Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615011713/dk5034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615011713/dk5034IIIsup4.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520615011713/dk5034sup5.pdf |
B-IncStrDB reference: 11322EzrAh2
CCDC references: 1407468; 1407469; 1407470
B3.041O10.479Si0.959Sr4 | V = 259.04 Å3 |
Mr = 577.9 | Z = 1 |
Orthorhombic, Pnma | F(000) = 264 |
Hall symbol: -P -2xabc;-2yb;-2zac | Dx = 3.705 Mg m−3 |
a = 12.2774 Å | Mo Kα radiation, λ = 0.71073 Å |
b = 3.9006 Å | µ = 20.64 mm−1 |
c = 5.4091 Å | T = 293 K |
Radiation source: X-ray tube | θmax = 43.2°, θmin = 4.1° |
8190 measured reflections | h = −23→23 |
1031 independent reflections | k = −7→7 |
428 reflections with I > 3σ(I) | l = −9→3 |
Rint = 0.107 |
Refinement on F | 0 restraints |
R[F2 > 2σ(F2)] = 0.077 | 1 constraint |
wR(F2) = 0.091 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 2.34 | (Δ/σ)max = 0.001 |
1031 reflections | Δρmax = 3.58 e Å−3 |
29 parameters | Δρmin = −5.05 e Å−3 |
B3.041O10.479Si0.959Sr4 | V = 259.04 Å3 |
Mr = 577.9 | Z = 1 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 12.2774 Å | µ = 20.64 mm−1 |
b = 3.9006 Å | T = 293 K |
c = 5.4091 Å |
8190 measured reflections | 428 reflections with I > 3σ(I) |
1031 independent reflections | Rint = 0.107 |
R[F2 > 2σ(F2)] = 0.077 | 29 parameters |
wR(F2) = 0.091 | 0 restraints |
S = 2.34 | Δρmax = 3.58 e Å−3 |
1031 reflections | Δρmin = −5.05 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sr | 0.14594 (9) | 0.75 | 0.90476 (13) | 0.0386 (3) | |
B | 0.4073 (18) | 0.820 (4) | 0.914 (4) | 0.0208 (18)* | 0.3802 |
Si | 0.4199 (10) | 0.75 | 0.944 (2) | 0.0208 (18)* | 0.2395 |
O1 | 0.4236 (12) | 0.75 | 0.681 (2) | 0.024 (2)* | 0.5 |
O2 | 0.510 (3) | 0.527 (7) | 0.919 (3) | 0.078 (7)* | 0.3097 |
O3 | 0.3340 (9) | 0.75 | 0.1031 (11) | 0.056 (3) | |
O4 | 0.3665 (12) | 0.75 | 0.675 (2) | 0.025 (2)* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr | 0.0765 (8) | 0.0153 (3) | 0.0241 (4) | 0 | −0.0166 (4) | 0 |
O3 | 0.102 (8) | 0.026 (3) | 0.040 (4) | 0 | 0.024 (4) | 0 |
Sr—Sri | 3.9006 | B—Si | 0.355 (19) |
Sr—Srii | 3.9006 | B—Siii | 3.634 (15) |
Sr—B | 3.22 (2) | B—Sixvii | 3.17 (2) |
Sr—Biii | 3.526 (18) | B—Sixviii | 2.81 (2) |
Sr—Biv | 3.598 (18) | B—O1 | 1.30 (2) |
Sr—Bv | 3.209 (19) | B—O1ii | 3.845 (16) |
