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The structure of trisodium phosphide, Na
3P, known from X-ray powder diffraction data, has been refined based on single-crystal data. The compound crystallizes in the hexagonal
A3B (
A = alkali metal and
B = group 15 element) structure type and is isotypic with the homologous potassium phase. The framework is built of Na
+ and P
3- ions arranged in two kinds of layers perpendicular to the
c axis. Two of the Na atoms and the P atom reside at positions of
m2 (2
b), 3
m (4
f) and
m2 (2
c) site symmetry, respectively.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 165 K
- Mean () = 0.000 Å
- R factor = 0.039
- wR factor = 0.084
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
| Author Response: The measured fraction is close to one, but below by only 7 %.
However, the ratio of independent reflections to the number of independent
parameters is greater than 17. There is only one free positional parameter
for one atom, Na(2), in the three atom asymmetric unit at 1/3,2/3,z. We
determine z = 0.5806(2). This value would not change if we included the
few
uncollected reflections. So we feel that the test is not important for
this
case.
|
Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).
Crystal data top
Na3P | Dx = 1.779 Mg m−3 |
Mr = 99.94 | 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 = 4.9512 (5) Å | µ = 0.81 mm−1 |
c = 8.7874 (13) Å | T = 165 K |
V = 186.56 (4) Å3 | Block, red |
Z = 2 | 0.10 × 0.10 × 0.05 mm |
F(000) = 96 | |
Data collection top
Bruker SMART 1K CCD area-detector diffractometer | 155 independent reflections |
Radiation source: fine-focus sealed tube | 115 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
φ and ω scans | θmax = 32.2°, θmin = 4.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1999) | h = −7→7 |
Tmin = 0.920, Tmax = 0.960 | k = −7→7 |
1495 measured reflections | l = −12→13 |
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)] = 0.039 | w = 1/[σ2(Fo2) + (0.0321P)2 + 0.2162P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.084 | (Δ/σ)max < 0.001 |
S = 1.13 | Δρmax = 0.41 e Å−3 |
155 reflections | Δρmin = −0.49 e Å−3 |
9 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.16 (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 | |
Na1 | 0.0000 | 0.0000 | 0.2500 | 0.0360 (9) | |
