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Crystal structures of Sr3B2 + xSi1 − xO8 − x/2 solid solutions with nominal compositions x = 0.28, 0.53, 0.78 in the Sr3B2SiO8–Sr2B2O5 section of the SrO–B2O3–SiO2 system are refined using single-crystal X-ray diffraction data. Incommensurate structure modulations are mainly associated with various orientations of corner-sharing (B,Si)-polyhedra. Preference is given to the (3 + 2)-dimensional symmetry group Pnma(0βγ)000(0{\rm{\bar \beta }}γ)000 for a single crystal compared with an alternate model of a twin formed by monoclinic components, each of them corresponding to the (3 + 1)-dimensional symmetry group P21/n(0βγ). Single-phase polycrystalline samples of solid solutions are investigated by high-temperature X-ray powder diffraction in air. Orientation preferences of the BO3 units lead to a strong anisotropy of thermal expansion. Negative expansion is observed along the a axis over the temperature range 303–753 K. Anisotropy decreases both on heating and decreasing of the boron content.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615011713/dk5034sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034IIsup3.hkl
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034IIIsup4.hkl
Contains datablocks global, I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520615011713/dk5034sup5.pdf
Tables with structure and thermal expansion data

B-IncStrDB reference: 11322EzrAh2

CCDC references: 1407468; 1407469; 1407470

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(I) top
Crystal data top
B3.041O10.479Si0.959Sr4V = 259.04 Å3
Mr = 577.9Z = 1
Orthorhombic, PnmaF(000) = 264
Hall symbol: -P -2xabc;-2yb;-2zacDx = 3.705 Mg m3
a = 12.2774 ÅMo Kα radiation, λ = 0.71073 Å
b = 3.9006 ŵ = 20.64 mm1
c = 5.4091 ÅT = 293 K
Data collection top
Radiation source: X-ray tubeθmax = 43.2°, θmin = 4.1°
8190 measured reflectionsh = 2323
1031 independent reflectionsk = 77
428 reflections with I > 3σ(I)l = 93
Rint = 0.107
Refinement top
Refinement on F0 restraints
R[F2 > 2σ(F2)] = 0.0771 constraint
wR(F2) = 0.091Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 2.34(Δ/σ)max = 0.001
1031 reflectionsΔρmax = 3.58 e Å3
29 parametersΔρmin = 5.05 e Å3
Crystal data top
B3.041O10.479Si0.959Sr4V = 259.04 Å3
Mr = 577.9Z = 1
Orthorhombic, PnmaMo Kα radiation
a = 12.2774 ŵ = 20.64 mm1
b = 3.9006 ÅT = 293 K
c = 5.4091 Å
Data collection top
8190 measured reflections428 reflections with I > 3σ(I)
1031 independent reflectionsRint = 0.107
Refinement top
R[F2 > 2σ(F2)] = 0.07729 parameters
wR(F2) = 0.0910 restraints
S = 2.34Δρmax = 3.58 e Å3