Sr—Bvi | 3.288 (19) | B—O1xvii | 3.75 (2) |
Sr—Bvii | 3.41 (2) | B—O1xviii | 3.46 (2) |
Sr—Bviii | 3.41 (2) | B—O2 | 1.71 (4) |
Sr—Bix | 3.22 (2) | B—O2ii | 3.03 (3) |
Sr—Bx | 3.209 (19) | B—O2xvii | 3.38 (3) |
Sr—Bxi | 3.288 (19) | B—O2xviii | 1.58 (3) |
Sr—Bxii | 3.526 (18) | B—O2xix | 1.92 (3) |
Sr—Bxiii | 3.598 (18) | B—O2xx | 2.88 (3) |
Sr—Si | 3.370 (13) | B—O2xxii | 3.54 (3) |
Sr—Siiii | 3.266 (9) | B—O2ix | 1.40 (4) |
Sr—Siiv | 3.601 (10) | B—O3xvi | 1.39 (2) |
Sr—Siv | 3.266 (9) | B—O3xxiii | 3.875 (16) |
Sr—Sivi | 3.601 (10) | B—O3vi | 3.80 (2) |
Sr—Sivii | 3.355 (12) | B—O3xxiv | 3.88 (2) |
Sr—O1 | 3.618 (14) | B—O3xxv | 3.59 (2) |
Sr—O1iv | 2.600 (8) | B—O4 | 1.41 (2) |
Sr—O1vi | 2.600 (8) | B—O4ii | 3.881 (17) |
Sr—O1vii | 2.768 (14) | B—O4xviii | 3.93 (2) |
Sr—O2iii | 3.43 (2) | Si—Sii | 3.9006 |
Sr—O2iv | 3.55 (2) | Si—Siii | 3.9006 |
Sr—O2xiv | 3.88 (3) | Si—Sixvii | 2.835 (13) |
Sr—O2vii | 2.57 (3) | Si—Sixviii | 2.835 (13) |
Sr—O2viii | 2.57 (3) | Si—O1 | 1.425 (16) |
Sr—O2xv | 3.88 (3) | Si—O1xvi | 3.985 (16) |
Sr—O2xii | 3.43 (2) | Si—O1xvii | 3.408 (14) |
Sr—O2xiii | 3.55 (2) | Si—O1xviii | 3.408 (14) |
Sr—O3xvi | 2.546 (10) | Si—O2 | 1.42 (3) |
Sr—O3iv | 2.555 (4) | Si—O2ii | 3.23 (3) |
Sr—O3vi | 2.555 (4) | Si—O2xvii | 3.04 (3) |
Sr—O4 | 2.979 (14) | Si—O2xviii | 1.56 (3) |
Sr—O4iv | 2.444 (7) | Si—O2xix | 1.56 (3) |
Sr—O4vi | 2.444 (7) | Si—O2xx | 3.04 (3) |
Sr—O4vii | 3.458 (15) | Si—O2xxii | 3.23 (3) |
B—Bi | 3.90 (2) | Si—O2ix | 1.42 (3) |
B—Bii | 3.90 (2) | Si—O3xvi | 1.362 (15) |
B—Bxvii | 3.14 (3) | Si—O3xxiv | 3.606 (14) |
B—Bxviii | 3.14 (3) | Si—O3xxv | 3.606 (14) |
B—Bxix | 3.51 (3) | Si—O4 | 1.593 (17) |
B—Bxx | 2.83 (3) | Si—O4xvii | 3.862 (16) |
B—Bix | 0.55 (2) | Si—O4xviii | 3.862 (16) |
B—Bxxi | 3.35 (2) |
Symmetry codes: (i) x, y−1, z; (ii) x, y+1, z; (iii) −x+1/2, −y+1, z−1/2; (iv) −x+1/2, −y+1, z+1/2; (v) −x+1/2, −y+2, z−1/2; (vi) −x+1/2, −y+2, z+1/2; (vii) x−1/2, −y+3/2, −z+3/2; (viii) x−1/2, y, −z+3/2; (ix) x, −y+3/2, z; (x) −x+1/2, y−1/2, z−1/2; (xi) −x+1/2, y−1/2, z+1/2; (xii) −x+1/2, y+1/2, z−1/2; (xiii) −x+1/2, y+1/2, z+1/2; (xiv) x−1/2, −y+1/2, −z+3/2; (xv) x−1/2, y+1, −z+3/2; (xvi) x, y, z+1; (xvii) −x+1, y−1/2, −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, y−1/2, −z+1; (xxv) −x+1, y+1/2, −z+1. |
