The crystal structure of Li
3P has been reinvestigated and confirmed by single-crystal data. The structure is built of Li
+ and P
3- ions stacked in two kinds of layers perpendicular to the
c axis. Atoms Li1, Li2 and P reside at positions of
m2, 3
m and
2 site symmetry, respectively. The only free parameter,
z, for Li2 is found to be 0.5839 (4).
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 167 K
- Mean () = 0.000 Å
- R factor = 0.015
- wR factor = 0.034
- Data-to-parameter ratio = 8.6
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91
| Author Response: There is only one free positional parameter for one atom, Li2, in the
three atom asymmetric unit at 1/3,2/3,z. We determine z = 0.5839(4). This value
would not change if we included the one uncollected reflections (resolution
range 1.0 \~ 0.9). So we feel that the test is not important for this case.
|
Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.62
PLAT731_ALERT_1_C Bond Calc 2.4414(4), Rep 2.44138(17) ...... 2.35 su-Ra
LI1 -P1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 2.4414(4), Rep 2.44138(18) ...... 2.22 su-Ra
LI1 -P1 1.555 1.565
PLAT731_ALERT_1_C Bond Calc 2.4414(4), Rep 2.44138(17) ...... 2.35 su-Ra
LI1 -P1 1.555 1.455
PLAT731_ALERT_1_C Bond Calc 2.4414(4), Rep 2.44138(17) ...... 2.35 su-Ra
P1 -LI1 1.555 1.655
PLAT731_ALERT_1_C Bond Calc 2.4414(4), Rep 2.44138(17) ...... 2.35 su-Ra
P1 -LI1 1.555 1.545
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
6 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
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2; data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).
Crystal data top
Li3P | Dx = 1.470 Mg m−3 |
Mr = 51.79 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 196 reflections |
Hall symbol: -P 6c 2c | θ = 3.3–40.2° |
a = 4.2286 (3) Å | µ = 0.71 mm−1 |
c = 7.5566 (13) Å | T = 167 K |
V = 117.02 (2) Å3 | Block, red |
Z = 2 | 0.07 × 0.07 × 0.06 mm |
F(000) = 48 | |
Data collection top
Bruker APEX II diffractometer | 69 independent reflections |
Radiation source: fine-focus sealed tube | 65 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 27.6°, θmin = 5.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −5→5 |
Tmin = 0.952, Tmax = 0.959 | k = −5→5 |
965 measured reflections | l = −9→9 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.015 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.034 | w = 1/[σ2(Fo2) + (0.0226P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.23 | (Δ/σ)max < 0.001 |
