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Almost absorption- and extinction-free single-crystal synchrotron X-ray diffraction data were measured at 150, 200 and 295 K for β-Si3N4, silicon nitride, at a wavelength of 0.7 Å. The true symmetry of this material has been the subject of minor controversy for several decades. No compelling evidence favouring the low-symmetry P63 model was identified in this study.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810401393X/av5009sup1.cif
Contains datablocks 295K-C, 295K-N, 200K-C, 200K-N, 150K-C, 150K-N

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810401393X/av5009295K-Csup2.hkl
Contains datablock 295K-C

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810401393X/av5009200K-Csup3.hkl
Contains datablock 200K-C

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010876810401393X/av5009150K-Csup4.hkl
Contains datablock 150K-C

Computing details top

For all compounds, data collection: Diff14A, Vaalsta & Hester 1997; cell refinement: Xtal3.7 LATCON; data reduction: Xtal DIFDAT SORTRF ABSORB ADDREF; program(s) used to solve structure: already known structure; program(s) used to refine structure: Xtal CRYLSQ; molecular graphics: Xtal; software used to prepare material for publication: Xtal BONDLA CIFIO.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
(295K-C) top
Crystal data top
N4Si3Dx = 3.202 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75022 Å
Hexagonal, P63/mCell parameters from 21 reflections
Hall symbol: -p 6cθ = 45.8–63.9°
a = 7.6044 (1) ŵ = 1.53 mm1
c = 2.9063 (1) ÅT = 295 K
V = 145.55 (1) Å3Spheroid, colourless
Z = 1.50.08 × 0.08 × 0.08 × 0.04 (radius) mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
792 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.025
Double Si monochromatorθmax = 65.0°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: for a sphere
?
k = 1818
Tmin = 0.939, Tmax = 0.940l = 77
8577 measured reflections6 standard reflections every 100 reflections
800 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.020(Δ/σ)max = 0.00029
wR(F2) = 0.015Δρmax = 0.61 e Å3
S = 2.01Δρmin = 0.53 e Å3
796 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
16 parametersExtinction coefficient: 1587 (307)
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75022 Å
Hexagonal, P63/mµ = 1.53 mm1
a = 7.6044 (1) ÅT = 295 K
c = 2.9063 (1) Å0.08 × 0.08 × 0.08 × 0.04 (radius) mm
V = 145.55 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
792 reflections with F > .00 sig(F )
Absorption correction: for a sphere
?
Rint = 0.025
Tmin = 0.939, Tmax = 0.9406 standard reflections every 100 reflections
8577 measured reflections intensity decay: none
800 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.015Δρmax = 0.61 e Å3
S = 2.01Δρmin = 0.53 e Å3
796 reflectionsAbsolute structure: see text
16 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.768477 (16)0.174557 (15)0.250000.00293 (3)
N10.03050 (4)0.33024 (4)0.250000.00413 (6)
N20.666660.333330.250000.00398 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00312 (3)0.00284 (3)0.00270 (3)0.00139 (3)0.000000.00000
N10.00312 (7)0.00548 (7)0.00297 (7)0.00153 (6)0.000000.00000
N20.00332 (7)0.00332 (7)0.00530 (12)0.00166 (4)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7298 (1)Si—N11.7357 (2)
Si—N11.7357 (3)Si—N11.7357 (2)
N2—Si—N1106.602 (13)Si—N1—Si123.038 (8)
N2—Si—N1110.103 (13)Si—N1—Si123.038 (8)
N2—Si—N1110.103 (13)Si—N1—Si113.697 (15)
N1—Si—N1108.024 (12)Si—N2—Si119.998 (6)
N1—Si—N1108.024 (12)Si—N2—Si120.002 (5)
N1—Si—N1113.697 (12)Si—N2—Si120.001 (7)
(295K-N) top
Crystal data top
N4Si3Dx = 3.202 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75022 Å