B3.376O10.312Si0.624Sr4 | V = 254.55 (9) Å3 |
Mr = 569.5 | Z = 1 |
Orthorhombic, Pnma† | F(000) = 260 |
q1 = 0.033000b* + 0.418000c*; q2 = -0.033000b* + 0.418000c* | Dx = 3.715 Mg m−3 |
a = 12.178 (2) Å | Mo Kα radiation, λ = 0.71069 Å |
b = 3.8801 (8) Å | µ = 20.96 mm−1 |
c = 5.3870 (11) Å | T = 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. |
IPDS Stoe diffractometer | 441 reflections with I > 3σ(I) |
Radiation source: X-ray tube | Rint = 0.054 |
Graphite monochromator | θmax = 29.2°, θmin = 2.3° |
??integration method?? scans | h = −16→15 |
4274 measured reflections | k = −5→5 |
1403 independent reflections | l = −7→7 |
Refinement on F | 0 restraints |
R[F2 > 2σ(F2)] = 0.061 | 4 constraints |
wR(F2) = 0.068 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 2.35 | (Δ/σ)max = 0.005 |
1403 reflections | Δρmax = 0.94 e Å−3 |
35 parameters | Δρmin = −1.19 e Å−3 |
B3.376O10.312Si0.624Sr4 | c = 5.3870 (11) Å |
Mr = 569.5 | V = 254.55 (9) Å3 |
Orthorhombic, Pnma† | Z = 1 |
q1 = 0.033000b* + 0.418000c*; q2 = -0.033000b* + 0.418000c* | Mo Kα radiation |
a = 12.178 (2) Å | µ = 20.96 mm−1 |
b = 3.8801 (8) Å | T = 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. |
IPDS Stoe diffractometer | 441 reflections with I > 3σ(I) |
4274 measured reflections | Rint = 0.054 |
1403 independent reflections |
R[F2 > 2σ(F2)] = 0.061 | 35 parameters |
wR(F2) = 0.068 | 0 restraints |
S = 2.35 | Δρmax = 0.94 e Å−3 |
1403 reflections | Δρmin = −1.19 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sr | 0.14481 (6) | 0.75 | 0.90534 (10) | 0.02953 (19) | |
B | 0.4089 (10) | 0.815 (2) | 0.916 (2) | 0.0202 (15)* | 0.422 |
Si | 0.4202 (11) | 0.75 | 0.949 (2) | 0.0202 (15)* | 0.156 |
O1 | 0.4301 (7) | 0.75 | 0.6826 (15) | 0.0221 (11)* | 0.5 |
O2 | 0.5088 (11) | 0.519 (4) | 0.917 (2) | 0.049 (3)* | 0.289 |
O3 | 0.3323 (4) | 0.75 | 0.1005 (9) | 0.0354 (13)* | |
O4 | 0.3681 (7) | 0.75 | 0.6769 (15) | 0.0221 (11)* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr | 0.0546 (4) | 0.0136 (2) | 0.0204 (3) | 0 | −0.0167 (3) | 0 |
Average | Minimum | Maximum | |
Sr—Sri | 3.880133 (18) | 3.88010 (4) | 3.88020 (4) |
Sr—Srii | 3.880132 (18) | 3.88010 (4) | 3.88020 (4) |
Sr—B | 3.227 (13) | 3.097 (13) | 3.358 (13) |
Sr—Biii | 3.492 (12) | 3.437 (12) | 3.548 (12) |
Sr—Biv | 3.576 (12) | 3.550 (12) | 3.604 (12) |
