Rhombohedral boron subnitride, B₁₃N₂, by X-ray powder diffraction

The structure of the title compound consists of distorted B₁₂ icosa­hedra linked by N-B-N chains. The compound crystallizes in the rhombohedral space group Rm (No. 166). The unit cell contains four symmetry-independent atom sites, three of which are occupied by boron [in the 18h, 18h (site symmetry m) and 3b (site symmetry m) Wyckoff positions] and one by nitro­gen (in the 6c Wyckoff position, site symmetry 3m). Two of the B atoms form the icosa­hedra, while N atoms link the icosa­hedra together. The main feature of the structure is that the 3b position is occupied by the B atom, which makes the structure different from those of B₆O, for which these atom sites are vacant, and B_4+xC_1-x, for which this position is randomly occupied by both B and C atoms.

S1. Comment

The fortunate combination of lightness, hardness, strength, chemical inertness and high cross section for neutron absorption has suited boron and boron-rich phases (B₆O, B_{4 + x}C_1-x etc.) to many technological applications (Emin, 1987; McMillan, 2002). Very recently, we have synthesized a new member of this group, boron subnitride `B<sub>6</sub>N'. From the electron energy loss spectroscopy data, the stoichiometry of the phase has been determined to be B<sub>6±1</sub>N, and from the X-ray study as B<sub>13</sub>N<sub>2</sub>. The phase has a structure similar in some respect to those of α -rhombohedral boron (Decker & Kasper, 1959), B<sub>4 + x</sub>C<sub>1 - x</sub> (Kirfel et al., 1979; Aselage et al., 1997) and B<sub>6</sub>O (Higashi et al., 1991; Aselage et al., 1997). However, the relative line intensities correspond to none of these three structures. The similarity is greatest to B<sub>4 + x</sub>C<sub>1 - x</sub>, which has the same unit cell, space group and atom sites as the nitride. Studies of the carbide by X-ray diffraction, Raman spectroscopy and, especially, <sup>13</sup>C and <sup>11</sup>B nuclear magnetic resonance revealed that a very complicated atomic distribution of carbon all over the lattice takes place via C/B disorder, resulting in C—C—C, B—B—C and C—B—C intericosahedral chains, as well as B<sub>11</sub>C and B<sub>12</sub> icosahedra (Aselage et al., 1997; Tallant et al., 1989; Bullett, 1982; Lundstrom, 1997). In the case of `B₆N', our Raman data have supported the suggestion that the `B₆N' structure is similar to that of boron carbide, B_{4 + x}C_{1 - x}, but with no evidence of N/B disorder of the type seen in the carbide. Thus, the nitride features N—B—N linkages, but no N—N—N linkages, which would be much less stable than the carbon analogues in any case.

In the present work, the structure of the new boron subnitride B₁₃N₂ has been determined by Rietveld refinement of powder diffraction data collected at ambient conditions (Fig. 1). The Bragg lines of the compound have been indexed in the rhombohedral cell, with lattice parameters a = 5.4455 (2) Å and c = 12.2649 (9) Å. In order to check all possibilities of the atom type distribution over symmetry-independent site positions, we have performed a Rietveld refinement of several unit cells of the `B₆N' compound. All the cells contained atoms B1 and B2 (18h Wyckoff position), while the 6c and 3b Wyckoff positions were allowed to be occupied by either B or N atoms. Satisfactory refinement was achieved only in the case of the starting unit cell containing two symmetry-independent B atoms of the 18h Wickoff position, one independent N atom in the 6c position, and one B atom in the 3b position (Fig. 2). The site occupancies of the atoms of each crystallographic type are close to unity, so the synthesized phase has the B₁₃N₂ stoichiometry.

Related literature

For related literature, see: Aselage et al. (1997); Bullett (1982); Decker & Kasper (1959); Emin (1987); Franklin (1950, 1951); Higashi et al. (1991); Kirfel et al. (1979); Lundstrom (1997); McMillan (2002); Ploog et al. (1972); Solozhenko & Peun (1997); Tallant et al. (1989).

