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The structure of tris­odium phosphide, Na3P, 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 P3- 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 \overline{6}m2 (2b), 3m (4f) and \overline{6}m2 (2c) site symmetry, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031168/wm6094sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031168/wm6094Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 165 K
  • Mean [sigma]() = 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

Computing details top

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).

Trisodium phosphide top
Crystal data top
Na3PDx = 1.779 Mg m3
Mr = 99.94Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmcCell parameters from 196 reflections
Hall symbol: -P 6c 2cθ = 3.3–40.2°
a = 4.9512 (5) ŵ = 0.81 mm1
c = 8.7874 (13) ÅT = 165 K
V = 186.56 (4) Å3Block, red
Z = 20.10 × 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 tube115 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
φ and ω scansθmax = 32.2°, θmin = 4.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1999)
h = 77
Tmin = 0.920, Tmax = 0.960k = 77
1495 measured reflectionsl = 1213
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary 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 = 1.13Δρmax = 0.41 e Å3
155 reflectionsΔρmin = 0.49 e Å3
9 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction 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
xyzUiso*/Ueq
Na10.00000.00000.25000.0360 (9)
Na20.33330.66670.58062 (18)0.0379 (6)
P0.33330.66670.25000.0095 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0127 (8)0.0127 (8)0.083 (3)0.0063 (4)0.0000.000
Na20.0501 (9)0.0501 (9)0.0134 (8)0.0251 (4)0.0000.000
P0.0088 (4)0.0088 (4)0.0109 (6)0.0044 (2)0.0000.000
Geometric parameters (Å, º) top
Na1—Pi2.8586 (3)Na2—Na2vi3.1904 (15)
Na1—Pii2.8586 (3)Na2—Pxi3.2229 (8)
Na1—P2.8586 (3)Na2—Piv3.2229 (8)
Na1—Na2iii3.2229 (8)Na2—Na1iv3.2229 (8)
Na1—Na2iv3.2229 (8)Na2—Na1vi3.2229 (8)
Na1—Na2v3.2229 (8)Na2—Na1viii3.2229 (8)
Na1—Na2vi3.2229 (8)Na2—Pvi3.2229 (8)
Na1—Na2vii3.2229 (8)P—Na1xii2.8586 (3)
Na1—Na2viii3.2229 (8)P—Na1xiii2.8586 (3)
Na1—Na24.0758 (12)P—Na2xiv2.9053 (17)
Na1—Na2ix4.0758 (12)P—Na2iii3.2229 (8)
Na1—Na2i4.0758 (12)P—Na2xi3.2229 (8)
Na2—P2.9053 (17)P—Na2iv3.2229 (8)
Na2—Na2x2.977 (3)P—Na2xv3.2229 (8)
Na2—Na2iv3.1904 (15)P—Na2vi3.2229 (8)
