Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768108004175/bs5058sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768108004175/bs5058prsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768108004175/bs5058ndsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768108004175/bs5058gdsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768108004175/bs5058tbsup5.hkl |
For all compounds, data collection: CrysAlis 1.171.32.6; cell refinement: CrysAlis 1.171.32.6; data reduction: CrysAlis 1.171.32.6; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Pr2S5Sn | F(000) = 496 |
Mr = 560.81 | Dx = 5.382 Mg m−3 |
Orthorhombic, Pbam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2 2ab | Cell parameters from 424 reflections |
a = 7.8195 (9) Å | θ = 3.2–27.5° |
b = 11.2145 (14) Å | µ = 18.82 mm−1 |
c = 3.9462 (5) Å | T = 293 K |
V = 346.05 (7) Å3 | Prism, dark red |
Z = 2 | 0.09 × 0.08 × 0.06 mm |
KUMA KM-4 with area CCD detector diffractometer | 452 independent reflections |
Radiation source: fine-focus sealed tube | 424 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω–scan | h = −10→9 |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | k = −12→14 |
Tmin = 0.239, Tmax = 0.458 | l = −5→4 |
4036 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.013 | w = 1/[σ2(Fo2) + (0.0102P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.025 | (Δ/σ)max = 0.001 |
S = 1.12 | Δρmax = 0.64 e Å−3 |
452 reflections | Δρmin = −0.70 e Å−3 |
28 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0093 (4) |
Pr2S5Sn | V = 346.05 (7) Å3 |
Mr = 560.81 | Z = 2 |
Orthorhombic, Pbam | Mo Kα radiation |
a = 7.8195 (9) Å | µ = 18.82 mm−1 |
b = 11.2145 (14) Å | T = 293 K |
c = 3.9462 (5) Å | 0.09 × 0.08 × 0.06 mm |
KUMA KM-4 with area CCD detector diffractometer | 452 independent reflections |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | 424 reflections with I > 2σ(I) |
Tmin = 0.239, Tmax = 0.458 | Rint = 0.041 |
4036 measured reflections |
R[F2 > 2σ(F2)] = 0.013 | 28 parameters |
wR(F2) = 0.025 | 0 restraints |
S = 1.12 | Δρmax = 0.64 e Å−3 |
452 reflections | Δρmin = −0.70 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
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. |
x | y | z | Uiso*/Ueq | ||
ND1 | 0.43360 (3) | 0.169372 (18) | 0.5000 | 0.00845 (9) | |
Sn1 | 0.0000 | 0.0000 | 0.0000 | 0.00849 (11) | |
S1 | 0.81432 (12) | 0.07439 (8) | 0.5000 | 0.0097 (2) | |
S2 | 0.15009 (12) | 0.20120 (8) | 0.0000 | 0.0083 (2) | |
S3 | 0.5000 | 0.0000 | 0.0000 | 0.0094 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
ND1 | 0.01044 (13) | 0.00759 (13) | 0.00732 (14) | 0.00072 (7) | 0.000 | 0.000 |
Sn1 | 0.0101 (2) | 0.00657 (18) | 0.0088 (2) | −0.00151 (13) | 0.000 | 0.000 |
S1 | 0.0084 (5) | 0.0123 (5) | 0.0084 (5) | 0.0017 (3) | 0.000 | 0.000 |
S2 | 0.0088 (5) | 0.0072 (4) | 0.0090 (5) | −0.0003 (3) | 0.000 | 0.000 |
S3 | 0.0114 (7) | 0.0084 (6) | 0.0085 (8) | 0.0011 (5) | 0.000 | 0.000 |
ND1—S3 | 2.7876 (3) | Sn1—S1viii | 2.5879 (6) |
ND1—S3i | 2.7876 (3) | Sn1—S1v | 2.5879 (6) |
ND1—S2ii | 2.9775 (7) | Sn1—S1ix | 2.5879 (6) |
ND1—S2iii | 2.9775 (7) | Sn1—S1x | 2.5879 (6) |
ND1—S2 | 2.9892 (8) | S1—Sn1xi | 2.5879 (6) |
ND1—S2i | 2.9892 (8) | S1—Sn1xii | 2.5879 (6) |
