Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802010218/br6051sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802010218/br6051Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Mo-O) = 0.003 Å
- R factor = 0.031
- wR factor = 0.073
- Data-to-parameter ratio = 31.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_732 Alert C Angle Calc 176.41(4), Rep 176.41(1) .... 2.67 s.u-Ratio MO4 -MO1 -MO2 1.555 1.555 1.555 General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.438 Tmax scaled 0.438 Tmin scaled 0.331
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: WinGX (Farrugia, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.
CaMo5O8 | F(000) = 1176 |
Mr = 647.78 | Dx = 6.702 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 7.550 (5) Å | θ = 8.3–16.1° |
b = 9.068 (5) Å | µ = 10.31 mm−1 |
c = 9.983 (5) Å | T = 293 K |
β = 110.07 (4)° | Irregular, black |
V = 642.0 (6) Å3 | 0.12 × 0.11 × 0.08 mm |
Z = 4 |
Enraf-Nonius CAD-4 diffractometer | 2812 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 39.9°, θmin = 2.9° |
θ–2θ scans | h = 0→13 |
Absorption correction: ψ scan (North et al. 1968) | k = 0→16 |
Tmin = 0.755, Tmax = 1.00 | l = −18→16 |
4174 measured reflections | 3 standard reflections every 60 min |
3965 independent reflections | intensity decay: none |
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)] = 0.031 | w = 1/[σ2(Fo2) + (0.0301P)2 + 0.820P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.073 | (Δ/σ)max = 0.001 |
S = 1.05 | Δρmax = 1.99 e Å−3 |
3965 reflections | Δρmin = −2.44 e Å−3 |
128 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00189 (13) |
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 | ||
Ca | 0.26502 (12) | 0.50520 (10) | 0.52649 (9) | 0.01094 (13) | |
Mo1 | 0.61063 (4) | −0.11555 (3) | 0.48386 (3) | 0.00331 (5) | |
Mo2 | 0.38311 (4) | −0.11560 (3) | 0.68223 (3) | 0.00319 (5) | |
Mo3 | 0.17729 (4) | −0.12651 (3) | 0.38673 (3) | 0.00322 (5) | |
Mo4 | 0.81176 (4) | −0.13391 (3) | 0.30011 (3) | 0.00319 (5) | |
Mo5 | 0.00045 (4) | −0.12368 (3) | 0.58644 (3) | 0.00299 (5) | |
O1 | 0.3994 (4) | 0.0079 (3) | 0.8417 (3) | 0.0044 (4) | |
O2 | 0.0073 (4) | −0.2212 (3) | 0.9361 (3) | 0.0044 (4) | |
O3 | −0.0133 (4) | 0.0007 (3) | 0.2366 (3) | 0.0049 (4) | |
O4 | 0.4009 (4) | −0.2532 (3) | 0.0205 (3) | 0.0047 (4) | |
O5 | 0.8011 (4) | −0.2458 (3) | 0.1175 (3) | 0.0056 (4) | |
O6 | 0.2055 (4) | −0.2469 (3) | 0.2170 (3) | 0.0054 (4) | |
O7 | 0.6066 (4) | −0.2339 (3) | 0.8309 (3) | 0.0051 (4) | |