Sr—Bv | 3.201 (12) | 3.140 (13) | 3.261 (13) |
Sr—Bvi | 3.292 (12) | 3.264 (13) | 3.322 (13) |
Sr—Bvii | 3.363 (13) | 3.234 (13) | 3.492 (13) |
Sr—Bviii | 3.363 (13) | 3.234 (13) | 3.492 (13) |
Sr—Bix | 3.227 (13) | 3.097 (13) | 3.358 (13) |
Sr—Bx | 3.201 (12) | 3.140 (13) | 3.261 (13) |
Sr—Bxi | 3.292 (12) | 3.264 (13) | 3.322 (13) |
Sr—Bxii | 3.492 (12) | 3.437 (12) | 3.548 (12) |
Sr—Bxiii | 3.576 (12) | 3.550 (12) | 3.604 (12) |
Sr—Si | 3.362 (14) | 3.230 (14) | 3.494 (14) |
Sr—Siiii | 3.232 (11) | 3.170 (12) | 3.294 (12) |
Sr—Siiv | 3.600 (12) | 3.573 (12) | 3.629 (12) |
Sr—Siv | 3.232 (11) | 3.170 (12) | 3.294 (12) |
Sr—Sivi | 3.600 (12) | 3.573 (12) | 3.629 (12) |
Sr—Sivii | 3.336 (14) | 3.209 (14) | 3.463 (14) |
Sr—O1 | 3.677 (10) | 3.563 (10) | 3.790 (10) |
Sr—O1iv | 2.613 (6) | 2.581 (7) | 2.648 (7) |
Sr—O1vi | 2.613 (6) | 2.581 (7) | 2.648 (7) |
Sr—O1vii | 2.657 (10) | 2.524 (10) | 2.791 (10) |
Sr—O2iii | 3.393 (13) | 3.294 (13) | 3.496 (13) |
Sr—O2iv | 3.491 (13) | 3.447 (13) | 3.542 (13) |
Sr—O2xiv | 3.828 (16) | 3.756 (16) | 3.902 (16) |
Sr—O2vii | 2.561 (14) | 2.453 (14) | 2.671 (14) |
Sr—O2viii | 2.561 (14) | 2.453 (14) | 2.671 (14) |
Sr—O2xv | 3.828 (16) | 3.756 (16) | 3.902 (16) |
Sr—O2xii | 3.393 (13) | 3.294 (13) | 3.496 (13) |
Sr—O2xiii | 3.491 (13) | 3.447 (13) | 3.542 (13) |
Sr—O3xvi | 2.51 (2) | 2.43 (2) | 2.60 (2) |
Sr—O3iv | 2.561 (5) | 2.552 (7) | 2.578 (7) |
Sr—O3vi | 2.562 (5) | 2.552 (7) | 2.578 (7) |
Sr—O4 | 2.986 (10) | 2.879 (10) | 3.093 (10) |
Sr—O4iv | 2.435 (6) | 2.412 (6) | 2.460 (6) |
Sr—O4vi | 2.435 (6) | 2.412 (6) | 2.460 (6) |
Sr—O4vii | 3.399 (10) | 3.266 (10) | 3.532 (10) |
B—Bi | 3.880 (13) | 3.880 (13) | 3.880 (13) |
B—Bii | 3.880 (13) | 3.880 (13) | 3.880 (13) |
B—Bxvii | 3.083 (16) | 3.083 (16) | 3.083 (16) |
B—Bxviii | 3.083 (16) | 3.083 (16) | 3.083 (16) |
B—Bxix | 3.422 (15) | 3.422 (15) | 3.422 (15) |
B—Bxx | 2.794 (16) | 2.794 (16) | 2.794 (16) |
B—Bix | 0.503 (13) | 0.503 (13) | 0.503 (13) |
B—Bxxi | 3.377 (13) | 3.377 (13) | 3.377 (13) |
B—Si | 0.338 (14) | 0.338 (14) | 0.338 (14) |
B—Siii | 3.636 (9) | 3.636 (9) | 3.636 (9) |
B—Sixvii | 3.109 (15) | 3.109 (15) | 3.109 (15) |
B—Sixviii | 2.777 (16) | 2.777 (16) | 2.777 (16) |
B—O1 | 1.307 (15) | 1.307 (15) | 1.307 (15) |
B—O1ii | 3.849 (10) | 3.848 (10) | 3.848 (10) |