Hexagonal, P63Cell parameters from 21 reflections
Hall symbol: p 6cθ = 45.8–63.9°
a = 7.6044 (1) ŵ = 1.53 mm1
c = 2.9063 (1) ÅT = 295 K
V = 145.55 (1) Å3Spheroid, colourless
Z = 1.50.08 × 0.08 × 0.08 × 0.04 (radius) mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
792 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.025
Double Si monochromatorθmax = 65.0°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: for a sphere
?
k = 1818
Tmin = 0.939, Tmax = 0.940l = 77
8577 measured reflections6 standard reflections every 100 reflections
800 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.018(Δ/σ)max = 0.001
wR(F2) = 0.014Δρmax = 0.53 e Å3
S = 1.88Δρmin = 0.48 e Å3
796 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
22 parametersExtinction coefficient: 2099 (391)
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75022 Å
Hexagonal, P63µ = 1.53 mm1
a = 7.6044 (1) ÅT = 295 K
c = 2.9063 (1) Å0.08 × 0.08 × 0.08 × 0.04 (radius) mm
V = 145.55 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
792 reflections with F > .00 sig(F )
Absorption correction: for a sphere
?
Rint = 0.025
Tmin = 0.939, Tmax = 0.9406 standard reflections every 100 reflections
8577 measured reflections intensity decay: none
800 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0180 restraints
wR(F2) = 0.014Δρmax = 0.53 e Å3
S = 1.88Δρmin = 0.48 e Å3
796 reflectionsAbsolute structure: see text
22 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.768473 (15)0.174555 (15)0.250000.00299 (3)
N10.03055 (4)0.33028 (4)0.2487 (6)0.00418 (6)
N20.666660.333330.2515 (11)0.00401 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00316 (3)0.00289 (3)0.00278 (3)0.00142 (2)0.00135 (11)0.00108 (11)
N10.00311 (6)0.00553 (7)0.00304 (7)0.00151 (6)0.0011 (3)0.0007 (3)
N20.00334 (7)0.00334 (7)0.00534 (12)0.00167 (3)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7297 (1)Si—N11.7387 (14)
Si—N11.7361 (3)Si—N11.7323 (14)
N2—Si—N1106.601 (14)Si—N1—Si123.22 (8)
N2—Si—N1110.19 (10)Si—N1—Si122.83 (8)
N2—Si—N1110.00 (10)Si—N1—Si113.716 (15)
N1—Si—N1107.88 (5)Si—N2—Si119.997 (4)
N1—Si—N1108.17 (5)Si—N2—Si120.001 (4)
N1—Si—N1113.72 (4)Si—N2—Si120.000 (6)
(200K-C) top
Crystal data top
N4Si3Dx = 3.204 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63/mCell parameters from 12 reflections
Hall symbol: -p 6cθ = 52.4–56.0°
a = 7.6015 (3) ŵ = 1.54 mm1
c = 2.9061 (1) ÅT = 200 K
V = 145.43 (1) Å3Irregular, colourless
Z = 1.50.04 × 0.03 × 0.02 mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
852 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.028
Double Si monochromatorθmax = 68.9°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: analytical
?
k = 1818
Tmin = 0.932, Tmax = 0.972l = 77
12331 measured reflections6 standard reflections every 200 reflections
866 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.014(Δ/σ)max = 0.001
wR(F2) = 0.011Δρmax = 0.45 e Å3
S = 1.89Δρmin = 0.37 e Å3
866 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
16 parametersExtinction coefficient: 1296 (439)
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63/mµ = 1.54 mm1
a = 7.6015 (3) ÅT = 200 K
c = 2.9061 (1) Å0.04 × 0.03 × 0.02 mm
V = 145.43 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
852 reflections with F > .00 sig(F )
Absorption correction: analytical
?
Rint = 0.028
Tmin = 0.932, Tmax = 0.9726 standard reflections every 200 reflections
12331 measured reflections intensity decay: none
866 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0140 restraints
wR(F2) = 0.011Δρmax = 0.45 e Å3
S = 1.89Δρmin = 0.37 e Å3
866 reflectionsAbsolute structure: see text
16 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.768477 (9)0.174569 (9)0.250000.00286 (2)
