0237 (6) | 0.0182 (7) | 0.0100 (5) | −0.0006 (5) | −0.0076 (6) |
S3 | 0.0135 (6) | 0.0104 (5) | 0.0099 (4) | 0.0073 (5) | 0.0003 (5) | 0.0003 (5) |
Geometric parameters (Å, º) top
Gd—S2i | 2.7906 (12) | Ag2—S2xiii | 2.672 (5) |
Gd—S3ii | 2.8160 (12) | Ag2—S2xiv | 2.672 (5) |
Gd—S2iii | 2.8309 (12) | Ag2—S2viii | 2.743 (5) |
Gd—S2 | 2.8443 (14) | Ag2—S2xvii | 2.743 (5) |
Gd—S3iv | 2.9090 (13) | Ag2—S2xviii | 2.743 (5) |
Gd—S1v | 2.9466 (9) | Ag2—Ag2ix | 2.8830 (6) |
Gd—S3i | 3.0045 (12) | Ag2—Ag2xii | 2.8830 (6) |
Gd—S2iv | 3.1616 (15) | Ag2—Gdxviii | 3.355 (3) |
Gd—Ag1vi | 3.263 (7) | Ag2—Gdxvii | 3.355 (3) |
Gd—Ag2v | 3.355 (4) | Ge1—S1iv | 2.1765 (19) |
Gd—Ag2vii | 3.549 (5) | Ge1—S3iii | 2.2256 (13) |
Gd—Ag1viii | 3.693 (14) | Ge1—S3xix | 2.2256 (13) |
Ag1—Ag2iv | 0.75 (2) | Ge1—S3v | 2.2256 (12) |
Ag1—Ag2ix | 2.13 (2) | S1—Ge1xvi | 2.1765 (19) |
Ag1—S2v | 2.413 (8) | S1—Gdxx | 2.9466 (9) |
Ag1—S2x | 2.413 (8) | S1—Gdviii | 2.9466 (9) |
Ag1—S2xi | 2.413 (8) | S1—Gdxxi | 2.9466 (9) |
Ag1—Ag1ix | 2.8830 (6) | S2—Ag1viii | 2.413 (8) |
Ag1—Ag1xii | 2.8830 (6) | S2—Ag2vi | 2.672 (5) |
Ag1—Gdxiii | 3.263 (7) | S2—Ag2v | 2.743 (5) |
Ag1—Gdxiv | 3.263 (7) | S2—Gdxxi | 2.7906 (11) |
Ag1—Gdxv | 3.263 (7) | S2—Gdxxii | 2.8309 (12) |
Ag1—Gdx | 3.693 (14) | S2—Gdxvi | 3.1616 (15) |
Ag1—Gdxi | 3.693 (14) | S3—Ge1viii | 2.2256 (12) |
Ag2—Ag1xvi | 0.75 (2) | S3—Gdxxiii | 2.8160 (12) |
Ag2—Ag1xii | 2.13 (2) | S3—Gdxvi | 2.9090 (13) |
Ag2—S2xv | 2.672 (5) | S3—Gdxxi | 3.0045 (12) |
| | | |
S2i—Gd—S3ii | 102.59 (4) | Gdxiii—Ag1—Gdx | 164.3 (8) |
S2i—Gd—S2iii | 89.80 (5) | Gdxiv—Ag1—Gdx | 75.14 (11) |
S3ii—Gd—S2iii | 140.84 (4) | Gdxv—Ag1—Gdx | 75.14 (11) |
S2i—Gd—S2 | 81.61 (4) | Ag2iv—Ag1—Gdxi | 57.9 (3) |
S3ii—Gd—S2 | 137.18 (4) | Ag2ix—Ag1—Gdxi | 122.1 (3) |
S2iii—Gd—S2 | 80.91 (3) | S2v—Ag1—Gdxi | 124.2 (3) |
S2i—Gd—S3iv | 140.77 (4) | S2x—Ag1—Gdxi | 125.1 (3) |
S3ii—Gd—S3iv | 75.80 (5) | S2xi—Ag1—Gdxi | 50.4 (2) |
S2iii—Gd—S3iv | 71.53 (3) | Ag1ix—Ag1—Gdxi | 57.9 (3) |
S2—Gd—S3iv | 126.56 (3) | Ag1xii—Ag1—Gdxi | 122.1 (3) |
S2i—Gd—S1v | 147.63 (3) | Gdxiii—Ag1—Gdxi | 75.14 (11) |
S3ii—Gd—S1v | 71.34 (4) | Gdxiv—Ag1—Gdxi | 164.3 (8) |
S2iii—Gd—S1v | 115.33 (3) | Gdxv—Ag1—Gdxi | 75.14 (11) |
S2—Gd—S1v | 82.65 (4) | Gdx—Ag1—Gdxi | 94.4 (5) |
S3iv—Gd—S1v | 70.08 (4) | Ag1xvi—Ag2—Ag1xii | 180.00 (3) |
S2i—Gd—S3i | 69.67 (3) | Ag1xvi—Ag2—S2xv | 120.96 (18) |
S3ii—Gd—S3i | 71.86 (2) | Ag1xii—Ag2—S2xv | 59.04 (17) |
S2iii—Gd—S3i | 146.14 (4) | Ag1xvi—Ag2—S2xiii | 120.96 (17) |
S2—Gd—S3i | 69.95 (3) | Ag1xii—Ag2—S2xiii | 59.04 (17) |
S3iv—Gd—S3i | 140.47 (3) | S2xv—Ag2—S2xiii | 95.9 (2) |
S1v—Gd—S3i | 78.40 (3) | Ag1xvi—Ag2—S2xiv | 120.96 (18) |
S2i—Gd—S2iv | 76.15 (3) | Ag1xii—Ag2—S2xiv | 59.04 (17) |
S3ii—Gd—S2iv | 71.75 (3) | S2xv—Ag2—S2xiv | 95.9 (2) |
S2iii—Gd—S2iv | 75.61 (3) | S2xiii—Ag2—S2xiv | 95.9 (2) |
S2—Gd—S2iv | 147.45 (5) | Ag1xvi—Ag2—S2viii | 56.64 (17) |
S3iv—Gd—S2iv | 66.04 (3) | Ag1xii—Ag2—S2viii | 123.36 (17) |
S1v—Gd—S2iv | 127.82 (4) | S2xv—Ag2—S2viii | 177.6 (3) |
S3i—Gd—S2iv | 121.97 (3) | S2xiii—Ag2—S2viii | 85.69 (2) |
S2i—Gd—Ag1vi | 46.17 (9) | S2xiv—Ag2—S2viii | 85.69 (2) |
S3ii—Gd—Ag1vi | 124.6 (4) | Ag1xvi—Ag2—S2xvii | 56.64 (16) |
S2iii—Gd—Ag1vi | 45.98 (9) | Ag1xii—Ag2—S2xvii | 123.36 (17) |
S2—Gd—Ag1vi | 89.3 (4) | S2xv—Ag2—S2xvii | 85.69 (2) |
S3iv—Gd—Ag1vi | 101.8 (3) | S2xiii—Ag2—S2xvii | 85.69 (2) |
S1v—Gd—Ag1vi | 160.90 (19) | S2xiv—Ag2—S2xvii | 177.6 (3) |
S3i—Gd—Ag1vi | 115.01 (18) | S2viii—Ag2—S2xvii | 92.7 (2) |
S2iv—Gd—Ag1vi | 58.2 (4) | Ag1xvi—Ag2—S2xviii | 56.64 (16) |
S2i—Gd—Ag2v | 50.52 (6) | Ag1xii—Ag2—S2xviii | 123.36 (16) |
S3ii—Gd—Ag2v | 152.98 (8) | S2xv—Ag2—S2xviii | 85.69 (2) |
S2iii—Gd—Ag2v | 50.30 (6) | S2xiii—Ag2—S2xviii | 177.6 (3) |
S2—Gd—Ag2v | 51.72 (15) | S2xiv—Ag2—S2xviii | 85.69 (2) |
S3iv—Gd—Ag2v | 121.83 (7) | S2viii—Ag2—S2xviii | 92.7 (2) |
S1v—Gd—Ag2v | 131.70 (15) | S2xvii—Ag2—S2xviii | 92.7 (2) |
S3i—Gd—Ag2v | 96.85 (9) | Ag1xvi—Ag2—Ag2ix | 180.00 (2) |
S2iv—Gd—Ag2v | 95.74 (15) | Ag1xii—Ag2—Ag2ix | 0.000 (3) |
Ag1vi—Gd—Ag2v | 37.5 (3) | S2xv—Ag2—Ag2ix | 59.04 (17) |
S2i—Gd—Ag2vii | 49.52 (5) | S2xiii—Ag2—Ag2ix | 59.04 (17) |
S3ii—Gd—Ag2vii | 114.12 (13) | S2xiv—Ag2—Ag2ix | 59.04 (17) |
S2iii—Gd—Ag2vii | 49.37 (5) | S2viii—Ag2—Ag2ix | 123.36 (17) |
S2—Gd—Ag2vii | 100.99 (14) | S2xvii—Ag2—Ag2ix | 123.36 (17) |
S3iv—Gd—Ag2vii | 94.53 (9) | S2xviii—Ag2—Ag2ix | 123.36 (16) |
S1v—Gd—Ag2vii | 162.42 (3) | Ag1xvi—Ag2—Ag2xii | 0.000 (12) |
S3i—Gd—Ag2vii | 119.08 (5) | Ag1xii—Ag2—Ag2xii | 180.000 (5) |
S2iv—Gd—Ag2vii | 46.48 (14) | S2xv—Ag2—Ag2xii | 120.96 (18) |
Ag1vi—Gd—Ag2vii | 11.7 (3) | S2xiii—Ag2—Ag2xii | 120.96 (17) |
Ag2v—Gd—Ag2vii | 49.26 (2) | S2xiv—Ag2—Ag2xii | 120.96 (17) |
S2i—Gd—Ag1viii | 55.56 (18) | S2viii—Ag2—Ag2xii | 56.64 (17) |
S3ii—Gd—Ag1viii | 156.62 (6) | S2xvii—Ag2—Ag2xii | 56.64 (17) |
S2iii—Gd—Ag1viii | 55.37 (18) | S2xviii—Ag2—Ag2xii | 56.64 (17) |
S2—Gd—Ag1viii | 40.8 (3) | Ag2ix—Ag2—Ag2xii | 180.000 (3) |
S3iv—Gd—Ag1viii | 125.75 (11) | Ag1xvi—Ag2—Gdxviii | 111.13 (16) |
S1v—Gd—Ag1viii | 121.5 (3) | Ag1xii—Ag2—Gdxviii | 68.87 (15) |
S3i—Gd—Ag1viii | 90.9 (2) | S2xv—Ag2—Gdxviii | 53.72 (8) |
S2iv—Gd—Ag1viii | 106.7 (3) | S2xiii—Ag2—Gdxviii | 127.9 (3) |
Ag1vi—Gd—Ag1viii | 48.49 (10) | S2xiv—Ag2—Gdxviii | 54.62 (8) |
Ag2v—Gd—Ag1viii | 10.9 (2) | S2viii—Ag2—Gdxviii | 126.43 (6) |
Ag2vii—Gd—Ag1viii | 60.2 (3) | S2xvii—Ag2—Gdxviii | 125.56 (6) |
Ag2iv—Ag1—Ag2ix | 180.000 (1) | S2xviii—Ag2—Gdxviii | 54.49 (3) |
Ag2iv—Ag1—S2v | 108.3 (6) | Ag2ix—Ag2—Gdxviii | 68.87 (15) |
Ag2ix—Ag1—S2v | 71.7 (6) | Ag2xii—Ag2—Gdxviii | 111.13 (15) |
Ag2iv—Ag1—S2x | 108.3 (6) | Ag1xvi—Ag2—Gdxvii | 111.13 (15) |
Ag2ix—Ag1—S2x | 71.7 (6) | Ag1xii—Ag2—Gdxvii | 68.87 (15) |
S2v—Ag1—S2x | 110.6 (6) | S2xv—Ag2—Gdxvii | 54.62 (8) |
Ag2iv—Ag1—S2xi | 108.3 (6) | S2xiii—Ag2—Gdxvii | 53.72 (8) |
Ag2ix—Ag1—S2xi | 71.7 (6) | S2xiv—Ag2—Gdxvii | 127.9 (3) |
S2v—Ag1—S2xi | 110.6 (6) | S2viii—Ag2—Gdxvii | 125.56 (6) |
S2x—Ag1—S2xi | 110.6 (6) | S2xvii—Ag2—Gdxvii | 54.49 (3) |
Ag2iv—Ag1—Ag1ix | 0.000 (1) | S2xviii—Ag2—Gdxvii | 126.43 (6) |
Ag2ix—Ag1—Ag1ix | 180.000 (1) | Ag2ix—Ag2—Gdxvii | 68.87 (15) |
S2v—Ag1—Ag1ix | 108.3 (6) | Ag2xii—Ag2—Gdxvii | 111.13 (15) |
S2x—Ag1—Ag1ix | 108.3 (6) | Gdxviii—Ag2—Gdxvii | 107.77 (16) |
S2xi—Ag1—Ag1ix | 108.3 (6) | S1iv—Ge1—S3iii | 114.14 (3) |
Ag2iv—Ag1—Ag1xii | 180.000 (2) | S1iv—Ge1—S3xix | 114.14 (3) |
Ag2ix—Ag1—Ag1xii | 0.000 (1) | S3iii—Ge1—S3xix | 104.42 (4) |
S2v—Ag1—Ag1xii | 71.7 (6) | S1iv—Ge1—S3v | 114.14 (3) |
S2x—Ag1—Ag1xii | 71.7 (6) | S3iii—Ge1—S3v | 104.42 (4) |
S2xi—Ag1—Ag1xii | 71.7 (6) | S3xix—Ge1—S3v | 104.42 (4) |
Ag1ix—Ag1—Ag1xii | 180.000 (2) | Ge1xvi—S1—Gdxx | 113.54 (3) |
Ag2iv—Ag1—Gdxiii | 106.4 (4) | Ge1xvi—S1—Gdviii | 113.54 (3) |
Ag2ix—Ag1—Gdxiii | 73.6 (4) | Gdxx—S1—Gdviii | 105.12 (4) |
S2v—Ag1—Gdxiii | 56.55 (17) | Ge1xvi—S1—Gdxxi | 113.54 (3) |
