Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802022973/br6072sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802022973/br6072Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Mo-Mo) = 0.001 Å
- R factor = 0.041
- wR factor = 0.093
- Data-to-parameter ratio = 23.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry 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 1.060 Tmax scaled 0.538 Tmin scaled 0.427 REFLT_03 From the CIF: _diffrn_reflns_theta_max 37.90 From the CIF: _reflns_number_total 2540 Count of symmetry unique reflns 1435 Completeness (_total/calc) 177.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1105 Fraction of Friedel pairs measured 0.770 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT (Nonius, 1998); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); 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.
PrMo7.6O14 | F(000) = 1964 |
Mr = 1095.97 | Dx = 7.121 Mg m−3 |
Orthorhombic, Aba2 | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: A 2 -2ac | Cell parameters from 25995 reflections |
a = 9.1611 (4) Å | θ = 1.0–37.8° |
b = 9.9709 (9) Å | µ = 13.78 mm−1 |
c = 11.1916 (8) Å | T = 293 K |
V = 1022.29 (13) Å3 | Irregular, black |
Z = 4 | 0.06 × 0.05 × 0.05 mm |
Nonius KappaCCD diffractometer | 2540 independent reflections |
Radiation source: fine-focus sealed tube | 2249 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
φ scans (κ = 0) + additional ω scans | θmax = 37.9°, θmin = 3.5° |
Absorption correction: multi-scan (Blessing, 1995) | h = −15→15 |
Tmin = 0.403, Tmax = 0.508 | k = −17→16 |
11744 measured reflections | l = −19→16 |
Refinement on F2 | w = 1/[σ2(Fo2) + (0.0333P)2 + 22.8476P] where P = (Fo2 + 2Fc2)/3 |
Least-squares matrix: full | (Δ/σ)max = 0.001 |
R[F2 > 2σ(F2)] = 0.041 | Δρmax = 3.97 e Å−3 |
wR(F2) = 0.093 | Δρmin = −2.37 e Å−3 |
S = 1.10 | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
2540 reflections | Extinction coefficient: 0.00076 (8) |
108 parameters | Absolute structure: Flack (1983), 1118 Friedel pairs |
1 restraint | Absolute structure parameter: −0.01 (3) |
Primary atom site location: isomorphous structure methods |
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 | Occ. (<1) | |
Pr | 0.0000 | 0.0000 | −0.49898 (8) | 0.01351 (12) | |
Mo1 | 0.12171 (6) | −0.07440 (6) | −0.83846 (5) | 0.00714 (12) | |
Mo2 | 0.11808 (6) | 0.16064 (6) | 0.04122 (6) | 0.00751 (11) | |
Mo3 | 0.12480 (6) | −0.08226 (5) | −0.08178 (5) | 0.00711 (12) | |
Mo4 | 0.12393 (8) | 0.66281 (8) | −0.69447 (7) | 0.0093 (2) | 0.811 (4) |