N10.03049 (2)0.33026 (3)0.250000.00393 (4)
N20.666660.333330.250000.00382 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00313 (2)0.00294 (2)0.00243 (3)0.001459 (16)0.000000.00000
N10.00322 (4)0.00502 (4)0.00283 (4)0.00153 (3)0.000000.00000
N20.00342 (4)0.00342 (4)0.00464 (8)0.00171 (2)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7290 (1)Si—N11.7354 (1)
Si—N11.7351 (2)Si—N11.7354 (1)
N2—Si—N1106.600 (9)Si—N1—Si123.032 (5)
N2—Si—N1110.096 (8)Si—N1—Si123.032 (5)
N2—Si—N1110.096 (8)Si—N1—Si113.708 (10)
N1—Si—N1108.026 (8)Si—N2—Si119.998 (5)
N1—Si—N1108.026 (8)Si—N2—Si120.002 (4)
N1—Si—N1113.708 (8)Si—N2—Si120.001 (4)
(200K-N) top
Crystal data top
N4Si3Dx = 3.204 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63Cell parameters from 12 reflections
Hall symbol: p 6cθ = 52.4–56.0°
a = 7.6015 (3) ŵ = 1.54 mm1
c = 2.9061 (1) ÅT = 200 K
V = 145.43 (1) Å3Irregular, colourless
Z = 1.50.04 × 0.03 × 0.02 mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
852 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.028
Double Si monochromatorθmax = 68.9°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: analytical
?
k = 1818
Tmin = 0.932, Tmax = 0.972l = 77
12331 measured reflections6 standard reflections every 200 reflections
866 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.013(Δ/σ)max = 0.004
wR(F2) = 0.011Δρmax = 0.38 e Å3
S = 1.76Δρmin = 0.34 e Å3
866 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
21 parametersExtinction coefficient: 1600.000
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63µ = 1.54 mm1
a = 7.6015 (3) ÅT = 200 K
c = 2.9061 (1) Å0.04 × 0.03 × 0.02 mm
V = 145.43 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
852 reflections with F > .00 sig(F )
Absorption correction: analytical
?
Rint = 0.028
Tmin = 0.932, Tmax = 0.9726 standard reflections every 200 reflections
12331 measured reflections intensity decay: none
866 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0130 restraints
wR(F2) = 0.011Δρmax = 0.38 e Å3
S = 1.76Δρmin = 0.34 e Å3
866 reflectionsAbsolute structure: see text
21 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.768482 (9)0.174583 (9)0.250000.00272 (2)
N10.03051 (2)0.33030 (3)0.2485 (4)0.00380 (3)
N20.666660.333330.2469 (9)0.00366 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00298 (2)0.00279 (2)0.00230 (2)0.001377 (14)0.00009 (11)0.00006 (11)
N10.00307 (4)0.00486 (4)0.00277 (4)0.00146 (3)0.0001 (2)0.0008 (2)
N20.00324 (4)0.00324 (4)0.00449 (9)0.00162 (2)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7290 (1)Si—N11.7352 (2)
Si—N11.7319 (10)Si—N11.7390 (10)
N2—Si—N1110.40 (8)Si—N1—Si123.25 (6)
N2—Si—N1106.599 (9)Si—N1—Si113.710 (9)
N2—Si—N1109.78 (8)Si—N1—Si122.82 (6)
N1—Si—N1108.19 (4)Si—N2—Si119.999 (5)
N1—Si—N1113.71 (3)Si—N2—Si119.998 (4)
N1—Si—N1107.87 (4)Si—N2—Si119.995 (5)
(150K-C) top
Crystal data top
N4Si3Dx = 3.204 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63/mCell parameters from 12 reflections
Hall symbol: -p 6cθ = 52.3–56.0°
a = 7.6020 (2) ŵ = 1.54 mm1
c = 2.9060 (1) ÅT = 150 K
V = 145.44 (1) Å3Irregular, colourless
Z = 1.50.04 × 0.03 × 0.02 mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
786 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.027
Double Si monochromatorθmax = 65.1°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: analytical
?
k = 1818
Tmin = 0.932, Tmax = 0.972l = 77
8549 measured reflections6 standard reflections every 100 reflections
796 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.014(Δ/σ)max = 0.002
wR(F2) = 0.014Δρmax = 0.51 e Å3
S = 1.84Δρmin = 0.40 e Å3
796 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
16 parametersExtinction coefficient: 2090 (375)