Na2—Na2xi3.1904 (15)P—Na2vii3.2229 (8)
Pi—Na1—Pii120.0P—Na2—Na1vi117.51 (3)
Pi—Na1—P120.0Na2x—Na2—Na1vi62.49 (3)
Pii—Na1—P120.0Na2iv—Na2—Na1vi178.86 (8)
Pi—Na1—Na2iii152.49 (3)Na2xi—Na2—Na1vi78.915 (18)
Pii—Na1—Na2iii63.674 (7)Na2vi—Na2—Na1vi78.915 (18)
P—Na1—Na2iii63.674 (7)Pxi—Na2—Na1vi52.653 (13)
Pi—Na1—Na2iv152.49 (3)Piv—Na2—Na1vi124.99 (5)
Pii—Na1—Na2iv63.674 (7)Na1iv—Na2—Na1vi100.37 (3)
P—Na1—Na2iv63.674 (7)P—Na2—Na1viii117.51 (3)
Na2iii—Na1—Na2iv55.01 (5)Na2x—Na2—Na1viii62.49 (3)
Pi—Na1—Na2v63.674 (7)Na2iv—Na2—Na1viii78.915 (18)
Pii—Na1—Na2v63.674 (7)Na2xi—Na2—Na1viii178.86 (8)
P—Na1—Na2v152.49 (3)Na2vi—Na2—Na1viii78.915 (18)
Na2iii—Na1—Na2v100.37 (3)Pxi—Na2—Na1viii124.99 (5)
Na2iv—Na1—Na2v127.347 (13)Piv—Na2—Na1viii52.653 (13)
Pi—Na1—Na2vi63.674 (7)Na1iv—Na2—Na1viii100.37 (3)
Pii—Na1—Na2vi152.49 (3)Na1vi—Na2—Na1viii100.37 (3)
P—Na1—Na2vi63.674 (7)P—Na2—Pvi117.51 (3)
Na2iii—Na1—Na2vi127.347 (13)Na2x—Na2—Pvi62.49 (3)
Na2iv—Na1—Na2vi100.37 (3)Na2iv—Na2—Pvi127.045 (8)
Na2v—Na1—Na2vi127.347 (13)Na2xi—Na2—Pvi127.045 (9)
Pi—Na1—Na2vii63.674 (7)Na2vi—Na2—Pvi53.87 (3)
Pii—Na1—Na2vii152.49 (3)Pxi—Na2—Pvi100.37 (3)
P—Na1—Na2vii63.674 (7)Piv—Na2—Pvi100.37 (3)
Na2iii—Na1—Na2vii100.37 (3)Na1iv—Na2—Pvi124.99 (5)
Na2iv—Na1—Na2vii127.347 (13)Na1vi—Na2—Pvi52.653 (13)
Na2v—Na1—Na2vii100.37 (3)Na1viii—Na2—Pvi52.653 (13)
Na2vi—Na1—Na2vii55.01 (5)P—Na2—Na144.536 (17)
Pi—Na1—Na2viii63.674 (7)Na2x—Na2—Na1135.464 (17)
Pii—Na1—Na2viii63.674 (7)Na2iv—Na2—Na150.89 (3)
P—Na1—Na2viii152.49 (3)Na2xi—Na2—Na1108.17 (7)
Na2iii—Na1—Na2viii127.347 (13)Na2vi—Na2—Na150.89 (3)
Na2iv—Na1—Na2viii100.37 (3)Pxi—Na2—Na1162.04 (4)
Na2v—Na1—Na2viii55.01 (5)Piv—Na2—Na191.041 (12)
Na2vi—Na1—Na2viii100.37 (3)Na1iv—Na2—Na1129.810 (16)
Na2vii—Na1—Na2viii127.347 (13)Na1vi—Na2—Na1129.810 (16)
Pi—Na1—Na2110.529 (6)Na1viii—Na2—Na172.970 (13)
Pii—Na1—Na2110.529 (6)Pvi—Na2—Na191.041 (12)
P—Na1—Na245.464 (17)Na1xii—P—Na1xiii120.0
Na2iii—Na1—Na291.041 (12)Na1xii—P—Na1120.0
Na2iv—Na1—Na250.190 (16)Na1xiii—P—Na1120.0
Na2v—Na1—Na2162.04 (4)Na1xii—P—Na2xiv90.0
Na2vi—Na1—Na250.190 (16)Na1xiii—P—Na2xiv90.0
Na2vii—Na1—Na291.041 (12)Na1—P—Na2xiv90.0
Na2viii—Na1—Na2107.030 (13)Na1xii—P—Na290.0
Pi—Na1—Na2ix110.529 (6)Na1xiii—P—Na290.0
Pii—Na1—Na2ix45.464 (17)Na1—P—Na290.0
P—Na1—Na2ix110.529 (6)Na2xiv—P—Na2180.0
Na2iii—Na1—Na2ix50.190 (16)Na1xii—P—Na2iii63.674 (7)
Na2iv—Na1—Na2ix91.041 (12)Na1xiii—P—Na2iii152.49 (3)