S2. Experimental

Boron subnitride, B₁₃N₂, was synthesized from the B–BN melt at 5 GPa using the multianvil X-ray system MAX80 at beamline F2.1, HASYLAB-DESY. The experimental setup has been described elsewhere (Solozhenko & Peun, 1997). The starting materials, β -rhombohedral boron (β -rh B) and hexagonal boron nitride (hBN), were mixed in the 5:1 molar ratio that corresponds to the B₆N stoichiometry, compressed to 5 GPa, heated to 2500 K and then quenched down to ambient conditions. Since the B₁₃N₂ phase crystallizes by peritectic reaction, the title compound has always been found in a mixture with β-rh boron, an I-tetragonal boron-like phase (Ploog et al., 1972) and hBN. According to Rietveld refinement, the sample contains about 22 vol% of B₁₃N₂.

S3. Refinement

Rietveld analysis of the powder diffraction pattern that contains six phases (five with already established structures and one new) made for a complicated refinement. The 2θ interval for the profile fitting (Fig. 1) was chosen so that the main lines of boron subnitride B₁₃N₂ have not been overlapped by the lines of other phases. The profile fitting of all the phases except B₁₃N₂ was performed employing both LeBail and Rietveld procedures using the literature data on the structures of corresponding phases.

Six phases were employed for profile fitting: B₁₃N₂ (phase 1), `B₅₀N₂' (phase 2), hBN (phase 3), β-rhombohedral boron (phase 4), boric acid H₃BO₃ (phase 5) and phase 6, which has the same structure as phase 3 but slightly different cell parameter c. Phase 6 was added to adjust the profile asymmetry of the 002 line due to a slight nonhomogeneity in the degree of ordering of hBN (Franklin, 1950, 1951). This has improved the fitting of the most intensive line of hBN (24–26° 2θ) and has not influenced fitting out of this range. The only line of phase 5 belongs to this 2θ range and does not affect the structure refinement of the principal phase. Phases 2 and 4 have some lines overlapping with the lines of B₁₃N₂, but these lines are noticeably narrower than those of phase 1; this difference has much facilitated the intensity extraction.

The sample contains approximately 22 vol% B₁₃N₂, 37 vol% hBN and about 41 vol% boron. The boron content (both β-rhombohedral boron and I-t boron-like phase) was estimated using the values of phase fractions for B₁₃N₂ and hBN and the total composition of the starting mixture (5B+BN). A very small amount of boric acid (0.001 vol%) was also observed. Its formation may be attributed to hBN hydrolysis that cannot be avoided in the high-pressure experiments.

Computing details

Data collection: program (reference)? for phase_4. Cell refinement: program (reference)? for phase_4. Data reduction: program (reference)? for phase_4. Program(s) used to solve structure: program (reference)? for phase_4. Program(s) used to refine structure: GSAS for phase_4. Molecular graphics: program (reference)? for phase_4. Software used to prepare material for publication: program (reference)? for phase_4.

Figures

Fig. 1. Rietveld full profile refinement of the X-ray powder diffraction pattern of B13N2 boron subnitride.

Fig. 2. The unit cell of B13N2. The unit cell contains four symmetry- independent atom sites, three of which are occupied by boron [i.e. B1, B2 and B4 in the 18h, 18h and 3b Wyckoff positions, respectively] and one by nitrogen (N3 in the 6c Wyckoff position). [Symmetry codes: (i) y - x + 1/3, - x + 2/3, z + 2/3; (-i) x - y + 2/3, x + 1/3, - z + 1/3; (ii) x + 2/3, y + 1/3, z + 1/3; (-ii) -x + 1/3, -y + 2/3, -z + 2/3; (iii) x + 1/3, x - y + 2/3, z + 2/3; (-iii) -x + 2/3, y - x + 1/3, - z + 1/3.]

(phase_1) boron nitride

Crystal data

B13N2	Z = 3
Mr = 168.54	F(000) = 235
Trigonal, R3m	Dx = 2.666 Mg m^−3
Hall symbol: -R 3 2"	Cu Kα radiation, λ = 1.540598 Å
a = 5.4455 (2) Å	T = 297 K
c = 12.2649 (9) Å	black
V = 314.97 (4) Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Special details

Geometry. N—B—N chains

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B1	0.1725 (14)	0.8275 (14)	0.0371 (13)	0.025*
B2	0.1198 (7)	0.8803 (7)	0.8834 (8)	0.025*
N3	0.0	0.0	0.3744 (13)	0.025*
B4	0.0	0.0	0.5	0.025*

Geometric parameters (Å, º)