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63/mµ = 1.54 mm1
a = 7.6020 (2) ÅT = 150 K
c = 2.9060 (1) Å0.04 × 0.03 × 0.02 mm
V = 145.44 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
786 reflections with F > .00 sig(F )
Absorption correction: analytical
?
Rint = 0.027
Tmin = 0.932, Tmax = 0.9726 standard reflections every 100 reflections
8549 measured reflections intensity decay: none
796 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0140 restraints
wR(F2) = 0.014Δρmax = 0.51 e Å3
S = 1.84Δρmin = 0.40 e Å3
796 reflectionsAbsolute structure: see text
16 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.768477 (12)0.174561 (12)0.250000.00248 (2)
N10.03050 (3)0.33025 (3)0.250000.00352 (5)
N20.666660.333330.250000.00343 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00272 (3)0.00255 (3)0.00211 (3)0.00127 (2)0.000000.00000
N10.00293 (5)0.00444 (5)0.00259 (5)0.00139 (4)0.000000.00000
N20.00306 (5)0.00306 (5)0.00415 (9)0.00153 (3)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7292 (1)Si—N11.7354 (1)
Si—N11.7352 (2)Si—N11.7354 (1)
N2—Si—N1106.601 (11)Si—N1—Si123.033 (7)
N2—Si—N1110.098 (10)Si—N1—Si123.033 (7)
N2—Si—N1110.098 (10)Si—N1—Si113.708 (12)
N1—Si—N1108.023 (9)Si—N2—Si119.998 (4)
N1—Si—N1108.023 (9)Si—N2—Si120.002 (5)
N1—Si—N1113.708 (10)Si—N2—Si120.001 (4)
(150K-N) top
Crystal data top
N4Si3Dx = 3.204 Mg m3
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63Cell parameters from 12 reflections
Hall symbol: p 6cθ = 52.3–56.0°
a = 7.6020 (2) ŵ = 1.54 mm1
c = 2.9060 (1) ÅT = 150 K
V = 145.44 (1) Å3Irregular, colourless
Z = 1.50.04 × 0.03 × 0.02 mm
F(000) = 140
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
787 reflections with F > .00 sig(F )
Radiation source: SynchrotronRint = 0.027
Double Si monochromatorθmax = 65.1°, θmin = 3.3°
%w/2%q scansh = 1818
Absorption correction: analytical
?
k = 1818
Tmin = 0.932, Tmax = 0.972l = 77
8549 measured reflections6 standard reflections every 100 reflections
800 independent reflections intensity decay: none
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.015(Δ/σ)max = 0.001
wR(F2) = 0.014Δρmax = 0.44 e Å3
S = 1.84Δρmin = 0.44 e Å3
265 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
22 parametersExtinction coefficient: 384 (489)
0 restraintsAbsolute structure: see text
Crystal data top
N4Si3Z = 1.5
Mr = 140.31Syn x radiation, λ = 0.75037 Å
Hexagonal, P63µ = 1.54 mm1
a = 7.6020 (2) ÅT = 150 K
c = 2.9060 (1) Å0.04 × 0.03 × 0.02 mm
V = 145.44 (1) Å3
Data collection top
PF-BL14A Rigaku 4circle
diffractometer
787 reflections with F > .00 sig(F )
Absorption correction: analytical
?
Rint = 0.027
Tmin = 0.932, Tmax = 0.9726 standard reflections every 100 reflections
8549 measured reflections intensity decay: none
800 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0150 restraints
wR(F2) = 0.014Δρmax = 0.44 e Å3
S = 1.84Δρmin = 0.44 e Å3
265 reflectionsAbsolute structure: see text
22 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si0.76847 (2)0.17453 (2)0.250000.00246 (4)
N10.03054 (5)0.33023 (6)0.2459 (6)0.00343 (7)
N20.666660.333330.2502 (17)0.00338 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si0.00268 (4)0.00254 (4)0.00209 (4)0.00126 (3)0.0001 (2)0.0002 (2)
N10.00287 (8)0.00428 (9)0.00252 (9)0.00133 (7)0.0000 (4)0.0009 (4)
N20.00304 (8)0.00304 (8)0.00406 (14)0.00152 (4)0.000000.00000
Geometric parameters (Å, º) top
Si—N21.7294 (1)Si—N11.7451 (15)
Si—N11.7355 (4)Si—N11.7252 (15)
N2—Si—N1106.602 (18)Si—N1—Si123.63 (9)
N2—Si—N1110.00 (15)Si—N1—Si122.42 (9)
N2—Si—N1110.20 (15)Si—N1—Si113.73 (2)
N1—Si—N1107.56 (6)Si—N2—Si119.997 (7)
N1—Si—N1108.46 (6)Si—N2—Si120.002 (6)
N1—Si—N1113.73 (5)Si—N2—Si120.001 (8)