ND1—S1iv | 3.0211 (10) | S1—ND1iii | 3.0211 (10) |
ND1—S1 | 3.1618 (10) | S2—ND1xiii | 2.9775 (7) |
ND1—ND1v | 3.9382 (6) | S2—ND1iv | 2.9775 (7) |
ND1—ND1i | 3.9462 (5) | S2—ND1vi | 2.9892 (8) |
ND1—ND1vi | 3.9462 (5) | S3—ND1x | 2.7876 (3) |
Sn1—S2vii | 2.5433 (9) | S3—ND1vi | 2.7876 (3) |
Sn1—S2 | 2.5433 (9) | S3—ND1v | 2.7876 (3) |
S3—ND1—S3i | 90.116 (12) | S3i—ND1—ND1vi | 135.058 (6) |
S3—ND1—S2ii | 134.053 (19) | S2ii—ND1—ND1vi | 131.504 (13) |
S3i—ND1—S2ii | 75.949 (17) | S2iii—ND1—ND1vi | 48.496 (13) |
S3—ND1—S2iii | 75.949 (17) | S2—ND1—ND1vi | 48.694 (13) |
S3i—ND1—S2iii | 134.053 (19) | S2i—ND1—ND1vi | 131.306 (13) |
S2ii—ND1—S2iii | 83.01 (3) | S1iv—ND1—ND1vi | 90.0 |
S3—ND1—S2 | 75.658 (16) | S1—ND1—ND1vi | 90.0 |
S3i—ND1—S2 | 133.371 (18) | ND1v—ND1—ND1vi | 90.0 |
S2ii—ND1—S2 | 143.212 (13) | ND1i—ND1—ND1vi | 180.000 (17) |
S2iii—ND1—S2 | 85.758 (11) | S2vii—Sn1—S2 | 180.000 (19) |
S3—ND1—S2i | 133.371 (18) | S2vii—Sn1—S1viii | 91.55 (3) |
S3i—ND1—S2i | 75.658 (16) | S2—Sn1—S1viii | 88.45 (3) |
S2ii—ND1—S2i | 85.758 (11) | S2vii—Sn1—S1v | 88.45 (3) |
S2iii—ND1—S2i | 143.212 (13) | S2—Sn1—S1v | 91.55 (3) |
S2—ND1—S2i | 82.61 (3) | S1viii—Sn1—S1v | 180.00 (4) |
S3—ND1—S1iv | 134.879 (6) | S2vii—Sn1—S1ix | 91.55 (3) |
S3i—ND1—S1iv | 134.879 (6) | S2—Sn1—S1ix | 88.45 (3) |
S2ii—ND1—S1iv | 73.25 (2) | S1viii—Sn1—S1ix | 99.36 (3) |
S2iii—ND1—S1iv | 73.25 (2) | S1v—Sn1—S1ix | 80.64 (3) |
S2—ND1—S1iv | 69.97 (2) | S2vii—Sn1—S1x | 88.45 (3) |
S2i—ND1—S1iv | 69.97 (2) | S2—Sn1—S1x | 91.55 (3) |
S3—ND1—S1 | 66.115 (12) | S1viii—Sn1—S1x | 80.64 (3) |
S3i—ND1—S1 | 66.115 (12) | S1v—Sn1—S1x | 99.36 (3) |
S2ii—ND1—S1 | 68.22 (2) | S1ix—Sn1—S1x | 180.00 (3) |
S2iii—ND1—S1 | 68.22 (2) | Sn1xi—S1—Sn1xii | 99.36 (3) |
S2—ND1—S1 | 137.606 (14) | Sn1xi—S1—ND1iii | 97.67 (2) |
S2i—ND1—S1 | 137.606 (14) | Sn1xii—S1—ND1iii | 97.67 (2) |
S1iv—ND1—S1 | 127.67 (3) | Sn1xi—S1—ND1 | 129.558 (17) |
S3—ND1—ND1v | 45.058 (6) | Sn1xii—S1—ND1 | 129.558 (17) |
S3i—ND1—ND1v | 45.058 (6) | ND1iii—S1—ND1 | 88.30 (2) |
S2ii—ND1—ND1v | 108.682 (19) | Sn1—S2—ND1xiii | 99.79 (3) |
S2iii—ND1—ND1v | 108.682 (19) | Sn1—S2—ND1iv | 99.79 (3) |
S2—ND1—ND1v | 108.103 (18) | ND1xiii—S2—ND1iv | 83.01 (3) |
S2i—ND1—ND1v | 108.103 (18) | Sn1—S2—ND1 | 103.67 (3) |
S1iv—ND1—ND1v | 177.30 (2) | ND1xiii—S2—ND1 | 156.53 (3) |
S1—ND1—ND1v | 55.026 (17) | ND1iv—S2—ND1 | 92.433 (11) |
S3—ND1—ND1i | 135.058 (6) | Sn1—S2—ND1vi | 103.67 (3) |
S3i—ND1—ND1i | 44.942 (6) | ND1xiii—S2—ND1vi | 92.433 (12) |
S2ii—ND1—ND1i | 48.496 (13) | ND1iv—S2—ND1vi | 156.53 (3) |
S2iii—ND1—ND1i | 131.504 (13) | ND1—S2—ND1vi | 82.61 (3) |
S2—ND1—ND1i | 131.306 (13) | ND1—S3—ND1x | 180.000 (8) |
S2i—ND1—ND1i | 48.694 (13) | ND1—S3—ND1vi | 90.116 (12) |
S1iv—ND1—ND1i | 90.0 | ND1x—S3—ND1vi | 89.884 (12) |
S1—ND1—ND1i | 90.0 | ND1—S3—ND1v | 89.884 (12) |
ND1v—ND1—ND1i | 90.0 | ND1x—S3—ND1v | 90.116 (12) |
S3—ND1—ND1vi | 44.942 (6) | ND1vi—S3—ND1v | 180.000 (6) |
Symmetry codes: (i) x, y, z+1; (ii) x+1/2, −y+1/2, z+1; (iii) x+1/2, −y+1/2, z; (iv) x−1/2, −y+1/2, z; (v) −x+1, −y, −z+1; (vi) x, y, z−1; (vii) −x, −y, −z; (viii) x−1, y, z−1; (ix) x−1, y, z; (x) −x+1, −y, −z; (xi) x+1, y, z+1; (xii) x+1, y, z; (xiii) x−1/2, −y+1/2, z−1. |