S2x—Ag1—Gdxiii | 145.3 (10) | Gdxx—S1—Gdxxi | 105.12 (4) |
S2xi—Ag1—Gdxiii | 57.53 (17) | Gdviii—S1—Gdxxi | 105.12 (4) |
Ag1ix—Ag1—Gdxiii | 106.4 (4) | Ag1viii—S2—Ag2vi | 49.2 (5) |
Ag1xii—Ag1—Gdxiii | 73.6 (4) | Ag2vi—S2—Ag2v | 64.33 (3) |
Ag2iv—Ag1—Gdxiv | 106.4 (4) | Ag1viii—S2—Gdxxi | 77.28 (9) |
Ag2ix—Ag1—Gdxiv | 73.6 (4) | Ag2vi—S2—Gdxxi | 75.76 (3) |
S2v—Ag1—Gdxiv | 57.53 (17) | Ag2v—S2—Gdxxi | 79.78 (5) |
S2x—Ag1—Gdxiv | 56.55 (17) | Ag1viii—S2—Gdxxii | 76.49 (10) |
S2xi—Ag1—Gdxiv | 145.3 (10) | Ag2vi—S2—Gdxxii | 75.08 (4) |
Ag1ix—Ag1—Gdxiv | 106.4 (4) | Ag2v—S2—Gdxxii | 79.08 (5) |
Ag1xii—Ag1—Gdxiv | 73.6 (4) | Gdxxi—S2—Gdxxii | 149.27 (5) |
Gdxiii—Ag1—Gdxiv | 112.3 (4) | Ag1viii—S2—Gd | 88.9 (6) |
Ag2iv—Ag1—Gdxv | 106.4 (4) | Ag2vi—S2—Gd | 138.11 (18) |
Ag2ix—Ag1—Gdxv | 73.6 (4) | Ag2v—S2—Gd | 73.78 (17) |
S2v—Ag1—Gdxv | 145.3 (10) | Gdxxi—S2—Gd | 98.07 (4) |
S2x—Ag1—Gdxv | 57.53 (17) | Gdxxii—S2—Gd | 97.14 (4) |
S2xi—Ag1—Gdxv | 56.55 (17) | Ag1viii—S2—Gdxvi | 123.7 (6) |
Ag1ix—Ag1—Gdxv | 106.4 (4) | Ag2vi—S2—Gdxvi | 74.42 (18) |
Ag1xii—Ag1—Gdxv | 73.6 (4) | Ag2v—S2—Gdxvi | 138.74 (17) |
Gdxiii—Ag1—Gdxv | 112.3 (4) | Gdxxi—S2—Gdxvi | 91.05 (3) |
Gdxiv—Ag1—Gdxv | 112.3 (4) | Gdxxii—S2—Gdxvi | 90.31 (3) |
Ag2iv—Ag1—Gdx | 57.9 (3) | Gd—S2—Gdxvi | 147.45 (5) |
Ag2ix—Ag1—Gdx | 122.1 (3) | Ge1viii—S3—Gdxxiii | 91.08 (4) |
S2v—Ag1—Gdx | 125.1 (3) | Ge1viii—S3—Gdxvi | 88.69 (4) |
S2x—Ag1—Gdx | 50.4 (2) | Gdxxiii—S3—Gdxvi | 109.62 (4) |
S2xi—Ag1—Gdx | 124.2 (3) | Ge1viii—S3—Gdxxi | 119.54 (5) |
Ag1ix—Ag1—Gdx | 57.9 (3) | Gdxxiii—S3—Gdxxi | 143.30 (4) |
Ag1xii—Ag1—Gdx | 122.1 (3) | Gdxvi—S3—Gdxxi | 92.02 (3) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) −x+y+1, −x+1, z−1; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) x+1, y+1, z−1; (viii) −x+1, −y+1, z+1/2; (ix) −x, −y, z−1/2; (x) y−1, −x+y, z−1/2; (xi) x−y, x−1, z−1/2; (xii) −x, −y, z+1/2; (xiii) −y+1, x−y, z; (xiv) −x+y, −x+1, z; (xv) x−1, y−1, z; (xvi) x, y, z+1; (xvii) x−y, x−1, z+1/2; (xviii) y−1, −x+y, z+1/2; (xix) x−y, x, z−1/2; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) −y+1, x−y, z+1. |
Crystal data top
Ag0.59GeS7Tb3 | Dx = 5.679 Mg m−3 |
Mr = 836.87 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 597 reflections |
Hall symbol: P 6c | θ = 4.1–25.6° |
a = 9.9003 (14) Å | µ = 27.01 mm−1 |
c = 5.7654 (12) Å | T = 295 K |
V = 489.39 (14) Å3 | Prism, dark red |
Z = 2 | 0.12 × 0.11 × 0.08 mm |
F(000) = 733 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 602 independent reflections |
Radiation source: fine-focus sealed tube | 597 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 25.6°, θmin = 4.1° |
ω–scan | h = −10→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.044, Tmax = 0.187 | l = −7→6 |
4229 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0175P)2 + 1.1981P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.001 |
wR(F2) = 0.038 | Δρmax = 0.84 e Å−3 |
S = 1.17 | Δρmin = −1.39 e Å−3 |
602 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
39 parameters | Extinction coefficient: 0.0055 (3) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (2) |
Crystal data top
Ag0.59GeS7Tb3 | Z = 2 |
Mr = 836.87 | Mo Kα radiation |
Hexagonal, P63 | µ = 27.01 mm−1 |
a = 9.9003 (14) Å | T = 295 K |
c = 5.7654 (12) Å | 0.12 × 0.11 × 0.08 mm |
V = 489.39 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 602 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 597 reflections with I > 2σ(I) |
Tmin = 0.044, Tmax = 0.187 | Rint = 0.039 |
4229 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.017 | 1 restraint |
wR(F2) = 0.038 | Δρmax = 0.84 e Å−3 |
S = 1.17 | Δρmin = −1.39 e Å−3 |
602 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs |
39 parameters | Absolute structure parameter: 0.00 (2) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Tb | 0.86677 (3) | 0.64133 (3) | 0.25005 (13) | 0.01415 (13) | |
Ag2 | 0.0000 | 0.0000 | 0.0324 (9) | 0.0939 (17) | 0.586 (6) |
Ge1 | 0.3333 | 0.6667 | 0.33058 (18) | 0.0103 (3) | |
S1 | 0.3333 | 0.6667 | 0.9534 (5) | 0.0108 (6) | |
S2 | 0.90025 (18) | 0.7379 (2) | 0.7165 (3) | 0.0192 (4) | |
S3 | 0.57908 (19) | 0.47987 (18) | 0.9894 (3) | 0.0120 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tb | 0.01170 (17) | 0.01089 (16) | 0.0201 (2) | 0.00580 (11) | −0.00178 (17) | −0.00055 (17) |
Ag2 | 0.0111 (8) | 0.0111 (8) | 0.260 (5) | 0.0055 (4) | 0.000 | 0.000 |
Ge1 | 0.0112 (4) | 0.0112 (4) | 0.0084 (6) | 0.00560 (18) | 0.000 | 0.000 |
S1 | 0.0140 (9) | 0.0140 (9) | 0.0045 (15) | 0.0070 (4) | 0.000 | 0.000 |
S2 | 0.0128 (7) | 0.0251 (8) | 0.0216 (10) | 0.0109 (6) | −0.0018 (7) | −0.0106 (8) |
S3 | 0.0154 (8) | 0.0123 (8) | 0.0113 (7) | 0.0091 (7) | −0.0004 (7) | −0.0013 (6) |
Geometric parameters (Å, º) top
Tb—S2i | 2.7693 (15) | Ag2—Tbxvii | 3.353 (2) |
Tb—S3ii | 2.8051 (17) | Ag2—Tbviii | 3.509 (3) |
Tb—S2iii | 2.8147 (16) | Ge1—S1iv | 2.175 (3) |
Tb—S2 | 2.818 (2) | Ge1—S3iii | 2.2256 (17) |
Tb—S3iv | 2.8937 (17) | Ge1—S3xviii | 2.2256 (17) |
Tb—S1v | 2.9251 (12) | Ge1—S3v | 2.2256 (17) |
Tb—S3i | 2.9996 (17) | S1—Ge1xix | 2.175 (3) |
Tb—S2iv | 3.189 (2) | S1—Tbxx | 2.9251 (12) |
Tb—Ag2vi | 3.353 (2) | S1—Tbvii | 2.9251 (12) |
Tb—Ag2vii | 3.509 (3) | S1—Tbxxi | 2.9251 (12) |
Ag2—S2v | 2.504 (3) | S2—Ag2vii | 2.504 (3) |
Ag2—S2viii | 2.504 (3) | S2—Tbxxi | 2.7693 (15) |
Ag2—S2ix | 2.504 (3) | S2—Tbxxii | 2.8147 (16) |
Ag2—Ag2x | 2.8827 (6) | S2—Ag2xxiii | 2.909 (4) |
Ag2—Ag2xi | 2.8827 (6) | S2—Tbxix | 3.189 (2) |
Ag2—S2xii | 2.909 (4) | S3—Ge1vii | 2.2256 (17) |
Ag2—S2xiii | 2.909 (4) | S3—Tbxxiv | 2.8051 (17) |
Ag2—S2xiv | 2.909 (4) | S3—Tbxix | 2.8937 (17) |
Ag2—Tbxv | 3.353 (2) | S3—Tbxxi | 2.9996 (17) |
Ag2—Tbxvi | 3.353 (2) | | |
| | | |
S2i—Tb—S3ii | 101.56 (5) | S2xiii—Ag2—S2xiv | 84.96 (13) |
S2i—Tb—S2iii | 89.41 (7) | S2v—Ag2—Tbxv | 54.11 (5) |
S3ii—Tb—S2iii | 140.59 (6) | S2viii—Ag2—Tbxv | 132.9 (2) |
S2i—Tb—S2 | 82.06 (5) | S2ix—Ag2—Tbxv | 55.18 (6) |
S3ii—Tb—S2 | 137.38 (5) | Ag2x—Ag2—Tbxv | 68.02 (8) |
S2iii—Tb—S2 | 81.26 (5) | Ag2xi—Ag2—Tbxv | 111.98 (8) |
S2i—Tb—S3iv | 140.15 (6) | S2xii—Ag2—Tbxv | 127.04 (5) |
S3ii—Tb—S3iv | 76.11 (7) | S2xiii—Ag2—Tbxv | 126.11 (5) |
S2iii—Tb—S3iv | 71.65 (4) | S2xiv—Ag2—Tbxv | 60.74 (4) |
S2—Tb—S3iv | 126.83 (5) | S2v—Ag2—Tbxvi | 132.9 (2) |
S2i—Tb—S1v | 147.60 (5) | S2viii—Ag2—Tbxvi | 55.18 (6) |
S3ii—Tb—S1v | 71.70 (5) | S2ix—Ag2—Tbxvi | 54.11 (5) |
S2iii—Tb—S1v | 116.29 (4) | Ag2x—Ag2—Tbxvi | 68.02 (8) |
S2—Tb—S1v | 82.81 (6) | Ag2xi—Ag2—Tbxvi | 111.98 (8) |
S3iv—Tb—S1v | 70.47 (5) | S2xii—Ag2—Tbxvi | 60.74 (4) |
S2i—Tb—S3i | 70.02 (5) | S2xiii—Ag2—Tbxvi | 127.04 (5) |
S3ii—Tb—S3i | 71.56 (3) | S2xiv—Ag2—Tbxvi | 126.11 (5) |
S2iii—Tb—S3i | 146.36 (5) | Tbxv—Ag2—Tbxvi | 106.85 (9) |
S2—Tb—S3i | 70.04 (5) | S2v—Ag2—Tbxvii | 55.18 (6) |
S3iv—Tb—S3i | 140.33 (4) | S2viii—Ag2—Tbxvii | 54.11 (5) |
S1v—Tb—S3i | 77.92 (4) | S2ix—Ag2—Tbxvii | 132.9 (2) |
S2i—Tb—S2iv | 75.63 (5) | Ag2x—Ag2—Tbxvii | 68.02 (8) |