1031 reflectionsΔρmin = 5.05 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sr0.14594 (9)0.750.90476 (13)0.0386 (3)
B0.4073 (18)0.820 (4)0.914 (4)0.0208 (18)*0.3802
Si0.4199 (10)0.750.944 (2)0.0208 (18)*0.2395
O10.4236 (12)0.750.681 (2)0.024 (2)*0.5
O20.510 (3)0.527 (7)0.919 (3)0.078 (7)*0.3097
O30.3340 (9)0.750.1031 (11)0.056 (3)
O40.3665 (12)0.750.675 (2)0.025 (2)*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr0.0765 (8)0.0153 (3)0.0241 (4)00.0166 (4)0
O30.102 (8)0.026 (3)0.040 (4)00.024 (4)0
Bond lengths (Å) top
Sr—Sri3.9006B—Si0.355 (19)
Sr—Srii3.9006B—Siii3.634 (15)
Sr—B3.22 (2)B—Sixvii3.17 (2)
Sr—Biii3.526 (18)B—Sixviii2.81 (2)
Sr—Biv3.598 (18)B—O11.30 (2)
Sr—Bv3.209 (19)B—O1ii3.845 (16)
Sr—Bvi3.288 (19)B—O1xvii3.75 (2)
Sr—Bvii3.41 (2)B—O1xviii3.46 (2)
Sr—Bviii3.41 (2)B—O21.71 (4)
Sr—Bix3.22 (2)B—O2ii3.03 (3)
Sr—Bx3.209 (19)B—O2xvii3.38 (3)
Sr—Bxi3.288 (19)B—O2xviii1.58 (3)
Sr—Bxii3.526 (18)B—O2xix1.92 (3)
Sr—Bxiii3.598 (18)B—O2xx2.88 (3)
Sr—Si3.370 (13)B—O2xxii3.54 (3)
Sr—Siiii3.266 (9)B—O2ix1.40 (4)
Sr—Siiv3.601 (10)B—O3xvi1.39 (2)
Sr—Siv3.266 (9)B—O3xxiii3.875 (16)
Sr—Sivi3.601 (10)B—O3vi3.80 (2)
Sr—Sivii3.355 (12)B—O3xxiv3.88 (2)
Sr—O13.618 (14)B—O3xxv3.59 (2)
Sr—O1iv2.600 (8)B—O41.41 (2)
Sr—O1vi2.600 (8)B—O4ii3.881 (17)
Sr—O1vii2.768 (14)B—O4xviii3.93 (2)
Sr—O2iii3.43 (2)Si—Sii3.9006
Sr—O2iv3.55 (2)Si—Siii3.9006
Sr—O2xiv3.88 (3)Si—Sixvii2.835 (13)
Sr—O2vii2.57 (3)Si—Sixviii2.835 (13)
Sr—O2viii2.57 (3)Si—O11.425 (16)
Sr—O2xv3.88 (3)Si—O1xvi3.985 (16)
Sr—O2xii3.43 (2)Si—O1xvii3.408 (14)
Sr—O2xiii3.55 (2)Si—O1xviii3.408 (14)
Sr—O3xvi2.546 (10)Si—O21.42 (3)
Sr—O3iv2.555 (4)Si—O2ii3.23 (3)
Sr—O3vi2.555 (4)Si—O2xvii3.04 (3)
Sr—O42.979 (14)Si—O2xviii1.56 (3)
Sr—O4iv2.444 (7)Si—O2xix1.56 (3)
Sr—O4vi2.444 (7)Si—O2xx3.04 (3)
Sr—O4vii3.458 (15)Si—O2xxii3.23 (3)
B—Bi3.90 (2)Si—O2ix1.42 (3)
B—Bii3.90 (2)Si—O3xvi1.362 (15)
B—Bxvii3.14 (3)Si—O3xxiv3.606 (14)
B—Bxviii3.14 (3)Si—O3xxv3.606 (14)
B—Bxix3.51 (3)Si—O41.593 (17)
B—Bxx2.83 (3)Si—O4xvii3.862 (16)
B—Bix0.55 (2)Si—O4xviii3.862 (16)
B—Bxxi3.35 (2)
Symmetry codes: (i) x, y1, z; (ii) x, y+1, z; (iii) x+1/2, y+1, z1/2; (iv) x+1/2, y+1, z+1/2; (v) x+1/2, y+2, z1/2; (vi) x+1/2, y+2, z+1/2; (vii) x1/2, y+3/2, z+3/2; (viii) x1/2, y, z+3/2; (ix) x, y+3/2, z; (x) x+1/2, y1/2, z1/2; (xi) x+1/2, y1/2, z+1/2; (xii) x+1/2, y+1/2, z1/2; (xiii) x+1/2, y+1/2, z+1/2; (xiv) x1/2, y+1/2, z+3/2; (xv) x1/2, y+1, z+3/2; (xvi) x, y, z+1; (xvii) x+1, y1/2, z+2; (xviii) x+1, y+1/2, z+2; (xix) x+1, y+1, z+2; (xx) x+1, y+2, z+2; (xxi) x, y+5/2, z; (xxii) x, y+1/2, z; (xxiii) x, y+1, z+1; (xxiv) x+1, y1/2, z+1; (xxv) x+1, y+1/2, z+1.
