Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101003389/jz1447sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101003389/jz1447Isup2.hkl |
For related literature, see: Gautier et al. (1998); Gougeon (1984); Gougeon et al. (1987, 1988, 1989a, 1989b, 1990); Gougeon, Padiou, Le Marouille, Potel & Sergent (1984); Picard et al. (1999, 2000); Potel (1981); Thomas et al. (1997).
Single crystals of Rb5Mo27Se31 grew during an attempt to obtain Rb4Mo21Se25, using a mixture of Rb2Mo6Se6, MoSe2 and Mo in the proportion 2:6.5:2.5. The ternary compound Rb2Mo6Se6 was synthesized from an ion exchange reaction of In2Mo6Se6 with RbCl at 1073 K, as previously described by? (ref?). All materials were handled in an argon-filled glove box. The initial mixture (ca 5 g) was cold-pressed and loaded into a molybdenum crucible, which was sealed under a low argon pressure using an arc welding system. The charge was heated at the rate of 300 K h-1 up to 1973 K, at which temperature it was held for 6 h, then cooled at 100 K h-1 down to 1373 K and finally furnace cooled.
Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT; data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.
Rb5Mo27Se31 | Dx = 6.164 Mg m−3 |
Mr = 5465.49 | Mo Kα radiation, λ = 0.71069 Å |
Hexagonal, P63/m | Cell parameters from 104176 reflections |
Hall symbol: -P 6c | θ = 1–40.3° |
a = 9.5208 (1) Å | µ = 28.79 mm−1 |
c = 37.5113 (5) Å | T = 293 K |
V = 2944.69 (6) Å3 | Irregular, black |
Z = 2 | 0.07 × 0.05 × 0.04 mm |
F(000) = 4746 |
Nonius KappaCCD diffractometer | 6242 independent reflections |
Radiation source: fine-focus sealed tube | 3113 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.086 |
ϕ scans (κ = 0) + additional ω scans | θmax = 40.2°, θmin = 1.1° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −17→15 |
Tmin = 0.090, Tmax = 0.162 | k = −17→17 |
58800 measured reflections | l = −64→68 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.047 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.120 | w = 1/[σ2(Fo2) + (0.0416P)2 + 3.5266P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
6242 reflections | Δρmax = 3.12 e Å−3 |
100 parameters | Δρmin = −2.54 e Å−3 |
Rb5Mo27Se31 | Z = 2 |
Mr = 5465.49 | Mo Kα radiation |
Hexagonal, P63/m | µ = 28.79 mm−1 |
a = 9.5208 (1) Å | T = 293 K |
c = 37.5113 (5) Å | 0.07 × 0.05 × 0.04 mm |
V = 2944.69 (6) Å3 |
Nonius KappaCCD diffractometer | 6242 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | 3113 reflections with I > 2σ(I) |
Tmin = 0.090, Tmax = 0.162 | Rint = 0.086 |
58800 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 100 parameters |
wR(F2) = 0.120 | 0 restraints |
S = 1.05 | Δρmax = 3.12 e Å−3 |
6242 reflections | Δρmin = −2.54 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 | ||
Mo1 | 0.68788 (6) | 0.18345 (6) | 0.129568 (13) | 0.01198 (10) | |
Mo2 | 0.83648 (6) | 0.35023 (6) | 0.190441 (12) | 0.01106 (9) | |
Mo3 | 0.68517 (8) | 0.18169 (8) | 1/4 | 0.01097 (12) | |
Mo4 | 0.17057 (6) | 0.02231 (6) | 0.090982 (13) | 0.01163 (9) | |
Mo5 | 0.15373 (6) | 0.17004 (6) | 0.029262 (12) | 0.01094 (9) | |
Se1 | 0.37474 (7) | −0.00033 (7) | 0.134332 (15) | 0.01397 (12) | |
Se2 | 0.70155 (8) | 0.03716 (7) | 0.189686 (15) | 0.01495 (12) | |
Se3 | 0.36906 (10) | −0.00258 (10) | 1/4 | 0.01501 (16) | |
Se4 | 0.29239 (7) | 0.33446 (7) | 0.085536 (15) | 0.01370 (11) | |
Se5 | −0.03282 (7) | 0.29696 (7) | 0.031140 (15) | 0.01417 (12) | |
Se6 | 2/3 | 1/3 | 0.07612 (3) | 0.01492 (19) | |
Se7 | 0 | 0 | 0.14460 (3) | 0.01451 (19) | |
Rb1 | 0 | 0 | 1/4 | 0.0419 (5) | |
Rb2 | 1/3 | −1/3 | 0.02324 (4) | 0.0353 (3) | |
Rb3 | 1/3 | −1/3 | 0.18715 (4) | 0.0369 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0132 (2) | 0.0125 (2) | 0.0102 (2) | 0.00636 (19) | −0.00065 (17) | −0.00056 (17) |
Mo2 | 0.0116 (2) | 0.0126 (2) | 0.0093 (2) | 0.00629 (18) | 0.00037 (17) | −0.00004 (17) |
Mo3 | 0.0121 (3) | 0.0122 (3) | 0.0089 (3) | 0.0064 (3) | 0 | 0 |
Mo4 | 0.0127 (2) | 0.0125 (2) | 0.0100 (2) | 0.00651 (18) | −0.00031 (17) | 0.00008 (17) |
Mo5 | 0.0120 (2) | 0.0124 (2) | 0.0090 (2) | 0.00646 (18) | −0.00036 (16) | −0.00009 (16) |
Se1 | 0.0147 (3) | 0.0145 (3) | 0.0121 (3) | 0.0068 (2) | −0.0020 (2) | −0.0008 (2) |
Se2 | 0.0189 (3) | 0.0150 (3) | 0.0130 (3) | 0.0100 (2) | −0.0003 (2) | −0.0007 (2) |
Se3 | 0.0150 (4) | 0.0144 (4) | 0.0126 (4) | 0.0050 (3) | 0 | 0 |
Se4 | 0.0138 (3) | 0.0139 (3) | 0.0124 (3) | 0.0062 (2) | −0.0022 (2) | −0.0013 (2) |
Se5 | 0.0173 (3) | 0.0135 (3) | 0.0133 (3) | 0.0089 (2) | 0.0001 (2) | 0.0000 (2) |
Se6 | 0.0169 (3) | 0.0169 (3) | 0.0109 (5) | 0.00846 (14) | 0 | 0 |
Se7 | 0.0169 (3) | 0.0169 (3) | 0.0098 (4) | 0.00844 (14) | 0 | 0 |