Nd2S5Sn | F(000) = 500 |
Mr = 567.47 | Dx = 5.504 Mg m−3 |
Orthorhombic, Pbam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2 2ab | Cell parameters from 392 reflections |
a = 7.7721 (14) Å | θ = 3.2–26.7° |
b = 11.218 (2) Å | µ = 19.96 mm−1 |
c = 3.9272 (9) Å | T = 293 K |
V = 342.41 (12) Å3 | Prism, black |
Z = 2 | 0.22 × 0.21 × 0.19 mm |
KUMA KM-4 with area CCD detector diffractometer | 402 independent reflections |
Radiation source: fine-focus sealed tube | 392 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.094 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.7°, θmin = 3.2° |
ω–scan | h = −8→9 |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | k = −14→14 |
Tmin = 0.123, Tmax = 0.258 | l = −4→4 |
3642 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.026 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.067 | w = 1/[σ2(Fo2) + (0.030P)2 + 3.9487P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
402 reflections | Δρmax = 1.33 e Å−3 |
27 parameters | Δρmin = −1.83 e Å−3 |
Nd2S5Sn | V = 342.41 (12) Å3 |
Mr = 567.47 | Z = 2 |
Orthorhombic, Pbam | Mo Kα radiation |
a = 7.7721 (14) Å | µ = 19.96 mm−1 |
b = 11.218 (2) Å | T = 293 K |
c = 3.9272 (9) Å | 0.22 × 0.21 × 0.19 mm |
KUMA KM-4 with area CCD detector diffractometer | 402 independent reflections |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | 392 reflections with I > 2σ(I) |
Tmin = 0.123, Tmax = 0.258 | Rint = 0.094 |
3642 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 27 parameters |
wR(F2) = 0.067 | 0 restraints |
S = 1.09 | Δρmax = 1.33 e Å−3 |
402 reflections | Δρmin = −1.83 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
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. |
x | y | z | Uiso*/Ueq | ||
Nd1 | 0.43909 (6) | 0.16988 (4) | 0.5000 | 0.0100 (2) | |
Sn1 | 0.0000 | 0.0000 | 0.0000 | 0.0101 (3) | |
S1 | 0.8162 (3) | 0.0772 (2) | 0.5000 | 0.0117 (5) | |
S2 | 0.1544 (3) | 0.20048 (19) | 0.0000 | 0.0103 (5) | |
S3 | 0.5000 | 0.0000 | 0.0000 | 0.0107 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.0097 (3) | 0.0105 (3) | 0.0100 (3) | 0.00091 (16) | 0.000 | 0.000 |
Sn1 | 0.0107 (5) | 0.0087 (5) | 0.0110 (5) | −0.0023 (3) | 0.000 | 0.000 |
S1 | 0.0078 (10) | 0.0141 (11) | 0.0132 (11) | 0.0029 (8) | 0.000 | 0.000 |
S2 | 0.0076 (9) | 0.0092 (10) | 0.0142 (12) | 0.0012 (8) | 0.000 | 0.000 |
S3 | 0.0112 (15) | 0.0087 (14) | 0.0123 (15) | 0.0005 (11) | 0.000 | 0.000 |
Nd1—S3 | 2.7770 (5) | Sn1—S1viii | 2.5782 (14) |
Nd1—S3i | 2.7770 (5) | Sn1—S1vi | 2.5782 (14) |
Nd1—S2ii | 2.9618 (16) | Sn1—S1ix | 2.5782 (14) |
Nd1—S2iii | 2.9618 (16) | Sn1—S1x | 2.5782 (14) |
Nd1—S2 | 2.9779 (17) | S1—Sn1xi | 2.5782 (14) |
Nd1—S2i | 2.9779 (17) | S1—Sn1xii | 2.5782 (14) |
Nd1—S1iv | 2.993 (2) | S1—Nd1iii | 2.993 (2) |
Nd1—S1 | 3.110 (2) | S2—Nd1xiii | 2.9618 (16) |
Nd1—Nd1i | 3.9272 (9) | S2—Nd1iv | 2.9618 (16) |
Nd1—Nd1v | 3.9272 (9) | S2—Nd1v | 2.9779 (17) |
Nd1—Nd1vi | 3.9274 (11) | S3—Nd1x | 2.7770 (5) |
Sn1—S2 | 2.549 (2) | S3—Nd1vi | 2.7770 (5) |
Sn1—S2vii | 2.549 (2) | S3—Nd1v | 2.7770 (5) |
S3—Nd1—S3i | 90.00 (2) | S3i—Nd1—Nd1vi | 44.999 (11) |
S3—Nd1—S2ii | 135.19 (4) | S2ii—Nd1—Nd1vi | 109.90 (4) |
S3i—Nd1—S2ii | 76.81 (4) | S2iii—Nd1—Nd1vi | 109.90 (4) |