Na2 | 0.3333 | 0.6667 | 0.58062 (18) | 0.0379 (6) | |
P | 0.3333 | 0.6667 | 0.2500 | 0.0095 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0127 (8) | 0.0127 (8) | 0.083 (3) | 0.0063 (4) | 0.000 | 0.000 |
Na2 | 0.0501 (9) | 0.0501 (9) | 0.0134 (8) | 0.0251 (4) | 0.000 | 0.000 |
P | 0.0088 (4) | 0.0088 (4) | 0.0109 (6) | 0.0044 (2) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Na1—Pi | 2.8586 (3) | Na2—Na2vi | 3.1904 (15) |
Na1—Pii | 2.8586 (3) | Na2—Pxi | 3.2229 (8) |
Na1—P | 2.8586 (3) | Na2—Piv | 3.2229 (8) |
Na1—Na2iii | 3.2229 (8) | Na2—Na1iv | 3.2229 (8) |
Na1—Na2iv | 3.2229 (8) | Na2—Na1vi | 3.2229 (8) |
Na1—Na2v | 3.2229 (8) | Na2—Na1viii | 3.2229 (8) |
Na1—Na2vi | 3.2229 (8) | Na2—Pvi | 3.2229 (8) |
Na1—Na2vii | 3.2229 (8) | P—Na1xii | 2.8586 (3) |
Na1—Na2viii | 3.2229 (8) | P—Na1xiii | 2.8586 (3) |
Na1—Na2 | 4.0758 (12) | P—Na2xiv | 2.9053 (17) |
Na1—Na2ix | 4.0758 (12) | P—Na2iii | 3.2229 (8) |
Na1—Na2i | 4.0758 (12) | P—Na2xi | 3.2229 (8) |
Na2—P | 2.9053 (17) | P—Na2iv | 3.2229 (8) |
Na2—Na2x | 2.977 (3) | P—Na2xv | 3.2229 (8) |
Na2—Na2iv | 3.1904 (15) | P—Na2vi | 3.2229 (8) |
Na2—Na2xi | 3.1904 (15) | P—Na2vii | 3.2229 (8) |
| | | |
Pi—Na1—Pii | 120.0 | P—Na2—Na1vi | 117.51 (3) |
Pi—Na1—P | 120.0 | Na2x—Na2—Na1vi | 62.49 (3) |
Pii—Na1—P | 120.0 | Na2iv—Na2—Na1vi | 178.86 (8) |
Pi—Na1—Na2iii | 152.49 (3) | Na2xi—Na2—Na1vi | 78.915 (18) |
Pii—Na1—Na2iii | 63.674 (7) | Na2vi—Na2—Na1vi | 78.915 (18) |
P—Na1—Na2iii | 63.674 (7) | Pxi—Na2—Na1vi | 52.653 (13) |
Pi—Na1—Na2iv | 152.49 (3) | Piv—Na2—Na1vi | 124.99 (5) |
Pii—Na1—Na2iv | 63.674 (7) | Na1iv—Na2—Na1vi | 100.37 (3) |
P—Na1—Na2iv | 63.674 (7) | P—Na2—Na1viii | 117.51 (3) |
Na2iii—Na1—Na2iv | 55.01 (5) | Na2x—Na2—Na1viii | 62.49 (3) |
Pi—Na1—Na2v | 63.674 (7) | Na2iv—Na2—Na1viii | 78.915 (18) |
Pii—Na1—Na2v | 63.674 (7) | Na2xi—Na2—Na1viii | 178.86 (8) |
P—Na1—Na2v | 152.49 (3) | Na2vi—Na2—Na1viii | 78.915 (18) |
Na2iii—Na1—Na2v | 100.37 (3) | Pxi—Na2—Na1viii | 124.99 (5) |
Na2iv—Na1—Na2v | 127.347 (13) | Piv—Na2—Na1viii | 52.653 (13) |
Pi—Na1—Na2vi | 63.674 (7) | Na1iv—Na2—Na1viii | 100.37 (3) |
Pii—Na1—Na2vi | 152.49 (3) | Na1vi—Na2—Na1viii | 100.37 (3) |
P—Na1—Na2vi | 63.674 (7) | P—Na2—Pvi | 117.51 (3) |
Na2iii—Na1—Na2vi | 127.347 (13) | Na2x—Na2—Pvi | 62.49 (3) |
Na2iv—Na1—Na2vi | 100.37 (3) | Na2iv—Na2—Pvi | 127.045 (8) |