B1—B1^i	1.865 (17)	N3—B1^xi	1.517 (12)
B1—B1^ii	1.865 (17)	N3—B1^xii	1.517 (12)
B1—B2^iii	1.950 (9)	N3—B1^xiii	1.517 (12)
B1—B2^iv	1.742 (14)	N3—B4	1.541 (16)
B1—B2^v	1.743 (14)	B4—B1^xiv	2.197 (13)
B1—N3^vi	1.517 (12)	B4—B1^xv	2.197 (13)
B1—B4^vi	2.197 (13)	B4—B1^xvi	2.197 (13)
B2—B1^vii	1.950 (9)	B4—B1^xi	2.197 (13)
B2—B1^iv	1.743 (14)	B4—B1^xii	2.197 (13)
B2—B1^v	1.742 (14)	B4—B1^xiii	2.197 (13)
B2—B2^viii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^ix	1.956 (12)	B4—N3^xvii	1.541 (16)
B2—B2^x	1.514 (11)
B1^i—B1—B1^ii	98.2 (12)	B1^vii—B2—B2^x	129.4 (10)
B1^i—B1—B2^iii	54.3 (8)	B1^iv—B2—B1^v	107.9 (12)
B1^i—B1—B2^iv	65.4 (5)	B1^iv—B2—B2^viii	104.3 (3)
B1^i—B1—B2^v	115.5 (6)	B1^iv—B2—B2^ix	55.9 (5)
B1^i—B1—N3^vi	116.8 (8)	B1^iv—B2—B2^x	124.0 (4)
B1^ii—B1—B2^iii	54.3 (8)	B1^v—B2—B2^viii	55.9 (5)
B1^ii—B1—B2^iv	115.5 (6)	B1^v—B2—B2^ix	104.3 (3)
B1^ii—B1—B2^v	65.4 (5)	B1^v—B2—B2^x	124.1 (4)
B1^ii—B1—N3^vi	116.8 (8)	B2^viii—B2—B2^ix	60.0
B2^iii—B1—B2^iv	112.7 (7)	B2^viii—B2—B2^x	120.5 (6)
B2^iii—B1—B2^v	112.7 (7)	B2^ix—B2—B2^x	120.4 (6)
B2^iii—B1—N3^vi	106.6 (15)	B1^xi—N3—B1^xii	119.90 (13)
B2^iv—B1—B2^v	68.3 (10)	B1^xi—N3—B1^xiii	119.90 (13)
B2^iv—B1—N3^vi	126.3 (9)	B1^xi—N3—B4	91.8 (11)
B2^v—B1—N3^vi	126.3 (9)	B1^xii—N3—B1^xiii	119.90 (13)
B1^vii—B2—B1^iv	60.3 (7)	B1^xii—N3—B4	91.8 (11)
B1^vii—B2—B1^v	60.3 (7)	B1^xiii—N3—B4	91.8 (11)
B1^vii—B2—B2^viii	102.8 (4)	N3—B4—N3^xvii	180.0
B1^vii—B2—B2^ix	102.8 (4)

Symmetry codes: (i) y−1, y−x, −z; (ii) x−y+1, x+1, −z; (iii) x, y, z−1; (iv) y−1, y−x, −z+1; (v) x−y+1, x+1, −z+1; (vi) x+1/3, y+2/3, z−1/3; (vii) x, y, z+1; (viii) −y+1, x−y+2, z; (ix) y−x−1, −x+1, z; (x) −x−1/3, −y+1/3, −z+1/3; (xi) x−1/3, y−2/3, z+1/3; (xii) −y+2/3, x−y+1/3, z+1/3; (xiii) y−x−1/3, −x+1/3, z+1/3; (xiv) −x−1/3, −y−2/3, −z−2/3; (xv) y−4/3, y−x−5/3, −z−2/3; (xvi) x−y−1/3, x−5/3, −z−2/3; (xvii) −x, −y, −z+1.