S3—Nd1—S2iii | 76.81 (4) | S2—Nd1—Nd1vi | 106.92 (4) |
S3i—Nd1—S2iii | 135.19 (4) | S2i—Nd1—Nd1vi | 106.92 (4) |
S2ii—Nd1—S2iii | 83.06 (6) | S1iv—Nd1—Nd1vi | 175.35 (5) |
S3—Nd1—S2 | 74.90 (4) | S1—Nd1—Nd1vi | 56.52 (4) |
S3i—Nd1—S2 | 132.22 (4) | Nd1i—Nd1—Nd1vi | 90.0 |
S2ii—Nd1—S2 | 143.17 (3) | Nd1v—Nd1—Nd1vi | 90.0 |
S2iii—Nd1—S2 | 85.76 (2) | S2—Sn1—S2vii | 180.00 (5) |
S3—Nd1—S2i | 132.22 (4) | S2—Sn1—S1viii | 87.96 (6) |
S3i—Nd1—S2i | 74.90 (4) | S2vii—Sn1—S1viii | 92.04 (6) |
S2ii—Nd1—S2i | 85.76 (2) | S2—Sn1—S1vi | 92.04 (6) |
S2iii—Nd1—S2i | 143.17 (3) | S2vii—Sn1—S1vi | 87.96 (6) |
S2—Nd1—S2i | 82.51 (6) | S1viii—Sn1—S1vi | 180.0 |
S3—Nd1—S1iv | 134.813 (11) | S2—Sn1—S1ix | 87.96 (6) |
S3i—Nd1—S1iv | 134.813 (11) | S2vii—Sn1—S1ix | 92.04 (6) |
S2ii—Nd1—S1iv | 73.44 (5) | S1viii—Sn1—S1ix | 99.21 (7) |
S2iii—Nd1—S1iv | 73.44 (5) | S1vi—Sn1—S1ix | 80.79 (7) |
S2—Nd1—S1iv | 69.74 (5) | S2—Sn1—S1x | 92.04 (6) |
S2i—Nd1—S1iv | 69.74 (5) | S2vii—Sn1—S1x | 87.96 (6) |
S3—Nd1—S1 | 67.04 (3) | S1viii—Sn1—S1x | 80.79 (7) |
S3i—Nd1—S1 | 67.04 (3) | S1vi—Sn1—S1x | 99.21 (7) |
S2ii—Nd1—S1 | 68.38 (5) | S1ix—Sn1—S1x | 180.00 (12) |
S2iii—Nd1—S1 | 68.38 (5) | Sn1xi—S1—Sn1xii | 99.21 (7) |
S2—Nd1—S1 | 137.62 (3) | Sn1xi—S1—Nd1iii | 98.15 (6) |
S2i—Nd1—S1 | 137.62 (3) | Sn1xii—S1—Nd1iii | 98.15 (6) |
S1iv—Nd1—S1 | 128.13 (6) | Sn1xi—S1—Nd1 | 129.38 (4) |
S3—Nd1—Nd1i | 134.999 (10) | Sn1xii—S1—Nd1 | 129.38 (4) |
S3i—Nd1—Nd1i | 45.001 (11) | Nd1iii—S1—Nd1 | 89.08 (6) |
S2ii—Nd1—Nd1i | 48.47 (3) | Sn1—S2—Nd1xiii | 99.62 (6) |
S2iii—Nd1—Nd1i | 131.53 (3) | Sn1—S2—Nd1iv | 99.62 (6) |
S2—Nd1—Nd1i | 131.25 (3) | Nd1xiii—S2—Nd1iv | 83.06 (6) |
S2i—Nd1—Nd1i | 48.75 (3) | Sn1—S2—Nd1 | 104.36 (6) |
S1iv—Nd1—Nd1i | 90.0 | Nd1xiii—S2—Nd1 | 156.01 (8) |
S1—Nd1—Nd1i | 90.0 | Nd1iv—S2—Nd1 | 92.25 (2) |
S3—Nd1—Nd1v | 45.001 (11) | Sn1—S2—Nd1v | 104.36 (6) |
S3i—Nd1—Nd1v | 134.999 (11) | Nd1xiii—S2—Nd1v | 92.25 (2) |
S2ii—Nd1—Nd1v | 131.53 (3) | Nd1iv—S2—Nd1v | 156.01 (8) |
S2iii—Nd1—Nd1v | 48.47 (3) | Nd1—S2—Nd1v | 82.51 (6) |
S2—Nd1—Nd1v | 48.75 (3) | Nd1x—S3—Nd1 | 180.00 (2) |
S2i—Nd1—Nd1v | 131.25 (3) | Nd1x—S3—Nd1vi | 90.00 (2) |
S1iv—Nd1—Nd1v | 90.0 | Nd1—S3—Nd1vi | 90.00 (2) |
S1—Nd1—Nd1v | 90.0 | Nd1x—S3—Nd1v | 90.00 (2) |
Nd1i—Nd1—Nd1v | 180.00 (4) | Nd1—S3—Nd1v | 90.00 (2) |
S3—Nd1—Nd1vi | 44.999 (11) | Nd1vi—S3—Nd1v | 180.000 (13) |
Symmetry codes: (i) x, y, z+1; (ii) x+1/2, −y+1/2, z+1; (iii) x+1/2, −y+1/2, z; (iv) x−1/2, −y+1/2, z; (v) x, y, z−1; (vi) −x+1, −y, −z+1; (vii) −x, −y, −z; (viii) x−1, y, z−1; (ix) x−1, y, z; (x) −x+1, −y, −z; (xi) x+1, y, z+1; (xii) x+1, y, z; (xiii) x−1/2, −y+1/2, z−1. |
Gd2S5Sn | F(000) = 516 |
Mr = 593.49 | Dx = 5.907 Mg m−3 |
Orthorhombic, Pbam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2 2ab | Cell parameters from 348 reflections |
a = 7.7330 (17) Å | θ = 3.2–26.7° |
b = 11.290 (2) Å | µ = 24.80 mm−1 |
c = 3.8217 (9) Å | T = 293 K |
V = 333.66 (13) Å3 | Prism, black |
Z = 2 | 0.10 × 0.03 × 0.02 mm |
KUMA KM-4 with area CCD detector diffractometer | 401 independent reflections |
Radiation source: fine-focus sealed tube | 348 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.7°, θmin = 3.2° |
ω–scan | h = −9→9 |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | k = −14→14 |