S3ii—Tb—S2iv | 71.44 (5) | Ag2xi—Ag2—Tbxvii | 111.98 (8) |
S2iii—Tb—S2iv | 75.03 (5) | S2xii—Ag2—Tbxvii | 126.11 (5) |
S2—Tb—S2iv | 147.33 (6) | S2xiii—Ag2—Tbxvii | 60.74 (4) |
S3iv—Tb—S2iv | 65.84 (5) | S2xiv—Ag2—Tbxvii | 127.04 (5) |
S1v—Tb—S2iv | 127.87 (6) | Tbxv—Ag2—Tbxvii | 106.85 (9) |
S3i—Tb—S2iv | 122.00 (4) | Tbxvi—Ag2—Tbxvii | 106.85 (9) |
S2i—Tb—Ag2vi | 47.11 (4) | S2v—Ag2—Tbviii | 127.23 (4) |
S3ii—Tb—Ag2vi | 119.12 (9) | S2viii—Ag2—Tbviii | 52.73 (6) |
S2iii—Tb—Ag2vi | 46.92 (4) | S2ix—Ag2—Tbviii | 126.20 (4) |
S2—Tb—Ag2vi | 94.62 (9) | Ag2x—Ag2—Tbviii | 117.63 (8) |
S3iv—Tb—Ag2vi | 98.51 (7) | Ag2xi—Ag2—Tbviii | 62.37 (8) |
S1v—Tb—Ag2vi | 163.109 (17) | S2xii—Ag2—Tbviii | 50.06 (5) |
S3i—Tb—Ag2vi | 116.99 (4) | S2xiii—Ag2—Tbviii | 50.98 (5) |
S2iv—Tb—Ag2vi | 52.73 (9) | S2xiv—Ag2—Tbviii | 113.61 (16) |
S2i—Tb—Ag2vii | 53.64 (5) | Tbxv—Ag2—Tbviii | 174.35 (16) |
S3ii—Tb—Ag2vii | 154.83 (4) | Tbxvi—Ag2—Tbviii | 76.283 (11) |
S2iii—Tb—Ag2vii | 53.40 (5) | Tbxvii—Ag2—Tbviii | 76.283 (11) |
S2—Tb—Ag2vii | 45.01 (8) | S1iv—Ge1—S3iii | 114.29 (5) |
S3iv—Tb—Ag2vii | 124.61 (4) | S1iv—Ge1—S3xviii | 114.29 (5) |
S1v—Tb—Ag2vii | 125.80 (9) | S3iii—Ge1—S3xviii | 104.25 (6) |
S3i—Tb—Ag2vii | 93.19 (6) | S1iv—Ge1—S3v | 114.29 (5) |
S2iv—Tb—Ag2vii | 102.34 (9) | S3iii—Ge1—S3v | 104.25 (6) |
Ag2vi—Tb—Ag2vii | 49.618 (13) | S3xviii—Ge1—S3v | 104.25 (6) |
S2v—Ag2—S2viii | 103.32 (14) | Ge1xix—S1—Tbxx | 113.62 (5) |
S2v—Ag2—S2ix | 103.32 (14) | Ge1xix—S1—Tbvii | 113.62 (5) |
S2viii—Ag2—S2ix | 103.32 (14) | Tbxx—S1—Tbvii | 105.02 (6) |
S2v—Ag2—Ag2x | 64.91 (12) | Ge1xix—S1—Tbxxi | 113.62 (5) |
S2viii—Ag2—Ag2x | 64.91 (12) | Tbxx—S1—Tbxxi | 105.02 (6) |
S2ix—Ag2—Ag2x | 64.91 (12) | Tbvii—S1—Tbxxi | 105.02 (6) |
S2v—Ag2—Ag2xi | 115.09 (12) | Ag2vii—S2—Tbxxi | 78.77 (5) |
S2viii—Ag2—Ag2xi | 115.09 (12) | Ag2vii—S2—Tbxxii | 77.91 (5) |
S2ix—Ag2—Ag2xi | 115.09 (12) | Tbxxi—S2—Tbxxii | 149.29 (7) |
Ag2x—Ag2—Ag2xi | 180.0 | Ag2vii—S2—Tb | 82.27 (12) |
S2v—Ag2—S2xii | 166.3 (2) | Tbxxi—S2—Tb | 98.72 (6) |
S2viii—Ag2—S2xii | 84.97 (4) | Tbxxii—S2—Tb | 97.65 (5) |
S2ix—Ag2—S2xii | 84.97 (4) | Ag2vii—S2—Ag2xxiii | 63.85 (5) |
Ag2x—Ag2—S2xii | 128.76 (9) | Tbxxi—S2—Ag2xxiii | 76.30 (4) |
Ag2xi—Ag2—S2xii | 51.24 (9) | Tbxxii—S2—Ag2xxiii | 75.61 (4) |
S2v—Ag2—S2xiii | 84.97 (4) | Tb—S2—Ag2xxiii | 146.11 (10) |
S2viii—Ag2—S2xiii | 84.97 (4) | Ag2vii—S2—Tbxix | 130.37 (13) |
S2ix—Ag2—S2xiii | 166.3 (2) | Tbxxi—S2—Tbxix | 90.44 (5) |
Ag2x—Ag2—S2xiii | 128.76 (9) | Tbxxii—S2—Tbxix | 89.63 (5) |
Ag2xi—Ag2—S2xiii | 51.24 (9) | Tb—S2—Tbxix | 147.33 (6) |
S2xii—Ag2—S2xiii | 84.96 (13) | Ag2xxiii—S2—Tbxix | 66.53 (9) |
S2v—Ag2—S2xiv | 84.97 (4) | Ge1vii—S3—Tbxxiv | 90.96 (5) |
S2viii—Ag2—S2xiv | 166.3 (2) | Ge1vii—S3—Tbxix | 88.68 (5) |
S2ix—Ag2—S2xiv | 84.97 (4) | Tbxxiv—S3—Tbxix | 109.07 (6) |
Ag2x—Ag2—S2xiv | 128.76 (9) | Ge1vii—S3—Tbxxi | 119.16 (7) |
Ag2xi—Ag2—S2xiv | 51.24 (9) | Tbxxiv—S3—Tbxxi | 144.01 (6) |
S2xii—Ag2—S2xiv | 84.96 (13) | Tbxix—S3—Tbxxi | 91.99 (5) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) −x+y+1, −x+1, z−1; (iii) y, −x+y+1, z−1/2; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) −x+1, −y+1, z+1/2; (viii) y−1, −x+y, z−1/2; (ix) x−y, x−1, z−1/2; (x) −x, −y, z+1/2; (xi) −x, −y, z−1/2; (xii) x−1, y−1, z−1; (xiii) −x+y, −x+1, z−1; (xiv) −y+1, x−y, z−1; (xv) −y+1, x−y, z; (xvi) x−1, y−1, z; (xvii) −x+y, −x+1, z; (xviii) x−y, x, z−1/2; (xix) x, y, z+1; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) x+1, y+1, z+1; (xxiv) −y+1, x−y, z+1. |
Crystal data top
Ag0.51Dy3GeS7 | Dx = 5.795 Mg m−3 |
Mr = 840.06 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 644 reflections |
Hall symbol: P 6c | θ = 4.3–26.4° |
a = 9.8003 (14) Å | µ = 28.56 mm−1 |
c = 5.7879 (12) Å | T = 295 K |
V = 481.43 (14) Å3 | Prism, dark red |
Z = 2 | 0.12 × 0.10 × 0.09 mm |
F(000) = 732 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 655 independent reflections |
Radiation source: fine-focus sealed tube | 644 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 4.3° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→10 |
Tmin = 0.035, Tmax = 0.244 | l = −7→7 |
5667 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0114P)2 + 0.9002P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.015 | (Δ/σ)max = 0.001 |
wR(F2) = 0.032 | Δρmax = 0.99 e Å−3 |
S = 1.12 | Δρmin = −1.03 e Å−3 |
655 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
39 parameters | Extinction coefficient: 0.0034 (2) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 293 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.005 (19) |
Crystal data top
Ag0.51Dy3GeS7 | Z = 2 |
Mr = 840.06 | Mo Kα radiation |
Hexagonal, P63 | µ = 28.56 mm−1 |
a = 9.8003 (14) Å | T = 295 K |
c = 5.7879 (12) Å | 0.12 × 0.10 × 0.09 mm |
V = 481.43 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 655 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 644 reflections with I > 2σ(I) |
Tmin = 0.035, Tmax = 0.244 | Rint = 0.046 |
5667 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.015 | 1 restraint |
wR(F2) = 0.032 | Δρmax = 0.99 e Å−3 |
S = 1.12 | Δρmin = −1.03 e Å−3 |
655 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 293 Friedel pairs |
39 parameters | Absolute structure parameter: −0.005 (19) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Dy | 0.86393 (3) | 0.64111 (3) | 0.24397 (11) | 0.01554 (10) | |
Ag2 | 0.0000 | 0.0000 | 0.0017 (9) | 0.0735 (13) | 0.517 (5) |
Ge1 | 0.3333 | 0.6667 | 0.32315 (16) | 0.0100 (2) | |
S1 | 0.3333 | 0.6667 | 0.9457 (4) | 0.0110 (5) | |
S2 | 0.89852 (18) | 0.7401 (2) | 0.7034 (2) | 0.0197 (4) | |
S3 | 0.57703 (18) | 0.47943 (18) | 0.9824 (2) | 0.0123 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Dy | 0.01188 (14) | 0.01160 (14) | 0.02330 (15) | 0.00598 (10) | −0.00218 (19) | −0.00039 (17) |
Ag2 | 0.0108 (7) | 0.0108 (7) | 0.199 (3) | 0.0054 (4) | 0.000 | 0.000 |
Ge1 | 0.0113 (3) | 0.0113 (3) | 0.0076 (4) | 0.00564 (17) | 0.000 | 0.000 |
S1 | 0.0137 (8) | 0.0137 (8) | 0.0057 (11) | 0.0069 (4) | 0.000 | 0.000 |
S2 | 0.0119 (7) | 0.0251 (8) | 0.0232 (10) | 0.0100 (6) | −0.0014 (6) | −0.0127 (7) |
S3 | 0.0165 (8) | 0.0122 (7) | 0.0114 (6) | 0.0096 (7) | −0.0002 (7) | −0.0008 (6) |
Geometric parameters (Å, º) top
Dy—S2i | 2.7330 (15) | Ag2—Dyxvii | 3.380 (2) |
Dy—S2ii | 2.7879 (15) | Ag2—Dyviii | 3.418 (2) |
Dy—S2 | 2.7922 (16) | Ge1—S1iv | 2.185 (2) |
Dy—S3iii | 2.7946 (16) | Ge1—S3ii | 2.2202 (16) |
Dy—S3iv | 2.8727 (16) | Ge1—S3xviii | 2.2202 (16) |
Dy—S1v | 2.8926 (11) | Ge1—S3v | 2.2202 (16) |
Dy—S3i | 2.9970 (16) | S1—Ge1xix | 2.185 (2) |
Dy—S2iv | 3.2430 (17) | S1—Dyxx | 2.8926 (11) |
Dy—Ag2vi | 3.380 (2) | S1—Dyvii | 2.8926 (11) |
Dy—Ag2vii | 3.418 (2) | S1—Dyxxi | 2.8926 (11) |
Ag2—S2v | 2.511 (3) | S2—Ag2vii | 2.511 (3) |
Ag2—S2viii | 2.511 (3) | S2—Dyxxi | 2.7330 (15) |
Ag2—S2ix | 2.511 (3) | S2—Dyxxii | 2.7879 (15) |