(II) top
Crystal data top
B3.376O10.312Si0.624Sr4V = 254.55 (9) Å3
Mr = 569.5Z = 1
Orthorhombic, PnmaF(000) = 260
q1 = 0.033000b* + 0.418000c*; q2 = -0.033000b* + 0.418000c*Dx = 3.715 Mg m3
a = 12.178 (2) ÅMo Kα radiation, λ = 0.71069 Å
b = 3.8801 (8) ŵ = 20.96 mm1
c = 5.3870 (11) ÅT = 293 K
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

Data collection top
IPDS Stoe
diffractometer
441 reflections with I > 3σ(I)
Radiation source: X-ray tubeRint = 0.054
Graphite monochromatorθmax = 29.2°, θmin = 2.3°
??integration method?? scansh = 1615
4274 measured reflectionsk = 55
1403 independent reflectionsl = 77
Refinement top
Refinement on F0 restraints
R[F2 > 2σ(F2)] = 0.0614 constraints
wR(F2) = 0.068Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 2.35(Δ/σ)max = 0.005
1403 reflectionsΔρmax = 0.94 e Å3
35 parametersΔρmin = 1.19 e Å3
Crystal data top
B3.376O10.312Si0.624Sr4c = 5.3870 (11) Å
Mr = 569.5V = 254.55 (9) Å3
Orthorhombic, PnmaZ = 1
q1 = 0.033000b* + 0.418000c*; q2 = -0.033000b* + 0.418000c*Mo Kα radiation
a = 12.178 (2) ŵ = 20.96 mm1
b = 3.8801 (8) ÅT = 293 K
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

Data collection top
IPDS Stoe
diffractometer
441 reflections with I > 3σ(I)
4274 measured reflectionsRint = 0.054
1403 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06135 parameters
wR(F2) = 0.0680 restraints
S = 2.35Δρmax = 0.94 e Å3
1403 reflectionsΔρmin = 1.19 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sr0.14481 (6)0.750.90534 (10)0.02953 (19)
B0.4089 (10)0.815 (2)0.916 (2)0.0202 (15)*0.422
Si0.4202 (11)0.750.949 (2)0.0202 (15)*0.156
O10.4301 (7)0.750.6826 (15)0.0221 (11)*0.5
O20.5088 (11)0.519 (4)0.917 (2)0.049 (3)*0.289
O30.3323 (4)0.750.1005 (9)0.0354 (13)*
O40.3681 (7)0.750.6769 (15)0.0221 (11)*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr0.0546 (4)0.0136 (2)0.0204 (3)00.0167 (3)0
Bond lengths (Å) top
AverageMinimumMaximum
Sr—Sri3.880133 (18)3.88010 (4)3.88020 (4)
Sr—Srii3.880132 (18)3.88010 (4)3.88020 (4)
Sr—B3.227 (13)3.097 (13)3.358 (13)
Sr—Biii3.492 (12)3.437 (12)3.548 (12)
Sr—Biv3.576 (12)3.550 (12)3.604 (12)