Tmin = 0.242, Tmax = 0.546 | l = −4→4 |
3712 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.018 | w = 1/[σ2(Fo2) + (0.0053P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.027 | (Δ/σ)max < 0.001 |
S = 0.87 | Δρmax = 0.77 e Å−3 |
401 reflections | Δρmin = −0.96 e Å−3 |
28 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0222 (6) |
Gd2S5Sn | V = 333.66 (13) Å3 |
Mr = 593.49 | Z = 2 |
Orthorhombic, Pbam | Mo Kα radiation |
a = 7.7330 (17) Å | µ = 24.80 mm−1 |
b = 11.290 (2) Å | T = 293 K |
c = 3.8217 (9) Å | 0.10 × 0.03 × 0.02 mm |
KUMA KM-4 with area CCD detector diffractometer | 401 independent reflections |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | 348 reflections with I > 2σ(I) |
Tmin = 0.242, Tmax = 0.546 | Rint = 0.062 |
3712 measured reflections |
R[F2 > 2σ(F2)] = 0.018 | 28 parameters |
wR(F2) = 0.027 | 0 restraints |
S = 0.87 | Δρmax = 0.77 e Å−3 |
401 reflections | Δρmin = −0.96 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
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. |
x | y | z | Uiso*/Ueq | ||
Gd1 | 0.46231 (5) | 0.17255 (4) | 0.5000 | 0.00938 (16) | |
Sn1 | 0.0000 | 0.0000 | 0.0000 | 0.0090 (2) | |
S1 | 0.8270 (2) | 0.09066 (18) | 0.5000 | 0.0097 (5) | |
S2 | 0.1701 (2) | 0.19536 (18) | 0.0000 | 0.0086 (4) | |
S3 | 0.5000 | 0.0000 | 0.0000 | 0.0095 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.0113 (2) | 0.0095 (2) | 0.0073 (2) | 0.00074 (19) | 0.000 | 0.000 |
Sn1 | 0.0116 (5) | 0.0085 (4) | 0.0069 (4) | −0.0001 (3) | 0.000 | 0.000 |
S1 | 0.0107 (10) | 0.0105 (10) | 0.0079 (11) | 0.0018 (9) | 0.000 | 0.000 |
S2 | 0.0091 (9) | 0.0089 (11) | 0.0077 (10) | −0.0011 (8) | 0.000 | 0.000 |
S3 | 0.0114 (16) | 0.0113 (14) | 0.0057 (13) | −0.0010 (11) | 0.000 | 0.000 |
Gd1—S3 | 2.7444 (5) | Sn1—S1vi | 2.5472 (13) |
Gd1—S3i | 2.7444 (5) | Sn1—S1ix | 2.5472 (13) |
Gd1—S1ii | 2.871 (2) | Sn1—S2x | 2.568 (2) |
Gd1—S2iii | 2.9082 (15) | Sn1—S2 | 2.568 (2) |
Gd1—S2iv | 2.9082 (15) | S1—Sn1xi | 2.5472 (13) |
Gd1—S1 | 2.968 (2) | S1—Sn1xii | 2.5472 (13) |
Gd1—S2 | 2.9704 (15) | S1—Gd1iv | 2.871 (2) |
Gd1—S2i | 2.9704 (15) | S2—Gd1ii | 2.9082 (15) |
Gd1—Gd1v | 3.8217 (9) | S2—Gd1xiii | 2.9082 (15) |
Gd1—Gd1i | 3.8217 (9) | S2—Gd1v | 2.9704 (15) |
Gd1—Gd1vi | 3.9396 (12) | S3—Gd1ix | 2.7444 (5) |
Sn1—S1vii | 2.5472 (13) | S3—Gd1v | 2.7444 (5) |
Sn1—S1viii | 2.5472 (13) | S3—Gd1vi | 2.7444 (5) |
S3—Gd1—S3i | 88.26 (2) | S3i—Gd1—Gd1vi | 44.130 (11) |
S3—Gd1—S1ii | 134.407 (14) | S1ii—Gd1—Gd1vi | 167.14 (4) |
S3i—Gd1—S1ii | 134.407 (14) | S2iii—Gd1—Gd1vi | 115.17 (4) |
S3—Gd1—S2iii | 139.71 (4) | S2iv—Gd1—Gd1vi | 115.17 (4) |
S3i—Gd1—S2iii | 81.25 (3) | S1—Gd1—Gd1vi | 63.34 (4) |
S1ii—Gd1—S2iii | 73.97 (5) | S2—Gd1—Gd1vi | 101.44 (4) |
S3—Gd1—S2iv | 81.25 (3) | S2i—Gd1—Gd1vi | 101.44 (4) |
S3i—Gd1—S2iv | 139.71 (4) | Gd1v—Gd1—Gd1vi | 90.0 |
S1ii—Gd1—S2iv | 73.97 (5) | Gd1i—Gd1—Gd1vi | 90.0 |
S2iii—Gd1—S2iv | 82.15 (5) | S1vii—Sn1—S1viii | 97.21 (7) |
S3—Gd1—S1 | 71.21 (3) | S1vii—Sn1—S1vi | 180.0 |
S3i—Gd1—S1 | 71.21 (3) | S1viii—Sn1—S1vi | 82.79 (7) |
S1ii—Gd1—S1 | 129.52 (5) | S1vii—Sn1—S1ix | 82.79 (7) |
S2iii—Gd1—S1 | 68.57 (5) | S1viii—Sn1—S1ix | 180.00 (7) |