Ag2—S2x | 2.816 (4) | S2—Ag2xxiii | 2.816 (4) |
Ag2—S2xi | 2.816 (4) | S2—Dyxix | 3.2430 (17) |
Ag2—S2xii | 2.816 (4) | S3—Ge1vii | 2.2202 (16) |
Ag2—Ag2xiii | 2.8939 (6) | S3—Dyxxiv | 2.7946 (16) |
Ag2—Ag2xiv | 2.8939 (6) | S3—Dyxix | 2.8727 (16) |
Ag2—Dyxv | 3.380 (2) | S3—Dyxxi | 2.9970 (16) |
Ag2—Dyxvi | 3.380 (2) | | |
| | | |
S2i—Dy—S2ii | 88.48 (7) | Ag2xiii—Ag2—Ag2xiv | 180.0 |
S2i—Dy—S2 | 82.68 (5) | S2v—Ag2—Dyxv | 52.81 (6) |
S2ii—Dy—S2 | 81.70 (4) | S2viii—Ag2—Dyxv | 127.80 (19) |
S2i—Dy—S3iii | 100.10 (5) | S2ix—Ag2—Dyxv | 54.08 (6) |
S2ii—Dy—S3iii | 140.01 (5) | S2x—Ag2—Dyxv | 128.44 (5) |
S2—Dy—S3iii | 137.91 (5) | S2xi—Ag2—Dyxv | 127.28 (5) |
S2i—Dy—S3iv | 138.99 (5) | S2xii—Ag2—Dyxv | 62.34 (4) |
S2ii—Dy—S3iv | 72.14 (4) | Ag2xiii—Ag2—Dyxv | 114.51 (8) |
S2—Dy—S3iv | 127.50 (4) | Ag2xiv—Ag2—Dyxv | 65.49 (8) |
S3iii—Dy—S3iv | 76.22 (6) | S2v—Ag2—Dyxvi | 127.80 (19) |
S2i—Dy—S1v | 147.56 (4) | S2viii—Ag2—Dyxvi | 54.08 (6) |
S2ii—Dy—S1v | 117.99 (4) | S2ix—Ag2—Dyxvi | 52.81 (6) |
S2—Dy—S1v | 83.09 (6) | S2x—Ag2—Dyxvi | 62.34 (4) |
S3iii—Dy—S1v | 72.32 (4) | S2xi—Ag2—Dyxvi | 128.44 (5) |
S3iv—Dy—S1v | 71.21 (4) | S2xii—Ag2—Dyxvi | 127.28 (5) |
S2i—Dy—S3i | 70.61 (5) | Ag2xiii—Ag2—Dyxvi | 114.51 (8) |
S2ii—Dy—S3i | 146.52 (5) | Ag2xiv—Ag2—Dyxvi | 65.49 (8) |
S2—Dy—S3i | 70.21 (4) | Dyxv—Ag2—Dyxvi | 104.00 (10) |
S3iii—Dy—S3i | 71.32 (3) | S2v—Ag2—Dyxvii | 54.08 (6) |
S3iv—Dy—S3i | 140.07 (4) | S2viii—Ag2—Dyxvii | 52.81 (6) |
S1v—Dy—S3i | 77.17 (3) | S2ix—Ag2—Dyxvii | 127.80 (19) |
S2i—Dy—S2iv | 74.74 (4) | S2x—Ag2—Dyxvii | 127.28 (5) |
S2ii—Dy—S2iv | 74.05 (4) | S2xi—Ag2—Dyxvii | 62.34 (4) |
S2—Dy—S2iv | 146.99 (6) | S2xii—Ag2—Dyxvii | 128.44 (5) |
S3iii—Dy—S2iv | 70.87 (4) | Ag2xiii—Ag2—Dyxvii | 114.51 (8) |
S3iv—Dy—S2iv | 65.40 (4) | Ag2xiv—Ag2—Dyxvii | 65.49 (8) |
S1v—Dy—S2iv | 128.07 (5) | Dyxv—Ag2—Dyxvii | 104.00 (10) |
S3i—Dy—S2iv | 122.04 (4) | Dyxvi—Ag2—Dyxvii | 104.00 (10) |
S2i—Dy—Ag2vi | 47.06 (4) | S2v—Ag2—Dyviii | 127.59 (3) |
S2ii—Dy—Ag2vi | 46.85 (4) | S2viii—Ag2—Dyviii | 53.57 (4) |
S2—Dy—Ag2vi | 96.74 (9) | S2ix—Ag2—Dyviii | 126.32 (3) |
S3iii—Dy—Ag2vi | 115.94 (9) | S2x—Ag2—Dyviii | 50.89 (6) |
S3iv—Dy—Ag2vi | 97.09 (6) | S2xi—Ag2—Dyviii | 52.04 (6) |
S1v—Dy—Ag2vi | 164.310 (10) | S2xii—Ag2—Dyviii | 116.29 (17) |
S3i—Dy—Ag2vi | 117.64 (4) | Ag2xiii—Ag2—Dyviii | 64.12 (8) |
S2iv—Dy—Ag2vi | 50.26 (9) | Ag2xiv—Ag2—Dyviii | 115.88 (8) |
S2i—Dy—Ag2vii | 53.07 (5) | Dyxv—Ag2—Dyviii | 178.63 (17) |
S2ii—Dy—Ag2vii | 52.78 (5) | Dyxvi—Ag2—Dyviii | 76.803 (7) |
S2—Dy—Ag2vii | 46.36 (9) | Dyxvii—Ag2—Dyviii | 76.803 (7) |
S3iii—Dy—Ag2vii | 153.01 (5) | S1iv—Ge1—S3ii | 114.54 (4) |
S3iv—Dy—Ag2vii | 124.63 (4) | S1iv—Ge1—S3xviii | 114.54 (4) |
S1v—Dy—Ag2vii | 127.61 (9) | S3ii—Ge1—S3xviii | 103.96 (5) |
S3i—Dy—Ag2vii | 93.94 (6) | S1iv—Ge1—S3v | 114.54 (4) |
S2iv—Dy—Ag2vii | 100.65 (9) | S3ii—Ge1—S3v | 103.96 (5) |
Ag2vi—Dy—Ag2vii | 50.384 (12) | S3xviii—Ge1—S3v | 103.96 (5) |
S2v—Ag2—S2viii | 100.14 (14) | Ge1xix—S1—Dyxx | 113.80 (4) |
S2v—Ag2—S2ix | 100.14 (14) | Ge1xix—S1—Dyvii | 113.80 (4) |
S2viii—Ag2—S2ix | 100.14 (14) | Dyxx—S1—Dyvii | 104.82 (5) |
S2v—Ag2—S2x | 169.9 (2) | Ge1xix—S1—Dyxxi | 113.80 (4) |
S2viii—Ag2—S2x | 86.29 (4) | Dyxx—S1—Dyxxi | 104.82 (5) |
S2ix—Ag2—S2x | 86.29 (4) | Dyvii—S1—Dyxxi | 104.82 (5) |
S2v—Ag2—S2xi | 86.29 (4) | Ag2vii—S2—Dyxxi | 80.13 (5) |
S2viii—Ag2—S2xi | 86.29 (4) | Ag2vii—S2—Dyxxii | 79.07 (5) |
S2ix—Ag2—S2xi | 169.9 (2) | Dyxxi—S2—Dyxxii | 149.54 (7) |
S2x—Ag2—S2xi | 86.32 (13) | Ag2vii—S2—Dy | 80.07 (11) |
S2v—Ag2—S2xii | 86.29 (4) | Dyxxi—S2—Dy | 99.69 (5) |
S2viii—Ag2—S2xii | 169.9 (2) | Dyxxii—S2—Dy | 98.37 (5) |
S2ix—Ag2—S2xii | 86.29 (4) | Ag2vii—S2—Ag2xxiii | 65.52 (5) |
S2x—Ag2—S2xii | 86.32 (13) | Dyxxi—S2—Ag2xxiii | 76.04 (4) |
S2xi—Ag2—S2xii | 86.32 (13) | Dyxxii—S2—Ag2xxiii | 75.18 (4) |
S2v—Ag2—Ag2xiii | 117.69 (11) | Dy—S2—Ag2xxiii | 145.58 (10) |
S2viii—Ag2—Ag2xiii | 117.69 (11) | Ag2vii—S2—Dyxix | 132.91 (12) |
S2ix—Ag2—Ag2xiii | 117.69 (11) | Dyxxi—S2—Dyxix | 89.51 (4) |
S2x—Ag2—Ag2xiii | 52.17 (9) | Dyxxii—S2—Dyxix | 88.56 (4) |
S2xi—Ag2—Ag2xiii | 52.17 (9) | Dy—S2—Dyxix | 146.99 (6) |
S2xii—Ag2—Ag2xiii | 52.17 (9) | Ag2xxiii—S2—Dyxix | 67.39 (9) |
S2v—Ag2—Ag2xiv | 62.31 (11) | Ge1vii—S3—Dyxxiv | 90.91 (5) |
S2viii—Ag2—Ag2xiv | 62.31 (11) | Ge1vii—S3—Dyxix | 88.90 (5) |
S2ix—Ag2—Ag2xiv | 62.31 (11) | Dyxxiv—S3—Dyxix | 107.96 (5) |
S2x—Ag2—Ag2xiv | 127.83 (9) | Ge1vii—S3—Dyxxi | 118.61 (6) |
S2xi—Ag2—Ag2xiv | 127.83 (9) | Dyxxiv—S3—Dyxxi | 145.01 (6) |
S2xii—Ag2—Ag2xiv | 127.83 (9) | Dyxix—S3—Dyxxi | 91.99 (4) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) y, −x+y+1, z−1/2; (iii) −x+y+1, −x+1, z−1; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) −x+1, −y+1, z+1/2; (viii) y−1, −x+y, z−1/2; (ix) x−y, x−1, z−1/2; (x) x−1, y−1, z−1; (xi) −x+y, −x+1, z−1; (xii) −y+1, x−y, z−1; (xiii) −x, −y, z−1/2; (xiv) −x, −y, z+1/2; (xv) −y+1, x−y, z; (xvi) x−1, y−1, z; (xvii) −x+y, −x+1, z; (xviii) x−y, x, z−1/2; (xix) x, y, z+1; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) x+1, y+1, z+1; (xxiv) −y+1, x−y, z+1. |
Crystal data top
Ag0.50GeHo3S7 | Dx = 5.895 Mg m−3 |
Mr = 845.73 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 630 reflections |
Hall symbol: P 6c | θ = 4.3–26.7° |
a = 9.7401 (14) Å | µ = 30.22 mm−1 |
c = 5.7994 (12) Å | T = 295 K |
V = 476.48 (14) Å3 | Prism, dark red |
Z = 2 | 0.09 × 0.07 × 0.03 mm |
F(000) = 737 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 649 independent reflections |
Radiation source: fine-focus sealed tube | 630 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.7°, θmin = 4.3° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.061, Tmax = 0.304 | l = −7→6 |
5792 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.004P)2 + 2.2568P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.001 |
wR(F2) = 0.033 | Δρmax = 0.79 e Å−3 |
S = 1.19 | Δρmin = −2.26 e Å−3 |
649 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
38 parameters | Extinction coefficient: 0.0054 (2) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 275 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.04 (2) |
Crystal data top
Ag0.50GeHo3S7 | Z = 2 |
Mr = 845.73 | Mo Kα radiation |
Hexagonal, P63 | µ = 30.22 mm−1 |
a = 9.7401 (14) Å | T = 295 K |
c = 5.7994 (12) Å | 0.09 × 0.07 × 0.03 mm |
V = 476.48 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 649 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 630 reflections with I > 2σ(I) |
Tmin = 0.061, Tmax = 0.304 | Rint = 0.045 |
5792 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.017 | 1 restraint |
wR(F2) = 0.033 | Δρmax = 0.79 e Å−3 |
S = 1.19 | Δρmin = −2.26 e Å−3 |
649 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 275 Friedel pairs |
38 parameters | Absolute structure parameter: −0.04 (2) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ho | 0.86127 (3) | 0.64077 (3) | 0.24376 (13) | 0.01686 (11) | |