(phase_2) boron nitride

Crystal data

BNx	Z = 50
Mr = 10.81	F(000) = 240
Tetragonal, P4n2	Dx = 2.21 Mg m^−3
Hall symbol: P -4 -2n	Cu Kα radiation, λ = 1.540598 Å
a = 8.7979 (18) Å	T = 297 K
c = 5.037 (3) Å	black
V = 389.91 Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B3	0.328	0.095	0.395	0.025*
B4	0.095	0.328	0.395	0.025*
B5	0.223	0.078	0.105	0.025*
B6	0.078	0.223	0.105	0.025*
B7	0.127	0.127	0.395	0.025*
B8	0.25	0.25	−0.078	0.025*

Geometric parameters (Å, º)

B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B2^i	1.950 (9)	N3—B1	1.517 (12)
B1—B2	1.742 (14)	N3—B4	1.541 (16)
B1—B2	1.743 (14)	B4—B1	2.197 (13)
B1—N3	1.517 (12)	B4—B1	2.197 (13)
B1—B4	2.197 (13)	B4—B1	2.197 (13)
B2—B1^ii	1.950 (9)	B4—B1	2.197 (13)
B2—B1	1.743 (14)	B4—B1	2.197 (13)
B2—B1	1.742 (14)	B4—B1	2.197 (13)
B2—B2^iii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^iv	1.956 (12)	B4—N3	1.541 (16)
B2—B2	1.514 (11)
B1—B1—B1	98.2 (12)	B1^ii—B2—B2	129.4 (10)
B1—B1—B2^i	54.3 (8)	B1—B2—B1	107.9 (12)
B1—B1—B2	65.4 (5)	B1—B2—B2^iii	104.3 (3)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	55.9 (5)
B1—B1—N3	116.8 (8)	B1—B2—B2	124.0 (4)
B1—B1—B2^i	54.3 (8)	B1—B2—B2^iii	55.9 (5)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	104.3 (3)
B1—B1—B2	65.4 (5)	B1—B2—B2	124.1 (4)
B1—B1—N3	116.8 (8)	B2^iii—B2—B2^iv	60.0
B2^i—B1—B2	112.7 (7)	B2^iii—B2—B2	120.5 (6)
B2^i—B1—B2	112.7 (7)	B2^iv—B2—B2	120.4 (6)
B2^i—B1—N3	106.6 (15)	B1—N3—B1	119.90 (13)
B2—B1—B2	68.3 (10)	B1—N3—B1	119.90 (13)
B2—B1—N3	126.3 (9)	B1—N3—B4	91.8 (11)
B2—B1—N3	126.3 (9)	B1—N3—B1	119.90 (13)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B2^iii	102.8 (4)	N3—B4—N3	180.0
B1^ii—B2—B2^iv	102.8 (4)

Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) y+1, −x+2, −z; (iv) −x−1, −y+1, z.

(phase_3) boron nitride

Crystal data

BN	Z = 2
Mr = 24.82	F(000) = 24
Hexagonal, P6m2	Dx = 2.298 Mg m^−3
Hall symbol: P -6 2	Cu Kα radiation, λ = 1.540598 Å
a = 2.49824 (8) Å	T = 297 K
c = 6.6357 (2) Å	black
V = 35.87 (1) Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B1	0.0	0.0	0.5	0.025*
B2	0.3333	0.6667	0.0	0.025*
N3	0.0	0.0	0.0	0.025*
N4	0.3333	0.6667	0.5	0.025*

Geometric parameters (Å, º)

B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B2^i	1.950 (9)	N3—B1	1.517 (12)
B1—B2	1.742 (14)	N3—B4	1.541 (16)
B1—B2	1.743 (14)	B4—B1	2.197 (13)
B1—N3	1.517 (12)	B4—B1	2.197 (13)
B1—B4	2.197 (13)	B4—B1	2.197 (13)
B2—B1^ii	1.950 (9)	B4—B1	2.197 (13)
B2—B1	1.743 (14)	B4—B1	2.197 (13)
B2—B1	1.742 (14)	B4—B1	2.197 (13)
B2—B2^iii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^iv	1.956 (12)	B4—N3	1.541 (16)
B2—B2	1.514 (11)
B1—B1—B1	98.2 (12)	B1^ii—B2—B2	129.4 (10)
B1—B1—B2^i	54.3 (8)	B1—B2—B1	107.9 (12)
B1—B1—B2	65.4 (5)	B1—B2—B2^iii	104.3 (3)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	55.9 (5)
B1—B1—N3	116.8 (8)	B1—B2—B2	124.0 (4)
B1—B1—B2^i	54.3 (8)	B1—B2—B2^iii	55.9 (5)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	104.3 (3)
B1—B1—B2	65.4 (5)	B1—B2—B2	124.1 (4)
B1—B1—N3	116.8 (8)	B2^iii—B2—B2^iv	60.0
B2^i—B1—B2	112.7 (7)	B2^iii—B2—B2	120.5 (6)
B2^i—B1—B2	112.7 (7)	B2^iv—B2—B2	120.4 (6)
B2^i—B1—N3	106.6 (15)	B1—N3—B1	119.90 (13)
B2—B1—B2	68.3 (10)	B1—N3—B1	119.90 (13)
B2—B1—N3	126.3 (9)	B1—N3—B4	91.8 (11)
B2—B1—N3	126.3 (9)	B1—N3—B1	119.90 (13)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B2^iii	102.8 (4)	N3—B4—N3	180.0
B1^ii—B2—B2^iv	102.8 (4)

Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) y−x+1, −x+2, −z; (iv) −y−1, x−y+1, z.

(phase_4) boron

Crystal data

B	Z = 105
Mr = 10.81	F(000) = 520
Trigonal, R3mr	Dx = 2.29 Mg m^−3
Hall symbol: -P 3 2	Cu Kα radiation, λ = 1.540598 Å
a = 10.1398 (3) Å	T = 297 K
c = 10.1398 Å	black
V = 823.05 Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B1	0.0025	0.0025	0.168	0.025*
B2	0.1008	0.1008	0.8374	0.025*
B3	0.9933	0.9933	0.6698	0.025*
B4	0.1032	0.1032	0.4921	0.025*
B5	0.17777	0.3473	0.0033	0.025*
B6	0.1673	0.5521	0.8921	0.025*
B7	0.1983	0.1983	0.6874	0.025*
B8	0.3765	0.6826	0.2024	0.025*
B9	0.3622	0.5811	0.0976	0.025*
B10	0.1991	0.1991	0.5061	0.025*
B11	0.3873	0.3873	0.569	0.025*
B12	0.4895	0.4895	0.2178	0.025*
B13	0.3843	0.3843	0.2131	0.025*
B14	0.3848	0.3848	0.3848	0.025*
B15	0.5	0.5	0.5	0.025*

Geometric parameters (Å, º)

B1—B1^i	1.865 (17)	N3—B1	1.517 (12)
B1—B1^ii	1.865 (17)	N3—B1	1.517 (12)
B1—B2^iii	1.950 (9)	N3—B1	1.517 (12)
B1—B2^iv	1.742 (14)	N3—B4	1.541 (16)
B1—B2^v	1.743 (14)	B4—B1	2.197 (13)
B1—N3	1.517 (12)	B4—B1	2.197 (13)
B1—B4	2.197 (13)	B4—B1	2.197 (13)
B2—B1^vi	1.950 (9)	B4—B1	2.197 (13)
B2—B1^iv	1.743 (14)	B4—B1	2.197 (13)
B2—B1^v	1.742 (14)	B4—B1	2.197 (13)
B2—B2^vii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^viii	1.956 (12)	B4—N3^ix	1.541 (16)
B2—B2	1.514 (11)
B1^i—B1—B1^ii	98.2 (12)	B1^vi—B2—B2	129.4 (10)
B1^i—B1—B2^iii	54.3 (8)	B1^iv—B2—B1^v	107.9 (12)
B1^i—B1—B2^iv	65.4 (5)	B1^iv—B2—B2^vii	104.3 (3)
B1^i—B1—B2^v	115.5 (6)	B1^iv—B2—B2^viii	55.9 (5)
B1^i—B1—N3	116.8 (8)	B1^iv—B2—B2	124.0 (4)
B1^ii—B1—B2^iii	54.3 (8)	B1^v—B2—B2^vii	55.9 (5)
B1^ii—B1—B2^iv	115.5 (6)	B1^v—B2—B2^viii	104.3 (3)
B1^ii—B1—B2^v	65.4 (5)	B1^v—B2—B2	124.1 (4)
B1^ii—B1—N3	116.8 (8)	B2^vii—B2—B2^viii	60.0
B2^iii—B1—B2^iv	112.7 (7)	B2^vii—B2—B2	120.5 (6)
B2^iii—B1—B2^v	112.7 (7)	B2^viii—B2—B2	120.4 (6)
B2^iii—B1—N3	106.6 (15)	B1—N3—B1	119.90 (13)
B2^iv—B1—B2^v	68.3 (10)	B1—N3—B1	119.90 (13)
B2^iv—B1—N3	126.3 (9)	B1—N3—B4	91.8 (11)
B2^v—B1—N3	126.3 (9)	B1—N3—B1	119.90 (13)
B1^vi—B2—B1^iv	60.3 (7)	B1—N3—B4	91.8 (11)
B1^vi—B2—B1^v	60.3 (7)	B1—N3—B4	91.8 (11)
B1^vi—B2—B2^vii	102.8 (4)	N3—B4—N3^ix	180.0
B1^vi—B2—B2^viii	102.8 (4)