S2iv—Gd1—S1 | 68.57 (5) | S1vi—Sn1—S1ix | 97.21 (7) |
S3—Gd1—S2 | 72.21 (3) | S1vii—Sn1—S2x | 94.37 (5) |
S3i—Gd1—S2 | 126.17 (4) | S1viii—Sn1—S2x | 94.37 (5) |
S1ii—Gd1—S2 | 69.03 (5) | S1vi—Sn1—S2x | 85.63 (5) |
S2iii—Gd1—S2 | 142.99 (3) | S1ix—Sn1—S2x | 85.63 (5) |
S2iv—Gd1—S2 | 87.32 (2) | S1vii—Sn1—S2 | 85.63 (5) |
S1—Gd1—S2 | 138.58 (3) | S1viii—Sn1—S2 | 85.63 (5) |
S3—Gd1—S2i | 126.17 (4) | S1vi—Sn1—S2 | 94.37 (5) |
S3i—Gd1—S2i | 72.21 (3) | S1ix—Sn1—S2 | 94.37 (5) |
S1ii—Gd1—S2i | 69.03 (5) | S2x—Sn1—S2 | 180.00 (8) |
S2iii—Gd1—S2i | 87.32 (2) | Sn1xi—S1—Sn1xii | 97.21 (7) |
S2iv—Gd1—S2i | 142.99 (3) | Sn1xi—S1—Gd1iv | 100.53 (5) |
S1—Gd1—S2i | 138.58 (3) | Sn1xii—S1—Gd1iv | 100.53 (5) |
S2—Gd1—S2i | 80.08 (5) | Sn1xi—S1—Gd1 | 128.62 (4) |
S3—Gd1—Gd1v | 45.870 (11) | Sn1xii—S1—Gd1 | 128.62 (4) |
S3i—Gd1—Gd1v | 134.130 (11) | Gd1iv—S1—Gd1 | 93.22 (6) |
S1ii—Gd1—Gd1v | 90.0 | Sn1—S2—Gd1ii | 99.05 (5) |
S2iii—Gd1—Gd1v | 131.08 (3) | Sn1—S2—Gd1xiii | 99.05 (5) |
S2iv—Gd1—Gd1v | 48.92 (3) | Gd1ii—S2—Gd1xiii | 82.15 (5) |
S1—Gd1—Gd1v | 90.0 | Sn1—S2—Gd1 | 108.37 (6) |
S2—Gd1—Gd1v | 49.96 (2) | Gd1ii—S2—Gd1 | 92.41 (3) |
S2i—Gd1—Gd1v | 130.04 (3) | Gd1xiii—S2—Gd1 | 152.56 (7) |
S3—Gd1—Gd1i | 134.130 (11) | Sn1—S2—Gd1v | 108.37 (6) |
S3i—Gd1—Gd1i | 45.870 (11) | Gd1ii—S2—Gd1v | 152.56 (7) |
S1ii—Gd1—Gd1i | 90.0 | Gd1xiii—S2—Gd1v | 92.41 (3) |
S2iii—Gd1—Gd1i | 48.92 (3) | Gd1—S2—Gd1v | 80.08 (5) |
S2iv—Gd1—Gd1i | 131.08 (3) | Gd1—S3—Gd1ix | 180.000 (12) |
S1—Gd1—Gd1i | 90.0 | Gd1—S3—Gd1v | 88.26 (2) |
S2—Gd1—Gd1i | 130.04 (2) | Gd1ix—S3—Gd1v | 91.74 (2) |
S2i—Gd1—Gd1i | 49.96 (2) | Gd1—S3—Gd1vi | 91.74 (2) |
Gd1v—Gd1—Gd1i | 180.000 (17) | Gd1ix—S3—Gd1vi | 88.26 (2) |
S3—Gd1—Gd1vi | 44.130 (11) | Gd1v—S3—Gd1vi | 180.000 (12) |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, z; (iii) x+1/2, −y+1/2, z+1; (iv) x+1/2, −y+1/2, z; (v) x, y, z−1; (vi) −x+1, −y, −z+1; (vii) x−1, y, z−1; (viii) x−1, y, z; (ix) −x+1, −y, −z; (x) −x, −y, −z; (xi) x+1, y, z+1; (xii) x+1, y, z; (xiii) x−1/2, −y+1/2, z−1. |
S5SnTb2 | F(000) = 520 |
Mr = 596.83 | Dx = 6.002 Mg m−3 |
Orthorhombic, Pbam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2 2ab | Cell parameters from 436 reflections |
a = 7.717 (2) Å | θ = 3.6–28.3° |
b = 11.2460 (15) Å | µ = 26.38 mm−1 |
c = 3.8056 (8) Å | T = 293 K |
V = 330.27 (13) Å3 | Prism, black |
Z = 2 | 0.11 × 0.06 × 0.03 mm |
KUMA KM-4 with area CCD detector diffractometer | 467 independent reflections |
Radiation source: fine-focus sealed tube | 436 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 28.3°, θmin = 3.6° |
ω–scan | h = −10→9 |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | k = −14→14 |
Tmin = 0.155, Tmax = 0.422 | l = −5→5 |
4139 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.016 | w = 1/[σ2(Fo2) + (0.0124P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.028 | (Δ/σ)max < 0.001 |
S = 1.04 | Δρmax = 0.95 e Å−3 |
467 reflections | Δρmin = −1.06 e Å−3 |
28 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0076 (3) |
S5SnTb2 | V = 330.27 (13) Å3 |
Mr = 596.83 | Z = 2 |
Orthorhombic, Pbam | Mo Kα radiation |
a = 7.717 (2) Å | µ = 26.38 mm−1 |
b = 11.2460 (15) Å | T = 293 K |
c = 3.8056 (8) Å | 0.11 × 0.06 × 0.03 mm |