Na2v—Na1—Na2vi | 127.347 (13) | Na2xi—Na2—Pvi | 127.045 (9) |
Pi—Na1—Na2vii | 63.674 (7) | Na2vi—Na2—Pvi | 53.87 (3) |
Pii—Na1—Na2vii | 152.49 (3) | Pxi—Na2—Pvi | 100.37 (3) |
P—Na1—Na2vii | 63.674 (7) | Piv—Na2—Pvi | 100.37 (3) |
Na2iii—Na1—Na2vii | 100.37 (3) | Na1iv—Na2—Pvi | 124.99 (5) |
Na2iv—Na1—Na2vii | 127.347 (13) | Na1vi—Na2—Pvi | 52.653 (13) |
Na2v—Na1—Na2vii | 100.37 (3) | Na1viii—Na2—Pvi | 52.653 (13) |
Na2vi—Na1—Na2vii | 55.01 (5) | P—Na2—Na1 | 44.536 (17) |
Pi—Na1—Na2viii | 63.674 (7) | Na2x—Na2—Na1 | 135.464 (17) |
Pii—Na1—Na2viii | 63.674 (7) | Na2iv—Na2—Na1 | 50.89 (3) |
P—Na1—Na2viii | 152.49 (3) | Na2xi—Na2—Na1 | 108.17 (7) |
Na2iii—Na1—Na2viii | 127.347 (13) | Na2vi—Na2—Na1 | 50.89 (3) |
Na2iv—Na1—Na2viii | 100.37 (3) | Pxi—Na2—Na1 | 162.04 (4) |
Na2v—Na1—Na2viii | 55.01 (5) | Piv—Na2—Na1 | 91.041 (12) |
Na2vi—Na1—Na2viii | 100.37 (3) | Na1iv—Na2—Na1 | 129.810 (16) |
Na2vii—Na1—Na2viii | 127.347 (13) | Na1vi—Na2—Na1 | 129.810 (16) |
Pi—Na1—Na2 | 110.529 (6) | Na1viii—Na2—Na1 | 72.970 (13) |
Pii—Na1—Na2 | 110.529 (6) | Pvi—Na2—Na1 | 91.041 (12) |
P—Na1—Na2 | 45.464 (17) | Na1xii—P—Na1xiii | 120.0 |
Na2iii—Na1—Na2 | 91.041 (12) | Na1xii—P—Na1 | 120.0 |
Na2iv—Na1—Na2 | 50.190 (16) | Na1xiii—P—Na1 | 120.0 |
Na2v—Na1—Na2 | 162.04 (4) | Na1xii—P—Na2xiv | 90.0 |
Na2vi—Na1—Na2 | 50.190 (16) | Na1xiii—P—Na2xiv | 90.0 |
Na2vii—Na1—Na2 | 91.041 (12) | Na1—P—Na2xiv | 90.0 |
Na2viii—Na1—Na2 | 107.030 (13) | Na1xii—P—Na2 | 90.0 |
Pi—Na1—Na2ix | 110.529 (6) | Na1xiii—P—Na2 | 90.0 |
Pii—Na1—Na2ix | 45.464 (17) | Na1—P—Na2 | 90.0 |
P—Na1—Na2ix | 110.529 (6) | Na2xiv—P—Na2 | 180.0 |
Na2iii—Na1—Na2ix | 50.190 (16) | Na1xii—P—Na2iii | 63.674 (7) |
Na2iv—Na1—Na2ix | 91.041 (12) | Na1xiii—P—Na2iii | 152.49 (3) |
Na2v—Na1—Na2ix | 50.190 (16) | Na1—P—Na2iii | 63.674 (7) |
Na2vi—Na1—Na2ix | 162.04 (4) | Na2xiv—P—Na2iii | 62.49 (3) |
Na2vii—Na1—Na2ix | 107.030 (13) | Na2—P—Na2iii | 117.51 (3) |
Na2viii—Na1—Na2ix | 91.041 (12) | Na1xii—P—Na2xi | 63.674 (7) |
Na2—Na1—Na2ix | 138.942 (13) | Na1xiii—P—Na2xi | 63.674 (7) |
Pi—Na1—Na2i | 45.464 (17) | Na1—P—Na2xi | 152.49 (3) |
Pii—Na1—Na2i | 110.529 (6) | Na2xiv—P—Na2xi | 117.51 (3) |
P—Na1—Na2i | 110.529 (6) | Na2—P—Na2xi | 62.49 (3) |
Na2iii—Na1—Na2i | 162.04 (4) | Na2iii—P—Na2xi | 127.347 (13) |
Na2iv—Na1—Na2i | 107.030 (13) | Na1xii—P—Na2iv | 63.674 (7) |