Ag2 | 0.0000 | 0.0000 | 0.9801 (12) | 0.0699 (11) | 0.50 |
Ge1 | 0.3333 | 0.6667 | 0.32172 (19) | 0.0101 (3) | |
S1 | 0.3333 | 0.6667 | 0.9456 (5) | 0.0104 (6) | |
S2 | 0.8968 (2) | 0.7410 (2) | 0.6976 (3) | 0.0204 (5) | |
S3 | 0.5748 (2) | 0.4782 (2) | 0.9815 (3) | 0.0130 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ho | 0.01145 (15) | 0.01179 (15) | 0.02747 (19) | 0.00591 (12) | −0.0023 (2) | 0.0000 (2) |
Ag2 | 0.0155 (6) | 0.0155 (6) | 0.179 (3) | 0.0078 (3) | 0.000 | 0.000 |
Ge1 | 0.0112 (4) | 0.0112 (4) | 0.0079 (6) | 0.00562 (19) | 0.000 | 0.000 |
S1 | 0.0127 (9) | 0.0127 (9) | 0.0058 (15) | 0.0064 (5) | 0.000 | 0.000 |
S2 | 0.0112 (8) | 0.0234 (9) | 0.0278 (15) | 0.0095 (7) | −0.0009 (7) | −0.0124 (8) |
S3 | 0.0169 (9) | 0.0133 (8) | 0.0126 (8) | 0.0104 (7) | −0.0006 (8) | −0.0005 (8) |
Geometric parameters (Å, º) top
Ho—S2i | 2.7141 (17) | Ag2—Hoviii | 3.349 (3) |
Ho—S2 | 2.768 (2) | Ag2—Hoxv | 3.417 (3) |
Ho—S2ii | 2.7731 (17) | Ge1—S1iv | 2.181 (3) |
Ho—S3iii | 2.7845 (19) | Ge1—S3ii | 2.2169 (18) |
Ho—S3iv | 2.8617 (19) | Ge1—S3xvi | 2.2169 (18) |
Ho—S1v | 2.8730 (14) | Ge1—S3v | 2.2169 (18) |
Ho—S3i | 3.0063 (18) | S1—Ge1xvii | 2.181 (3) |
Ho—Ag2v | 3.349 (3) | S1—Hoxviii | 2.8730 (13) |
Ho—Ag2vi | 3.417 (3) | S1—Hovii | 2.8730 (13) |
Ag2—S2vii | 2.535 (4) | S1—Hoxix | 2.8730 (13) |
Ag2—S2viii | 2.535 (4) | S2—Ag2v | 2.535 (4) |
Ag2—S2ix | 2.535 (4) | S2—Hoxix | 2.7141 (17) |
Ag2—S2x | 2.743 (5) | S2—Ag2xx | 2.743 (5) |
Ag2—S2xi | 2.743 (5) | S2—Hoxxi | 2.7731 (17) |
Ag2—S2xii | 2.743 (5) | S3—Ge1vii | 2.2169 (18) |
Ag2—Ag2xiii | 2.8997 (6) | S3—Hoxv | 2.7845 (19) |
Ag2—Ag2xiv | 2.8997 (6) | S3—Hoxvii | 2.8617 (19) |
Ag2—Hoix | 3.349 (3) | S3—Hoxix | 3.0063 (18) |
Ag2—Hovii | 3.349 (3) | | |
| | | |
S2i—Ho—S2 | 83.19 (6) | S2viii—Ag2—Hoix | 126.14 (4) |
S2i—Ho—S2ii | 87.93 (8) | S2ix—Ag2—Hoix | 53.99 (5) |
S2—Ho—S2ii | 82.11 (5) | S2x—Ag2—Hoix | 51.75 (7) |
S2i—Ho—S3iii | 98.76 (6) | S2xi—Ag2—Hoix | 53.03 (7) |
S2—Ho—S3iii | 138.23 (6) | S2xii—Ag2—Hoix | 119.2 (2) |
S2ii—Ho—S3iii | 139.49 (6) | Ag2xiii—Ag2—Hoix | 114.15 (12) |
S2i—Ho—S3iv | 138.26 (6) | Ag2xiv—Ag2—Hoix | 65.85 (11) |
S2—Ho—S3iv | 128.02 (5) | S2vii—Ag2—Hovii | 53.99 (5) |
S2ii—Ho—S3iv | 72.58 (5) | S2viii—Ag2—Hovii | 127.50 (4) |
S3iii—Ho—S3iv | 76.30 (7) | S2ix—Ag2—Hovii | 126.14 (4) |
S2i—Ho—S1v | 147.28 (5) | S2x—Ag2—Hovii | 119.2 (2) |
S2—Ho—S1v | 83.18 (7) | S2xi—Ag2—Hovii | 51.75 (7) |
S2ii—Ho—S1v | 119.33 (4) | S2xii—Ag2—Hovii | 53.03 (7) |
S3iii—Ho—S1v | 72.90 (5) | Ag2xiii—Ag2—Hovii | 114.15 (11) |
S3iv—Ho—S1v | 71.78 (6) | Ag2xiv—Ag2—Hovii | 65.85 (12) |
S2i—Ho—S3i | 70.93 (5) | Hoix—Ag2—Hovii | 104.41 (13) |
S2—Ho—S3i | 70.44 (5) | S2vii—Ag2—Hoviii | 126.14 (4) |
S2ii—Ho—S3i | 146.77 (5) | S2viii—Ag2—Hoviii | 53.99 (5) |
S3iii—Ho—S3i | 70.95 (3) | S2ix—Ag2—Hoviii | 127.50 (4) |
S3iv—Ho—S3i | 139.65 (5) | S2x—Ag2—Hoviii | 53.03 (7) |
S1v—Ho—S3i | 76.49 (4) | S2xi—Ag2—Hoviii | 119.2 (2) |
S2i—Ho—Ag2v | 52.52 (7) | S2xii—Ag2—Hoviii | 51.75 (7) |
S2—Ho—Ag2v | 47.81 (12) | Ag2xiii—Ag2—Hoviii | 114.15 (11) |
S2ii—Ho—Ag2v | 52.20 (7) | Ag2xiv—Ag2—Hoviii | 65.85 (12) |
S3iii—Ho—Ag2v | 151.24 (7) | Hoix—Ag2—Hoviii | 104.41 (13) |
S3iv—Ho—Ag2v | 124.60 (6) | Hovii—Ag2—Hoviii | 104.41 (13) |
S1v—Ho—Ag2v | 129.30 (13) | S2vii—Ag2—Hoxv | 51.70 (7) |
S3i—Ho—Ag2v | 94.77 (8) | S2viii—Ag2—Hoxv | 53.05 (8) |
S2i—Ho—Ag2vi | 47.15 (5) | S2ix—Ag2—Hoxv | 123.6 (3) |
S2—Ho—Ag2vi | 98.54 (12) | S2x—Ag2—Hoxv | 129.38 (5) |
S2ii—Ho—Ag2vi | 46.94 (5) | S2xi—Ag2—Hoxv | 128.11 (5) |
S3iii—Ho—Ag2vi | 113.31 (11) | S2xii—Ag2—Hoxv | 63.27 (5) |
S3iv—Ho—Ag2vi | 96.06 (8) | Ag2xiii—Ag2—Hoxv | 63.42 (11) |
S1v—Ho—Ag2vi | 165.13 (2) | Ag2xiv—Ag2—Hoxv | 116.58 (11) |
S3i—Ho—Ag2vi | 118.08 (5) | Hoix—Ag2—Hoxv | 177.6 (2) |
Ag2v—Ho—Ag2vi | 50.735 (13) | Hovii—Ag2—Hoxv | 77.003 (9) |
S2vii—Ag2—S2viii | 97.40 (19) | Hoviii—Ag2—Hoxv | 77.003 (9) |
S2vii—Ag2—S2ix | 97.40 (19) | S1iv—Ge1—S3ii | 114.70 (6) |
S2viii—Ag2—S2ix | 97.40 (19) | S1iv—Ge1—S3xvi | 114.70 (6) |
S2vii—Ag2—S2x | 173.1 (3) | S3ii—Ge1—S3xvi | 103.77 (6) |
S2viii—Ag2—S2x | 87.10 (4) | S1iv—Ge1—S3v | 114.70 (6) |
S2ix—Ag2—S2x | 87.10 (4) | S3ii—Ge1—S3v | 103.77 (6) |
S2vii—Ag2—S2xi | 87.10 (4) | S3xvi—Ge1—S3v | 103.77 (6) |
S2viii—Ag2—S2xi | 173.1 (3) | Ge1xvii—S1—Hoxviii | 114.05 (6) |
S2ix—Ag2—S2xi | 87.10 (4) | Ge1xvii—S1—Hovii | 114.05 (6) |
S2x—Ag2—S2xi | 87.98 (18) | Hoxviii—S1—Hovii | 104.53 (7) |
S2vii—Ag2—S2xii | 87.10 (4) | Ge1xvii—S1—Hoxix | 114.05 (6) |
S2viii—Ag2—S2xii | 87.10 (4) | Hoxviii—S1—Hoxix | 104.53 (7) |
S2ix—Ag2—S2xii | 173.1 (3) | Hovii—S1—Hoxix | 104.53 (7) |
S2x—Ag2—S2xii | 87.98 (18) | Ag2v—S2—Hoxix | 81.16 (6) |
S2xi—Ag2—S2xii | 87.98 (18) | Ag2v—S2—Ag2xx | 66.52 (5) |
S2vii—Ag2—Ag2xiii | 60.17 (15) | Hoxix—S2—Ag2xx | 75.73 (5) |
S2viii—Ag2—Ag2xiii | 60.17 (15) | Ag2v—S2—Ho | 78.20 (15) |
S2ix—Ag2—Ag2xiii | 60.17 (15) | Hoxix—S2—Ho | 100.43 (6) |
S2x—Ag2—Ag2xiii | 126.68 (13) | Ag2xx—S2—Ho | 144.70 (14) |
S2xi—Ag2—Ag2xiii | 126.68 (13) | Ag2v—S2—Hoxxi | 80.01 (6) |
S2xii—Ag2—Ag2xiii | 126.68 (13) | Hoxix—S2—Hoxxi | 149.46 (8) |
S2vii—Ag2—Ag2xiv | 119.83 (15) | Ag2xx—S2—Hoxxi | 74.78 (5) |
S2viii—Ag2—Ag2xiv | 119.83 (15) | Ho—S2—Hoxxi | 98.98 (6) |
S2ix—Ag2—Ag2xiv | 119.83 (15) | Ge1vii—S3—Hoxv | 90.96 (6) |
S2x—Ag2—Ag2xiv | 53.32 (13) | Ge1vii—S3—Hoxvii | 88.96 (6) |
S2xi—Ag2—Ag2xiv | 53.32 (13) | Hoxv—S3—Hoxvii | 107.19 (7) |
S2xii—Ag2—Ag2xiv | 53.32 (13) | Ge1vii—S3—Hoxix | 118.19 (8) |
Ag2xiii—Ag2—Ag2xiv | 180.000 (3) | Hoxv—S3—Hoxix | 145.83 (7) |
S2vii—Ag2—Hoix | 127.50 (4) | Hoxvii—S3—Hoxix | 91.74 (5) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) y, −x+y+1, z−1/2; (iii) −x+y+1, −x+1, z−1; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z−1; (vii) −x+1, −y+1, z+1/2; (viii) x−y, x−1, z+1/2; (ix) y−1, −x+y, z+1/2; (x) x−1, y−1, z; (xi) −x+y, −x+1, z; (xii) −y+1, x−y, z; (xiii) −x, −y, z+1/2; (xiv) −x, −y, z−1/2; (xv) −y+1, x−y, z+1; (xvi) x−y, x, z−1/2; (xvii) x, y, z+1; (xviii) x−y, x, z+1/2; (xix) y, −x+y+1, z+1/2; (xx) x+1, y+1, z; (xxi) x−y+1, x, z+1/2. |
Crystal data top
Ag0.50Er3GeS7 | Dx = 5.970 Mg m−3 |
Mr = 852.72 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 628 reflections |
Hall symbol: P 6c | θ = 4.2–26.4° |
a = 9.6921 (14) Å | µ = 31.87 mm−1 |
c = 5.8308 (12) Å | T = 295 K |
V = 474.35 (14) Å3 | Prism, dark red |
Z = 2 | 0.13 × 0.10 × 0.08 mm |
F(000) = 743 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 633 independent reflections |
Radiation source: fine-focus sealed tube | 628 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 4.2° |
ω–scan | h = −12→12 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→11 |
Tmin = 0.038, Tmax = 0.131 | l = −7→7 |
4994 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0131P)2 + 7.731P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max = 0.001 |
wR(F2) = 0.053 | Δρmax = 0.86 e Å−3 |
S = 1.15 | Δρmin = −2.84 e Å−3 |