Symmetry codes: (i) −z−1, −x, −y; (ii) −y+1, −z+1, −x; (iii) x, y, z−1; (iv) −z−1, −x, −y+1; (v) −y+1, −z+1, −x+1; (vi) x, y, z+1; (vii) z+1, x+2, y; (viii) y−1, z+1, x; (ix) −x, −y, −z+1.

(phase_5) boric acid

Crystal data

H3BO3	Z = 6
Mr = 58.81	F(000) = 174
Trigonal, P32	Dx = 1.42 Mg m^−3
Hall symbol: P 32	Cu Kα radiation, λ = 1.540598 Å
a = 7.0453 Å	T = 297 K
c = 9.60 (1) Å	black
V = 412.67 Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B1	0.1837	0.6403	0.2849	0.025*
B2	0.518	0.3069	0.2964	0.025*
O3	0.0621	0.7393	0.2805	0.025*
O4	0.0864	0.4195	0.2808	0.025*
O5	0.409	0.765	0.2869	0.025*
O6	0.6437	0.2103	0.2929	0.025*
O7	0.295	0.1832	0.2998	0.025*
O8	0.6136	0.5294	0.2904	0.025*

Geometric parameters (Å, º)

B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B2^i	1.950 (9)	N3—B1	1.517 (12)
B1—B2	1.742 (14)	N3—B4	1.541 (16)
B1—B2	1.743 (14)	B4—B1	2.197 (13)
B1—N3	1.517 (12)	B4—B1	2.197 (13)
B1—B4	2.197 (13)	B4—B1	2.197 (13)
B2—B1^ii	1.950 (9)	B4—B1	2.197 (13)
B2—B1	1.743 (14)	B4—B1	2.197 (13)
B2—B1	1.742 (14)	B4—B1	2.197 (13)
B2—B2^iii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^iv	1.956 (12)	B4—N3	1.541 (16)
B2—B2	1.514 (11)
B1—B1—B1	98.2 (12)	B1^ii—B2—B2	129.4 (10)
B1—B1—B2^i	54.3 (8)	B1—B2—B1	107.9 (12)
B1—B1—B2	65.4 (5)	B1—B2—B2^iii	104.3 (3)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	55.9 (5)
B1—B1—N3	116.8 (8)	B1—B2—B2	124.0 (4)
B1—B1—B2^i	54.3 (8)	B1—B2—B2^iii	55.9 (5)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	104.3 (3)
B1—B1—B2	65.4 (5)	B1—B2—B2	124.1 (4)
B1—B1—N3	116.8 (8)	B2^iii—B2—B2^iv	60.0
B2^i—B1—B2	112.7 (7)	B2^iii—B2—B2	120.5 (6)
B2^i—B1—B2	112.7 (7)	B2^iv—B2—B2	120.4 (6)
B2^i—B1—N3	106.6 (15)	B1—N3—B1	119.90 (13)
B2—B1—B2	68.3 (10)	B1—N3—B1	119.90 (13)
B2—B1—N3	126.3 (9)	B1—N3—B4	91.8 (11)
B2—B1—N3	126.3 (9)	B1—N3—B1	119.90 (13)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B2^iii	102.8 (4)	N3—B4—N3	180.0
B1^ii—B2—B2^iv	102.8 (4)

Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) −y+1, x−y+2, z+2/3; (iv) y−x−1, −x+1, z+1/3.