Sr—Bv3.201 (12)3.140 (13)3.261 (13)
Sr—Bvi3.292 (12)3.264 (13)3.322 (13)
Sr—Bvii3.363 (13)3.234 (13)3.492 (13)
Sr—Bviii3.363 (13)3.234 (13)3.492 (13)
Sr—Bix3.227 (13)3.097 (13)3.358 (13)
Sr—Bx3.201 (12)3.140 (13)3.261 (13)
Sr—Bxi3.292 (12)3.264 (13)3.322 (13)
Sr—Bxii3.492 (12)3.437 (12)3.548 (12)
Sr—Bxiii3.576 (12)3.550 (12)3.604 (12)
Sr—Si3.362 (14)3.230 (14)3.494 (14)
Sr—Siiii3.232 (11)3.170 (12)3.294 (12)
Sr—Siiv3.600 (12)3.573 (12)3.629 (12)
Sr—Siv3.232 (11)3.170 (12)3.294 (12)
Sr—Sivi3.600 (12)3.573 (12)3.629 (12)
Sr—Sivii3.336 (14)3.209 (14)3.463 (14)
Sr—O13.677 (10)3.563 (10)3.790 (10)
Sr—O1iv2.613 (6)2.581 (7)2.648 (7)
Sr—O1vi2.613 (6)2.581 (7)2.648 (7)
Sr—O1vii2.657 (10)2.524 (10)2.791 (10)
Sr—O2iii3.393 (13)3.294 (13)3.496 (13)
Sr—O2iv3.491 (13)3.447 (13)3.542 (13)
Sr—O2xiv3.828 (16)3.756 (16)3.902 (16)
Sr—O2vii2.561 (14)2.453 (14)2.671 (14)
Sr—O2viii2.561 (14)2.453 (14)2.671 (14)
Sr—O2xv3.828 (16)3.756 (16)3.902 (16)
Sr—O2xii3.393 (13)3.294 (13)3.496 (13)
Sr—O2xiii3.491 (13)3.447 (13)3.542 (13)
Sr—O3xvi2.51 (2)2.43 (2)2.60 (2)
Sr—O3iv2.561 (5)2.552 (7)2.578 (7)
Sr—O3vi2.562 (5)2.552 (7)2.578 (7)
Sr—O42.986 (10)2.879 (10)3.093 (10)
Sr—O4iv2.435 (6)2.412 (6)2.460 (6)
Sr—O4vi2.435 (6)2.412 (6)2.460 (6)
Sr—O4vii3.399 (10)3.266 (10)3.532 (10)
B—Bi3.880 (13)3.880 (13)3.880 (13)
B—Bii3.880 (13)3.880 (13)3.880 (13)
B—Bxvii3.083 (16)3.083 (16)3.083 (16)
B—Bxviii3.083 (16)3.083 (16)3.083 (16)
B—Bxix3.422 (15)3.422 (15)3.422 (15)
B—Bxx2.794 (16)2.794 (16)2.794 (16)
B—Bix0.503 (13)0.503 (13)0.503 (13)
B—Bxxi3.377 (13)3.377 (13)3.377 (13)
B—Si0.338 (14)0.338 (14)0.338 (14)
B—Siii3.636 (9)3.636 (9)3.636 (9)
B—Sixvii3.109 (15)3.109 (15)3.109 (15)
B—Sixviii2.777 (16)2.777 (16)2.777 (16)
B—O11.307 (15)1.307 (15)1.307 (15)
B—O1ii3.849 (10)3.848 (10)3.848 (10)
B—O1xvii3.650 (13)3.650 (13)3.650 (13)
B—O1xviii3.372 (14)3.372 (14)3.372 (14)
B—O21.673 (19)1.673 (19)1.673 (19)
B—O2ii2.989 (19)2.989 (19)2.989 (19)
B—O2xvii3.371 (19)3.371 (19)3.371 (19)
B—O2xviii1.564 (18)1.564 (18)1.564 (18)
B—O2xix1.869 (18)1.869 (18)1.869 (18)
B—O2xx2.917 (19)2.917 (19)2.917 (19)
B—O2xxii3.455 (19)3.455 (19)3.455 (19)