Rb1 | 0.0267 (5) | 0.0267 (5) | 0.0723 (16) | 0.0133 (3) | 0 | 0 |
Rb2 | 0.0262 (4) | 0.0262 (4) | 0.0535 (9) | 0.01312 (19) | 0 | 0 |
Rb3 | 0.0268 (4) | 0.0268 (4) | 0.0570 (9) | 0.01339 (19) | 0 | 0 |
Mo1—Se6 | 2.5269 (9) | Se3—Mo3ii | 2.6340 (10) |
Mo1—Se1 | 2.6010 (7) | Se3—Mo2vii | 2.6854 (6) |
Mo1—Se1i | 2.6044 (7) | Se3—Mo2ii | 2.6854 (6) |
Mo1—Se4i | 2.6319 (7) | Se3—Rb1 | 3.5261 (8) |
Mo1—Mo1i | 2.6638 (8) | Se3—Rb3 | 3.8103 (11) |
Mo1—Mo1ii | 2.6638 (8) | Se3—Rb3vi | 3.8103 (11) |
Mo1—Se2 | 2.6876 (7) | Se4—Mo4ix | 2.6173 (8) |
Mo1—Mo2 | 2.7369 (7) | Se4—Mo1ii | 2.6319 (7) |
Mo1—Mo2ii | 2.7720 (7) | Se4—Rb2xiii | 3.7926 (10) |
Mo1—Mo4i | 3.2780 (7) | Se5—Mo5ix | 2.5905 (8) |
Mo1—Mo2i | 3.8344 (7) | Se5—Mo4ix | 2.6824 (7) |
Mo1—Se7iii | 4.1700 (5) | Se5—Mo5xi | 2.6893 (7) |
Mo1—Se5iii | 4.3586 (8) | Se5—Rb2xiii | 3.5156 (6) |
Mo1—Mo3 | 4.5176 (5) | Se5—Rb2xiv | 3.6685 (10) |
Mo1—Mo4iv | 4.5987 (7) | Se5—Mo1xv | 4.3586 (7) |
Mo2—Se1i | 2.5594 (7) | Se6—Mo1i | 2.5269 (9) |
Mo2—Se2 | 2.5896 (8) | Se6—Mo1ii | 2.5269 (9) |
Mo2—Se2i | 2.6069 (8) | Se6—Rb2xvi | 3.7270 (18) |
Mo2—Mo2ii | 2.6719 (8) | Se7—Mo4viii | 2.5262 (9) |
Mo2—Mo2i | 2.6719 (8) | Se7—Mo4ix | 2.5262 (9) |
Mo2—Se3i | 2.6854 (6) | Se7—Rb1 | 3.9539 (10) |
Mo2—Mo3 | 2.7074 (6) | Se7—Mo1x | 4.1701 (5) |
Mo2—Mo3i | 2.7207 (6) | Se7—Mo1ii | 4.1701 (5) |
Mo2—Mo1i | 2.7720 (7) | Se7—Mo1xv | 4.1701 (5) |
Mo2—Mo1ii | 3.8344 (7) | Rb1—Se3viii | 3.5261 (9) |
Mo2—Rb3v | 4.1494 (5) | Rb1—Se3ix | 3.5261 (8) |
Mo3—Se3 | 2.6183 (11) | Rb1—Se2vii | 3.7847 (6) |
Mo3—Se3i | 2.6340 (10) | Rb1—Se2x | 3.7847 (6) |
Mo3—Mo3i | 2.6663 (12) | Rb1—Se2xvii | 3.7847 (6) |
Mo3—Mo3ii | 2.6663 (12) | Rb1—Se2xviii | 3.7847 (6) |
Mo3—Se2vi | 2.6928 (7) | Rb1—Se2xv | 3.7847 (6) |
Mo3—Se2 | 2.6928 (7) | Rb1—Se2ii | 3.7847 (6) |
Mo3—Mo2vi | 2.7074 (6) | Rb1—Se7vi | 3.9539 (10) |
Mo3—Mo2vii | 2.7207 (6) | Rb1—Mo3ii | 4.1428 (7) |
Mo3—Mo2ii | 2.7207 (6) | Rb1—Mo3x | 4.1428 (7) |
Mo3—Rb1iii | 4.1428 (7) | Rb1—Mo3xv | 4.1428 (7) |
Mo3—Mo1vi | 4.5176 (5) | Rb1—Rb3vi | 5.9810 (6) |
Mo4—Se7 | 2.5262 (9) | Rb2—Se5viii | 3.5156 (6) |
Mo4—Se4 | 2.6024 (7) | Rb2—Se5xix | 3.5156 (6) |
Mo4—Se4viii | 2.6173 (8) | Rb2—Se5i | 3.5156 (6) |
Mo4—Se1 | 2.6246 (7) | Rb2—Se5xiv | 3.6685 (10) |
Mo4—Mo4viii | 2.6480 (8) | Rb2—Se5xx | 3.6685 (10) |
Mo4—Mo4ix | 2.6480 (8) | Rb2—Se5xxi | 3.6685 (10) |
Mo4—Se5viii | 2.6824 (7) | Rb2—Se6xvi | 3.7270 (18) |
Mo4—Mo5 | 2.7549 (6) | Rb2—Se4i | 3.7926 (10) |
Mo4—Mo5viii | 2.8044 (7) | Rb2—Se4viii | 3.7926 (10) |
Mo4—Mo1ii | 3.2780 (7) | Rb2—Se4xix | 3.7926 (10) |
Mo4—Mo1x | 4.5987 (7) | Rb2—Mo5viii | 4.1529 (5) |
Mo5—Se4 | 2.5657 (7) | Rb2—Mo5i | 4.1529 (5) |
Mo5—Se5viii | 2.5905 (8) | Rb2—Mo5xix | 4.1529 (5) |
Mo5—Se5 | 2.6011 (7) | Rb2—Rb2xxii | 5.7667 (9) |
Mo5—Mo5viii | 2.6797 (8) | Rb2—Rb2xvi | 5.7667 (9) |
Mo5—Mo5ix | 2.6797 (8) | Rb3—Se2x | 3.5179 (6) |
Mo5—Mo5xi | 2.6857 (8) | Rb3—Se2iv | 3.5179 (6) |
Mo5—Mo5xii | 2.6857 (8) | Rb3—Se1x | 3.5893 (10) |
Mo5—Se5xii | 2.6893 (7) | Rb3—Se1iv | 3.5893 (10) |
Mo5—Mo4ix | 2.8044 (7) | Rb3—Se3x | 3.8103 (11) |
Mo5—Rb2xiii | 4.1529 (5) | Rb3—Se3iv | 3.8103 (11) |
Se1—Mo2ii | 2.5594 (7) | Rb3—Mo2xxiii | 4.1494 (5) |
Se1—Mo1ii | 2.6044 (7) | Rb3—Mo2ii | 4.1494 (5) |
Se1—Rb3 | 3.5893 (10) | Rb3—Mo2xxiv | 4.1494 (5) |
Se2—Mo2ii | 2.6069 (8) | Rb3—Rb3vi | 4.715 (3) |
Se2—Rb3 | 3.5179 (6) | Rb3—Mo1x | 4.8642 (8) |
Se2—Rb1iii | 3.7847 (6) | ||
Se6—Mo1—Se1 | 92.640 (19) | Mo3—Se3—Rb1 | 144.18 (3) |
Se6—Mo1—Se1i | 92.56 (2) | Mo3ii—Se3—Rb1 | 83.17 (3) |
Se1—Mo1—Se1i | 171.94 (3) | Mo2vii—Se3—Rb1 | 102.44 (2) |
Se6—Mo1—Se4i | 88.06 (2) | Mo2ii—Se3—Rb1 | 102.44 (2) |
Se1—Mo1—Se4i | 84.05 (2) | Mo3—Se3—Rb3 | 98.71 (2) |
Se1i—Mo1—Se4i | 102.28 (2) | Mo3ii—Se3—Rb3 | 138.39 (2) |
Se6—Mo1—Mo1i | 58.191 (14) | Mo2vii—Se3—Rb3 | 143.99 (3) |
Se1—Mo1—Mo1i | 119.13 (2) | Mo2ii—Se3—Rb3 | 77.26 (2) |
Se1i—Mo1—Mo1i | 59.16 (2) | Rb1—Se3—Rb3 | 109.163 (18) |
Se4i—Mo1—Mo1i | 137.657 (19) | Mo3—Se3—Rb3vi | 98.71 (2) |
Se6—Mo1—Mo1ii | 58.191 (14) | Mo3ii—Se3—Rb3vi | 138.39 (2) |
Se1—Mo1—Mo1ii | 59.28 (2) | Mo2vii—Se3—Rb3vi | 77.26 (2) |
Se1i—Mo1—Mo1ii | 119.00 (2) | Mo2ii—Se3—Rb3vi | 143.99 (3) |
Se4i—Mo1—Mo1ii | 125.55 (2) | Rb1—Se3—Rb3vi | 109.163 (18) |
Mo1i—Mo1—Mo1ii | 60.0 | Rb3—Se3—Rb3vi | 76.44 (4) |
Se6—Mo1—Se2 | 175.31 (3) | Mo5—Se4—Mo4 | 64.421 (19) |
Se1—Mo1—Se2 | 85.98 (2) | Mo5—Se4—Mo4ix | 65.51 (2) |
Se1i—Mo1—Se2 | 88.35 (2) | Mo4—Se4—Mo4ix | 60.97 (2) |
Se4i—Mo1—Se2 | 96.25 (2) | Mo5—Se4—Mo1ii | 129.92 (3) |
Mo1i—Mo1—Se2 | 118.740 (18) | Mo4—Se4—Mo1ii | 77.55 (2) |
Mo1ii—Mo1—Se2 | 117.440 (19) | Mo4ix—Se4—Mo1ii | 122.35 (3) |
Se6—Mo1—Mo2 | 119.90 (2) | Mo5—Se4—Rb2xiii | 78.98 (2) |
Se1—Mo1—Mo2 | 114.78 (2) | Mo4—Se4—Rb2xiii | 143.33 (3) |