(phase_6) boron nitride

Crystal data

BN	Z = 2
Mr = 24.82	F(000) = 24
Hexagonal, P6m2	Dx = 2.236 Mg m^−3
Hall symbol: P -6 2	Cu Kα radiation, λ = 1.540598 Å
a = 2.54 Å	T = 297 K
c = 6.598 (3) Å	black
V = 36.86 Å^3	flat_sheet, 0.2 × 0.2 mm

Data collection

G3000 TEXT Inel diffractometer	Specimen mounting: Si syngle crystal (111)
Radiation source: copper x-ray tube, CuKα	Data collection mode: reflection
Yes monochromator	Scan method: Stationary detector

Refinement

Least-squares matrix: full	Excluded region(s): unavoidable non-uniform strain render impossible to adjust the profile function parameters in a wide angle range.
Rp = 0.100	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = 95.838 #3(GW) = 7.893 #4(LX) = 1.057 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -0.9606 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 8.000 #4(LX) = 5.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = 20.000 #3(GW) = 30.000 #4(LX) = 0.000 #5(LY) = 0.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 5.000 #2(GV) = -5.000 #3(GW) = 12.000 #4(LX) = 2.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = -1.7500 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -2.000 #3(GW) = 786.199 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 2.000 #2(GV) = -5.000 #3(GW) = 591.058 #4(LX) = 1.000 #5(LY) = 1.000 #6(trns) = 0.000 #7(asym) = 0.0000 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.136	14 parameters
Rexp = 0.034	0 restraints
R(F^2) = 0.02645	(Δ/σ)max = 0.21
χ^2 = 15.761	Background function: GSAS Background function number 2 with 2 terms. Cosine Fourier series 1: 305.650 2: 196.641
5000 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.65811 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 0.10000 h= 0.000 k= 0.000 l= 1.000

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
B1	0.0	0.0	0.5	0.025*
B2	0.3333	0.6667	0.0	0.025*
N3	0.0	0.0	0.0	0.025*
N4	0.3333	0.6667	0.5	0.025*

Geometric parameters (Å, º)

B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B1	1.865 (17)	N3—B1	1.517 (12)
B1—B2^i	1.950 (9)	N3—B1	1.517 (12)
B1—B2	1.742 (14)	N3—B4	1.541 (16)
B1—B2	1.743 (14)	B4—B1	2.197 (13)
B1—N3	1.517 (12)	B4—B1	2.197 (13)
B1—B4	2.197 (13)	B4—B1	2.197 (13)
B2—B1^ii	1.950 (9)	B4—B1	2.197 (13)
B2—B1	1.743 (14)	B4—B1	2.197 (13)
B2—B1	1.742 (14)	B4—B1	2.197 (13)
B2—B2^iii	1.956 (12)	B4—N3	1.541 (16)
B2—B2^iv	1.956 (12)	B4—N3	1.541 (16)
B2—B2	1.514 (11)
B1—B1—B1	98.2 (12)	B1^ii—B2—B2	129.4 (10)
B1—B1—B2^i	54.3 (8)	B1—B2—B1	107.9 (12)
B1—B1—B2	65.4 (5)	B1—B2—B2^iii	104.3 (3)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	55.9 (5)
B1—B1—N3	116.8 (8)	B1—B2—B2	124.0 (4)
B1—B1—B2^i	54.3 (8)	B1—B2—B2^iii	55.9 (5)
B1—B1—B2	115.5 (6)	B1—B2—B2^iv	104.3 (3)
B1—B1—B2	65.4 (5)	B1—B2—B2	124.1 (4)
B1—B1—N3	116.8 (8)	B2^iii—B2—B2^iv	60.0
B2^i—B1—B2	112.7 (7)	B2^iii—B2—B2	120.5 (6)
B2^i—B1—B2	112.7 (7)	B2^iv—B2—B2	120.4 (6)
B2^i—B1—N3	106.6 (15)	B1—N3—B1	119.90 (13)
B2—B1—B2	68.3 (10)	B1—N3—B1	119.90 (13)
B2—B1—N3	126.3 (9)	B1—N3—B4	91.8 (11)
B2—B1—N3	126.3 (9)	B1—N3—B1	119.90 (13)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B1	60.3 (7)	B1—N3—B4	91.8 (11)
B1^ii—B2—B2^iii	102.8 (4)	N3—B4—N3	180.0
B1^ii—B2—B2^iv	102.8 (4)

Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) y−x+1, −x+2, −z; (iv) −y−1, x−y+1, z.