KUMA KM-4 with area CCD detector diffractometer | 467 independent reflections |
Absorption correction: numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | 436 reflections with I > 2σ(I) |
Tmin = 0.155, Tmax = 0.422 | Rint = 0.042 |
4139 measured reflections |
R[F2 > 2σ(F2)] = 0.016 | 28 parameters |
wR(F2) = 0.028 | 0 restraints |
S = 1.04 | Δρmax = 0.95 e Å−3 |
467 reflections | Δρmin = −1.06 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
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. |
x | y | z | Uiso*/Ueq | ||
Tb1 | 0.46598 (3) | 0.17285 (2) | 0.5000 | 0.00959 (9) | |
Sn2 | 0.0000 | 0.0000 | 0.0000 | 0.00902 (12) | |
S1 | 0.82826 (17) | 0.09314 (10) | 0.5000 | 0.0098 (2) | |
S2 | 0.17306 (17) | 0.19510 (9) | 0.0000 | 0.0095 (2) | |
S3 | 0.5000 | 0.0000 | 0.0000 | 0.0100 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tb1 | 0.01379 (15) | 0.00798 (13) | 0.00699 (13) | 0.00089 (9) | 0.000 | 0.000 |
Sn2 | 0.0134 (3) | 0.0072 (2) | 0.0065 (2) | −0.00044 (17) | 0.000 | 0.000 |
S1 | 0.0104 (6) | 0.0105 (5) | 0.0084 (6) | 0.0019 (5) | 0.000 | 0.000 |
S2 | 0.0108 (6) | 0.0084 (5) | 0.0094 (6) | −0.0007 (4) | 0.000 | 0.000 |
S3 | 0.0138 (10) | 0.0080 (7) | 0.0081 (8) | 0.0001 (6) | 0.000 | 0.000 |
Tb1—S3 | 2.7328 (4) | Sn2—S1vi | 2.5445 (9) |
Tb1—S3i | 2.7328 (4) | Sn2—S1ix | 2.5445 (9) |
Tb1—S1ii | 2.8381 (12) | Sn2—S2x | 2.5686 (12) |
Tb1—S2iii | 2.8948 (10) | Sn2—S2 | 2.5686 (12) |
Tb1—S2iv | 2.8948 (10) | S1—Sn2xi | 2.5445 (9) |
Tb1—S1 | 2.9359 (15) | S1—Sn2xii | 2.5445 (9) |
Tb1—S2 | 2.9653 (12) | S1—Tb1iv | 2.8381 (12) |
Tb1—S2i | 2.9653 (12) | S2—Tb1ii | 2.8948 (10) |
Tb1—Tb1v | 3.8056 (8) | S2—Tb1xiii | 2.8948 (10) |
Tb1—Tb1i | 3.8056 (8) | S2—Tb1v | 2.9653 (12) |
Tb1—Tb1vi | 3.9231 (7) | S3—Tb1ix | 2.7328 (4) |
Sn2—S1vii | 2.5445 (9) | S3—Tb1vi | 2.7328 (4) |
Sn2—S1viii | 2.5445 (9) | S3—Tb1v | 2.7328 (4) |
S3—Tb1—S3i | 88.258 (16) | S3i—Tb1—Tb1vi | 44.129 (8) |
S3—Tb1—S1ii | 134.069 (10) | S1ii—Tb1—Tb1vi | 165.70 (3) |
S3i—Tb1—S1ii | 134.069 (10) | S2iii—Tb1—Tb1vi | 115.75 (2) |
S3—Tb1—S2iii | 140.31 (3) | S2iv—Tb1—Tb1vi | 115.75 (2) |
S3i—Tb1—S2iii | 81.62 (2) | S1—Tb1—Tb1vi | 64.53 (2) |
S1ii—Tb1—S2iii | 74.40 (3) | S2—Tb1—Tb1vi | 100.70 (2) |
S3—Tb1—S2iv | 81.62 (2) | S2i—Tb1—Tb1vi | 100.70 (2) |
S3i—Tb1—S2iv | 140.31 (3) | Tb1v—Tb1—Tb1vi | 90.0 |
S1ii—Tb1—S2iv | 74.40 (3) | Tb1i—Tb1—Tb1vi | 90.0 |
S2iii—Tb1—S2iv | 82.19 (4) | S1vii—Sn2—S1viii | 96.80 (4) |
S3—Tb1—S1 | 72.021 (17) | S1vii—Sn2—S1vi | 180.00 (5) |
S3i—Tb1—S1 | 72.021 (17) | S1viii—Sn2—S1vi | 83.20 (4) |
S1ii—Tb1—S1 | 129.77 (4) | S1vii—Sn2—S1ix | 83.20 (4) |
S2iii—Tb1—S1 | 68.34 (3) | S1viii—Sn2—S1ix | 180.0 |
S2iv—Tb1—S1 | 68.34 (3) | S1vi—Sn2—S1ix | 96.80 (4) |
S3—Tb1—S2 | 71.73 (2) | S1vii—Sn2—S2x | 94.64 (4) |
S3i—Tb1—S2 | 125.45 (2) | S1viii—Sn2—S2x | 94.64 (4) |
S1ii—Tb1—S2 | 68.67 (3) | S1vi—Sn2—S2x | 85.36 (4) |
S2iii—Tb1—S2 | 143.07 (2) | S1ix—Sn2—S2x | 85.36 (4) |
S2iv—Tb1—S2 | 87.46 (2) | S1vii—Sn2—S2 | 85.36 (4) |
S1—Tb1—S2 | 138.73 (2) | S1viii—Sn2—S2 | 85.36 (4) |
S3—Tb1—S2i | 125.45 (2) | S1vi—Sn2—S2 | 94.64 (4) |
S3i—Tb1—S2i | 71.73 (2) | S1ix—Sn2—S2 | 94.64 (4) |
S1ii—Tb1—S2i | 68.67 (3) | S2x—Sn2—S2 | 180.00 (2) |
S2iii—Tb1—S2i | 87.46 (2) | Sn2xi—S1—Sn2xii | 96.80 (4) |