Se1i—Mo1—Mo2 | 57.198 (18) | Mo4ix—Se4—Rb2xiii | 102.622 (19) |
Se4i—Mo1—Mo2 | 143.55 (3) | Mo1ii—Se4—Rb2xiii | 132.91 (2) |
Mo1i—Mo1—Mo2 | 61.746 (15) | Mo5ix—Se5—Mo5 | 62.15 (2) |
Mo1ii—Mo1—Mo2 | 90.457 (13) | Mo5ix—Se5—Mo4ix | 62.967 (19) |
Se2—Mo1—Mo2 | 57.021 (19) | Mo5—Se5—Mo4ix | 64.096 (19) |
Se6—Mo1—Mo2ii | 118.58 (2) | Mo5ix—Se5—Mo5xi | 61.12 (2) |
Se1—Mo1—Mo2ii | 56.786 (18) | Mo5—Se5—Mo5xi | 60.99 (2) |
Se1i—Mo1—Mo2ii | 115.21 (2) | Mo4ix—Se5—Mo5xi | 114.23 (2) |
Se4i—Mo1—Mo2ii | 131.26 (2) | Mo5ix—Se5—Rb2xiii | 145.81 (2) |
Mo1i—Mo1—Mo2ii | 89.701 (14) | Mo5—Se5—Rb2xiii | 84.103 (19) |
Mo1ii—Mo1—Mo2ii | 60.424 (16) | Mo4ix—Se5—Rb2xiii | 108.60 (3) |
Se2—Mo1—Mo2ii | 57.017 (19) | Mo5xi—Se5—Rb2xiii | 99.01 (3) |
Mo2—Mo1—Mo2ii | 58.02 (2) | Mo5ix—Se5—Rb2xiv | 97.20 (2) |
Se6—Mo1—Mo4i | 90.940 (19) | Mo5—Se5—Rb2xiv | 140.78 (3) |
Se1—Mo1—Mo4i | 134.58 (2) | Mo4ix—Se5—Rb2xiv | 138.75 (3) |
Se1i—Mo1—Mo4i | 51.456 (17) | Mo5xi—Se5—Rb2xiv | 79.95 (2) |
Se4i—Mo1—Mo4i | 50.824 (17) | Rb2xiii—Se5—Rb2xiv | 106.759 (17) |
Mo1i—Mo1—Mo4i | 100.92 (2) | Mo5ix—Se5—Mo1xv | 81.003 (18) |
Mo1ii—Mo1—Mo4i | 148.676 (15) | Mo5—Se5—Mo1xv | 112.42 (2) |
Se2—Mo1—Mo4i | 93.22 (2) | Mo4ix—Se5—Mo1xv | 48.652 (15) |
Mo2—Mo1—Mo4i | 102.141 (19) | Mo5xi—Se5—Mo1xv | 140.45 (2) |
Mo2ii—Mo1—Mo4i | 149.53 (2) | Rb2xiii—Se5—Mo1xv | 119.75 (3) |
Se6—Mo1—Mo2i | 89.06 (2) | Rb2xiv—Se5—Mo1xv | 94.96 (2) |
Se1—Mo1—Mo2i | 87.556 (19) | Mo1i—Se6—Mo1 | 63.62 (3) |
Se1i—Mo1—Mo2i | 86.375 (19) | Mo1i—Se6—Mo1ii | 63.62 (3) |
Se4i—Mo1—Mo2i | 170.99 (2) | Mo1—Se6—Mo1ii | 63.62 (3) |
Mo1i—Mo1—Mo2i | 45.541 (10) | Mo1i—Se6—Rb2xvi | 142.509 (18) |
Mo1ii—Mo1—Mo2i | 46.296 (10) | Mo1—Se6—Rb2xvi | 142.509 (17) |
Se2—Mo1—Mo2i | 86.402 (19) | Mo1ii—Se6—Rb2xvi | 142.509 (17) |
Mo2—Mo1—Mo2i | 44.172 (14) | Mo4—Se7—Mo4viii | 63.22 (3) |
Mo2ii—Mo1—Mo2i | 44.171 (14) | Mo4—Se7—Mo4ix | 63.22 (3) |
Mo4i—Mo1—Mo2i | 137.793 (18) | Mo4viii—Se7—Mo4ix | 63.22 (3) |
Se6—Mo1—Se7iii | 128.22 (2) | Mo4—Se7—Rb1 | 142.758 (17) |
Se1—Mo1—Se7iii | 121.743 (19) | Mo4viii—Se7—Rb1 | 142.758 (17) |
Se1i—Mo1—Se7iii | 58.704 (15) | Mo4ix—Se7—Rb1 | 142.758 (17) |
Se4i—Mo1—Se7iii | 61.768 (19) | Mo4—Se7—Mo1x | 82.848 (17) |
Mo1i—Mo1—Se7iii | 117.72 (2) | Mo4viii—Se7—Mo1x | 51.811 (13) |
Mo1ii—Mo1—Se7iii | 171.981 (16) | Mo4ix—Se7—Mo1x | 114.83 (3) |
Se2—Mo1—Se7iii | 55.96 (2) | Rb1—Se7—Mo1x | 97.769 (15) |
Mo2—Mo1—Se7iii | 81.969 (19) | Mo4—Se7—Mo1ii | 51.811 (13) |
Mo2ii—Mo1—Se7iii | 112.77 (2) | Mo4viii—Se7—Mo1ii | 114.83 (3) |
Mo4i—Mo1—Se7iii | 37.281 (16) | Mo4ix—Se7—Mo1ii | 82.848 (17) |
Mo2i—Mo1—Se7iii | 126.124 (18) | Rb1—Se7—Mo1ii | 97.769 (15) |
Se6—Mo1—Se5iii | 53.056 (16) | Mo1x—Se7—Mo1ii | 118.203 (7) |
Se1—Mo1—Se5iii | 125.24 (2) | Mo4—Se7—Mo1xv | 114.83 (3) |
Se1i—Mo1—Se5iii | 62.797 (17) | Mo4viii—Se7—Mo1xv | 82.848 (17) |
Se4i—Mo1—Se5iii | 57.391 (17) | Mo4ix—Se7—Mo1xv | 51.811 (13) |
Mo1i—Mo1—Se5iii | 80.906 (15) | Rb1—Se7—Mo1xv | 97.769 (15) |
Mo1ii—Mo1—Se5iii | 111.124 (11) | Mo1x—Se7—Mo1xv | 118.203 (7) |
Se2—Mo1—Se5iii | 131.12 (2) | Mo1ii—Se7—Mo1xv | 118.203 (7) |
Mo2—Mo1—Se5iii | 119.247 (19) | Se3viii—Rb1—Se3ix | 120.0 |
Mo2ii—Mo1—Se5iii | 169.94 (2) | Se3viii—Rb1—Se3 | 120.0 |
Mo4i—Mo1—Se5iii | 37.901 (12) | Se3ix—Rb1—Se3 | 120.0 |
Mo2i—Mo1—Se5iii | 126.397 (16) | Se3viii—Rb1—Se2vii | 142.941 (9) |
Se7iii—Mo1—Se5iii | 75.177 (17) | Se3ix—Rb1—Se2vii | 70.546 (14) |
Se6—Mo1—Mo3 | 142.52 (2) | Se3—Rb1—Se2vii | 62.292 (13) |
Se1—Mo1—Mo3 | 85.773 (18) | Se3viii—Rb1—Se2x | 62.292 (13) |
Se1i—Mo1—Mo3 | 86.353 (18) | Se3ix—Rb1—Se2x | 142.941 (9) |
Se4i—Mo1—Mo3 | 128.80 (2) | Se3—Rb1—Se2x | 70.546 (14) |
Mo1i—Mo1—Mo3 | 90.157 (10) | Se2vii—Rb1—Se2x | 132.741 (6) |
Mo1ii—Mo1—Mo3 | 89.870 (10) | Se3viii—Rb1—Se2xvii | 62.292 (13) |
Se2—Mo1—Mo3 | 32.933 (16) | Se3ix—Rb1—Se2xvii | 142.941 (9) |
Mo2—Mo1—Mo3 | 33.714 (14) | Se3—Rb1—Se2xvii | 70.546 (14) |
Mo2ii—Mo1—Mo3 | 34.299 (13) | Se2vii—Rb1—Se2xvii | 87.934 (13) |
Mo4i—Mo1—Mo3 | 116.405 (17) | Se2x—Rb1—Se2xvii | 73.425 (18) |
Mo2i—Mo1—Mo3 | 53.471 (12) | Se3viii—Rb1—Se2xviii | 70.546 (14) |
Se7iii—Mo1—Mo3 | 82.370 (18) | Se3ix—Rb1—Se2xviii | 62.292 (13) |
Se5iii—Mo1—Mo3 | 148.174 (16) | Se3—Rb1—Se2xviii | 142.941 (9) |
Se6—Mo1—Mo4iv | 108.44 (2) | Se2vii—Rb1—Se2xviii | 87.934 (13) |
Se1—Mo1—Mo4iv | 102.907 (18) | Se2x—Rb1—Se2xviii | 132.741 (6) |
Se1i—Mo1—Mo4iv | 81.243 (17) | Se2xvii—Rb1—Se2xviii | 87.934 (13) |
Se4i—Mo1—Mo4iv | 28.739 (15) | Se3viii—Rb1—Se2xv | 70.546 (14) |
Mo1i—Mo1—Mo4iv | 135.31 (2) | Se3ix—Rb1—Se2xv | 62.292 (13) |
Mo1ii—Mo1—Mo4iv | 154.176 (18) | Se3—Rb1—Se2xv | 142.941 (9) |
Se2—Mo1—Mo4iv | 76.244 (17) | Se2vii—Rb1—Se2xv | 132.741 (6) |