B—O1xvii | 3.650 (13) | 3.650 (13) | 3.650 (13) |
B—O1xviii | 3.372 (14) | 3.372 (14) | 3.372 (14) |
B—O2 | 1.673 (19) | 1.673 (19) | 1.673 (19) |
B—O2ii | 2.989 (19) | 2.989 (19) | 2.989 (19) |
B—O2xvii | 3.371 (19) | 3.371 (19) | 3.371 (19) |
B—O2xviii | 1.564 (18) | 1.564 (18) | 1.564 (18) |
B—O2xix | 1.869 (18) | 1.869 (18) | 1.869 (18) |
B—O2xx | 2.917 (19) | 2.917 (19) | 2.917 (19) |
B—O2xxii | 3.455 (19) | 3.455 (19) | 3.455 (19) |
B—O2ix | 1.376 (19) | 1.376 (19) | 1.376 (19) |
B—O3xvi | 1.39 (2) | 1.25 (2) | 1.54 (2) |
B—O3xxiii | 3.879 (11) | 3.830 (12) | 3.935 (12) |
B—O3iv | 4.05 (2) | 3.88 (2) | 4.20 (2) |
B—O3vi | 3.80 (2) | 3.62 (2) | 3.96 (2) |
B—O3xxiv | 3.85 (2) | 3.66 (2) | 4.02 (2) |
B—O3xxv | 3.59 (2) | 3.39 (2) | 3.77 (2) |
B—O4 | 1.403 (15) | 1.403 (15) | 1.403 (15) |
B—O4ii | 3.882 (10) | 3.882 (10) | 3.882 (10) |
B—O4xviii | 3.878 (14) | 3.878 (14) | 3.878 (14) |
Si—Sii | 3.8801 | 3.8801 | 3.8801 |
Si—Siii | 3.8801 | 3.8801 | 3.8801 |
Si—Sixvii | 2.801 (14) | 2.801 (14) | 2.801 (14) |
Si—Sixviii | 2.801 (14) | 2.801 (14) | 2.801 (14) |
Si—O1 | 1.440 (15) | 1.440 (15) | 1.440 (15) |
Si—O1xvi | 3.954 (15) | 3.954 (15) | 3.954 (15) |
Si—O1xvii | 3.320 (13) | 3.320 (13) | 3.320 (13) |
Si—O1xviii | 3.320 (13) | 3.320 (13) | 3.320 (13) |
Si—O2 | 1.414 (18) | 1.414 (18) | 1.414 (18) |
Si—O2ii | 3.176 (17) | 3.176 (17) | 3.176 (17) |
Si—O2xvii | 3.054 (17) | 3.054 (17) | 3.054 (17) |
Si—O2xviii | 1.536 (18) | 1.536 (18) | 1.536 (18) |
Si—O2xix | 1.536 (18) | 1.536 (18) | 1.536 (18) |
Si—O2xx | 3.054 (17) | 3.054 (17) | 3.054 (17) |
Si—O2xxii | 3.176 (17) | 3.176 (17) | 3.176 (17) |
Si—O2ix | 1.414 (18) | 1.414 (18) | 1.414 (18) |
Si—O3xvi | 1.35 (2) | 1.18 (2) | 1.52 (2) |
Si—O3iv | 4.10 (2) | 3.93 (2) | 4.26 (2) |
Si—O3vi | 4.10 (2) | 3.93 (2) | 4.26 (2) |
Si—O3xxiv | 3.60 (2) | 3.41 (2) | 3.78 (2) |
Si—O3xxv | 3.60 (2) | 3.41 (2) | 3.78 (2) |
Si—O4 | 1.597 (16) | 1.597 (16) | 1.597 (16) |
Si—O4xvi | 3.972 (16) | 3.972 (16) | 3.972 (16) |
Si—O4xvii | 3.804 (14) | 3.804 (14) | 3.804 (14) |
Si—O4xviii | 3.804 (14) | 3.804 (14) | 3.804 (14) |