Na2v—Na1—Na2ix50.190 (16)Na1—P—Na2iii63.674 (7)
Na2vi—Na1—Na2ix162.04 (4)Na2xiv—P—Na2iii62.49 (3)
Na2vii—Na1—Na2ix107.030 (13)Na2—P—Na2iii117.51 (3)
Na2viii—Na1—Na2ix91.041 (12)Na1xii—P—Na2xi63.674 (7)
Na2—Na1—Na2ix138.942 (13)Na1xiii—P—Na2xi63.674 (7)
Pi—Na1—Na2i45.464 (17)Na1—P—Na2xi152.49 (3)
Pii—Na1—Na2i110.529 (6)Na2xiv—P—Na2xi117.51 (3)
P—Na1—Na2i110.529 (6)Na2—P—Na2xi62.49 (3)
Na2iii—Na1—Na2i162.04 (4)Na2iii—P—Na2xi127.347 (13)
Na2iv—Na1—Na2i107.030 (13)Na1xii—P—Na2iv63.674 (7)
Na2v—Na1—Na2i91.041 (12)Na1xiii—P—Na2iv152.49 (3)
Na2vi—Na1—Na2i50.190 (16)Na1—P—Na2iv63.674 (7)
Na2vii—Na1—Na2i91.041 (12)Na2xiv—P—Na2iv117.51 (3)
Na2viii—Na1—Na2i50.190 (16)Na2—P—Na2iv62.49 (3)
Na2—Na1—Na2i74.80 (3)Na2iii—P—Na2iv55.01 (5)
Na2ix—Na1—Na2i138.942 (13)Na2xi—P—Na2iv100.37 (3)
P—Na2—Na2x180.0Na1xii—P—Na2xv63.674 (7)
P—Na2—Na2iv63.64 (5)Na1xiii—P—Na2xv63.674 (7)
Na2x—Na2—Na2iv116.36 (5)Na1—P—Na2xv152.49 (3)
P—Na2—Na2xi63.64 (5)Na2xiv—P—Na2xv62.49 (3)
Na2x—Na2—Na2xi116.36 (5)Na2—P—Na2xv117.51 (3)
Na2iv—Na2—Na2xi101.78 (6)Na2iii—P—Na2xv100.37 (3)
P—Na2—Na2vi63.64 (5)Na2xi—P—Na2xv55.01 (5)
Na2x—Na2—Na2vi116.36 (5)Na2iv—P—Na2xv127.347 (13)
Na2iv—Na2—Na2vi101.78 (6)Na1xii—P—Na2vi152.49 (3)
Na2xi—Na2—Na2vi101.78 (6)Na1xiii—P—Na2vi63.674 (7)
P—Na2—Pxi117.51 (3)Na1—P—Na2vi63.674 (7)
Na2x—Na2—Pxi62.49 (3)Na2xiv—P—Na2vi117.51 (3)
Na2iv—Na2—Pxi127.045 (9)Na2—P—Na2vi62.49 (3)
Na2xi—Na2—Pxi53.87 (3)Na2iii—P—Na2vi127.347 (13)
Na2vi—Na2—Pxi127.045 (9)Na2xi—P—Na2vi100.37 (3)
P—Na2—Piv117.51 (3)Na2iv—P—Na2vi100.37 (3)
Na2x—Na2—Piv62.49 (3)Na2xv—P—Na2vi127.347 (14)
Na2iv—Na2—Piv53.87 (3)Na1xii—P—Na2vii152.49 (3)
Na2xi—Na2—Piv127.045 (9)Na1xiii—P—Na2vii63.674 (7)
Na2vi—Na2—Piv127.045 (9)Na1—P—Na2vii63.674 (7)
Pxi—Na2—Piv100.37 (3)Na2xiv—P—Na2vii62.49 (3)
P—Na2—Na1iv117.51 (3)Na2—P—Na2vii117.51 (3)
Na2x—Na2—Na1iv62.49 (3)Na2iii—P—Na2vii100.37 (3)
Na2iv—Na2—Na1iv78.915 (18)Na2xi—P—Na2vii127.347 (14)
Na2xi—Na2—Na1iv78.915 (18)Na2iv—P—Na2vii127.347 (13)
Na2vi—Na2—Na1iv178.86 (8)Na2xv—P—Na2vii100.37 (3)
Pxi—Na2—Na1iv52.653 (13)Na2vi—P—Na2vii55.01 (5)
Piv—Na2—Na1iv52.653 (13)
Symmetry codes: (i) x, y1, z; (ii) x1, y1, z; (iii) x, y+1, z1/2; (iv) x, y+1, z+1; (v) x, y, z1/2; (vi) x+1, y+1, z+1; (vii) x+1, y+1, z1/2; (viii) x, y, z+1; (ix) x1, y1, 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, z1/2.
 

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