Mo2—Mo1—Mo4iv | 114.924 (18) | Se2x—Rb1—Se2xv | 87.934 (13) |
Mo2ii—Mo1—Mo4iv | 128.284 (19) | Se2xvii—Rb1—Se2xv | 132.741 (6) |
Mo4i—Mo1—Mo4iv | 34.383 (14) | Se2xviii—Rb1—Se2xv | 73.425 (18) |
Mo2i—Mo1—Mo4iv | 158.875 (16) | Se3viii—Rb1—Se2ii | 142.941 (9) |
Se7iii—Mo1—Mo4iv | 33.029 (13) | Se3ix—Rb1—Se2ii | 70.546 (14) |
Se5iii—Mo1—Mo4iv | 61.745 (12) | Se3—Rb1—Se2ii | 62.292 (13) |
Mo3—Mo1—Mo4iv | 108.387 (14) | Se2vii—Rb1—Se2ii | 73.425 (18) |
Se1i—Mo2—Se2 | 91.49 (2) | Se2x—Rb1—Se2ii | 87.934 (13) |
Se1i—Mo2—Se2i | 88.55 (2) | Se2xvii—Rb1—Se2ii | 132.741 (6) |
Se2—Mo2—Se2i | 177.74 (3) | Se2xviii—Rb1—Se2ii | 132.741 (6) |
Se1i—Mo2—Mo2ii | 120.433 (19) | Se2xv—Rb1—Se2ii | 87.934 (13) |
Se2—Mo2—Mo2ii | 59.38 (3) | Se3viii—Rb1—Se7vi | 90.0 |
Se2i—Mo2—Mo2ii | 118.74 (2) | Se3ix—Rb1—Se7vi | 90.0 |
Se1i—Mo2—Mo2i | 118.534 (19) | Se3—Rb1—Se7vi | 90.0 |
Se2—Mo2—Mo2i | 119.37 (3) | Se2vii—Rb1—Se7vi | 53.287 (9) |
Se2i—Mo2—Mo2i | 58.74 (2) | Se2x—Rb1—Se7vi | 126.713 (9) |
Mo2ii—Mo2—Mo2i | 60.0 | Se2xvii—Rb1—Se7vi | 53.287 (9) |
Se1i—Mo2—Se3i | 111.63 (2) | Se2xviii—Rb1—Se7vi | 53.287 (9) |
Se2—Mo2—Se3i | 91.77 (3) | Se2xv—Rb1—Se7vi | 126.713 (9) |
Se2i—Mo2—Se3i | 90.32 (3) | Se2ii—Rb1—Se7vi | 126.713 (9) |
Mo2ii—Mo2—Se3i | 119.22 (2) | Se3viii—Rb1—Se7 | 90.0 |
Mo2i—Mo2—Se3i | 118.19 (2) | Se3ix—Rb1—Se7 | 90.0 |
Se1i—Mo2—Mo3 | 148.49 (3) | Se3—Rb1—Se7 | 90.0 |
Se2—Mo2—Mo3 | 61.06 (2) | Se2vii—Rb1—Se7 | 126.713 (9) |
Se2i—Mo2—Mo3 | 119.51 (2) | Se2x—Rb1—Se7 | 53.287 (9) |
Mo2ii—Mo2—Mo3 | 60.762 (17) | Se2xvii—Rb1—Se7 | 126.713 (9) |
Mo2i—Mo2—Mo3 | 90.083 (17) | Se2xviii—Rb1—Se7 | 126.713 (9) |
Se3i—Mo2—Mo3 | 58.47 (2) | Se2xv—Rb1—Se7 | 53.287 (9) |
Se1i—Mo2—Mo3i | 145.58 (3) | Se2ii—Rb1—Se7 | 53.287 (9) |
Se2—Mo2—Mo3i | 119.88 (3) | Se7vi—Rb1—Se7 | 180.0 |
Se2i—Mo2—Mo3i | 60.68 (2) | Se3viii—Rb1—Mo3ii | 159.146 (16) |
Mo2ii—Mo2—Mo3i | 89.797 (17) | Se3ix—Rb1—Mo3ii | 80.854 (16) |
Mo2i—Mo2—Mo3i | 60.263 (16) | Se3—Rb1—Mo3ii | 39.146 (16) |
Se3i—Mo2—Mo3i | 57.93 (2) | Se2vii—Rb1—Mo3ii | 39.389 (9) |
Mo3—Mo2—Mo3i | 58.84 (3) | Se2x—Rb1—Mo3ii | 101.656 (11) |
Se1i—Mo2—Mo1 | 58.795 (18) | Se2xvii—Rb1—Mo3ii | 101.656 (11) |
Se2—Mo2—Mo1 | 60.531 (19) | Se2xviii—Rb1—Mo3ii | 124.807 (11) |
Se2i—Mo2—Mo1 | 117.69 (2) | Se2xv—Rb1—Mo3ii | 124.807 (11) |
Mo2ii—Mo2—Mo1 | 61.647 (16) | Se2ii—Rb1—Mo3ii | 39.389 (9) |
Mo2i—Mo2—Mo1 | 90.286 (14) | Se7vi—Rb1—Mo3ii | 90.0 |
Se3i—Mo2—Mo1 | 148.44 (3) | Se7—Rb1—Mo3ii | 90.0 |
Mo3—Mo2—Mo1 | 112.15 (2) | Se3viii—Rb1—Mo3x | 39.146 (16) |
Mo3i—Mo2—Mo1 | 147.48 (3) | Se3ix—Rb1—Mo3x | 159.146 (16) |
Se1i—Mo2—Mo1i | 58.237 (19) | Se3—Rb1—Mo3x | 80.854 (16) |
Se2—Mo2—Mo1i | 118.34 (2) | Se2vii—Rb1—Mo3x | 124.807 (11) |
Se2i—Mo2—Mo1i | 59.862 (19) | Se2x—Rb1—Mo3x | 39.389 (9) |
Mo2ii—Mo2—Mo1i | 89.535 (13) | Se2xvii—Rb1—Mo3x | 39.389 (9) |
Mo2i—Mo2—Mo1i | 60.330 (15) | Se2xviii—Rb1—Mo3x | 101.656 (11) |
Se3i—Mo2—Mo1i | 147.01 (3) | Se2xv—Rb1—Mo3x | 101.656 (11) |
Mo3—Mo2—Mo1i | 146.78 (2) | Se2ii—Rb1—Mo3x | 124.807 (11) |
Mo3i—Mo2—Mo1i | 110.66 (2) | Se7vi—Rb1—Mo3x | 90.0 |
Mo1—Mo2—Mo1i | 57.83 (2) | Se7—Rb1—Mo3x | 90.0 |
Se1i—Mo2—Mo1ii | 88.109 (19) | Mo3ii—Rb1—Mo3x | 120.0 |
Se2—Mo2—Mo1ii | 88.58 (2) | Se3viii—Rb1—Mo3xv | 80.854 (16) |
Se2i—Mo2—Mo1ii | 89.16 (2) | Se3ix—Rb1—Mo3xv | 39.146 (16) |
Mo2ii—Mo2—Mo1ii | 45.542 (10) | Se3—Rb1—Mo3xv | 159.146 (16) |
Mo2i—Mo2—Mo1ii | 46.294 (10) | Se2vii—Rb1—Mo3xv | 101.656 (11) |
Se3i—Mo2—Mo1ii | 160.24 (2) | Se2x—Rb1—Mo3xv | 124.807 (11) |
Mo3—Mo2—Mo1ii | 105.13 (2) | Se2xvii—Rb1—Mo3xv | 124.807 (11) |
Mo3i—Mo2—Mo1ii | 105.186 (19) | Se2xviii—Rb1—Mo3xv | 39.389 (9) |
Mo1—Mo2—Mo1ii | 44.002 (14) | Se2xv—Rb1—Mo3xv | 39.389 (9) |
Mo1i—Mo2—Mo1ii | 44.004 (14) | Se2ii—Rb1—Mo3xv | 101.656 (11) |
Se1i—Mo2—Rb3v | 59.17 (2) | Se7vi—Rb1—Mo3xv | 90.0 |
Se2—Mo2—Rb3v | 124.38 (2) | Se7—Rb1—Mo3xv | 90.0 |
Se2i—Mo2—Rb3v | 57.457 (16) | Mo3ii—Rb1—Mo3xv | 120.0 |
Mo2ii—Mo2—Rb3v | 175.84 (2) | Mo3x—Rb1—Mo3xv | 120.0 |
Mo2i—Mo2—Rb3v | 116.19 (2) | Se3viii—Rb1—Rb3vi | 90.317 (12) |
Se3i—Mo2—Rb3v | 63.60 (3) | Se3ix—Rb1—Rb3vi | 142.479 (12) |
Mo3—Mo2—Rb3v | 122.04 (3) | Se3—Rb1—Rb3vi | 36.997 (12) |
Mo3i—Mo2—Rb3v | 89.43 (3) | Se2vii—Rb1—Rb3vi | 71.938 (11) |
Mo1—Mo2—Rb3v | 117.87 (3) | Se2x—Rb1—Rb3vi | 68.780 (14) |
Mo1i—Mo2—Rb3v | 86.91 (2) | Se2xvii—Rb1—Rb3vi | 33.571 (12) |
Mo1ii—Mo2—Rb3v | 130.90 (2) | Se2xviii—Rb1—Rb3vi | 115.872 (15) |
Se3—Mo3—Se3i | 178.99 (3) | Se2xv—Rb1—Rb3vi | 155.177 (12) |
Se3—Mo3—Mo3i | 119.78 (3) | Se2ii—Rb1—Rb3vi | 99.277 (12) |
Se3i—Mo3—Mo3i | 59.20 (3) | Se7vi—Rb1—Rb3vi | 66.787 (13) |
Se3—Mo3—Mo3ii | 59.78 (3) | Se7—Rb1—Rb3vi | 113.213 (13) |
Se3i—Mo3—Mo3ii | 119.20 (3) | Mo3ii—Rb1—Rb3vi | 70.589 (8) |