Symmetry codes: (i) x1, x2−1, x3, x4, x5; (ii) x1, x2+1, x3, x4, x5; (iii) −x1+1/2, −x2+1, x3−1/2, x5, x4; (iv) −x1+1/2, −x2+1, x3+1/2, x5, x4; (v) −x1+1/2, −x2+2, x3−1/2, x5, x4; (vi) −x1+1/2, −x2+2, x3+1/2, x5, x4; (vii) x1−1/2, −x2+3/2, −x3+3/2, −x4, −x5; (viii) x1−1/2, x2, −x3+3/2, −x5, −x4; (ix) x1, −x2+3/2, x3, x5, x4; (x) −x1+1/2, x2−1/2, x3−1/2, x4, x5; (xi) −x1+1/2, x2−1/2, x3+1/2, x4, x5; (xii) −x1+1/2, x2+1/2, x3−1/2, x4, x5; (xiii) −x1+1/2, x2+1/2, x3+1/2, x4, x5; (xiv) x1−1/2, −x2+1/2, −x3+3/2, −x4, −x5; (xv) x1−1/2, x2+1, −x3+3/2, −x5, −x4; (xvi) x1, x2, x3+1, x4, x5; (xvii) −x1+1, x2−1/2, −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, x2−1/2, −x3+1, −x5, −x4; (xxv) −x1+1, x2+1/2, −x3+1, −x5, −x4. |
B3.704O10.148Si0.296Sr4 | V = 251.18 Å3 |
Mr = 561.2 | Z = 1 |
Orthorhombic, Pnma† | F(000) = 256 |
q1 = 0.041000b* + 0.378000c*; q2 = -0.041000b* + 0.378000c* | Dx = 3.71 Mg m−3 |
a = 12.089 Å | Mo Kα radiation, λ = 0.71069 Å |
b = 3.8635 Å | µ = 21.20 mm−1 |
c = 5.378 Å | T = 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. |
IPDS Stoe diffractometer | 431 reflections with I > 3σ(I) |
Radiation source: X-ray tube | Rint = 0.087 |
Graphite monochromator | θmax = 29.2°, θmin = 2.2° |
??integration method?? scans | h = −16→16 |
4765 measured reflections | k = −5→5 |
1431 independent reflections | l = −7→7 |
Refinement on F | 0 restraints |
R[F2 > 2σ(F2)] = 0.081 | 4 constraints |
wR(F2) = 0.083 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 2.64 | (Δ/σ)max = 0.006 |
1431 reflections | Δρmax = 1.09 e Å−3 |
35 parameters | Δρmin = −4.63 e Å−3 |
B3.704O10.148Si0.296Sr4 | c = 5.378 Å |
Mr = 561.2 | V = 251.18 Å3 |
Orthorhombic, Pnma† | Z = 1 |
q1 = 0.041000b* + 0.378000c*; q2 = -0.041000b* + 0.378000c* | Mo Kα radiation |
a = 12.089 Å | µ = 21.20 mm−1 |
b = 3.8635 Å | T = 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. |
IPDS Stoe diffractometer | 431 reflections with I > 3σ(I) |
4765 measured reflections | Rint = 0.087 |
1431 independent reflections |
R[F2 > 2σ(F2)] = 0.081 | 35 parameters |
wR(F2) = 0.083 | 0 restraints |
S = 2.64 | Δρmax = 1.09 e Å−3 |
1431 reflections | Δρmin = −4.63 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sr | 0.14443 (7) | 0.75 | 0.90653 (14) | 0.0238 (3) | |
B | 0.4082 (12) | 0.816 (2) | 0.924 (3) | 0.019 (3)* | 0.463 |
Si | 0.422 (3) | 0.75 | 0.952 (8) | 0.019 (3)* | 0.074 |
O1 | 0.4304 (10) | 0.75 | 0.692 (2) | 0.0244 (15)* | 0.5 |
O2 | 0.5067 (15) | 0.493 (5) | 0.908 (3) | 0.046 (4)* | 0.2685 |