O1 | 0.2426 (7) | 0.3322 (5) | −0.2052 (5) | 0.0076 (9) | |
O2 | 0.2468 (7) | 0.0841 (5) | −0.3338 (6) | 0.0105 (9) | |
O3 | 0.0155 (6) | 0.2513 (6) | −0.3355 (5) | 0.0091 (9) | |
O4 | 0.2319 (5) | 0.3462 (5) | −0.9577 (6) | 0.0099 (9) | |
O5 | 0.2674 (6) | 0.0812 (5) | −0.0774 (6) | 0.0122 (10) | |
O6 | −0.0075 (6) | 0.2605 (6) | −0.0790 (6) | 0.0154 (11) | |
O7 | 0.0000 | 0.0000 | −0.7139 (7) | 0.0083 (13) | |
O8 | 0.0000 | 0.0000 | −0.2230 (9) | 0.0191 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pr | 0.0119 (2) | 0.0128 (2) | 0.0158 (2) | 0.00103 (19) | 0.000 | 0.000 |
Mo1 | 0.0056 (2) | 0.0073 (2) | 0.0084 (3) | 0.00063 (16) | −0.0005 (2) | 0.00000 (19) |
Mo2 | 0.0059 (2) | 0.0070 (2) | 0.0097 (2) | 0.00050 (16) | −0.0011 (2) | −0.0011 (2) |
Mo3 | 0.0056 (2) | 0.0082 (2) | 0.0076 (3) | 0.00108 (16) | −0.00012 (19) | 0.0004 (2) |
Mo4 | 0.0080 (3) | 0.0083 (3) | 0.0117 (4) | 0.0021 (2) | −0.0027 (2) | −0.0031 (3) |
O1 | 0.0080 (18) | 0.0057 (18) | 0.009 (2) | 0.0008 (19) | −0.0038 (16) | 0.0004 (17) |
O2 | 0.0114 (19) | 0.0103 (19) | 0.010 (2) | 0.002 (2) | 0.003 (2) | −0.001 (2) |
O3 | 0.008 (2) | 0.0089 (19) | 0.011 (2) | −0.0015 (15) | −0.0004 (18) | 0.0037 (19) |
O4 | 0.0071 (18) | 0.009 (2) | 0.014 (2) | −0.0008 (15) | 0.002 (2) | 0.002 (2) |
O5 | 0.015 (2) | 0.010 (2) | 0.011 (2) | −0.0021 (17) | 0.006 (2) | −0.002 (2) |
O6 | 0.013 (2) | 0.016 (2) | 0.017 (3) | −0.0044 (19) | −0.008 (3) | 0.007 (2) |
O7 | 0.006 (3) | 0.005 (3) | 0.014 (4) | 0.002 (3) | 0.000 | 0.000 |
O8 | 0.018 (4) | 0.026 (4) | 0.013 (4) | 0.004 (4) | 0.000 | 0.000 |
Pr—O7 | 2.405 (8) | Mo2—O4xiii | 2.124 (5) |
Pr—O5i | 2.443 (6) | Mo2—Mo4v | 2.6384 (11) |
Pr—O5ii | 2.443 (6) | Mo2—Mo1xiii | 2.7031 (8) |
Pr—O6iii | 2.552 (6) | Mo2—Mo1xiv | 2.7163 (8) |
Pr—O6iv | 2.552 (6) | Mo2—Mo3vii | 2.7306 (8) |
Pr—O4v | 2.661 (5) | Mo2—Mo3 | 2.7864 (8) |
Pr—O4vi | 2.661 (5) | Mo2—Prxv | 3.5808 (6) |
Pr—O2 | 3.038 (7) | Mo2—Prxvi | 3.8742 (6) |
Pr—O2vii | 3.038 (7) | Mo3—O1viii | 2.027 (6) |
Pr—O8 | 3.088 (10) | Mo3—O4xvii | 2.040 (6) |
Pr—O3 | 3.106 (6) | Mo3—O6vii | 2.077 (6) |
Pr—O3vii | 3.106 (6) | Mo3—O5 | 2.090 (5) |
Pr—Mo2iii | 3.5808 (6) | Mo3—O8 | 2.116 (7) |
Pr—Mo2iv | 3.5808 (6) | Mo3—Mo1xiii | 2.7244 (9) |
Pr—Mo3i | 3.6532 (6) | Mo3—Mo4vi | 2.7254 (11) |
Pr—Mo3ii | 3.6532 (6) | Mo3—Mo2vii | 2.7306 (8) |
Pr—Mo2i | 3.8742 (6) | Mo3—Mo4v | 2.7499 (10) |
Mo1—O7 | 1.933 (6) | Mo3—Mo3vii | 2.8141 (11) |
Mo1—O2i | 1.988 (6) | Mo3—Prxvi | 3.6532 (6) |