Mo3i—Mo3—Mo3ii | 60.0 | Mo3x—Rb1—Rb3vi | 54.839 (9) |
Se3—Mo3—Se2vi | 89.91 (2) | Mo3xv—Rb1—Rb3vi | 155.261 (12) |
Se3i—Mo3—Se2vi | 90.64 (2) | Se5viii—Rb2—Se5xix | 119.297 (7) |
Mo3i—Mo3—Se2vi | 118.13 (2) | Se5viii—Rb2—Se5i | 119.297 (7) |
Mo3ii—Mo3—Se2vi | 117.89 (2) | Se5xix—Rb2—Se5i | 119.297 (7) |
Se3—Mo3—Se2 | 89.91 (2) | Se5viii—Rb2—Se5xiv | 63.808 (18) |
Se3i—Mo3—Se2 | 90.64 (2) | Se5xix—Rb2—Se5xiv | 73.241 (17) |
Mo3i—Mo3—Se2 | 118.13 (2) | Se5i—Rb2—Se5xiv | 150.50 (4) |
Mo3ii—Mo3—Se2 | 117.89 (2) | Se5viii—Rb2—Se5xx | 150.50 (4) |
Se2vi—Mo3—Se2 | 114.32 (3) | Se5xix—Rb2—Se5xx | 63.808 (18) |
Se3—Mo3—Mo2vi | 119.332 (18) | Se5i—Rb2—Se5xx | 73.241 (17) |
Se3i—Mo3—Mo2vi | 60.346 (17) | Se5xiv—Rb2—Se5xx | 92.08 (3) |
Mo3i—Mo3—Mo2vi | 60.831 (19) | Se5viii—Rb2—Se5xxi | 73.241 (17) |
Mo3ii—Mo3—Mo2vi | 90.203 (17) | Se5xix—Rb2—Se5xxi | 150.50 (4) |
Se2vi—Mo3—Mo2vi | 57.311 (17) | Se5i—Rb2—Se5xxi | 63.808 (18) |
Se2—Mo3—Mo2vi | 147.84 (3) | Se5xiv—Rb2—Se5xxi | 92.08 (3) |
Se3—Mo3—Mo2 | 119.332 (18) | Se5xx—Rb2—Se5xxi | 92.08 (3) |
Se3i—Mo3—Mo2 | 60.346 (17) | Se5viii—Rb2—Se6xvi | 94.84 (2) |
Mo3i—Mo3—Mo2 | 60.831 (19) | Se5xix—Rb2—Se6xvi | 94.84 (2) |
Mo3ii—Mo3—Mo2 | 90.203 (17) | Se5i—Rb2—Se6xvi | 94.84 (2) |
Se2vi—Mo3—Mo2 | 147.84 (3) | Se5xiv—Rb2—Se6xvi | 56.22 (2) |
Se2—Mo3—Mo2 | 57.311 (17) | Se5xx—Rb2—Se6xvi | 56.22 (2) |
Mo2vi—Mo3—Mo2 | 111.22 (3) | Se5xxi—Rb2—Se6xvi | 56.22 (2) |
Se3—Mo3—Mo2vii | 60.357 (16) | Se5viii—Rb2—Se4i | 68.962 (17) |
Se3i—Mo3—Mo2vii | 119.306 (18) | Se5xix—Rb2—Se4i | 136.64 (4) |
Mo3i—Mo3—Mo2vii | 89.915 (17) | Se5i—Rb2—Se4i | 58.404 (16) |
Mo3ii—Mo3—Mo2vii | 60.330 (19) | Se5xiv—Rb2—Se4i | 132.707 (12) |
Se2vi—Mo3—Mo2vii | 57.571 (17) | Se5xx—Rb2—Se4i | 131.417 (12) |
Se2—Mo3—Mo2vii | 147.52 (3) | Se5xxi—Rb2—Se4i | 71.823 (13) |
Mo2vi—Mo3—Mo2vii | 58.98 (2) | Se6xvi—Rb2—Se4i | 128.037 (19) |
Mo2—Mo3—Mo2vii | 147.12 (3) | Se5viii—Rb2—Se4viii | 58.404 (16) |
Se3—Mo3—Mo2ii | 60.357 (16) | Se5xix—Rb2—Se4viii | 68.962 (17) |
Se3i—Mo3—Mo2ii | 119.306 (18) | Se5i—Rb2—Se4viii | 136.64 (4) |
Mo3i—Mo3—Mo2ii | 89.915 (17) | Se5xiv—Rb2—Se4viii | 71.823 (13) |
Mo3ii—Mo3—Mo2ii | 60.330 (19) | Se5xx—Rb2—Se4viii | 132.707 (12) |
Se2vi—Mo3—Mo2ii | 147.52 (3) | Se5xxi—Rb2—Se4viii | 131.417 (12) |
Se2—Mo3—Mo2ii | 57.571 (17) | Se6xvi—Rb2—Se4viii | 128.037 (19) |
Mo2vi—Mo3—Mo2ii | 147.12 (3) | Se4i—Rb2—Se4viii | 86.02 (3) |
Mo2—Mo3—Mo2ii | 58.98 (2) | Se5viii—Rb2—Se4xix | 136.64 (4) |
Mo2vii—Mo3—Mo2ii | 110.40 (3) | Se5xix—Rb2—Se4xix | 58.404 (16) |
Se3—Mo3—Rb1iii | 123.33 (3) | Se5i—Rb2—Se4xix | 68.962 (17) |
Se3i—Mo3—Rb1iii | 57.68 (2) | Se5xiv—Rb2—Se4xix | 131.417 (12) |
Mo3i—Mo3—Rb1iii | 116.89 (3) | Se5xx—Rb2—Se4xix | 71.823 (13) |
Mo3ii—Mo3—Rb1iii | 176.89 (3) | Se5xxi—Rb2—Se4xix | 132.707 (12) |
Se2vi—Mo3—Rb1iii | 63.113 (17) | Se6xvi—Rb2—Se4xix | 128.037 (19) |
Se2—Mo3—Rb1iii | 63.113 (17) | Se4i—Rb2—Se4xix | 86.02 (3) |
Mo2vi—Mo3—Rb1iii | 88.040 (18) | Se4viii—Rb2—Se4xix | 86.02 (3) |
Mo2—Mo3—Rb1iii | 88.039 (18) | Se5viii—Rb2—Mo5viii | 38.538 (11) |
Mo2vii—Mo3—Rb1iii | 120.644 (16) | Se5xix—Rb2—Mo5viii | 81.180 (12) |
Mo2ii—Mo3—Rb1iii | 120.644 (16) | Se5i—Rb2—Mo5viii | 157.185 (19) |
Se3—Mo3—Mo1vi | 90.287 (10) | Se5xiv—Rb2—Mo5viii | 39.615 (11) |
Se3i—Mo3—Mo1vi | 89.713 (10) | Se5xx—Rb2—Mo5viii | 128.31 (2) |
Mo3i—Mo3—Mo1vi | 89.839 (10) | Se5xxi—Rb2—Mo5viii | 103.955 (17) |
Mo3ii—Mo3—Mo1vi | 90.126 (10) | Se6xvi—Rb2—Mo5viii | 93.12 (2) |
Se2vi—Mo3—Mo1vi | 32.862 (14) | Se4i—Rb2—Mo5viii | 100.23 (2) |
Se2—Mo3—Mo1vi | 147.18 (2) | Se4viii—Rb2—Mo5viii | 37.331 (11) |
Mo2vi—Mo3—Mo1vi | 34.132 (12) | Se4xix—Rb2—Mo5viii | 121.13 (3) |
Mo2—Mo3—Mo1vi | 145.35 (2) | Se5viii—Rb2—Mo5i | 81.180 (12) |
Mo2vii—Mo3—Mo1vi | 35.039 (12) | Se5xix—Rb2—Mo5i | 157.185 (19) |
Mo2ii—Mo3—Mo1vi | 145.44 (2) | Se5i—Rb2—Mo5i | 38.538 (11) |
Rb1iii—Mo3—Mo1vi | 89.860 (10) | Se5xiv—Rb2—Mo5i | 128.31 (2) |
Se7—Mo4—Se4 | 93.40 (2) | Se5xx—Rb2—Mo5i | 103.955 (17) |
Se7—Mo4—Se4viii | 93.039 (19) | Se5xxi—Rb2—Mo5i | 39.615 (11) |
Se4—Mo4—Se4viii | 170.94 (3) | Se6xvi—Rb2—Mo5i | 93.12 (2) |
Se7—Mo4—Se1 | 88.35 (2) | Se4i—Rb2—Mo5i | 37.331 (11) |
Se4—Mo4—Se1 | 102.53 (2) | Se4viii—Rb2—Mo5i | 121.13 (3) |
Se4viii—Mo4—Se1 | 84.02 (2) | Se4xix—Rb2—Mo5i | 100.23 (2) |
Se7—Mo4—Mo4viii | 58.392 (14) | Mo5viii—Rb2—Mo5i | 119.707 (4) |
Se4—Mo4—Mo4viii | 119.59 (2) | Se5viii—Rb2—Mo5xix | 157.185 (19) |
Se4viii—Mo4—Mo4viii | 59.24 (2) | Se5xix—Rb2—Mo5xix | 38.537 (11) |
Se1—Mo4—Mo4viii | 125.61 (2) | Se5i—Rb2—Mo5xix | 81.180 (12) |
Se7—Mo4—Mo4ix | 58.392 (14) | Se5xiv—Rb2—Mo5xix | 103.955 (17) |
Se4—Mo4—Mo4ix | 59.79 (2) | Se5xx—Rb2—Mo5xix | 39.615 (11) |
Se4viii—Mo4—Mo4ix | 119.04 (2) | Se5xxi—Rb2—Mo5xix | 128.31 (2) |