O3 | 0.3336 (6) | 0.75 | 0.0995 (13) | 0.0335 (17)* | |
O4 | 0.3669 (10) | 0.75 | 0.683 (2) | 0.0244 (15)* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr | 0.0433 (7) | 0.0125 (3) | 0.0157 (5) | 0 | −0.0109 (5) | 0 |
Average | Minimum | Maximum | |
Sr—Sri | 3.86360 (5) | 3.86350 (12) | 3.86387 (12) |
Sr—Srii | 3.86360 (5) | 3.86350 (12) | 3.86387 (12) |
Sr—Sriii | 4.109 (7) | 3.929 (7) | 4.306 (7) |
Sr—Sriv | 4.110 (7) | 3.929 (7) | 4.306 (7) |
Sr—B | 3.198 (16) | 3.019 (16) | 3.384 (16) |
Sr—Bv | 3.454 (16) | 3.415 (16) | 3.498 (16) |
Sr—Bvi | 3.599 (16) | 3.495 (16) | 3.710 (16) |
Sr—Bvii | 3.155 (17) | 3.112 (17) | 3.204 (17) |
Sr—Bviii | 3.313 (17) | 3.200 (17) | 3.433 (17) |
Sr—Bix | 3.378 (17) | 3.270 (17) | 3.488 (17) |
Sr—Bx | 3.378 (17) | 3.270 (17) | 3.488 (17) |
Sr—Bxi | 3.198 (16) | 3.019 (16) | 3.384 (16) |
Sr—Bxii | 3.155 (17) | 3.112 (17) | 3.204 (17) |
Sr—Bxiii | 3.313 (17) | 3.200 (17) | 3.433 (17) |
Sr—Bxiv | 3.454 (16) | 3.415 (16) | 3.498 (16) |
Sr—Bxv | 3.599 (16) | 3.495 (16) | 3.710 (16) |
Sr—Si | 3.36 (4) | 3.19 (4) | 3.54 (4) |
Sr—Siv | 3.22 (3) | 3.19 (3) | 3.25 (3) |
Sr—Sivi | 3.61 (4) | 3.49 (4) | 3.73 (4) |
Sr—Sivii | 3.22 (3) | 3.19 (3) | 3.25 (3) |
Sr—Siviii | 3.61 (4) | 3.49 (4) | 3.73 (4) |
Sr—Siix | 3.31 (4) | 3.22 (4) | 3.41 (4) |
Sr—O1 | 3.655 (14) | 3.437 (14) | 3.851 (14) |
Sr—O1vi | 2.623 (9) | 2.515 (10) | 2.739 (10) |
Sr—O1viii | 2.623 (9) | 2.515 (10) | 2.739 (10) |
Sr—O1ix | 2.647 (14) | 2.481 (14) | 2.807 (14) |
Sr—O2v | 3.384 (19) | 3.348 (19) | 3.417 (19) |
Sr—O2vi | 3.424 (19) | 3.270 (19) | 3.568 (19) |
Sr—O2xvi | 3.72 (2) | 3.69 (2) | 3.77 (2) |
Sr—O2ix | 2.570 (19) | 2.517 (19) | 2.641 (19) |
Sr—O2x | 2.570 (19) | 2.517 (19) | 2.641 (19) |
Sr—O2xvii | 3.72 (2) | 3.69 (2) | 3.77 (2) |
Sr—O2xiv | 3.383 (19) | 3.348 (19) | 3.417 (19) |
Sr—O2xv | 3.423 (19) | 3.270 (19) | 3.568 (19) |
Sr—O3xviii | 2.51 (3) | 2.42 (4) | 2.60 (4) |
Sr—O3vi | 2.560 (8) | 2.479 (11) | 2.669 (11) |
Sr—O3viii | 2.560 (8) | 2.479 (11) | 2.668 (11) |
Sr—O4 | 2.934 (13) | 2.737 (14) | 3.156 (14) |
Sr—O4vi | 2.447 (8) | 2.389 (9) | 2.517 (9) |
Sr—O4viii | 2.448 (8) | 2.391 (9) | 2.517 (9) |
Sr—O4ix | 3.388 (13) | 3.221 (13) | 3.562 (13) |
B—Bi | 3.864 (13) | 3.864 (13) | 3.864 (13) |
B—Bii | 3.864 (13) | 3.864 (13) | 3.864 (13) |