B—O2ix1.376 (19)1.376 (19)1.376 (19)
B—O3xvi1.39 (2)1.25 (2)1.54 (2)
B—O3xxiii3.879 (11)3.830 (12)3.935 (12)
B—O3iv4.05 (2)3.88 (2)4.20 (2)
B—O3vi3.80 (2)3.62 (2)3.96 (2)
B—O3xxiv3.85 (2)3.66 (2)4.02 (2)
B—O3xxv3.59 (2)3.39 (2)3.77 (2)
B—O41.403 (15)1.403 (15)1.403 (15)
B—O4ii3.882 (10)3.882 (10)3.882 (10)
B—O4xviii3.878 (14)3.878 (14)3.878 (14)
Si—Sii3.88013.88013.8801
Si—Siii3.88013.88013.8801
Si—Sixvii2.801 (14)2.801 (14)2.801 (14)
Si—Sixviii2.801 (14)2.801 (14)2.801 (14)
Si—O11.440 (15)1.440 (15)1.440 (15)
Si—O1xvi3.954 (15)3.954 (15)3.954 (15)
Si—O1xvii3.320 (13)3.320 (13)3.320 (13)
Si—O1xviii3.320 (13)3.320 (13)3.320 (13)
Si—O21.414 (18)1.414 (18)1.414 (18)
Si—O2ii3.176 (17)3.176 (17)3.176 (17)
Si—O2xvii3.054 (17)3.054 (17)3.054 (17)
Si—O2xviii1.536 (18)1.536 (18)1.536 (18)
Si—O2xix1.536 (18)1.536 (18)1.536 (18)
Si—O2xx3.054 (17)3.054 (17)3.054 (17)
Si—O2xxii3.176 (17)3.176 (17)3.176 (17)
Si—O2ix1.414 (18)1.414 (18)1.414 (18)
Si—O3xvi1.35 (2)1.18 (2)1.52 (2)
Si—O3iv4.10 (2)3.93 (2)4.26 (2)
Si—O3vi4.10 (2)3.93 (2)4.26 (2)
Si—O3xxiv3.60 (2)3.41 (2)3.78 (2)
Si—O3xxv3.60 (2)3.41 (2)3.78 (2)
Si—O41.597 (16)1.597 (16)1.597 (16)
Si—O4xvi3.972 (16)3.972 (16)3.972 (16)
Si—O4xvii3.804 (14)3.804 (14)3.804 (14)
Si—O4xviii3.804 (14)3.804 (14)3.804 (14)
Symmetry codes: (i) x1, x21, x3, x4, x5; (ii) x1, x2+1, x3, x4, x5; (iii) x1+1/2, x2+1, x31/2, x5, x4; (iv) x1+1/2, x2+1, x3+1/2, x5, x4; (v) x1+1/2, x2+2, x31/2, x5, x4; (vi) x1+1/2, x2+2, x3+1/2, x5, x4; (vii) x11/2, x2+3/2, x3+3/2, x4, x5; (viii) x11/2, x2, x3+3/2, x5, x4; (ix) x1, x2+3/2, x3, x5, x4; (x) x1+1/2, x21/2, x31/2, x4, x5; (xi) x1+1/2, x21/2, x3+1/2, x4, x5; (xii) x1+1/2, x2+1/2, x31/2, x4, x5; (xiii) x1+1/2, x2+1/2, x3+1/2, x4, x5; (xiv) x11/2, x2+1/2, x3+3/2, x4, x5; (xv) x11/2, x2+1, x3+3/2, x5, x4; (xvi) x1, x2, x3+1, x4, x5; (xvii) x1+1, x21/2, x3+2, x5, x4; (xviii) x1+1, x2+1/2, x3+2, x5, x4; (xix) x1+1, x2+1, x3+2, x4, x5; (xx) x1+1, x2+2, x3+2, x4, x5; (xxi) x1, x2+5/2, x3, x5, x4; (xxii) x1, x2+1/2, x3, x5, x4; (xxiii) x1, x2+1, x3+1, x4, x5; (xxiv) x1+1, x21/2, x3+1, x5, x4; (xxv) x1+1, x2+1/2, x3+1, x5, x4.