S2iv—Tb1—S2i | 143.07 (2) | Sn2xi—S1—Tb1iv | 100.76 (4) |
S1—Tb1—S2i | 138.73 (2) | Sn2xii—S1—Tb1iv | 100.76 (4) |
S2—Tb1—S2i | 79.84 (4) | Sn2xi—S1—Tb1 | 128.44 (3) |
S3—Tb1—Tb1v | 45.871 (8) | Sn2xii—S1—Tb1 | 128.44 (3) |
S3i—Tb1—Tb1v | 134.129 (8) | Tb1iv—S1—Tb1 | 94.21 (4) |
S1ii—Tb1—Tb1v | 90.0 | Sn2—S2—Tb1ii | 98.70 (4) |
S2iii—Tb1—Tb1v | 131.096 (18) | Sn2—S2—Tb1xiii | 98.70 (4) |
S2iv—Tb1—Tb1v | 48.904 (18) | Tb1ii—S2—Tb1xiii | 82.19 (4) |
S1—Tb1—Tb1v | 90.0 | Sn2—S2—Tb1 | 108.92 (3) |
S2—Tb1—Tb1v | 50.08 (2) | Tb1ii—S2—Tb1 | 92.42 (2) |
S2i—Tb1—Tb1v | 129.92 (2) | Tb1xiii—S2—Tb1 | 152.36 (4) |
S3—Tb1—Tb1i | 134.129 (8) | Sn2—S2—Tb1v | 108.92 (3) |
S3i—Tb1—Tb1i | 45.871 (8) | Tb1ii—S2—Tb1v | 152.36 (4) |
S1ii—Tb1—Tb1i | 90.0 | Tb1xiii—S2—Tb1v | 92.42 (2) |
S2iii—Tb1—Tb1i | 48.904 (18) | Tb1—S2—Tb1v | 79.84 (4) |
S2iv—Tb1—Tb1i | 131.096 (18) | Tb1ix—S3—Tb1 | 180.000 (11) |
S1—Tb1—Tb1i | 90.0 | Tb1ix—S3—Tb1vi | 88.258 (16) |
S2—Tb1—Tb1i | 129.92 (2) | Tb1—S3—Tb1vi | 91.742 (16) |
S2i—Tb1—Tb1i | 50.08 (2) | Tb1ix—S3—Tb1v | 91.742 (16) |
Tb1v—Tb1—Tb1i | 180.000 (17) | Tb1—S3—Tb1v | 88.258 (16) |
S3—Tb1—Tb1vi | 44.129 (8) | Tb1vi—S3—Tb1v | 180.000 (12) |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, z; (iii) x+1/2, −y+1/2, z+1; (iv) x+1/2, −y+1/2, z; (v) x, y, z−1; (vi) −x+1, −y, −z+1; (vii) x−1, y, z−1; (viii) x−1, y, z; (ix) −x+1, −y, −z; (x) −x, −y, −z; (xi) x+1, y, z+1; (xii) x+1, y, z; (xiii) x−1/2, −y+1/2, z−1. |
Experimental details
(pr) | (nd) | (gd) | (tb) | |
Crystal data | ||||
Chemical formula | Pr2S5Sn | Nd2S5Sn | Gd2S5Sn | S5SnTb2 |
Mr | 560.81 | 567.47 | 593.49 | 596.83 |
Crystal system, space group | Orthorhombic, Pbam | Orthorhombic, Pbam | Orthorhombic, Pbam | Orthorhombic, Pbam |
Temperature (K) | 293 | 293 | 293 | 293 |
a, b, c (Å) | 7.8195 (9), 11.2145 (14), 3.9462 (5) | 7.7721 (14), 11.218 (2), 3.9272 (9) | 7.7330 (17), 11.290 (2), 3.8217 (9) | 7.717 (2), 11.2460 (15), 3.8056 (8) |
V (Å3) | 346.05 (7) | 342.41 (12) | 333.66 (13) | 330.27 (13) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 18.82 | 19.96 | 24.80 | 26.38 |
Crystal size (mm) | 0.09 × 0.08 × 0.06 | 0.22 × 0.21 × 0.19 | 0.10 × 0.03 × 0.02 | 0.11 × 0.06 × 0.03 |
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 M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | Numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | Numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 | Numerical M. Mayer, CrysAlis Data Reduction Program, Oxford Diffraction Ltd, 2007 |
Tmin, Tmax | 0.239, 0.458 | 0.123, 0.258 | 0.242, 0.546 | 0.155, 0.422 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4036, 452, 424 | 3642, 402, 392 | 3712, 401, 348 | 4139, 467, 436 |
Rint | 0.041 | 0.094 | 0.062 | 0.042 |
(sin θ/λ)max (Å−1) | 0.649 | 0.631 | 0.632 | 0.666 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.013, 0.025, 1.12 | 0.026, 0.067, 1.09 | 0.018, 0.027, 0.87 | 0.016, 0.028, 1.04 |
No. of reflections | 452 | 402 | 401 | 467 |
No. of parameters | 28 | 27 | 28 | 28 |
Δρmax, Δρmin (e Å−3) | 0.64, −0.70 | 1.33, −1.83 | 0.77, −0.96 | 0.95, −1.06 |
Computer programs: CrysAlis 1.171.32.6, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).
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