Se1—Mo4—Mo4ix | 138.331 (19) | Se6xvi—Rb2—Mo5xix | 93.12 (2) |
Mo4viii—Mo4—Mo4ix | 60.0 | Se4i—Rb2—Mo5xix | 121.13 (3) |
Se7—Mo4—Se5viii | 175.47 (3) | Se4viii—Rb2—Mo5xix | 100.23 (2) |
Se4—Mo4—Se5viii | 88.33 (2) | Se4xix—Rb2—Mo5xix | 37.331 (11) |
Se4viii—Mo4—Se5viii | 84.80 (2) | Mo5viii—Rb2—Mo5xix | 119.707 (4) |
Se1—Mo4—Se5viii | 95.37 (2) | Mo5i—Rb2—Mo5xix | 119.707 (4) |
Mo4viii—Mo4—Se5viii | 117.150 (18) | Se5viii—Rb2—Rb2xxii | 91.005 (10) |
Mo4ix—Mo4—Se5viii | 119.342 (18) | Se5xix—Rb2—Rb2xxii | 37.526 (9) |
Se7—Mo4—Mo5 | 120.86 (2) | Se5i—Rb2—Rb2xxii | 148.43 (2) |
Se4—Mo4—Mo5 | 57.144 (18) | Se5xiv—Rb2—Rb2xxii | 35.715 (14) |
Se4viii—Mo4—Mo5 | 113.93 (2) | Se5xx—Rb2—Rb2xxii | 75.76 (2) |
Se1—Mo4—Mo5 | 142.86 (2) | Se5xxi—Rb2—Rb2xxii | 123.62 (4) |
Mo4viii—Mo4—Mo5 | 90.854 (13) | Se6xvi—Rb2—Rb2xxii | 72.40 (3) |
Mo4ix—Mo4—Mo5 | 62.501 (15) | Se4i—Rb2—Rb2xxii | 151.01 (3) |
Se5viii—Mo4—Mo5 | 56.887 (19) | Se4viii—Rb2—Rb2xxii | 65.336 (13) |
Se7—Mo4—Mo5viii | 118.98 (2) | Se4xix—Rb2—Rb2xxii | 95.821 (14) |
Se4—Mo4—Mo5viii | 114.76 (2) | Mo5viii—Rb2—Rb2xxii | 54.301 (7) |
Se4viii—Mo4—Mo5viii | 56.360 (18) | Mo5i—Rb2—Rb2xxii | 163.00 (4) |
Se1—Mo4—Mo5viii | 130.58 (2) | Mo5xix—Rb2—Rb2xxii | 71.128 (7) |
Mo4viii—Mo4—Mo5viii | 60.617 (15) | Se5viii—Rb2—Rb2xvi | 37.526 (9) |
Mo4ix—Mo4—Mo5viii | 89.777 (13) | Se5xix—Rb2—Rb2xvi | 148.43 (2) |
Se5viii—Mo4—Mo5viii | 56.545 (18) | Se5i—Rb2—Rb2xvi | 91.005 (10) |
Mo5—Mo4—Mo5viii | 57.63 (2) | Se5xiv—Rb2—Rb2xvi | 75.76 (2) |
Se7—Mo4—Mo1ii | 90.908 (19) | Se5xx—Rb2—Rb2xvi | 123.62 (4) |
Se4—Mo4—Mo1ii | 51.630 (17) | Se5xxi—Rb2—Rb2xvi | 35.715 (14) |
Se4viii—Mo4—Mo1ii | 134.61 (2) | Se6xvi—Rb2—Rb2xvi | 72.40 (3) |
Se1—Mo4—Mo1ii | 50.904 (16) | Se4i—Rb2—Rb2xvi | 65.336 (13) |
Mo4viii—Mo4—Mo1ii | 148.877 (15) | Se4viii—Rb2—Rb2xvi | 95.821 (14) |
Mo4ix—Mo4—Mo1ii | 101.26 (2) | Se4xix—Rb2—Rb2xvi | 151.01 (3) |
Se5viii—Mo4—Mo1ii | 93.45 (2) | Mo5viii—Rb2—Rb2xvi | 71.128 (7) |
Mo5—Mo4—Mo1ii | 102.283 (19) | Mo5i—Rb2—Rb2xvi | 54.301 (7) |
Mo5viii—Mo4—Mo1ii | 149.26 (2) | Mo5xix—Rb2—Rb2xvi | 163.00 (4) |
Se7—Mo4—Mo1x | 64.123 (11) | Rb2xxii—Rb2—Rb2xvi | 111.28 (3) |
Se4—Mo4—Mo1x | 156.69 (2) | Se2x—Rb3—Se2 | 119.928 (3) |
Se4viii—Mo4—Mo1x | 28.916 (14) | Se2x—Rb3—Se2iv | 119.928 (2) |
Se1—Mo4—Mo1x | 83.847 (17) | Se2—Rb3—Se2iv | 119.928 (3) |
Mo4viii—Mo4—Mo1x | 44.353 (16) | Se2x—Rb3—Se1x | 60.983 (15) |
Mo4ix—Mo4—Mo1x | 100.549 (16) | Se2—Rb3—Se1x | 147.40 (4) |
Se5viii—Mo4—Mo1x | 113.637 (19) | Se2iv—Rb3—Se1x | 71.779 (16) |
Mo5—Mo4—Mo1x | 127.832 (18) | Se2x—Rb3—Se1 | 71.779 (16) |
Mo5viii—Mo4—Mo1x | 74.632 (14) | Se2—Rb3—Se1 | 60.983 (15) |
Mo1ii—Mo4—Mo1x | 129.857 (18) | Se2iv—Rb3—Se1 | 147.40 (4) |
Se7—Mo4—Mo1 | 108.28 (2) | Se1x—Rb3—Se1 | 92.46 (3) |
Se4—Mo4—Mo1 | 81.506 (17) | Se2x—Rb3—Se1iv | 147.40 (4) |
Se4viii—Mo4—Mo1 | 102.478 (18) | Se2—Rb3—Se1iv | 71.779 (16) |
Se1—Mo4—Mo1 | 28.208 (15) | Se2iv—Rb3—Se1iv | 60.983 (15) |
Mo4viii—Mo4—Mo1 | 153.693 (18) | Se1x—Rb3—Se1iv | 92.46 (3) |
Mo4ix—Mo4—Mo1 | 135.93 (2) | Se1—Rb3—Se1iv | 92.46 (3) |
Se5viii—Mo4—Mo1 | 76.111 (17) | Se2x—Rb3—Se3 | 70.324 (19) |
Mo5—Mo4—Mo1 | 114.845 (18) | Se2—Rb3—Se3 | 61.457 (18) |
Mo5viii—Mo4—Mo1 | 127.782 (18) | Se2iv—Rb3—Se3 | 139.85 (4) |
Mo1ii—Mo4—Mo1 | 34.662 (14) | Se1x—Rb3—Se3 | 131.307 (15) |
Mo1x—Mo4—Mo1 | 110.314 (15) | Se1—Rb3—Se3 | 71.732 (12) |
Se4—Mo5—Se5viii | 91.15 (2) | Se1iv—Rb3—Se3 | 132.686 (15) |
Se4—Mo5—Se5 | 87.52 (2) | Se2x—Rb3—Se3x | 61.457 (18) |
Se5viii—Mo5—Se5 | 176.21 (3) | Se2—Rb3—Se3x | 139.85 (4) |
Se4—Mo5—Mo5viii | 120.544 (18) | Se2iv—Rb3—Se3x | 70.324 (19) |
Se5viii—Mo5—Mo5viii | 59.12 (2) | Se1x—Rb3—Se3x | 71.732 (12) |
Se5—Mo5—Mo5viii | 118.71 (3) | Se1—Rb3—Se3x | 132.686 (15) |
Se4—Mo5—Mo5ix | 118.33 (2) | Se1iv—Rb3—Se3x | 131.307 (15) |
Se5viii—Mo5—Mo5ix | 119.10 (2) | Se3—Rb3—Se3x | 85.75 (3) |
Se5—Mo5—Mo5ix | 58.73 (3) | Se2x—Rb3—Se3iv | 139.85 (4) |
Mo5viii—Mo5—Mo5ix | 60.0 | Se2—Rb3—Se3iv | 70.324 (19) |
Se4—Mo5—Mo5xi | 145.00 (2) | Se2iv—Rb3—Se3iv | 61.457 (18) |
Se5viii—Mo5—Mo5xi | 121.09 (2) | Se1x—Rb3—Se3iv | 132.686 (15) |
Se5—Mo5—Mo5xi | 61.127 (17) | Se1—Rb3—Se3iv | 131.307 (15) |
Mo5viii—Mo5—Mo5xi | 90.0 | Se1iv—Rb3—Se3iv | 71.732 (12) |
Mo5ix—Mo5—Mo5xi | 60.074 (11) | Se3—Rb3—Se3iv | 85.75 (3) |
Se4—Mo5—Mo5xii | 148.51 (2) | Se3x—Rb3—Se3iv | 85.75 (3) |
Se5viii—Mo5—Mo5xii | 61.256 (17) | Se2x—Rb3—Mo2xxiii | 38.659 (12) |
Se5—Mo5—Mo5xii | 120.95 (2) | Se2—Rb3—Mo2xxiii | 158.432 (14) |
Mo5viii—Mo5—Mo5xii | 60.074 (11) | Se2iv—Rb3—Mo2xxiii | 81.285 (12) |
Mo5ix—Mo5—Mo5xii | 90.0 | Se1x—Rb3—Mo2xxiii | 37.756 (11) |
Mo5xi—Mo5—Mo5xii | 59.85 (2) | Se1—Rb3—Mo2xxiii | 103.863 (18) |
Se4—Mo5—Se5xii | 112.79 (2) | Se1iv—Rb3—Mo2xxiii | 126.89 (2) |