(III) top
Crystal data top
B3.704O10.148Si0.296Sr4V = 251.18 Å3
Mr = 561.2Z = 1
Orthorhombic, PnmaF(000) = 256
q1 = 0.041000b* + 0.378000c*; q2 = -0.041000b* + 0.378000c*Dx = 3.71 Mg m3
a = 12.089 ÅMo Kα radiation, λ = 0.71069 Å
b = 3.8635 ŵ = 21.20 mm1
c = 5.378 ÅT = 293 K
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

Data collection top
IPDS Stoe
diffractometer
431 reflections with I > 3σ(I)
Radiation source: X-ray tubeRint = 0.087
Graphite monochromatorθmax = 29.2°, θmin = 2.2°
??integration method?? scansh = 1616
4765 measured reflectionsk = 55
1431 independent reflectionsl = 77
Refinement top
Refinement on F0 restraints
R[F2 > 2σ(F2)] = 0.0814 constraints
wR(F2) = 0.083Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 2.64(Δ/σ)max = 0.006
1431 reflectionsΔρmax = 1.09 e Å3
35 parametersΔρmin = 4.63 e Å3
Crystal data top
B3.704O10.148Si0.296Sr4c = 5.378 Å
Mr = 561.2V = 251.18 Å3
Orthorhombic, PnmaZ = 1
q1 = 0.041000b* + 0.378000c*; q2 = -0.041000b* + 0.378000c*Mo Kα radiation
a = 12.089 ŵ = 21.20 mm1
b = 3.8635 ÅT = 293 K
† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

Data collection top
IPDS Stoe
diffractometer
431 reflections with I > 3σ(I)
4765 measured reflectionsRint = 0.087
1431 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.08135 parameters
wR(F2) = 0.0830 restraints
S = 2.64Δρmax = 1.09 e Å3
1431 reflectionsΔρmin = 4.63 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sr0.14443 (7)0.750.90653 (14)0.0238 (3)
B0.4082 (12)0.816 (2)0.924 (3)0.019 (3)*0.463
Si0.422 (3)0.750.952 (8)0.019 (3)*0.074
O10.4304 (10)0.750.692 (2)0.0244 (15)*0.5
O20.5067 (15)0.493 (5)0.908 (3)0.046 (4)*0.2685
O30.3336 (6)0.750.0995 (13)0.0335 (17)*
O40.3669 (10)0.750.683 (2)0.0244 (15)*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr0.0433 (7)0.0125 (3)0.0157 (5)00.0109 (5)0
Bond lengths (Å) top
AverageMinimumMaximum
Sr—Sri3.86360 (5)3.86350 (12)3.86387 (12)
Sr—Srii3.86360 (5)3.86350 (12)3.86387 (12)
Sr—Sriii4.109 (7)3.929 (7)4.306 (7)
Sr—Sriv4.110 (7)3.929 (7)4.306 (7)
Sr—B3.198 (16)3.019 (16)3.384 (16)
Sr—Bv3.454 (16)3.415 (16)3.498 (16)
Sr—Bvi3.599 (16)3.495 (16)3.710 (16)
Sr—Bvii3.155 (17)3.112 (17)3.204 (17)
Sr—Bviii3.313 (17)3.200 (17)3.433 (17)
Sr—Bix3.378 (17)3.270 (17)3.488 (17)
Sr—Bx3.378 (17)3.270 (17)3.488 (17)
Sr—Bxi3.198 (16)3.019 (16)3.384 (16)
Sr—Bxii3.155 (17)3.112 (17)3.204 (17)
Sr—Bxiii3.313 (17)3.200 (17)3.433 (17)
Sr—Bxiv3.454 (16)3.415 (16)3.498 (16)
Sr—Bxv3.599 (16)3.495 (16)3.710 (16)
Sr—Si3.36 (4)3.19 (4)3.54 (4)