O8 | 0.3842 (4) | −0.0014 (3) | 0.3326 (3) | 0.0055 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ca | 0.0099 (3) | 0.0114 (3) | 0.0104 (3) | −0.0003 (3) | 0.0021 (2) | 0.0009 (3) |
Mo1 | 0.00338 (10) | 0.00300 (11) | 0.00351 (10) | −0.00028 (8) | 0.00116 (8) | 0.00004 (8) |
Mo2 | 0.00314 (10) | 0.00313 (11) | 0.00320 (10) | 0.00024 (8) | 0.00094 (8) | 0.00026 (8) |
Mo3 | 0.00326 (10) | 0.00292 (11) | 0.00367 (10) | 0.00013 (9) | 0.00145 (8) | −0.00013 (8) |
Mo4 | 0.00375 (11) | 0.00313 (11) | 0.00276 (10) | 0.00015 (8) | 0.00123 (8) | −0.00013 (8) |
Mo5 | 0.00334 (10) | 0.00263 (10) | 0.00282 (10) | −0.00018 (9) | 0.00085 (8) | 0.00018 (8) |
O1 | 0.0044 (9) | 0.0048 (10) | 0.0022 (9) | 0.0017 (8) | −0.0010 (7) | 0.0002 (8) |
O2 | 0.0045 (10) | 0.0060 (10) | 0.0020 (9) | 0.0011 (8) | 0.0002 (8) | 0.0014 (7) |
O3 | 0.0065 (10) | 0.0038 (10) | 0.0060 (10) | 0.0007 (8) | 0.0041 (8) | 0.0016 (8) |
O4 | 0.0033 (10) | 0.0047 (10) | 0.0061 (10) | 0.0005 (7) | 0.0015 (8) | 0.0014 (8) |
O5 | 0.0053 (11) | 0.0058 (11) | 0.0059 (10) | −0.0006 (8) | 0.0023 (9) | −0.0020 (8) |
O6 | 0.0057 (11) | 0.0063 (10) | 0.0041 (10) | −0.0002 (8) | 0.0018 (8) | −0.0015 (8) |
O7 | 0.0047 (10) | 0.0057 (10) | 0.0039 (10) | 0.0023 (8) | 0.0002 (8) | 0.0005 (8) |
O8 | 0.0067 (10) | 0.0046 (10) | 0.0069 (10) | −0.0010 (8) | 0.0044 (8) | 0.0008 (8) |
Ca—O1i | 2.394 (3) | Mo4—O5 | 2.064 (3) |
Ca—O1ii | 2.421 (3) | Mo4—O1ix | 2.074 (3) |
Ca—O4iii | 2.481 (3) | Mo4—O2xv | 2.091 (3) |
Ca—O7ii | 2.592 (3) | Mo4—Mo3x | 2.5943 (19) |
Ca—O5iv | 2.647 (3) | Mo4—Mo5x | 2.7229 (16) |
Ca—O3v | 2.662 (3) | Mo4—Mo2ix | 2.7373 (12) |
Ca—O2i | 2.689 (3) | Mo4—Mo1 | 2.7587 (14) |
Ca—O8iii | 2.874 (3) | Mo4—Mo5ix | 2.7653 (13) |
Ca—O2vi | 3.018 (3) | Mo4—Caxvi | 3.3556 (18) |
Ca—O6iii | 3.035 (3) | Mo5—O5xvii | 2.021 (3) |
Ca—Mo4iv | 3.3556 (18) | Mo5—O6vii | 2.022 (3) |
Ca—Mo2ii | 3.378 (2) | Mo5—O3xiv | 2.063 (3) |
Mo1—O5vii | 2.028 (3) | Mo5—O2viii | 2.071 (3) |
Mo1—O7viii | 2.041 (3) | Mo5—Mo3xiv | 2.6957 (12) |
Mo1—O8ix | 2.106 (3) | Mo5—Mo2 | 2.715 (2) |
Mo1—O4vii | 2.111 (3) | Mo5—Mo4xiii | 2.7229 (16) |
Mo1—O8 | 2.122 (3) | Mo5—Mo3 | 2.7541 (13) |
Mo1—Mo2ix | 2.6830 (11) | Mo5—Mo4ix | 2.7653 (13) |
Mo1—Mo4 | 2.7587 (14) | Mo5—Mo1xiii | 2.765 (2) |
Mo1—Mo3ix | 2.7625 (13) | Mo5—Mo5xiv | 2.8288 (12) |
Mo1—Mo5x | 2.765 (2) | O1—Mo4ix | 2.074 (3) |
Mo1—Mo1ix | 2.7669 (13) | O1—Caiii | 2.394 (3) |
Mo1—Mo2 | 3.0343 (15) | O1—Caxi | 2.421 (3) |
Mo1—Mo3 | 3.078 (2) | O2—Mo3vii | 2.057 (3) |