Se5viii—Mo5—Se5xii | 92.01 (2) | Se3—Rb3—Mo2xxiii | 100.37 (2) |
Se5—Mo5—Se5xii | 91.779 (19) | Se3x—Rb3—Mo2xxiii | 39.142 (11) |
Mo5viii—Mo5—Se5xii | 117.931 (18) | Se3iv—Rb3—Mo2xxiii | 122.72 (3) |
Mo5ix—Mo5—Se5xii | 117.684 (19) | Se2x—Rb3—Mo2ii | 81.286 (12) |
Mo5xi—Mo5—Se5xii | 57.63 (2) | Se2—Rb3—Mo2ii | 38.659 (12) |
Mo5xii—Mo5—Se5xii | 57.89 (2) | Se2iv—Rb3—Mo2ii | 158.432 (14) |
Se4—Mo5—Mo4 | 58.435 (19) | Se1x—Rb3—Mo2ii | 126.89 (2) |
Se5viii—Mo5—Mo4 | 60.146 (18) | Se1—Rb3—Mo2ii | 37.756 (11) |
Se5—Mo5—Mo4 | 116.23 (2) | Se1iv—Rb3—Mo2ii | 103.863 (18) |
Mo5viii—Mo5—Mo4 | 62.115 (15) | Se3—Rb3—Mo2ii | 39.142 (11) |
Mo5ix—Mo5—Mo4 | 90.189 (13) | Se3x—Rb3—Mo2ii | 122.72 (3) |
Mo5xi—Mo5—Mo4 | 147.639 (18) | Se3iv—Rb3—Mo2ii | 100.37 (2) |
Mo5xii—Mo5—Mo4 | 112.009 (18) | Mo2xxiii—Rb3—Mo2ii | 119.912 (2) |
Se5xii—Mo5—Mo4 | 148.68 (3) | Se2x—Rb3—Mo2xxiv | 158.432 (14) |
Se4—Mo5—Mo4ix | 58.133 (19) | Se2—Rb3—Mo2xxiv | 81.286 (12) |
Se5viii—Mo5—Mo4ix | 116.98 (2) | Se2iv—Rb3—Mo2xxiv | 38.659 (12) |
Se5—Mo5—Mo4ix | 59.359 (18) | Se1x—Rb3—Mo2xxiv | 103.863 (18) |
Mo5viii—Mo5—Mo4ix | 89.136 (13) | Se1—Rb3—Mo2xxiv | 126.89 (2) |
Mo5ix—Mo5—Mo4ix | 60.259 (15) | Se1iv—Rb3—Mo2xxiv | 37.756 (11) |
Mo5xi—Mo5—Mo4ix | 110.478 (18) | Se3—Rb3—Mo2xxiv | 122.72 (3) |
Mo5xii—Mo5—Mo4ix | 146.076 (17) | Se3x—Rb3—Mo2xxiv | 100.37 (2) |
Se5xii—Mo5—Mo4ix | 148.50 (2) | Se3iv—Rb3—Mo2xxiv | 39.142 (11) |
Mo4—Mo5—Mo4ix | 56.88 (2) | Mo2xxiii—Rb3—Mo2xxiv | 119.912 (2) |
Se4—Mo5—Rb2xiii | 63.69 (2) | Mo2ii—Rb3—Mo2xxiv | 119.912 (2) |
Se5viii—Mo5—Rb2xiii | 125.012 (19) | Se2x—Rb3—Rb3vi | 88.45 (3) |
Se5—Mo5—Rb2xiii | 57.359 (16) | Se2—Rb3—Rb3vi | 88.45 (3) |
Mo5viii—Mo5—Rb2xiii | 174.86 (2) | Se2iv—Rb3—Rb3vi | 88.45 (3) |
Mo5ix—Mo5—Rb2xiii | 115.87 (2) | Se1x—Rb3—Rb3vi | 123.51 (2) |
Mo5xi—Mo5—Rb2xiii | 85.09 (2) | Se1—Rb3—Rb3vi | 123.51 (2) |
Mo5xii—Mo5—Rb2xiii | 118.22 (3) | Se1iv—Rb3—Rb3vi | 123.51 (2) |
Se5xii—Mo5—Rb2xiii | 60.43 (2) | Se3—Rb3—Rb3vi | 51.779 (19) |
Mo4—Mo5—Rb2xiii | 122.08 (3) | Se3x—Rb3—Rb3vi | 51.779 (19) |
Mo4ix—Mo5—Rb2xiii | 91.13 (2) | Se3iv—Rb3—Rb3vi | 51.779 (19) |
Mo2ii—Se1—Mo1 | 64.977 (19) | Mo2xxiii—Rb3—Rb3vi | 88.30 (2) |
Mo2ii—Se1—Mo1ii | 64.007 (19) | Mo2ii—Rb3—Rb3vi | 88.30 (2) |
Mo1—Se1—Mo1ii | 61.56 (2) | Mo2xxiv—Rb3—Rb3vi | 88.30 (2) |
Mo2ii—Se1—Mo4 | 129.64 (3) | Se2x—Rb3—Mo1x | 32.659 (13) |
Mo1—Se1—Mo4 | 123.30 (3) | Se2—Rb3—Mo1x | 132.30 (2) |
Mo1ii—Se1—Mo4 | 77.64 (2) | Se2iv—Rb3—Mo1x | 101.819 (16) |
Mo2ii—Se1—Rb3 | 83.07 (2) | Se1x—Rb3—Mo1x | 31.482 (12) |
Mo1—Se1—Rb3 | 102.409 (19) | Se1—Rb3—Mo1x | 71.475 (18) |
Mo1ii—Se1—Rb3 | 146.88 (3) | Se1iv—Rb3—Mo1x | 115.79 (3) |
Mo4—Se1—Rb3 | 130.98 (2) | Se3—Rb3—Mo1x | 101.265 (13) |
Mo2—Se2—Mo2ii | 61.88 (2) | Se3x—Rb3—Mo1x | 73.067 (11) |
Mo2—Se2—Mo1 | 62.447 (19) | Se3iv—Rb3—Mo1x | 156.95 (2) |
Mo2ii—Se2—Mo1 | 63.121 (19) | Mo2xxiii—Rb3—Mo1x | 34.684 (10) |
Mo2—Se2—Mo3 | 61.63 (2) | Mo2ii—Rb3—Mo1x | 98.722 (13) |
Mo2ii—Se2—Mo3 | 61.75 (2) | Mo2xxiv—Rb3—Mo1x | 135.26 (2) |
Mo1—Se2—Mo3 | 114.20 (3) | Rb3vi—Rb3—Mo1x | 116.365 (16) |
Mo2—Se2—Rb3 | 145.75 (2) | Se2x—Rb3—Mo1 | 101.819 (16) |
Mo2ii—Se2—Rb3 | 83.884 (19) | Se2—Rb3—Mo1 | 32.659 (13) |
Mo1—Se2—Rb3 | 102.40 (3) | Se2iv—Rb3—Mo1 | 132.30 (2) |
Mo3—Se2—Rb3 | 104.58 (3) | Se1x—Rb3—Mo1 | 115.79 (3) |
Mo2—Se2—Rb1iii | 97.90 (2) | Se1—Rb3—Mo1 | 31.482 (12) |
Mo2ii—Se2—Rb1iii | 139.19 (2) | Se1iv—Rb3—Mo1 | 71.475 (18) |
Mo1—Se2—Rb1iii | 141.55 (2) | Se3—Rb3—Mo1 | 73.067 (11) |
Mo3—Se2—Rb1iii | 77.498 (19) | Se3x—Rb3—Mo1 | 156.95 (2) |
Rb3—Se2—Rb1iii | 109.92 (2) | Se3iv—Rb3—Mo1 | 101.265 (13) |
Mo3—Se3—Mo3ii | 61.01 (3) | Mo2xxiii—Rb3—Mo1 | 135.26 (2) |
Mo3—Se3—Mo2vii | 61.711 (19) | Mo2ii—Rb3—Mo1 | 34.684 (10) |
Mo3ii—Se3—Mo2vii | 61.181 (18) | Mo2xxiv—Rb3—Mo1 | 98.722 (13) |
Mo3—Se3—Mo2ii | 61.712 (19) | Rb3vi—Rb3—Mo1 | 116.365 (16) |
Mo3ii—Se3—Mo2ii | 61.181 (18) | Mo1x—Rb3—Mo1 | 101.78 (2) |
Mo2vii—Se3—Mo2ii | 112.60 (3) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) x+1, y, z; (iv) −x+y+1, −x, z; (v) x+1, y+1, z; (vi) x, y, −z+1/2; (vii) −x+y+1, −x+1, −z+1/2; (viii) −x+y, −x, z; (ix) −y, x−y, z; (x) −y, x−y−1, z; (xi) x−y, x, −z; (xii) y, −x+y, −z; (xiii) x, y+1, z; (xiv) −x, −y, −z; (xv) x−1, y, z; (xvi) −x+1, −y, −z; (xvii) −y, x−y−1, −z+1/2; (xviii) x−1, y, −z+1/2; (xix) x, y−1, z; (xx) y, −x+y−1, −z; (xxi) x−y+1, x, −z; (xxii) −x, −y−1, −z; (xxiii) x−1, y−1, z; (xxiv) −y+1, x−y−1, z. |
Experimental details
Crystal data | |
Chemical formula | Rb5Mo27Se31 |
Mr | 5465.49 |
Crystal system, space group | Hexagonal, P63/m |
Temperature (K) | 293 |
a, c (Å) | 9.5208 (1), 37.5113 (5) |
V (Å3) | 2944.69 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 28.79 |