Sr—Siv3.22 (3)3.19 (3)3.25 (3)
Sr—Sivi3.61 (4)3.49 (4)3.73 (4)
Sr—Sivii3.22 (3)3.19 (3)3.25 (3)
Sr—Siviii3.61 (4)3.49 (4)3.73 (4)
Sr—Siix3.31 (4)3.22 (4)3.41 (4)
Sr—O13.655 (14)3.437 (14)3.851 (14)
Sr—O1vi2.623 (9)2.515 (10)2.739 (10)
Sr—O1viii2.623 (9)2.515 (10)2.739 (10)
Sr—O1ix2.647 (14)2.481 (14)2.807 (14)
Sr—O2v3.384 (19)3.348 (19)3.417 (19)
Sr—O2vi3.424 (19)3.270 (19)3.568 (19)
Sr—O2xvi3.72 (2)3.69 (2)3.77 (2)
Sr—O2ix2.570 (19)2.517 (19)2.641 (19)
Sr—O2x2.570 (19)2.517 (19)2.641 (19)
Sr—O2xvii3.72 (2)3.69 (2)3.77 (2)
Sr—O2xiv3.383 (19)3.348 (19)3.417 (19)
Sr—O2xv3.423 (19)3.270 (19)3.568 (19)
Sr—O3xviii2.51 (3)2.42 (4)2.60 (4)
Sr—O3vi2.560 (8)2.479 (11)2.669 (11)
Sr—O3viii2.560 (8)2.479 (11)2.668 (11)
Sr—O42.934 (13)2.737 (14)3.156 (14)
Sr—O4vi2.447 (8)2.389 (9)2.517 (9)
Sr—O4viii2.448 (8)2.391 (9)2.517 (9)
Sr—O4ix3.388 (13)3.221 (13)3.562 (13)
B—Bi3.864 (13)3.864 (13)3.864 (13)
B—Bii3.864 (13)3.864 (13)3.864 (13)
B—Bxix3.053 (19)3.053 (19)3.053 (19)
B—Bxx3.053 (19)3.053 (19)3.053 (19)
B—Bxxi3.400 (18)3.400 (18)3.400 (18)
B—Bxxii2.76 (2)2.76 (2)2.76 (2)
B—Bxi0.511 (13)0.511 (13)0.511 (13)
B—Bxxiii3.352 (13)3.352 (13)3.352 (13)
B—Si0.34 (3)0.34 (3)0.34 (3)
B—Siii3.615 (9)3.615 (9)3.615 (9)
B—Sixix3.07 (3)3.07 (3)3.07 (3)
B—Sixx2.73 (4)2.73 (4)2.73 (4)
B—O11.30 (2)1.30 (2)1.30 (2)
B—O1ii3.827 (11)3.827 (11)3.827 (11)
B—O1xix3.583 (17)3.583 (17)3.583 (17)
B—O1xx3.296 (18)3.296 (18)3.296 (18)
B—O21.73 (2)1.73 (2)1.73 (2)
B—O2ii2.88 (2)2.88 (2)2.88 (2)
B—O2xix3.46 (2)3.46 (2)3.46 (2)
B—O2xx1.53 (2)1.53 (2)1.53 (2)
B—O2xxi1.82 (2)1.82 (2)1.82 (2)
B—O2xxii3.00 (2)3.00 (2)3.00 (2)
B—O2xxiv3.35 (2)3.35 (2)3.35 (2)
B—O2xi1.40 (2)1.40 (2)1.40 (2)
B—O3xviii1.33 (3)1.19 (3)1.49 (3)
B—O3xxv3.838 (14)3.789 (15)3.897 (15)
B—O3vi4.06 (3)3.88 (3)4.22 (3)
B—O3viii3.80 (3)3.62 (4)3.98 (4)
B—O3xxvi3.82 (3)3.63 (4)4.00 (4)
B—O3xxvii3.56 (4)3.35 (4)3.75 (4)
B—O41.42 (2)1.42 (2)1.42 (2)
B—O4ii3.867 (11)3.867 (11)3.867 (11)
B—O4viii3.974 (18)3.974 (18)3.974 (18)
B—O4xx3.830 (18)3.830 (18)3.830 (18)
Si—Sii3.86353.86353.8635
Si—Siii3.86353.86353.8635
Si—Sixix2.75 (4)2.75 (4)2.75 (4)
Si—Sixx2.75 (4)2.75 (4)2.75 (4)
Si—O11.40 (4)1.40 (4)1.40 (4)
Si—O1xviii3.98 (4)3.98 (4)3.98 (4)
Si—O1xix3.25 (3)3.25 (3)3.25 (3)
Si—O1xx3.25 (3)3.25 (3)3.25 (3)
Si—O21.45 (4)1.45 (4)1.45 (4)
Si—O2ii3.06 (2)3.06 (2)3.06 (2)
Si—O2xix3.14 (3)3.14 (3)3.14 (3)
Si—O2xx1.48 (4)1.48 (4)1.48 (4)
Si—O2xxi1.48 (4)1.48 (4)1.48 (4)
Si—O2xxii3.14 (3)3.14 (3)3.14 (3)
Si—O2xxiv3.06 (2)3.06 (2)3.06 (2)
Si—O2xi1.45 (4)1.45 (4)1.45 (4)