69 reflections | Δρmax = 0.15 e Å−3 |
8 parameters | Δρmin = −0.12 e Å−3 |
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 | |
Li1 | 0.0000 | 1.0000 | 0.2500 | 0.0170 (8) | |
Li2 | 0.3333 | 0.6667 | 0.5839 (4) | 0.0164 (7) | |
P1 | 0.3333 | 0.6667 | 0.2500 | 0.0079 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Li1 | 0.0122 (11) | 0.0122 (11) | 0.027 (2) | 0.0061 (6) | 0.000 | 0.000 |
Li2 | 0.0192 (11) | 0.0192 (11) | 0.0109 (14) | 0.0096 (5) | 0.000 | 0.000 |
P1 | 0.0079 (3) | 0.0079 (3) | 0.0080 (4) | 0.00394 (14) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Li1—P1 | 2.4414 (2) | Li2—Li1vi | 2.7451 (14) |
Li1—P1i | 2.4414 (2) | Li2—Li1viii | 2.7451 (14) |
Li1—P1ii | 2.4414 (2) | Li2—P1xii | 2.7451 (14) |
Li1—Li2iii | 2.7451 (14) | Li2—Li2viii | 2.751 (3) |
Li1—Li2iv | 2.7451 (14) | Li2—Li2vi | 2.751 (3) |
Li1—Li2v | 2.7451 (14) | Li2—Li2xii | 2.751 (3) |
Li1—Li2vi | 2.7451 (14) | Li2—Li1xiii | 3.511 (2) |
Li1—Li2vii | 2.7451 (14) | P1—Li1xiv | 2.4414 (2) |
Li1—Li2viii | 2.7451 (14) | P1—Li1xiii | 2.4414 (2) |
Li1—Li2ix | 3.511 (2) | P1—Li2x | 2.523 (3) |
Li1—Li2x | 3.511 (2) | P1—Li2v | 2.7451 (14) |
Li1—Li2i | 3.511 (2) | P1—Li2vi | 2.7451 (14) |
Li2—Li2xi | 2.510 (6) | P1—Li2viii | 2.7451 (14) |
Li2—P1 | 2.523 (3) | P1—Li2vii | 2.7451 (14) |
Li2—P1vi | 2.7451 (14) | P1—Li2xii | 2.7451 (14) |
Li2—P1viii | 2.7451 (14) | P1—Li2xv | 2.7451 (14) |
Li2—Li1iv | 2.7451 (14) | | |
| | | |
P1—Li1—P1i | 120.0 | Li2xi—Li2—Li2viii | 117.45 (11) |
P1—Li1—P1ii | 120.0 | P1—Li2—Li2viii | 62.55 (11) |
P1i—Li1—P1ii | 120.0 | P1vi—Li2—Li2viii | 127.256 (14) |
P1—Li1—Li2iii | 152.79 (6) | P1viii—Li2—Li2viii | 54.66 (6) |
P1i—Li1—Li2iii | 63.597 (14) | Li1iv—Li2—Li2viii | 79.41 (3) |
P1ii—Li1—Li2iii | 63.597 (14) | Li1vi—Li2—Li2viii | 179.75 (17) |
P1—Li1—Li2iv | 152.79 (6) | Li1viii—Li2—Li2viii | 79.41 (3) |
P1i—Li1—Li2iv | 63.597 (14) | P1xii—Li2—Li2viii | 127.256 (14) |
P1ii—Li1—Li2iv | 63.597 (14) | Li2xi—Li2—Li2vi | 117.45 (11) |
Li2iii—Li1—Li2iv | 54.41 (11) | P1—Li2—Li2vi | 62.55 (11) |
P1—Li1—Li2v | 63.597 (14) | P1vi—Li2—Li2vi | 54.66 (6) |
P1i—Li1—Li2v | 152.79 (6) | P1viii—Li2—Li2vi | 127.256 (14) |
P1ii—Li1—Li2v | 63.597 (14) | Li1iv—Li2—Li2vi | 79.41 (3) |
Li2iii—Li1—Li2v | 100.75 (7) | Li1vi—Li2—Li2vi | 79.41 (3) |
Li2iv—Li1—Li2v | 127.19 (3) | Li1viii—Li2—Li2vi | 179.75 (17) |
P1—Li1—Li2vi | 63.597 (14) | P1xii—Li2—Li2vi | 127.256 (14) |
P1i—Li1—Li2vi | 63.597 (14) | Li2viii—Li2—Li2vi | 100.44 (14) |