Experimental details

(295K-C)(295K-N)(200K-C)(200K-N)
Crystal data
Chemical formulaN4Si3N4Si3N4Si3N4Si3
Mr140.31140.31140.31140.31
Crystal system, space groupHexagonal, P63/mHexagonal, P63Hexagonal, P63/mHexagonal, P63
Temperature (K)295295200200
a, c (Å)7.6044 (1), 2.9063 (1)7.6044 (1), 2.9063 (1)7.6015 (3), 2.9061 (1)7.6015 (3), 2.9061 (1)
V3)145.55 (1)145.55 (1)145.43 (1)145.43 (1)
Z1.51.51.51.5
Radiation typeSyn x, λ = 0.75022 ÅSyn x, λ = 0.75022 ÅSyn x, λ = 0.75037 ÅSyn x, λ = 0.75037 Å
µ (mm1)1.531.531.541.54
Crystal size (mm)0.08 × 0.08 × 0.08 × 0.04 (radius)0.08 × 0.08 × 0.08 × 0.04 (radius)0.04 × 0.03 × 0.020.04 × 0.03 × 0.02
Data collection
DiffractometerPF-BL14A Rigaku 4circle
diffractometer
PF-BL14A Rigaku 4circle
diffractometer
PF-BL14A Rigaku 4circle
diffractometer
PF-BL14A Rigaku 4circle
diffractometer
Absorption correctionFor a sphereFor a sphereAnalyticalAnalytical
Tmin, Tmax0.939, 0.9400.939, 0.9400.932, 0.9720.932, 0.972
No. of measured, independent and
observed [F > .00 sig(F )] reflections
8577, 800, 792 8577, 800, 792 12331, 866, 852 12331, 866, 852
Rint0.0250.0250.0280.028
(sin θ/λ)max1)1.2081.2081.2431.243
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.015, 2.01 0.018, 0.014, 1.88 0.014, 0.011, 1.89 0.013, 0.011, 1.76
No. of reflections796796866866
No. of parameters16221621
Δρmax, Δρmin (e Å3)0.61, 0.530.53, 0.480.45, 0.370.38, 0.34
Absolute structureSee textSee textSee textSee text


(150K-C)(150K-N)
Crystal data
Chemical formulaN4Si3N4Si3
Mr140.31140.31
Crystal system, space groupHexagonal, P63/mHexagonal, P63
Temperature (K)150150
a, c (Å)7.6020 (2), 2.9060 (1)7.6020 (2), 2.9060 (1)
V3)145.44 (1)145.44 (1)
Z1.51.5
Radiation typeSyn x, λ = 0.75037 ÅSyn x, λ = 0.75037 Å
µ (mm1)1.541.54
Crystal size (mm)0.04 × 0.03 × 0.020.04 × 0.03 × 0.02
Data collection
DiffractometerPF-BL14A Rigaku 4circle
diffractometer
PF-BL14A Rigaku 4circle
diffractometer
Absorption correctionAnalyticalAnalytical
Tmin, Tmax0.932, 0.9720.932, 0.972
No. of measured, independent and
observed [F > .00 sig(F )] reflections
8549, 796, 786 8549, 800, 787
Rint0.0270.027
(sin θ/λ)max1)1.2081.208
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.014, 0.014, 1.84 0.015, 0.014, 1.84
No. of reflections796265
No. of parameters1622
Δρmax, Δρmin (e Å3)0.51, 0.400.44, 0.44
Absolute structureSee textSee text

Computer programs: Diff14A, Vaalsta & Hester 1997, Xtal3.7 LATCON, Xtal DIFDAT SORTRF ABSORB ADDREF, already known structure, Xtal CRYLSQ, Xtal BONDLA CIFIO.

 

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