Mo1—O3iv | 1.992 (6) | Mo3—Mo4xviii | 3.6539 (10) |
Mo1—O4viii | 2.051 (6) | Mo3—Mo1xii | 3.6948 (8) |
Mo1—O1iv | 2.078 (6) | Mo4—O8xix | 2.0066 (18) |
Mo1—Mo1vii | 2.6784 (12) | Mo4—O1xix | 2.012 (5) |
Mo1—Mo2ix | 2.7031 (8) | Mo4—O6xix | 2.017 (7) |
Mo1—Mo2x | 2.7163 (8) | Mo4—O5xix | 2.026 (7) |
Mo1—Mo3ix | 2.7244 (9) | Mo4—O3xix | 2.063 (6) |
Mo1—Mo4xi | 3.0761 (10) | Mo4—O2xix | 2.077 (6) |
Mo1—Mo4viii | 3.6907 (10) | Mo4—Mo2xix | 2.6384 (11) |
Mo1—Mo3i | 3.6948 (8) | Mo4—Mo3iii | 2.7254 (11) |
Mo2—O2xii | 2.018 (7) | Mo4—Mo3xix | 2.7499 (10) |
Mo2—O6 | 2.031 (6) | Mo4—Mo1xx | 3.0761 (10) |
Mo2—O3vi | 2.043 (6) | Mo4—Mo3xxi | 3.6539 (10) |
Mo2—O5 | 2.064 (6) | Mo4—Mo1xxii | 3.6907 (10) |
O7—Mo1—O2i | 91.5 (2) | O1viii—Mo3—O5 | 88.2 (2) |
O7—Mo1—O3iv | 92.36 (17) | O4xvii—Mo3—O5 | 81.7 (2) |
O2i—Mo1—O3iv | 171.6 (2) | O6vii—Mo3—O5 | 172.2 (2) |
O7—Mo1—O4viii | 174.0 (2) | O1viii—Mo3—O8 | 88.7 (2) |
O2i—Mo1—O4viii | 85.9 (2) | O4xvii—Mo3—O8 | 172.6 (2) |
O3iv—Mo1—O4viii | 89.6 (2) | O6vii—Mo3—O8 | 93.62 (19) |
O7—Mo1—O1iv | 87.8 (2) | O5—Mo3—O8 | 93.02 (19) |
O2i—Mo1—O1iv | 90.8 (3) | O8xix—Mo4—O1xix | 167.2 (3) |
O3iv—Mo1—O1iv | 81.8 (2) | O8xix—Mo4—O6xix | 98.9 (2) |
O4viii—Mo1—O1iv | 86.9 (2) | O1xix—Mo4—O6xix | 87.4 (2) |
O2xii—Mo2—O6 | 172.8 (2) | O8xix—Mo4—O5xix | 98.3 (2) |
O2xii—Mo2—O3vi | 93.5 (3) | O1xix—Mo4—O5xix | 91.4 (2) |
O6—Mo2—O3vi | 84.1 (2) | O6xix—Mo4—O5xix | 99.6 (2) |
O2xii—Mo2—O5 | 83.9 (3) | O8xix—Mo4—O3xix | 87.2 (3) |
O6—Mo2—O5 | 97.9 (3) | O1xix—Mo4—O3xix | 81.7 (2) |
O3vi—Mo2—O5 | 175.1 (2) | O6xix—Mo4—O3xix | 89.8 (2) |
O2xii—Mo2—O4xiii | 91.4 (2) | O5xix—Mo4—O3xix | 168.1 (2) |
O6—Mo2—O4xiii | 81.7 (2) | O8xix—Mo4—O2xix | 83.2 (3) |
O3vi—Mo2—O4xiii | 85.2 (2) | O1xix—Mo4—O2xix | 88.8 (2) |
O5—Mo2—O4xiii | 90.7 (2) | O6xix—Mo4—O2xix | 170.7 (2) |
O1viii—Mo3—O4xvii | 86.1 (2) | O5xix—Mo4—O2xix | 89.0 (3) |
O1viii—Mo3—O6vii | 87.7 (2) | O3xix—Mo4—O2xix | 81.3 (2) |
O4xvii—Mo3—O6vii | 91.4 (2) |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) x−1/2, −y, z−1/2; (iii) −x, −y+1/2, z−1/2; (iv) x, y−1/2, z−1/2; (v) x, y−1/2, z+1/2; (vi) −x, −y+1/2, z+1/2; (vii) −x, −y, z; (viii) −x+1/2, y−1/2, z; (ix) x, y, z−1; (x) −x, −y, z−1; (xi) x, y−1, z; (xii) −x+1/2, y, z+1/2; (xiii) x, y, z+1; (xiv) −x, −y, z+1; (xv) x, y+1/2, z+1/2; (xvi) x+1/2, −y, z+1/2; (xvii) −x+1/2, y−1/2, z+1; (xviii) −x+1/2, y−1, z+1/2; (xix) x, y+1/2, z−1/2; (xx) x, y+1, z; (xxi) −x+1/2, y+1, z−1/2; (xxii) −x+1/2, y+1/2, z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register