P1ii—Li1—Li2vi | 152.79 (6) | Li2xi—Li2—Li2xii | 117.45 (11) |
Li2iii—Li1—Li2vi | 127.19 (3) | P1—Li2—Li2xii | 62.55 (11) |
Li2iv—Li1—Li2vi | 100.75 (7) | P1vi—Li2—Li2xii | 127.256 (14) |
Li2v—Li1—Li2vi | 127.19 (3) | P1viii—Li2—Li2xii | 127.256 (14) |
P1—Li1—Li2vii | 63.597 (14) | Li1iv—Li2—Li2xii | 179.75 (17) |
P1i—Li1—Li2vii | 63.597 (14) | Li1vi—Li2—Li2xii | 79.41 (3) |
P1ii—Li1—Li2vii | 152.79 (6) | Li1viii—Li2—Li2xii | 79.41 (3) |
Li2iii—Li1—Li2vii | 100.75 (7) | P1xii—Li2—Li2xii | 54.66 (6) |
Li2iv—Li1—Li2vii | 127.19 (3) | Li2viii—Li2—Li2xii | 100.44 (14) |
Li2v—Li1—Li2vii | 100.75 (7) | Li2vi—Li2—Li2xii | 100.44 (14) |
Li2vi—Li1—Li2vii | 54.41 (11) | Li2xi—Li2—Li1xiii | 135.95 (3) |
P1—Li1—Li2viii | 63.597 (14) | P1—Li2—Li1xiii | 44.05 (3) |
P1i—Li1—Li2viii | 152.79 (6) | P1vi—Li2—Li1xiii | 161.26 (9) |
P1ii—Li1—Li2viii | 63.597 (14) | P1viii—Li2—Li1xiii | 91.11 (2) |
Li2iii—Li1—Li2viii | 127.19 (3) | Li1iv—Li2—Li1xiii | 129.63 (3) |
Li2iv—Li1—Li2viii | 100.75 (7) | Li1vi—Li2—Li1xiii | 129.63 (3) |
Li2v—Li1—Li2viii | 54.41 (11) | Li1viii—Li2—Li1xiii | 73.15 (2) |
Li2vi—Li1—Li2viii | 100.75 (7) | P1xii—Li2—Li1xiii | 91.11 (2) |
Li2vii—Li1—Li2viii | 127.19 (3) | Li2viii—Li2—Li1xiii | 50.22 (7) |
P1—Li1—Li2ix | 110.345 (13) | Li2vi—Li2—Li1xiii | 106.60 (14) |
P1i—Li1—Li2ix | 110.345 (13) | Li2xii—Li2—Li1xiii | 50.22 (7) |
P1ii—Li1—Li2ix | 45.95 (3) | Li1—P1—Li1xiv | 120.0 |
Li2iii—Li1—Li2ix | 50.37 (3) | Li1—P1—Li1xiii | 120.0 |
Li2iv—Li1—Li2ix | 91.11 (2) | Li1xiv—P1—Li1xiii | 120.0 |
Li2v—Li1—Li2ix | 50.37 (3) | Li1—P1—Li2x | 90.0 |
Li2vi—Li1—Li2ix | 161.26 (9) | Li1xiv—P1—Li2x | 90.0 |
Li2vii—Li1—Li2ix | 106.85 (2) | Li1xiii—P1—Li2x | 90.0 |
Li2viii—Li1—Li2ix | 91.11 (2) | Li1—P1—Li2 | 90.0 |
P1—Li1—Li2x | 45.95 (3) | Li1xiv—P1—Li2 | 90.0 |
P1i—Li1—Li2x | 110.345 (13) | Li1xiii—P1—Li2 | 90.0 |
P1ii—Li1—Li2x | 110.345 (13) | Li2x—P1—Li2 | 180.0 |
Li2iii—Li1—Li2x | 106.85 (2) | Li1—P1—Li2v | 63.597 (14) |
Li2iv—Li1—Li2x | 161.26 (9) | Li1xiv—P1—Li2v | 152.79 (6) |
Li2v—Li1—Li2x | 50.37 (3) | Li1xiii—P1—Li2v | 63.597 (14) |
Li2vi—Li1—Li2x | 91.11 (2) | Li2x—P1—Li2v | 62.79 (6) |
Li2vii—Li1—Li2x | 50.37 (3) | Li2—P1—Li2v | 117.21 (6) |
Li2viii—Li1—Li2x | 91.11 (2) | Li1—P1—Li2vi | 63.597 (14) |
Li2ix—Li1—Li2x | 74.05 (5) | Li1xiv—P1—Li2vi | 63.597 (14) |
P1—Li1—Li2i | 110.345 (13) | Li1xiii—P1—Li2vi | 152.79 (6) |
P1i—Li1—Li2i | 45.95 (3) | Li2x—P1—Li2vi | 117.21 (6) |
P1ii—Li1—Li2i | 110.345 (13) | Li2—P1—Li2vi | 62.79 (6) |
