Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680501216X/mg6032sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680501216X/mg6032Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (d-O) = 0.008 Å
- H-atom completeness 1%
- R factor = 0.048
- wR factor = 0.143
- Data-to-parameter ratio = 27.4
checkCIF/PLATON results
No syntax errors found
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 687.08 TEST: Calculate formula weight from _atom_site_* atom mass num sum H 1.01 0.00 0.00 I 126.90 3.00 380.71 Nd 144.24 1.00 144.24 O 16.00 9.00 143.99 Calculated formula weight 668.95 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 687.08 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Nd PLAT431_ALERT_2_C Short Inter HL..A Contact I1 .. O4 .. 3.45 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H18 I3 Nd1 O9 Atom count from the _atom_site data: I3 Nd1 O9 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum H18 I3 Nd O9 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 36.00 0.00 36.00 I 6.00 6.00 0.00 Nd 2.00 2.00 0.00 O 18.00 18.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: Please provide missing details.
NdI3·9H2O | Dx = 2.723 Mg m−3 |
Mr = 687.08 | Melting point: not measured K |
Orthorhombic, Pmmn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ab 2a | Cell parameters from 1391 reflections |
a = 11.6604 (15) Å | θ = 1.9–28.0° |
b = 8.0103 (11) Å | µ = 8.64 mm−1 |
c = 8.9702 (16) Å | T = 278 K |
V = 837.8 (2) Å3 | Prismatic, pale yellow |
Z = 2 | 0.5 × 0.5 × 0.2 mm |
F(000) = 618 |
Stoe IPDS-I diffractometer | 1123 independent reflections |
Radiation source: fine-focus sealed tube | 843 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.095 |
2deg φ scans | θmax = 28.0°, θmin = 3.4° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2002) and X-SHAPE (Stoe & Cie, 1999)] | h = −14→15 |
Tmin = 0.058, Tmax = 0.509 | k = −9→10 |
7674 measured reflections | l = −11→11 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not defined |
R[F2 > 2σ(F2)] = 0.048 | w = 1/[σ2(Fo2) + (0.1174P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.143 | (Δ/σ)max < 0.001 |
S = 1.02 | Δρmax = 1.22 e Å−3 |
1123 reflections | Δρmin = −2.56 e Å−3 |
41 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.084 (7) |
Primary atom site location: structure-invariant direct 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 | ||
Nd | 0.2500 | 0.7500 | 0.66846 (8) | 0.0485 (3) | |
I1 | 0.49778 (5) | 0.2500 | 0.82838 (9) | 0.0692 (3) | |
I2 | 0.7500 | 0.7500 | 0.70705 (16) | 0.0690 (4) | |
O1 | 0.3791 (4) | 0.5273 (8) | 0.5654 (7) | 0.0708 (15) | |
O2 | 0.2500 | 0.7500 | 0.3877 (13) | 0.069 (3) | |
O3 | 0.2500 | 0.9567 (12) | 0.8798 (11) | 0.081 (2) | |
O4 | 0.4418 (6) | 0.7500 | 0.7948 (10) | 0.076 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd | 0.0369 (4) | 0.0686 (5) | 0.0400 (4) | 0.000 | 0.000 | 0.000 |
I1 | 0.0688 (5) | 0.0909 (7) | 0.0481 (5) | 0.000 | −0.0025 (3) | 0.000 |
I2 | 0.0583 (5) | 0.0855 (8) | 0.0632 (7) | 0.000 | 0.000 | 0.000 |
O1 | 0.058 (2) | 0.093 (4) | 0.061 (3) | 0.016 (2) | −0.002 (2) | −0.005 (3) |
O2 | 0.064 (5) | 0.095 (8) | 0.049 (6) | 0.000 | 0.000 | 0.000 |
O3 | 0.063 (3) | 0.110 (7) | 0.071 (5) | 0.000 | 0.000 | −0.026 (5) |
O4 | 0.058 (3) | 0.117 (7) | 0.052 (4) | 0.000 | −0.010 (3) | 0.000 |
Nd—O4 | 2.507 (7) | Nd—O1i | 2.511 (5) |
Nd—O4i | 2.507 (7) | Nd—O3 | 2.517 (9) |
Nd—O1ii | 2.511 (5) | Nd—O3i | 2.517 (9) |
Nd—O1 | 2.511 (5) | Nd—O2 | 2.519 (12) |
Nd—O1iii | 2.511 (5) | ||
O4—Nd—O4i | 126.3 (4) | O1—Nd—O3 | 138.15 (17) |
O4—Nd—O1ii | 134.53 (14) | O1iii—Nd—O3 | 79.0 (2) |
O4i—Nd—O1ii | 68.39 (18) | O1i—Nd—O3 | 79.0 (2) |
O4—Nd—O1 | 68.39 (18) | O4—Nd—O3i | 70.10 (16) |
O4i—Nd—O1 | 134.53 (14) | O4i—Nd—O3i | 70.10 (16) |
O1ii—Nd—O1 | 73.7 (3) | O1ii—Nd—O3i | 79.0 (2) |
O4—Nd—O1iii | 68.39 (18) | O1—Nd—O3i | 79.0 (2) |
O4i—Nd—O1iii | 134.53 (14) | O1iii—Nd—O3i | 138.15 (17) |
O1ii—Nd—O1iii | 136.8 (3) | O1i—Nd—O3i | 138.15 (17) |
O1—Nd—O1iii | 90.6 (3) | O3—Nd—O3i | 82.3 (5) |
O4—Nd—O1i | 134.53 (14) | O4—Nd—O2 | 116.9 (2) |
O4i—Nd—O1i | 68.39 (18) | O4i—Nd—O2 | 116.9 (2) |
O1ii—Nd—O1i | 90.6 (3) | O1ii—Nd—O2 | 68.38 (14) |
O1—Nd—O1i | 136.8 (3) | O1—Nd—O2 | 68.38 (14) |
O1iii—Nd—O1i | 73.7 (3) | O1iii—Nd—O2 | 68.38 (14) |
O4—Nd—O3 | 70.10 (16) | O1i—Nd—O2 | 68.38 (14) |
O4i—Nd—O3 | 70.10 (16) | O3—Nd—O2 | 138.9 (2) |
O1ii—Nd—O3 | 138.15 (17) | O3i—Nd—O2 | 138.9 (2) |
Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, y, z; (iii) x, −y+3/2, z. |
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