Mo2—O1 | 1.915 (3) | O2—Mo5vii | 2.071 (3) |
Mo2—O6vii | 1.948 (3) | O2—Mo4xvii | 2.091 (3) |
Mo2—O4vii | 2.047 (3) | O2—Caiii | 2.689 (3) |
Mo2—O8ix | 2.100 (3) | O2—Caxviii | 3.018 (3) |
Mo2—O7 | 2.117 (3) | O3—Mo4xiii | 2.052 (3) |
Mo2—Mo1ix | 2.6830 (11) | O3—Mo5xiv | 2.063 (3) |
Mo2—Mo5 | 2.715 (2) | O3—Caxix | 2.662 (3) |
Mo2—Mo4ix | 2.7373 (12) | O4—Mo2viii | 2.047 (3) |
Mo2—Mo3 | 2.8250 (17) | O4—Mo3viii | 2.068 (3) |
Mo2—Caxi | 3.378 (2) | O4—Mo1viii | 2.111 (3) |
Mo2—Caxii | 3.753 (2) | O4—Cai | 2.481 (3) |
Mo3—O3 | 2.042 (3) | O5—Mo5xv | 2.021 (3) |
Mo3—O2viii | 2.057 (3) | O5—Mo1viii | 2.028 (3) |
Mo3—O4vii | 2.068 (3) | O5—Caxvi | 2.647 (3) |
Mo3—O6 | 2.087 (3) | O6—Mo2viii | 1.948 (3) |
Mo3—O8 | 2.145 (3) | O6—Mo5viii | 2.022 (3) |
Mo3—Mo4xiii | 2.5943 (19) | O6—Cai | 3.035 (3) |
Mo3—Mo5xiv | 2.6957 (12) | O7—Mo1vii | 2.041 (3) |
Mo3—Mo5 | 2.7541 (13) | O7—Mo4vii | 2.063 (3) |
Mo3—Mo1ix | 2.7625 (13) | O7—Caxi | 2.592 (3) |
Mo3—Mo2 | 2.8250 (17) | O8—Mo2ix | 2.100 (3) |
Mo3—Caxii | 3.592 (2) | O8—Mo1ix | 2.106 (3) |
Mo4—O3x | 2.052 (3) | O8—Cai | 2.874 (3) |
Mo4—O7viii | 2.063 (3) | ||
O5vii—Mo1—O7viii | 84.42 (12) | Mo4xiii—Mo3—Mo5 | 61.12 (4) |
O5vii—Mo1—O8ix | 86.71 (12) | Mo5xiv—Mo3—Mo5 | 62.53 (2) |
O7viii—Mo1—O8ix | 168.26 (11) | Mo4xiii—Mo3—Mo1ix | 123.78 (3) |
O5vii—Mo1—O4vii | 86.62 (12) | Mo5xiv—Mo3—Mo1ix | 60.87 (4) |
O7viii—Mo1—O4vii | 86.15 (11) | Mo5—Mo3—Mo1ix | 90.07 (3) |
O8ix—Mo1—O4vii | 85.66 (11) | Mo4xiii—Mo3—Mo2 | 119.34 (4) |
O5vii—Mo1—O8 | 170.73 (11) | Mo5xiv—Mo3—Mo2 | 88.91 (3) |
O7viii—Mo1—O8 | 89.56 (11) | Mo5—Mo3—Mo2 | 58.22 (4) |
O8ix—Mo1—O8 | 98.24 (11) | Mo1ix—Mo3—Mo2 | 57.38 (2) |
O4vii—Mo1—O8 | 85.95 (11) | Mo4xiii—Mo3—Mo1 | 178.903 (15) |
Mo2ix—Mo1—Mo4 | 60.38 (3) | Mo5xiv—Mo3—Mo1 | 116.94 (3) |
Mo2ix—Mo1—Mo3ix | 62.48 (4) | Mo5—Mo3—Mo1 | 119.90 (4) |
Mo4—Mo1—Mo3ix | 89.77 (3) | Mo1ix—Mo3—Mo1 | 56.24 (3) |
Mo2ix—Mo1—Mo5x | 90.43 (3) | Mo2—Mo3—Mo1 | 61.68 (4) |
Mo4—Mo1—Mo5x | 59.06 (4) | O3x—Mo4—O7viii | 170.84 (10) |
Mo3ix—Mo1—Mo5x | 58.37 (3) | O3x—Mo4—O5 | 81.59 (11) |
Mo2ix—Mo1—Mo1ix | 67.64 (4) | O7viii—Mo4—O5 | 92.42 (11) |
Mo4—Mo1—Mo1ix | 127.97 (3) | O3x—Mo4—O1ix | 83.50 (11) |
Mo3ix—Mo1—Mo1ix | 67.66 (5) | O7viii—Mo4—O1ix | 88.92 (12) |
Mo5x—Mo1—Mo1ix | 125.83 (3) | O5—Mo4—O1ix | 83.13 (11) |
Mo2ix—Mo1—Mo2 | 122.51 (2) | O3x—Mo4—O2xv | 100.88 (11) |
Mo4—Mo1—Mo2 | 176.412 (15) | O7viii—Mo4—O2xv | 86.39 (12) |
Mo3ix—Mo1—Mo2 | 93.55 (3) | O5—Mo4—O2xv | 93.97 (11) |