Li2iii—Li1—Li2i | 91.11 (2) | Li2v—P1—Li2vi | 127.19 (3) |
Li2iv—Li1—Li2i | 50.37 (3) | Li1—P1—Li2viii | 63.597 (14) |
Li2v—Li1—Li2i | 161.26 (9) | Li1xiv—P1—Li2viii | 152.79 (6) |
Li2vi—Li1—Li2i | 50.37 (3) | Li1xiii—P1—Li2viii | 63.597 (14) |
Li2vii—Li1—Li2i | 91.11 (2) | Li2x—P1—Li2viii | 117.21 (6) |
Li2viii—Li1—Li2i | 106.85 (2) | Li2—P1—Li2viii | 62.79 (6) |
Li2ix—Li1—Li2i | 139.31 (3) | Li2v—P1—Li2viii | 54.41 (11) |
Li2x—Li1—Li2i | 139.31 (3) | Li2vi—P1—Li2viii | 100.75 (7) |
Li2xi—Li2—P1 | 180.000 (1) | Li1—P1—Li2vii | 63.597 (14) |
Li2xi—Li2—P1vi | 62.79 (6) | Li1xiv—P1—Li2vii | 63.597 (14) |
P1—Li2—P1vi | 117.21 (6) | Li1xiii—P1—Li2vii | 152.79 (6) |
Li2xi—Li2—P1viii | 62.79 (6) | Li2x—P1—Li2vii | 62.79 (6) |
P1—Li2—P1viii | 117.21 (6) | Li2—P1—Li2vii | 117.21 (6) |
P1vi—Li2—P1viii | 100.75 (7) | Li2v—P1—Li2vii | 100.75 (7) |
Li2xi—Li2—Li1iv | 62.79 (6) | Li2vi—P1—Li2vii | 54.41 (11) |
P1—Li2—Li1iv | 117.21 (6) | Li2viii—P1—Li2vii | 127.19 (3) |
P1vi—Li2—Li1iv | 52.81 (3) | Li1—P1—Li2xii | 152.79 (6) |
P1viii—Li2—Li1iv | 52.81 (3) | Li1xiv—P1—Li2xii | 63.597 (14) |
Li2xi—Li2—Li1vi | 62.79 (6) | Li1xiii—P1—Li2xii | 63.597 (14) |
P1—Li2—Li1vi | 117.21 (6) | Li2x—P1—Li2xii | 117.21 (6) |
P1vi—Li2—Li1vi | 52.81 (3) | Li2—P1—Li2xii | 62.79 (6) |
P1viii—Li2—Li1vi | 125.59 (11) | Li2v—P1—Li2xii | 127.19 (3) |
Li1iv—Li2—Li1vi | 100.75 (7) | Li2vi—P1—Li2xii | 100.75 (7) |
Li2xi—Li2—Li1viii | 62.79 (6) | Li2viii—P1—Li2xii | 100.75 (7) |
P1—Li2—Li1viii | 117.21 (6) | Li2vii—P1—Li2xii | 127.19 (3) |
P1vi—Li2—Li1viii | 125.59 (11) | Li1—P1—Li2xv | 152.79 (6) |
P1viii—Li2—Li1viii | 52.81 (3) | Li1xiv—P1—Li2xv | 63.597 (14) |
Li1iv—Li2—Li1viii | 100.75 (7) | Li1xiii—P1—Li2xv | 63.597 (14) |
Li1vi—Li2—Li1viii | 100.75 (7) | Li2x—P1—Li2xv | 62.79 (6) |
Li2xi—Li2—P1xii | 62.79 (6) | Li2—P1—Li2xv | 117.21 (6) |
P1—Li2—P1xii | 117.21 (6) | Li2v—P1—Li2xv | 100.75 (7) |
P1vi—Li2—P1xii | 100.75 (7) | Li2vi—P1—Li2xv | 127.19 (3) |
P1viii—Li2—P1xii | 100.75 (7) | Li2viii—P1—Li2xv | 127.19 (3) |
Li1iv—Li2—P1xii | 125.59 (11) | Li2vii—P1—Li2xv | 100.75 (7) |
Li1vi—Li2—P1xii | 52.81 (3) | Li2xii—P1—Li2xv | 54.41 (11) |
Li1viii—Li2—P1xii | 52.81 (3) | | |
Symmetry codes: (i) x, y+1, z; (ii) x−1, y, z; (iii) −x, −y+2, z−1/2; (iv) −x, −y+2, −z+1; (v) −x, −y+1, z−1/2; (vi) −x+1, −y+2, −z+1; (vii) −x+1, −y+2, z−1/2; (viii) −x, −y+1, −z+1; (ix) x−1, y, −z+1/2; (x) x, y, −z+1/2; (xi) x, y, −z+3/2; (xii) −x+1, −y+1, −z+1; (xiii) x, y−1, z; (xiv) x+1, y, z; (xv) −x+1, −y+1, z−1/2. |