633 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
38 parameters | Extinction coefficient: 0.0081 (5) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 280 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.03 (3) |
Crystal data top
Ag0.50Er3GeS7 | Z = 2 |
Mr = 852.72 | Mo Kα radiation |
Hexagonal, P63 | µ = 31.87 mm−1 |
a = 9.6921 (14) Å | T = 295 K |
c = 5.8308 (12) Å | 0.13 × 0.10 × 0.08 mm |
V = 474.35 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 633 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 628 reflections with I > 2σ(I) |
Tmin = 0.038, Tmax = 0.131 | Rint = 0.049 |
4994 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.022 | 1 restraint |
wR(F2) = 0.053 | Δρmax = 0.86 e Å−3 |
S = 1.15 | Δρmin = −2.84 e Å−3 |
633 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 280 Friedel pairs |
38 parameters | Absolute structure parameter: −0.03 (3) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Er | 0.85842 (5) | 0.64061 (5) | 0.24518 (19) | 0.02066 (18) | |
Ag2 | 0.0000 | 0.0000 | 0.9635 (19) | 0.076 (2) | 0.50 |
Ge1 | 0.3333 | 0.6667 | 0.3216 (3) | 0.0119 (4) | |
S1 | 0.3333 | 0.6667 | 0.9460 (7) | 0.0134 (9) | |
S2 | 0.8949 (3) | 0.7418 (3) | 0.6936 (5) | 0.0238 (7) | |
S3 | 0.5725 (3) | 0.4776 (3) | 0.9825 (4) | 0.0154 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Er | 0.0144 (2) | 0.0150 (2) | 0.0327 (3) | 0.00742 (17) | −0.0022 (3) | 0.0004 (3) |
Ag2 | 0.0231 (9) | 0.0231 (9) | 0.181 (7) | 0.0115 (5) | 0.000 | 0.000 |
Ge1 | 0.0140 (6) | 0.0140 (6) | 0.0077 (8) | 0.0070 (3) | 0.000 | 0.000 |
S1 | 0.0159 (13) | 0.0159 (13) | 0.008 (2) | 0.0079 (6) | 0.000 | 0.000 |
S2 | 0.0136 (11) | 0.0252 (13) | 0.0340 (19) | 0.0107 (10) | −0.0022 (10) | −0.0143 (11) |
S3 | 0.0202 (12) | 0.0155 (12) | 0.0148 (12) | 0.0122 (10) | −0.0006 (11) | −0.0001 (10) |
Geometric parameters (Å, º) top
Er—S2i | 2.699 (3) | Ag2—Erviii | 3.295 (4) |
Er—S2 | 2.753 (3) | Ag2—Erxv | 3.454 (5) |
Er—S2ii | 2.761 (3) | Ge1—S1iv | 2.190 (4) |
Er—S3iii | 2.784 (3) | Ge1—S3ii | 2.223 (3) |
Er—S3iv | 2.853 (3) | Ge1—S3xvi | 2.223 (3) |
Er—S1v | 2.8566 (19) | Ge1—S3v | 2.223 (3) |
Er—S3i | 3.020 (3) | S1—Ge1xvii | 2.190 (4) |
Er—Ag2v | 3.295 (4) | S1—Erxviii | 2.8566 (19) |
Er—Ag2vi | 3.454 (6) | S1—Ervii | 2.8566 (19) |
Ag2—S2vii | 2.560 (7) | S1—Erxix | 2.8566 (19) |
Ag2—S2viii | 2.560 (7) | S2—Ag2v | 2.560 (7) |
Ag2—S2ix | 2.560 (7) | S2—Ag2xx | 2.688 (7) |
Ag2—S2x | 2.688 (7) | S2—Erxix | 2.699 (2) |
Ag2—S2xi | 2.688 (7) | S2—Erxxi | 2.761 (3) |
Ag2—S2xii | 2.688 (7) | S3—Ge1vii | 2.223 (3) |
Ag2—Ag2xiii | 2.9154 (6) | S3—Erxv | 2.784 (3) |
Ag2—Ag2xiv | 2.9154 (6) | S3—Erxvii | 2.853 (3) |
Ag2—Erix | 3.295 (4) | S3—Erxix | 3.020 (3) |
Ag2—Ervii | 3.295 (4) | | |
| | | |
S2i—Er—S2 | 83.78 (8) | S2viii—Ag2—Erix | 125.81 (7) |
S2i—Er—S2ii | 87.49 (12) | S2ix—Ag2—Erix | 54.35 (7) |
S2—Er—S2ii | 82.62 (8) | S2x—Ag2—Erix | 52.43 (11) |
S2i—Er—S3iii | 97.24 (8) | S2xi—Ag2—Erix | 53.82 (11) |
S2—Er—S3iii | 138.35 (8) | S2xii—Ag2—Erix | 121.4 (4) |
S2ii—Er—S3iii | 138.98 (9) | Ag2xiii—Ag2—Erix | 67.27 (18) |
S2i—Er—S3iv | 137.50 (9) | Ag2xiv—Ag2—Erix | 112.73 (18) |
S2—Er—S3iv | 128.56 (8) | S2vii—Ag2—Ervii | 54.35 (7) |
S2ii—Er—S3iv | 72.95 (7) | S2viii—Ag2—Ervii | 127.26 (8) |
S3iii—Er—S3iv | 76.52 (10) | S2ix—Ag2—Ervii | 125.81 (7) |
S2i—Er—S1v | 146.88 (8) | S2x—Ag2—Ervii | 121.4 (4) |
S2—Er—S1v | 83.26 (10) | S2xi—Ag2—Ervii | 52.43 (11) |
S2ii—Er—S1v | 120.73 (7) | S2xii—Ag2—Ervii | 53.82 (11) |
S3iii—Er—S1v | 73.40 (8) | Ag2xiii—Ag2—Ervii | 67.27 (18) |
S3iv—Er—S1v | 72.38 (8) | Ag2xiv—Ag2—Ervii | 112.73 (18) |
S2i—Er—S3i | 71.23 (8) | Erix—Ag2—Ervii | 106.0 (2) |
S2—Er—S3i | 70.50 (7) | S2vii—Ag2—Erviii | 125.81 (7) |
S2ii—Er—S3i | 146.97 (8) | S2viii—Ag2—Erviii | 54.35 (7) |
S3iii—Er—S3i | 70.57 (4) | S2ix—Ag2—Erviii | 127.26 (7) |
S3iv—Er—S3i | 139.30 (7) | S2x—Ag2—Erviii | 53.82 (11) |
S1v—Er—S3i | 75.73 (6) | S2xi—Ag2—Erviii | 121.4 (4) |
S2i—Er—Ag2v | 52.15 (11) | S2xii—Ag2—Erviii | 52.43 (11) |
S2—Er—Ag2v | 49.08 (19) | Ag2xiii—Ag2—Erviii | 67.27 (18) |
S2ii—Er—Ag2v | 51.80 (10) | Ag2xiv—Ag2—Erviii | 112.73 (18) |
S3iii—Er—Ag2v | 149.39 (11) | Erix—Ag2—Erviii | 106.0 (2) |
S3iv—Er—Ag2v | 124.65 (10) | Ervii—Ag2—Erviii | 106.0 (2) |
S1v—Er—Ag2v | 130.8 (2) | S2vii—Ag2—Erxv | 50.69 (11) |
S3i—Er—Ag2v | 95.37 (12) | S2viii—Ag2—Erxv | 52.12 (12) |
S2i—Er—Ag2vi | 47.22 (8) | S2ix—Ag2—Erxv | 120.0 (4) |
S2—Er—Ag2vi | 100.19 (17) | S2x—Ag2—Erxv | 130.10 (7) |
S2ii—Er—Ag2vi | 47.02 (8) | S2xi—Ag2—Erxv | 128.73 (6) |
S3iii—Er—Ag2vi | 110.90 (16) | S2xii—Ag2—Erxv | 64.22 (7) |
S3iv—Er—Ag2vi | 95.13 (13) | Ag2xiii—Ag2—Erxv | 118.39 (17) |
S1v—Er—Ag2vi | 165.81 (5) | Ag2xiv—Ag2—Erxv | 61.61 (17) |
S3i—Er—Ag2vi | 118.43 (7) | Erix—Ag2—Erxv | 174.3 (3) |
Ag2v—Er—Ag2vi | 51.12 (2) | Ervii—Ag2—Erxv | 77.17 (2) |
S2vii—Ag2—S2viii | 95.0 (3) | Erviii—Ag2—Erxv | 77.17 (2) |
S2vii—Ag2—S2ix | 95.0 (3) | S1iv—Ge1—S3ii | 114.96 (8) |
S2viii—Ag2—S2ix | 95.0 (3) | S1iv—Ge1—S3xvi | 114.96 (8) |
S2vii—Ag2—S2x | 175.8 (4) | S3ii—Ge1—S3xvi | 103.46 (9) |
S2viii—Ag2—S2x | 87.80 (5) | S1iv—Ge1—S3v | 114.96 (8) |
S2ix—Ag2—S2x | 87.80 (5) | S3ii—Ge1—S3v | 103.46 (9) |
S2vii—Ag2—S2xi | 87.80 (5) | S3xvi—Ge1—S3v | 103.46 (9) |
S2viii—Ag2—S2xi | 175.8 (4) | Ge1xvii—S1—Erxviii | 114.20 (8) |
S2ix—Ag2—S2xi | 87.80 (5) | Ge1xvii—S1—Ervii | 114.20 (8) |
S2x—Ag2—S2xi | 89.2 (3) | Erxviii—S1—Ervii | 104.35 (9) |
S2vii—Ag2—S2xii | 87.80 (5) | Ge1xvii—S1—Erxix | 114.20 (8) |
S2viii—Ag2—S2xii | 87.80 (5) | Erxviii—S1—Erxix | 104.35 (9) |
S2ix—Ag2—S2xii | 175.8 (4) | Ervii—S1—Erxix | 104.35 (9) |
S2x—Ag2—S2xii | 89.2 (3) | Ag2v—S2—Ag2xx | 67.44 (7) |
S2xi—Ag2—S2xii | 89.2 (3) | Ag2v—S2—Erxix | 82.09 (10) |
S2vii—Ag2—Ag2xiii | 121.6 (2) | Ag2xx—S2—Erxix | 75.42 (7) |
S2viii—Ag2—Ag2xiii | 121.6 (2) | Ag2v—S2—Er | 76.6 (2) |
S2ix—Ag2—Ag2xiii | 121.6 (2) | Ag2xx—S2—Er | 144.0 (2) |
S2x—Ag2—Ag2xiii | 54.2 (2) | Erxix—S2—Er | 101.16 (9) |
S2xi—Ag2—Ag2xiii | 54.2 (2) | Ag2v—S2—Erxxi | 80.87 (10) |
S2xii—Ag2—Ag2xiii | 54.2 (2) | Ag2xx—S2—Erxxi | 74.39 (7) |
S2vii—Ag2—Ag2xiv | 58.4 (2) | Erxix—S2—Erxxi | 149.19 (11) |
S2viii—Ag2—Ag2xiv | 58.4 (2) | Er—S2—Erxxi | 99.59 (8) |
S2ix—Ag2—Ag2xiv | 58.4 (2) | Ge1vii—S3—Erxv | 90.90 (8) |
S2x—Ag2—Ag2xiv | 125.8 (2) | Ge1vii—S3—Erxvii | 89.11 (8) |
S2xi—Ag2—Ag2xiv | 125.8 (2) | Erxv—S3—Erxvii | 106.35 (9) |
S2xii—Ag2—Ag2xiv | 125.8 (2) | Ge1vii—S3—Erxix | 117.62 (11) |
Ag2xiii—Ag2—Ag2xiv | 180.000 (4) | Erxv—S3—Erxix | 146.82 (9) |
S2vii—Ag2—Erix | 127.26 (7) | Erxvii—S3—Erxix | 91.58 (7) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) y, −x+y+1, z−1/2; (iii) −x+y+1, −x+1, z−1; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z−1; (vii) −x+1, −y+1, z+1/2; (viii) x−y, x−1, z+1/2; (ix) y−1, −x+y, z+1/2; (x) x−1, y−1, z; (xi) −x+y, −x+1, z; (xii) −y+1, x−y, z; (xiii) −x, −y, z−1/2; (xiv) −x, −y, z+1/2; (xv) −y+1, x−y, z+1; (xvi) x−y, x, z−1/2; (xvii) x, y, z+1; (xviii) x−y, x, z+1/2; (xix) y, −x+y+1, z+1/2; (xx) x+1, y+1, z; (xxi) x−y+1, x, z+1/2. |