Mo5x—Mo1—Mo2 | 121.82 (4) | O1ix—Mo4—O2xv | 174.38 (10) |
Mo1ix—Mo1—Mo2 | 54.86 (3) | Mo3x—Mo4—Mo5x | 62.34 (4) |
Mo2ix—Mo1—Mo3 | 94.17 (3) | Mo3x—Mo4—Mo2ix | 119.40 (3) |
Mo4—Mo1—Mo3 | 123.82 (4) | Mo5x—Mo4—Mo2ix | 90.19 (3) |
Mo3ix—Mo1—Mo3 | 123.76 (3) | Mo3x—Mo4—Mo1 | 122.83 (4) |
Mo5x—Mo1—Mo3 | 175.386 (15) | Mo5x—Mo4—Mo1 | 60.59 (4) |
Mo1ix—Mo1—Mo3 | 56.10 (3) | Mo2ix—Mo4—Mo1 | 58.44 (2) |
Mo2—Mo1—Mo3 | 55.05 (4) | Mo3x—Mo4—Mo5ix | 60.29 (2) |
O1—Mo2—O6vii | 94.47 (12) | Mo5x—Mo4—Mo5ix | 62.05 (2) |
O1—Mo2—O4vii | 173.00 (11) | Mo2ix—Mo4—Mo5ix | 59.12 (4) |
O6vii—Mo2—O4vii | 90.23 (12) | Mo1—Mo4—Mo5ix | 89.92 (3) |
O1—Mo2—O8ix | 86.93 (12) | O5xvii—Mo5—O6vii | 90.40 (12) |
O6vii—Mo2—O8ix | 168.42 (11) | O5xvii—Mo5—O3xiv | 90.21 (11) |
O4vii—Mo2—O8ix | 87.43 (12) | O6vii—Mo5—O3xiv | 87.77 (11) |
O1—Mo2—O7 | 84.56 (11) | O5xvii—Mo5—O2viii | 85.33 (11) |
O6vii—Mo2—O7 | 89.00 (12) | O6vii—Mo5—O2viii | 82.47 (11) |
O4vii—Mo2—O7 | 90.35 (11) | O3xiv—Mo5—O2viii | 169.22 (11) |
O8ix—Mo2—O7 | 79.68 (12) | Mo3xiv—Mo5—Mo2 | 116.62 (3) |
Mo1ix—Mo2—Mo5 | 92.62 (3) | Mo3xiv—Mo5—Mo4xiii | 91.95 (3) |
Mo1ix—Mo2—Mo4ix | 61.18 (4) | Mo2—Mo5—Mo4xiii | 118.74 (4) |
Mo5—Mo2—Mo4ix | 60.95 (3) | Mo3xiv—Mo5—Mo3 | 117.47 (2) |
Mo1ix—Mo2—Mo3 | 60.14 (3) | Mo2—Mo5—Mo3 | 62.20 (4) |
Mo5—Mo2—Mo3 | 59.58 (4) | Mo4xiii—Mo5—Mo3 | 56.54 (4) |
Mo4ix—Mo2—Mo3 | 88.91 (3) | Mo3xiv—Mo5—Mo4ix | 56.71 (4) |
Mo1ix—Mo2—Mo1 | 57.49 (2) | Mo2—Mo5—Mo4ix | 59.92 (2) |
Mo5—Mo2—Mo1 | 122.85 (4) | Mo4xiii—Mo5—Mo4ix | 117.95 (2) |
Mo4ix—Mo2—Mo1 | 118.63 (3) | Mo3—Mo5—Mo4ix | 89.81 (3) |
Mo3—Mo2—Mo1 | 63.27 (5) | Mo3xiv—Mo5—Mo1xiii | 60.76 (2) |
O3—Mo3—O2viii | 102.40 (11) | Mo2—Mo5—Mo1xiii | 176.756 (15) |
O3—Mo3—O4vii | 170.32 (11) | Mo4xiii—Mo5—Mo1xiii | 60.35 (4) |
O2viii—Mo3—O4vii | 85.95 (12) | Mo3—Mo5—Mo1xiii | 116.80 (4) |
O3—Mo3—O6 | 86.68 (11) | Mo4ix—Mo5—Mo1xiii | 117.39 (3) |
O2viii—Mo3—O6 | 95.11 (11) | Mo3xiv—Mo5—Mo5xiv | 59.75 (4) |
O4vii—Mo3—O6 | 87.71 (11) | Mo2—Mo5—Mo5xiv | 88.45 (3) |
O3—Mo3—O8 | 84.66 (11) | Mo4xiii—Mo5—Mo5xiv | 59.71 (3) |
O2viii—Mo3—O8 | 169.69 (11) | Mo3—Mo5—Mo5xiv | 57.72 (2) |
O4vii—Mo3—O8 | 86.43 (11) | Mo4ix—Mo5—Mo5xiv | 58.24 (4) |
O6—Mo3—O8 | 77.65 (11) | Mo1xiii—Mo5—Mo5xiv | 88.48 (3) |
Mo4xiii—Mo3—Mo5xiv | 63.00 (3) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x, y−1, z; (xiii) x−1, y, z; (xiv) −x, −y, −z+1; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2; (xviii) −x, y−1/2, −z+3/2; (xix) −x, y−1/2, −z+1/2. |
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