Si—O3xviii1.33 (5)1.15 (5)1.52 (5)
Si—O3vi4.12 (5)3.94 (5)4.28 (5)
Si—O3viii4.12 (5)3.94 (5)4.28 (5)
Si—O3xxvi3.55 (5)3.35 (5)3.74 (5)
Si—O3xxvii3.55 (5)3.35 (5)3.74 (5)
Si—O41.60 (4)1.60 (4)1.60 (4)
Si—O4xviii3.98 (4)3.98 (4)3.98 (4)
Si—O4xix3.75 (4)3.75 (4)3.75 (4)
Si—O4xx3.75 (4)3.75 (4)3.75 (4)
Symmetry codes: (i) x1, x21, x3, x4, x5; (ii) x1, x2+1, x3, x4, x5; (iii) x1, x21/2, x3+2, x5, x4; (iv) x1, x2+1/2, x3+2, x5, x4; (v) x1+1/2, x2+1, x31/2, x5, x4; (vi) x1+1/2, x2+1, x3+1/2, x5, x4; (vii) x1+1/2, x2+2, x31/2, x5, x4; (viii) x1+1/2, x2+2, x3+1/2, x5, x4; (ix) x11/2, x2+3/2, x3+3/2, x4, x5; (x) x11/2, x2, x3+3/2, x5, x4; (xi) x1, x2+3/2, x3, x5, x4; (xii) x1+1/2, x21/2, x31/2, x4, x5; (xiii) x1+1/2, x21/2, x3+1/2, x4, x5; (xiv) x1+1/2, x2+1/2, x31/2, x4, x5; (xv) x1+1/2, x2+1/2, x3+1/2, x4, x5; (xvi) x11/2, x2+1/2, x3+3/2, x4, x5; (xvii) x11/2, x2+1, x3+3/2, x5, x4; (xviii) x1, x2, x3+1, x4, x5; (xix) x1+1, x21/2, x3+2, x5, x4; (xx) x1+1, x2+1/2, x3+2, x5, x4; (xxi) x1+1, x2+1, x3+2, x4, x5; (xxii) x1+1, x2+2, x3+2, x4, x5; (xxiii) x1, x2+5/2, x3, x5, x4; (xxiv) x1, x2+1/2, x3, x5, x4; (xxv) x1, x2+1, x3+1, x4, x5; (xxvi) x1+1, x21/2, x3+1, x5, x4; (xxvii) x1+1, x2+1/2, x3+1, x5, x4.

Experimental details

(I)(II)(III)
Crystal data
Chemical formulaB3.041O10.479Si0.959Sr4B3.376O10.312Si0.624Sr4B3.704O10.148Si0.296Sr4
Mr577.9569.5561.2
Crystal system, space groupOrthorhombic, PnmaOrthorhombic, PnmaOrthorhombic, Pnma
Temperature (K)293293293
a, b, c (Å)12.2774, 3.9006, 5.4091??
V3)259.0490, 90, 9090, 90, 90
Z1254.55 (9)251.18
Radiation typeMo Kα??
µ (mm1)20.64??
Crystal size (mm) × ×
Data collection
Diffractometer?IPDS Stoe
diffractometer
IPDS Stoe
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 3σ(I)] reflections
8190, 1031, 428 4274, 1403, 441 4765, 1431, 431
Rint0.1070.0540.087
(sin θ/λ)max1)0.9640.6850.686
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.077, 0.091, 2.34 0.061, 0.068, 2.35 0.081, 0.083, 2.64
No. of reflections103114031431
No. of parameters293535
Δρmax, Δρmin (e Å3)3.58, 5.050.94, 1.191.09, 4.63

† Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

‡ Symmetry operations: (1) x1, x2, x3, x4, x5; (2) −x1+1/2, −x2, x3+1/2, x5, x4; (3) −x1, x2+1/2, −x3, −x5, −x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4, −x5; (5) −x1, −x2, −x3, −x4, −x5; (6) x1+1/2, x2, −x3+1/2, −x5, −x4; (7) x1, −x2+1/2, x3, x5, x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4, x5.

 

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