Crystal size (mm) | 0.07 × 0.05 × 0.04 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995) |
Tmin, Tmax | 0.090, 0.162 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 58800, 6242, 3113 |
Rint | 0.086 |
(sin θ/λ)max (Å−1) | 0.909 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.120, 1.05 |
No. of reflections | 6242 |
No. of parameters | 100 |
Δρmax, Δρmin (e Å−3) | 3.12, −2.54 |
Computer programs: COLLECT (Nonius, 1998), COLLECT, DENZO and SCALEPACK (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Bergerhoff, 1996), SHELXL97.
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register
The crystal structures of reduced molybdenum chalcogenides are characterized by metal-metal bonding that manifests itself in discrete clusters of diverse sizes and geometries. Up to now, 11 different Mo clusters with nuclearities from three to 36 have been synthesized in solid-state chemistry. Clusters with nuclearities higher than six, i.e. Mo3n (n = 3, 4, 5, 6, 7, 8, 10 and 12), result from the one-dimensional trans-face-sharing of (n-1) Mo6 octahedra. The Mo3n clusters are surrounded by 3n+8 chalchogenide atoms to form Mo3nXi3n+2Xa6 units. Whereas the inner ligands, denoted Xi in the notation of Schäfer & von Schnering (1964), are only linked to one cluster, the six external Xa ligands are shared between adjacent clusters to create the Mo—X framework. Large voids between the Mo3nX3n+2 units are thus formed, in which the cations reside.
The crystal structures of these compounds can be based on only one or on two different types of Mo clusters. The first case is represented by the series of compounds Mn-2Mo3nX3n+2 (M = Rb or Cs and X = S, Se or Te; n = 3, 4, 5, 6, 7, 8, 10 or 12) containing Mo9, Mo12, Mo15, Mo18, Mo21, Mo24, Mo30 and Mo36 clusters (Gougeon, 1984; Gougeon et al., 1984, 1987, 1988, 1989a,b, 1990; Thomas et al., 1997; Picard, Gougeon & Potel, 1999; Picard, Halet et al., 1999). The second group is based on compounds containing clusters of odd and even nuclearity in equal proportion and is exemplified by the series of compounds Rb2nMo9X11Mo6nX6n+2 (n = 1, 2, 3, 4 or 5; Picard et al., 2000). Current interest in these Mo cluster compounds is associated not only with their fascinating structural aspect, but also with their interesting physical properties. Indeed, the sulfides and selenides generally present superconducting or metal-insulator transitions at low temperature.
We present here a new structural type, Rb5Mo27Se31, containing Mo12Sei14Sea6 and Mo15Sei17Sea6 cluster units in equal proportion. Both units share their Sea atoms according to the connective formulae Mo12Sei8Sei-a6/2Sei-a6/2 and Mo15Sei11Sei-a6/2Sei-a6/2 to form large cavities in which the Rb+ ions are located. The Mo12Se14Se6 and Mo15Se17Se6 cluster units are similar to those previously reported in the compounds Rb2Mo12Se14 (Gautier et al., 1998) and Rb3Mo15Se17 (Gougeon et al., 1989a), in which they occur separately. The Mo cores of both units result from the trans-face-sharing of three or four octahedral Mo6 clusters, respectively, and they can alternatively be described as resulting from the stacking of four and five Mo3 triangles, respectively.
The Mo12Se14Se6 unit possesses the same local symmetry (3 or C3i) as, and does not show any significant structural differences from, that observed in Rb2Mo12Se14. Indeed, the intracluster Mo—Mo and Mo—Se distances are similar to within 0.009 and 0.006 Å, respectively, in both compounds, indicating an identical cationic charge transfer toward the Mo12Se14Se6 units.
The symmetry of the Mo15Se17Se6 unit is 6 or C3 h, as in Rb3Mo15Se17. The different Mo—Mo and Mo—Se distances within the Mo15Se17Se6 unit also compare well with those found in Rb3Mo15Se17; the greatest deviations are 0.007 and 0.005 Å for the Mo—Mo and Mo—Se bonds, respectively.
The shortest Mo—Mo distance between the Mo12 and Mo15 clusters is 3.2780 (7) Å, similar to those found in Rb2Mo12Se14 [3.279 (1) Å] and Rb3Mo15Se17 [3.268 (2) Å]. The Rb1+ cation is surrounded by 11 Se atoms, forming a distorted trigonal prism capped on all faces. The other alkali-metal cations are arranged in finite chains along the threefold axis between two consecutive Mo15Se17Se6 units. The Rb2+ cations at both ends of the finite chains are in a tetra-capped trigonal prismatic environment of Se atoms, and the Rb3+ cations are in a tri-capped trigonal coordination. The latter environment is similar to that encountered in the quasi-one-dimensional compounds M2Mo6X6 (Potel, 1981). The Rb—Se distances vary over a wide range [3.5156 (6)–3.954 (1) Å]. The shortest spacing between adjacent Rb+ cations is 4.715 (3) Å.