Crystal data top
Ag0.50GeS7Y3 | Dx = 4.240 Mg m−3 |
Mr = 617.67 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63 | Cell parameters from 641 reflections |
Hall symbol: P 6c | θ = 4.2–26.3° |
a = 9.8090 (14) Å | µ = 23.31 mm−1 |
c = 5.8059 (12) Å | T = 295 K |
V = 483.78 (14) Å3 | Prism, dark red |
Z = 2 | 0.09 × 0.06 × 0.05 mm |
F(000) = 569 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 657 independent reflections |
Radiation source: fine-focus sealed tube | 641 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.3°, θmin = 4.2° |
ω–scan | h = −12→11 |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | k = −12→12 |
Tmin = 0.107, Tmax = 0.210 | l = −7→7 |
5168 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0228P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.021 | (Δ/σ)max < 0.001 |
wR(F2) = 0.044 | Δρmax = 0.60 e Å−3 |
S = 1.12 | Δρmin = −1.38 e Å−3 |
657 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
38 parameters | Extinction coefficient: 0.0058 (9) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 294 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.036 (11) |
Crystal data top
Ag0.50GeS7Y3 | Z = 2 |
Mr = 617.67 | Mo Kα radiation |
Hexagonal, P63 | µ = 23.31 mm−1 |
a = 9.8090 (14) Å | T = 295 K |
c = 5.8059 (12) Å | 0.09 × 0.06 × 0.05 mm |
V = 483.78 (14) Å3 | |
Data collection top
KUMA KM-4 with area CCD detector diffractometer | 657 independent reflections |
Absorption correction: numerical CrysAlis (Oxford Diffraction, 2007) | 641 reflections with I > 2σ(I) |
Tmin = 0.107, Tmax = 0.210 | Rint = 0.050 |
5168 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.021 | 1 restraint |
wR(F2) = 0.044 | Δρmax = 0.60 e Å−3 |
S = 1.12 | Δρmin = −1.38 e Å−3 |
657 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 294 Friedel pairs |
38 parameters | Absolute structure parameter: −0.036 (11) |
Special details top
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. |
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 > σ(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y | 0.86329 (5) | 0.64088 (5) | 0.24445 (13) | 0.01737 (15) | |
Ag2 | 0.0000 | 0.0000 | 0.0009 (7) | 0.0814 (10) | 0.50 |
Ge1 | 0.3333 | 0.6667 | 0.32329 (13) | 0.0112 (2) | |
S1 | 0.3333 | 0.6667 | 0.9465 (4) | 0.0115 (5) | |
S2 | 0.89780 (14) | 0.73969 (16) | 0.7021 (2) | 0.0207 (3) | |
S3 | 0.57643 (15) | 0.47892 (15) | 0.9833 (2) | 0.0136 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y | 0.0132 (2) | 0.0128 (2) | 0.0263 (3) | 0.00662 (18) | −0.0023 (2) | −0.0006 (2) |
Ag2 | 0.0172 (5) | 0.0172 (5) | 0.210 (3) | 0.0086 (2) | 0.000 | 0.000 |
Ge1 | 0.0124 (3) | 0.0124 (3) | 0.0088 (4) | 0.00618 (15) | 0.000 | 0.000 |
S1 | 0.0139 (7) | 0.0139 (7) | 0.0065 (11) | 0.0070 (3) | 0.000 | 0.000 |
S2 | 0.0126 (6) | 0.0267 (7) | 0.0243 (8) | 0.0108 (5) | −0.0017 (5) | −0.0117 (6) |
S3 | 0.0174 (6) | 0.0137 (6) | 0.0123 (6) | 0.0097 (5) | −0.0010 (6) | −0.0003 (5) |
Geometric parameters (Å, º) top
Y—S2i | 2.7361 (14) | Ag2—Yxvii | 3.3885 (19) |
Y—S2 | 2.7906 (16) | Ag2—Yix | 3.4207 (19) |
Y—S2ii | 2.7944 (13) | Ge1—S1iv | 2.188 (2) |
Y—S3iii | 2.7946 (14) | Ge1—S3ii | 2.2249 (14) |
Y—S3iv | 2.8758 (14) | Ge1—S3xviii | 2.2249 (14) |
Y—S1v | 2.8944 (11) | Ge1—S3v | 2.2249 (13) |
Y—S3i | 3.0089 (14) | S1—Ge1xix | 2.188 (2) |
Y—S2iv | 3.2618 (17) | S1—Yxx | 2.8944 (11) |
Y—Ag2vi | 3.3885 (19) | S1—Yvii | 2.8944 (11) |
Y—Ag2vii | 3.421 (2) | S1—Yxxi | 2.8944 (11) |
Ag2—S2v | 2.516 (2) | S2—Ag2vii | 2.516 (2) |
Ag2—S2viii | 2.516 (2) | S2—Yxxi | 2.7361 (13) |
Ag2—S2ix | 2.516 (2) | S2—Yxxii | 2.7944 (13) |
Ag2—S2x | 2.824 (3) | S2—Ag2xxiii | 2.824 (3) |
Ag2—S2xi | 2.824 (3) | S2—Yxix | 3.2618 (17) |
Ag2—S2xii | 2.824 (3) | S3—Ge1vii | 2.2249 (13) |
Ag2—Ag2xiii | 2.9029 (6) | S3—Yxxiv | 2.7946 (14) |
Ag2—Ag2xiv | 2.9029 (6) | S3—Yxix | 2.8758 (14) |
Ag2—Yxv | 3.3885 (19) | S3—Yxxi | 3.0089 (14) |
Ag2—Yxvi | 3.3885 (19) | | |
| | | |
S2i—Y—S2 | 82.92 (4) | Ag2xiii—Ag2—Ag2xiv | 180.0 |
S2i—Y—S2ii | 88.50 (6) | S2v—Ag2—Yxv | 52.73 (4) |
S2—Y—S2ii | 81.88 (4) | S2viii—Ag2—Yxv | 54.08 (5) |
S2i—Y—S3iii | 99.71 (4) | S2ix—Ag2—Yxv | 127.67 (15) |
S2—Y—S3iii | 137.94 (4) | S2x—Ag2—Yxv | 128.55 (4) |
S2ii—Y—S3iii | 139.84 (5) | S2xi—Ag2—Yxv | 127.33 (4) |
S2i—Y—S3iv | 138.86 (5) | S2xii—Ag2—Yxv | 62.57 (3) |
S2—Y—S3iv | 127.53 (4) | Ag2xiii—Ag2—Yxv | 65.34 (7) |
S2ii—Y—S3iv | 72.15 (4) | Ag2xiv—Ag2—Yxv | 114.66 (7) |
S3iii—Y—S3iv | 76.26 (5) | S2v—Ag2—Yxvi | 127.67 (15) |
S2i—Y—S1v | 147.46 (4) | S2viii—Ag2—Yxvi | 52.73 (4) |
S2—Y—S1v | 83.00 (5) | S2ix—Ag2—Yxvi | 54.08 (5) |
S2ii—Y—S1v | 118.23 (3) | S2x—Ag2—Yxvi | 62.57 (3) |
S3iii—Y—S1v | 72.48 (4) | S2xi—Ag2—Yxvi | 128.55 (4) |
S3iv—Y—S1v | 71.33 (4) | S2xii—Ag2—Yxvi | 127.33 (4) |
S2i—Y—S3i | 70.64 (4) | Ag2xiii—Ag2—Yxvi | 65.34 (7) |
S2—Y—S3i | 70.20 (4) | Ag2xiv—Ag2—Yxvi | 114.66 (7) |
S2ii—Y—S3i | 146.62 (4) | Yxv—Ag2—Yxvi | 103.82 (8) |
S3iii—Y—S3i | 71.28 (3) | S2v—Ag2—Yxvii | 54.08 (5) |
S3iv—Y—S3i | 139.99 (4) | S2viii—Ag2—Yxvii | 127.67 (15) |
S1v—Y—S3i | 77.00 (3) | S2ix—Ag2—Yxvii | 52.73 (4) |
S2i—Y—S2iv | 74.62 (4) | S2x—Ag2—Yxvii | 127.33 (4) |
S2—Y—S2iv | 147.08 (5) | S2xi—Ag2—Yxvii | 62.57 (3) |
S2ii—Y—S2iv | 73.90 (4) | S2xii—Ag2—Yxvii | 128.55 (4) |
S3iii—Y—S2iv | 70.70 (4) | Ag2xiii—Ag2—Yxvii | 65.34 (7) |
S3iv—Y—S2iv | 65.34 (4) | Ag2xiv—Ag2—Yxvii | 114.66 (7) |
S1v—Y—S2iv | 128.09 (5) | Yxv—Ag2—Yxvii | 103.82 (8) |
S3i—Y—S2iv | 122.05 (4) | Yxvi—Ag2—Yxvii | 103.82 (8) |
S2i—Y—Ag2vi | 47.03 (4) | S2v—Ag2—Yix | 127.60 (3) |
S2—Y—Ag2vi | 96.89 (7) | S2viii—Ag2—Yix | 126.26 (3) |
S2ii—Y—Ag2vi | 46.81 (4) | S2ix—Ag2—Yix | 53.48 (4) |
S3iii—Y—Ag2vi | 115.64 (7) | S2x—Ag2—Yix | 50.88 (5) |
S3iv—Y—Ag2vi | 97.10 (6) | S2xi—Ag2—Yix | 52.10 (4) |
S1v—Y—Ag2vi | 164.509 (17) | S2xii—Ag2—Yix | 116.28 (13) |
S3i—Y—Ag2vi | 117.64 (4) | Ag2xiii—Ag2—Yix | 115.81 (7) |
S2iv—Y—Ag2vi | 50.21 (7) | Ag2xiv—Ag2—Yix | 64.19 (7) |
S2i—Y—Ag2vii | 53.20 (4) | Yxv—Ag2—Yix | 178.85 (13) |
S2—Y—Ag2vii | 46.43 (7) | Yxvi—Ag2—Yix | 76.853 (8) |
S2ii—Y—Ag2vii | 52.89 (4) | Yxvii—Ag2—Yix | 76.853 (8) |
S3iii—Y—Ag2vii | 152.76 (4) | S1iv—Ge1—S3ii | 114.68 (4) |
S3iv—Y—Ag2vii | 124.74 (4) | S1iv—Ge1—S3xviii | 114.68 (4) |
S1v—Y—Ag2vii | 127.64 (8) | S3ii—Ge1—S3xviii | 103.79 (4) |
S3i—Y—Ag2vii | 93.92 (5) | S1iv—Ge1—S3v | 114.68 (4) |
S2iv—Y—Ag2vii | 100.67 (7) | S3ii—Ge1—S3v | 103.79 (4) |
Ag2vi—Y—Ag2vii | 50.467 (13) | S3xviii—Ge1—S3v | 103.79 (4) |
S2v—Ag2—S2viii | 100.17 (11) | Ge1xix—S1—Yxx | 113.90 (4) |
S2v—Ag2—S2ix | 100.17 (11) | Ge1xix—S1—Yvii | 113.90 (4) |
S2viii—Ag2—S2ix | 100.17 (11) | Yxx—S1—Yvii | 104.70 (5) |
S2v—Ag2—S2x | 169.76 (16) | Ge1xix—S1—Yxxi | 113.90 (4) |
S2viii—Ag2—S2x | 86.32 (3) | Yxx—S1—Yxxi | 104.70 (5) |
S2ix—Ag2—S2x | 86.32 (3) | Yvii—S1—Yxxi | 104.70 (5) |