Na2v—Na1—Na2i | 91.041 (12) | Na1xiii—P—Na2iv | 152.49 (3) |
Na2vi—Na1—Na2i | 50.190 (16) | Na1—P—Na2iv | 63.674 (7) |
Na2vii—Na1—Na2i | 91.041 (12) | Na2xiv—P—Na2iv | 117.51 (3) |
Na2viii—Na1—Na2i | 50.190 (16) | Na2—P—Na2iv | 62.49 (3) |
Na2—Na1—Na2i | 74.80 (3) | Na2iii—P—Na2iv | 55.01 (5) |
Na2ix—Na1—Na2i | 138.942 (13) | Na2xi—P—Na2iv | 100.37 (3) |
P—Na2—Na2x | 180.0 | Na1xii—P—Na2xv | 63.674 (7) |
P—Na2—Na2iv | 63.64 (5) | Na1xiii—P—Na2xv | 63.674 (7) |
Na2x—Na2—Na2iv | 116.36 (5) | Na1—P—Na2xv | 152.49 (3) |
P—Na2—Na2xi | 63.64 (5) | Na2xiv—P—Na2xv | 62.49 (3) |
Na2x—Na2—Na2xi | 116.36 (5) | Na2—P—Na2xv | 117.51 (3) |
Na2iv—Na2—Na2xi | 101.78 (6) | Na2iii—P—Na2xv | 100.37 (3) |
P—Na2—Na2vi | 63.64 (5) | Na2xi—P—Na2xv | 55.01 (5) |
Na2x—Na2—Na2vi | 116.36 (5) | Na2iv—P—Na2xv | 127.347 (13) |
Na2iv—Na2—Na2vi | 101.78 (6) | Na1xii—P—Na2vi | 152.49 (3) |
Na2xi—Na2—Na2vi | 101.78 (6) | Na1xiii—P—Na2vi | 63.674 (7) |
P—Na2—Pxi | 117.51 (3) | Na1—P—Na2vi | 63.674 (7) |
Na2x—Na2—Pxi | 62.49 (3) | Na2xiv—P—Na2vi | 117.51 (3) |
Na2iv—Na2—Pxi | 127.045 (9) | Na2—P—Na2vi | 62.49 (3) |
Na2xi—Na2—Pxi | 53.87 (3) | Na2iii—P—Na2vi | 127.347 (13) |
Na2vi—Na2—Pxi | 127.045 (9) | Na2xi—P—Na2vi | 100.37 (3) |
P—Na2—Piv | 117.51 (3) | Na2iv—P—Na2vi | 100.37 (3) |
Na2x—Na2—Piv | 62.49 (3) | Na2xv—P—Na2vi | 127.347 (14) |
Na2iv—Na2—Piv | 53.87 (3) | Na1xii—P—Na2vii | 152.49 (3) |
Na2xi—Na2—Piv | 127.045 (9) | Na1xiii—P—Na2vii | 63.674 (7) |
Na2vi—Na2—Piv | 127.045 (9) | Na1—P—Na2vii | 63.674 (7) |
Pxi—Na2—Piv | 100.37 (3) | Na2xiv—P—Na2vii | 62.49 (3) |
P—Na2—Na1iv | 117.51 (3) | Na2—P—Na2vii | 117.51 (3) |
Na2x—Na2—Na1iv | 62.49 (3) | Na2iii—P—Na2vii | 100.37 (3) |
Na2iv—Na2—Na1iv | 78.915 (18) | Na2xi—P—Na2vii | 127.347 (14) |
Na2xi—Na2—Na1iv | 78.915 (18) | Na2iv—P—Na2vii | 127.347 (13) |
Na2vi—Na2—Na1iv | 178.86 (8) | Na2xv—P—Na2vii | 100.37 (3) |
Pxi—Na2—Na1iv | 52.653 (13) | Na2vi—P—Na2vii | 55.01 (5) |
Piv—Na2—Na1iv | 52.653 (13) | | |
Symmetry codes: (i) x, y−1, z; (ii) x−1, y−1, z; (iii) −x, −y+1, z−1/2; (iv) −x, −y+1, −z+1; (v) −x, −y, z−1/2; (vi) −x+1, −y+1, −z+1; (vii) −x+1, −y+1, z−1/2; (viii) −x, −y, −z+1; (ix) x−1, y−1, −z+1/2; (x) x, y, −z+3/2; (xi) −x+1, −y+2, −z+1; (xii) x, y+1, z; (xiii) x+1, y+1, z; (xiv) x, y, −z+1/2; (xv) −x+1, −y+2, z−1/2. |
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