A novel (3,9)-connected lanthanide-based network of lanthanum trinitrite, La(NO2)3, was synthesized and characterized by single-crystal X-ray diffraction. The central LaIII atom is coordinated by nine O atoms from nine nitrite anions. These unidentate O atoms are arranged in a capped trigonal prism. The resulting [LaO9] polyhedron shows 3m symmetry.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 273 K
- R factor = 0.013
- wR factor = 0.029
- Data-to-parameter ratio = 8.9
checkCIF/PLATON results
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Alert level G
REFLT03_ALERT_4_G 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.
From the CIF: _diffrn_reflns_theta_max 26.99
From the CIF: _reflns_number_total 195
Count of symmetry unique reflns 114
Completeness (_total/calc) 171.05%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 81
Fraction of Friedel pairs measured 0.711
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
0 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Lanthanum(III) nitrite
top
Crystal data top
La(NO2)3 | Dx = 3.447 Mg m−3 |
Mr = 276.94 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 746 reflections |
Hall symbol: R 3 -2" | θ = 3.8–28.0° |
a = 10.6226 (19) Å | µ = 7.99 mm−1 |
c = 4.0954 (15) Å | T = 273 K |
V = 400.21 (18) Å3 | Needle, colorless |
Z = 3 | 0.12 × 0.01 × 0.01 mm |
F(000) = 378 | |
Data collection top
Bruker SMART APEX 2000 diffractometer | 195 independent reflections |
Radiation source: fine-focus sealed tube | 195 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 27.0°, θmin = 3.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.447, Tmax = 0.924 | k = −10→13 |
738 measured reflections | l = −3→5 |
Refinement top
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) + (0.0156P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.029 | (Δ/σ)max = 0.025 |
S = 1.14 | Δρmax = 0.35 e Å−3 |
195 reflections | Δρmin = −0.45 e Å−3 |
22 parameters | Absolute structure: Flack (1983), 40 Friedel pairs |
1 restraint | Absolute structure parameter: 0.06 (5) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
La1 | 0.0000 | 0.0000 | 0.2723 | 0.00817 (6) | |
O1 | −0.3960 (3) | −0.19798 (15) | 0.9551 (7) | 0.0199 (7) | |
O2 | −0.1705 (3) | −0.08523 (13) | 0.7754 (7) | 0.0125 (5) | |
N1 | −0.3069 (4) | −0.15346 (18) | 0.7324 (10) | 0.0218 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
La1 | 0.00908 (7) | 0.00908 (7) | 0.00635 (12) | 0.00454 (3) | 0.000 | 0.000 |
O1 | 0.0113 (11) | 0.0282 (11) | 0.0146 (17) | 0.0057 (6) | 0.0032 (11) | 0.0016 (5) |
O2 | 0.0066 (10) | 0.0155 (9) | 0.0124 (13) | 0.0033 (5) | 0.0006 (9) | 0.0003 (4) |
N1 | 0.0188 (15) | 0.0255 (12) | 0.0189 (18) | 0.0094 (8) | 0.0004 (13) | 0.0002 (6) |
Geometric parameters (Å, º) top
La1—O1i | 2.491 (3) | La1—O2 | 2.589 (3) |
La1—O1ii | 2.491 (3) | La1—La1iv | 4.0954 (15) |
La1—O1iii | 2.491 (3) | La1—La1ix | 4.0954 (15) |
La1—O2iv | 2.569 (3) | O1—N1 | 1.226 (5) |
La1—O2v | 2.569 (3) | O1—La1x | 2.491 (3) |
La1—O2vi | 2.569 (3) | O2—N1 | 1.268 (4) |
La1—O2vii | 2.589 (3) | O2—La1ix | 2.569 (3) |
La1—O2viii | 2.589 (3) | | |
| | | |
O1i—La1—O1ii | 119.932 (6) | O1iii—La1—O2 | 71.11 (6) |
O1i—La1—O1iii | 119.930 (6) | O2iv—La1—O2 | 105.11 (9) |
O1ii—La1—O1iii | 119.930 (6) | O2v—La1—O2 | 144.60 (4) |
O1i—La1—O2iv | 73.50 (6) | O2vi—La1—O2 | 144.60 (4) |
O1ii—La1—O2iv | 129.13 (9) | O2vii—La1—O2 | 63.27 (10) |
O1iii—La1—O2iv | 73.50 (6) | O2viii—La1—O2 | 63.27 (10) |
O1i—La1—O2v | 73.50 (6) | O1i—La1—La1iv | 91.52 (6) |
O1ii—La1—O2v | 73.50 (6) | O1ii—La1—La1iv | 91.52 (6) |
O1iii—La1—O2v | 129.13 (9) | O1iii—La1—La1iv | 91.52 (6) |
O2iv—La1—O2v | 63.82 (10) | O2iv—La1—La1iv | 37.61 (6) |
O1i—La1—O2vi | 129.13 (9) | O2v—La1—La1iv | 37.61 (6) |
O1ii—La1—O2vi | 73.50 (6) | O2vi—La1—La1iv | 37.61 (6) |
O1iii—La1—O2vi | 73.50 (6) | O2vii—La1—La1iv | 142.72 (6) |
O2iv—La1—O2vi | 63.82 (10) | O2viii—La1—La1iv | 142.72 (6) |
O2v—La1—O2vi | 63.82 (10) | O2—La1—La1iv | 142.72 (6) |
O1i—La1—O2vii | 125.76 (9) | O1i—La1—La1ix | 88.48 (6) |
O1ii—La1—O2vii | 71.11 (6) | O1ii—La1—La1ix | 88.48 (6) |
O1iii—La1—O2vii | 71.11 (6) | O1iii—La1—La1ix | 88.48 (6) |
O2iv—La1—O2vii | 144.60 (4) | O2iv—La1—La1ix | 142.39 (6) |
O2v—La1—O2vii | 144.60 (4) | O2v—La1—La1ix | 142.39 (6) |
O2vi—La1—O2vii | 105.11 (9) | O2vi—La1—La1ix | 142.39 (6) |
O1i—La1—O2viii | 71.11 (6) | O2vii—La1—La1ix | 37.28 (6) |
O1ii—La1—O2viii | 71.11 (6) | O2viii—La1—La1ix | 37.28 (6) |
O1iii—La1—O2viii | 125.76 (9) | O2—La1—La1ix | 37.28 (6) |
O2iv—La1—O2viii | 144.60 (4) | La1iv—La1—La1ix | 180.0 |
O2v—La1—O2viii | 105.11 (9) | N1—O1—La1x | 130.4 (2) |
O2vi—La1—O2viii | 144.60 (4) | N1—O2—La1ix | 135.6 (3) |
O2vii—La1—O2viii | 63.27 (10) | N1—O2—La1 | 119.3 (2) |
O1i—La1—O2 | 71.11 (6) | La1ix—O2—La1 | 105.11 (9) |
O1ii—La1—O2 | 125.76 (9) | O1—N1—O2 | 124.0 (4) |
Symmetry codes: (i) −x+y−1/3, −x−2/3, z−2/3; (ii) x+2/3, y+1/3, z−2/3; (iii) −y−1/3, x−y+1/3, z−2/3; (iv) x, y, z−1; (v) −y, x−y, z−1; (vi) −x+y, −x, z−1; (vii) −x+y, −x, z; (viii) −y, x−y, z; (ix) x, y, z+1; (x) x−2/3, y−1/3, z+2/3. |