S2v—Ag2—S2xi | 86.32 (3) | Ag2vii—S2—Yxxi | 80.24 (4) |
S2viii—Ag2—S2xi | 169.76 (16) | Ag2vii—S2—Y | 80.09 (9) |
S2ix—Ag2—S2xi | 86.32 (3) | Yxxi—S2—Y | 99.94 (4) |
S2x—Ag2—S2xi | 86.21 (11) | Ag2vii—S2—Yxxii | 79.11 (4) |
S2v—Ag2—S2xii | 86.32 (3) | Yxxi—S2—Yxxii | 149.35 (6) |
S2viii—Ag2—S2xii | 86.32 (3) | Y—S2—Yxxii | 98.53 (4) |
S2ix—Ag2—S2xii | 169.76 (16) | Ag2vii—S2—Ag2xxiii | 65.57 (4) |
S2x—Ag2—S2xii | 86.21 (11) | Yxxi—S2—Ag2xxiii | 75.92 (3) |
S2xi—Ag2—S2xii | 86.21 (11) | Y—S2—Ag2xxiii | 145.65 (9) |
S2v—Ag2—Ag2xiii | 62.33 (9) | Yxxii—S2—Ag2xxiii | 75.01 (3) |
S2viii—Ag2—Ag2xiii | 62.33 (9) | Ag2vii—S2—Yxix | 132.79 (10) |
S2ix—Ag2—Ag2xiii | 62.33 (9) | Yxxi—S2—Yxix | 89.31 (4) |
S2x—Ag2—Ag2xiii | 127.90 (7) | Y—S2—Yxix | 147.08 (5) |
S2xi—Ag2—Ag2xiii | 127.90 (7) | Yxxii—S2—Yxix | 88.31 (4) |
S2xii—Ag2—Ag2xiii | 127.90 (7) | Ag2xxiii—S2—Yxix | 67.22 (7) |
S2v—Ag2—Ag2xiv | 117.67 (9) | Ge1vii—S3—Yxxiv | 91.02 (5) |
S2viii—Ag2—Ag2xiv | 117.67 (9) | Ge1vii—S3—Yxix | 88.93 (4) |
S2ix—Ag2—Ag2xiv | 117.67 (9) | Yxxiv—S3—Yxix | 107.85 (5) |
S2x—Ag2—Ag2xiv | 52.10 (7) | Ge1vii—S3—Yxxi | 118.37 (5) |
S2xi—Ag2—Ag2xiv | 52.10 (7) | Yxxiv—S3—Yxxi | 145.19 (5) |
S2xii—Ag2—Ag2xiv | 52.10 (7) | Yxix—S3—Yxxi | 91.94 (4) |
Symmetry codes: (i) x−y+1, x, z−1/2; (ii) y, −x+y+1, z−1/2; (iii) −x+y+1, −x+1, z−1; (iv) x, y, z−1; (v) −x+1, −y+1, z−1/2; (vi) x+1, y+1, z; (vii) −x+1, −y+1, z+1/2; (viii) x−y, x−1, z−1/2; (ix) y−1, −x+y, z−1/2; (x) x−1, y−1, z−1; (xi) −x+y, −x+1, z−1; (xii) −y+1, x−y, z−1; (xiii) −x, −y, z+1/2; (xiv) −x, −y, z−1/2; (xv) −y+1, x−y, z; (xvi) x−1, y−1, z; (xvii) −x+y, −x+1, z; (xviii) x−y, x, z−1/2; (xix) x, y, z+1; (xx) x−y, x, z+1/2; (xxi) y, −x+y+1, z+1/2; (xxii) x−y+1, x, z+1/2; (xxiii) x+1, y+1, z+1; (xxiv) −y+1, x−y, z+1. |
Experimental details
| (la) | (ce) | (pr) | (nd) |
Crystal data |
Chemical formula | Ag0.82GeLa3S7 | Ag0.88Ce3GeS7 | Ag0.89GePr3S7 | Ag0.84GeNd3S7 |
Mr | 802.19 | 812.30 | 815.74 | 819.80 |
Crystal system, space group | Hexagonal, P63 | Hexagonal, P63 | Hexagonal, P63 | Hexagonal, P63 |
Temperature (K) | 295 | 295 | 295 | 295 |
a, c (Å) | 10.4056 (15), 5.8280 (12) | 10.3902 (15), 5.8425 (12) | 10.2290 (14), 5.7760 (11) | 10.1930 (14), 5.7693 (12) |
V (Å3) | 546.49 (16) | 546.23 (16) | 523.39 (14) | 519.11 (15) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 16.91 | 17.79 | 19.50 | 20.49 |
Crystal size (mm) | 0.09 × 0.04 × 0.03 | 0.09 × 0.08 × 0.06 | 0.10 × 0.09 × 0.07 | 0.11 × 0.09 × 0.08 |
|
Data collection |
Diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer |
Absorption correction | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) |
Tmin, Tmax | 0.097, 0.599 | 0.097, 0.599 | 0.163, 0.272 | 0.093, 0.261 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5858, 743, 729 | 6515, 726, 704 | 5174, 602, 585 | 5463, 713, 700 |
Rint | 0.039 | 0.043 | 0.059 | 0.038 |
(sin θ/λ)max (Å−1) | 0.625 | 0.625 | 0.595 | 0.625 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.011, 0.022, 1.04 | 0.021, 0.046, 1.06 | 0.025, 0.051, 1.09 | 0.016, 0.035, 1.08 |
No. of reflections | 743 | 726 | 602 | 713 |
No. of parameters | 43 | 43 | 43 | 43 |
No. of restraints | 1 | 1 | 1 | 1 |
Δρmax, Δρmin (e Å−3) | 0.37, −0.44 | 1.01, −0.70 | 1.22, −0.73 | 0.72, −0.75 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881, 334 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 319 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 320 Friedel pairs |
Absolute structure parameter | 0.014 (12) | −0.04 (2) | 0.05 (3) | −0.027 (19) |
| (sm) | (gd) | (tb) | (dy) |
Crystal data |
Chemical formula | Ag0.74GeS7Sm3 | Ag0.63Gd3GeS7 | Ag0.59GeS7Tb3 | Ag0.51Dy3GeS7 |
Mr | 827.34 | 836.18 | 836.87 | 840.06 |
Crystal system, space group | Hexagonal, P63 | Hexagonal, P63 | Hexagonal, P63 | Hexagonal, P63 |
Temperature (K) | 295 | 295 | 295 | 295 |
a, c (Å) | 10.0809 (14), 5.7604 (12) | 9.9637 (14), 5.7660 (12) | 9.9003 (14), 5.7654 (12) | 9.8003 (14), 5.7879 (12) |
V (Å3) | 506.97 (15) | 495.73 (14) | 489.39 (14) | 481.43 (14) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 22.80 | 25.41 | 27.01 | 28.56 |
Crystal size (mm) | 0.13 × 0.11 × 0.09 | 0.13 × 0.12 × 0.10 | 0.12 × 0.11 × 0.08 | 0.12 × 0.10 × 0.09 |
|
Data collection |
Diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer |
Absorption correction | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) |
Tmin, Tmax | 0.029, 0.242 | 0.024, 0.192 | 0.044, 0.187 | 0.035, 0.244 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4935, 604, 601 | 5095, 658, 657 | 4229, 602, 597 | 5667, 655, 644 |
Rint | 0.046 | 0.044 | 0.039 | 0.046 |
(sin θ/λ)max (Å−1) | 0.602 | 0.621 | 0.609 | 0.625 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.014, 0.034, 1.17 | 0.013, 0.029, 1.12 | 0.017, 0.038, 1.17 | 0.015, 0.032, 1.12 |
No. of reflections | 604 | 658 | 602 | 655 |
No. of parameters | 43 | 43 | 39 | 39 |
No. of restraints | 1 | 1 | 1 | 1 |
Δρmax, Δρmin (e Å−3) | 0.70, −0.51 | 0.58, −0.81 | 0.84, −1.39 | 0.99, −1.03 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881, 270 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 296 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 293 Friedel pairs |
Absolute structure parameter | −0.029 (18) | 0.006 (15) | 0.00 (2) | −0.005 (19) |
| (ho) | (er) | (y) |
Crystal data |
Chemical formula | Ag0.50GeHo3S7 | Ag0.50Er3GeS7 | Ag0.50GeS7Y3 |
Mr | 845.73 | 852.72 | 617.67 |
Crystal system, space group | Hexagonal, P63 | Hexagonal, P63 | Hexagonal, P63 |
Temperature (K) | 295 | 295 | 295 |
a, c (Å) | 9.7401 (14), 5.7994 (12) | 9.6921 (14), 5.8308 (12) | 9.8090 (14), 5.8059 (12) |
V (Å3) | 476.48 (14) | 474.35 (14) | 483.78 (14) |
Z | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 30.22 | 31.87 | 23.31 |
Crystal size (mm) | 0.09 × 0.07 × 0.03 | 0.13 × 0.10 × 0.08 | 0.09 × 0.06 × 0.05 |
|
Data collection |
Diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer | KUMA KM-4 with area CCD detector diffractometer |
Absorption correction | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) | Numerical CrysAlis (Oxford Diffraction, 2007) |
Tmin, Tmax | 0.061, 0.304 | 0.038, 0.131 | 0.107, 0.210 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5792, 649, 630 | 4994, 633, 628 | 5168, 657, 641 |
Rint | 0.045 | 0.049 | 0.050 |
(sin θ/λ)max (Å−1) | 0.633 | 0.625 | 0.624 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.033, 1.19 | 0.022, 0.053, 1.15 | 0.021, 0.044, 1.12 |
No. of reflections | 649 | 633 | 657 |
No. of parameters | 38 | 38 | 38 |
No. of restraints | 1 | 1 | 1 |
Δρmax, Δρmin (e Å−3) | 0.79, −2.26 | 0.86, −2.84 | 0.60, −1.38 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881, 275 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 280 Friedel pairs | Flack H D (1983), Acta Cryst. A39, 876-881, 294 Friedel pairs |
Absolute structure parameter | −0.04 (2) | −0.03 (3) | −0.036 (11) |
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