B—Bxix | 3.053 (19) | 3.053 (19) | 3.053 (19) |
B—Bxx | 3.053 (19) | 3.053 (19) | 3.053 (19) |
B—Bxxi | 3.400 (18) | 3.400 (18) | 3.400 (18) |
B—Bxxii | 2.76 (2) | 2.76 (2) | 2.76 (2) |
B—Bxi | 0.511 (13) | 0.511 (13) | 0.511 (13) |
B—Bxxiii | 3.352 (13) | 3.352 (13) | 3.352 (13) |
B—Si | 0.34 (3) | 0.34 (3) | 0.34 (3) |
B—Siii | 3.615 (9) | 3.615 (9) | 3.615 (9) |
B—Sixix | 3.07 (3) | 3.07 (3) | 3.07 (3) |
B—Sixx | 2.73 (4) | 2.73 (4) | 2.73 (4) |
B—O1 | 1.30 (2) | 1.30 (2) | 1.30 (2) |
B—O1ii | 3.827 (11) | 3.827 (11) | 3.827 (11) |
B—O1xix | 3.583 (17) | 3.583 (17) | 3.583 (17) |
B—O1xx | 3.296 (18) | 3.296 (18) | 3.296 (18) |
B—O2 | 1.73 (2) | 1.73 (2) | 1.73 (2) |
B—O2ii | 2.88 (2) | 2.88 (2) | 2.88 (2) |
B—O2xix | 3.46 (2) | 3.46 (2) | 3.46 (2) |
B—O2xx | 1.53 (2) | 1.53 (2) | 1.53 (2) |
B—O2xxi | 1.82 (2) | 1.82 (2) | 1.82 (2) |
B—O2xxii | 3.00 (2) | 3.00 (2) | 3.00 (2) |
B—O2xxiv | 3.35 (2) | 3.35 (2) | 3.35 (2) |
B—O2xi | 1.40 (2) | 1.40 (2) | 1.40 (2) |
B—O3xviii | 1.33 (3) | 1.19 (3) | 1.49 (3) |
B—O3xxv | 3.838 (14) | 3.789 (15) | 3.897 (15) |
B—O3vi | 4.06 (3) | 3.88 (3) | 4.22 (3) |
B—O3viii | 3.80 (3) | 3.62 (4) | 3.98 (4) |
B—O3xxvi | 3.82 (3) | 3.63 (4) | 4.00 (4) |
B—O3xxvii | 3.56 (4) | 3.35 (4) | 3.75 (4) |
B—O4 | 1.42 (2) | 1.42 (2) | 1.42 (2) |
B—O4ii | 3.867 (11) | 3.867 (11) | 3.867 (11) |
B—O4viii | 3.974 (18) | 3.974 (18) | 3.974 (18) |
B—O4xx | 3.830 (18) | 3.830 (18) | 3.830 (18) |
Si—Sii | 3.8635 | 3.8635 | 3.8635 |
Si—Siii | 3.8635 | 3.8635 | 3.8635 |
Si—Sixix | 2.75 (4) | 2.75 (4) | 2.75 (4) |
Si—Sixx | 2.75 (4) | 2.75 (4) | 2.75 (4) |
Si—O1 | 1.40 (4) | 1.40 (4) | 1.40 (4) |
Si—O1xviii | 3.98 (4) | 3.98 (4) | 3.98 (4) |
Si—O1xix | 3.25 (3) | 3.25 (3) | 3.25 (3) |
Si—O1xx | 3.25 (3) | 3.25 (3) | 3.25 (3) |
Si—O2 | 1.45 (4) | 1.45 (4) | 1.45 (4) |
Si—O2ii | 3.06 (2) | 3.06 (2) | 3.06 (2) |
Si—O2xix | 3.14 (3) | 3.14 (3) | 3.14 (3) |
Si—O2xx | 1.48 (4) | 1.48 (4) | 1.48 (4) |
Si—O2xxi | 1.48 (4) | 1.48 (4) | 1.48 (4) |
Si—O2xxii | 3.14 (3) | 3.14 (3) | 3.14 (3) |
Si—O2xxiv | 3.06 (2) | 3.06 (2) | 3.06 (2) |
Si—O2xi | 1.45 (4) | 1.45 (4) | 1.45 (4) |
Si—O3xviii | 1.33 (5) | 1.15 (5) | 1.52 (5) |
Si—O3vi | 4.12 (5) | 3.94 (5) | 4.28 (5) |
Si—O3viii | 4.12 (5) | 3.94 (5) | 4.28 (5) |
Si—O3xxvi | 3.55 (5) | 3.35 (5) | 3.74 (5) |
Si—O3xxvii | 3.55 (5) | 3.35 (5) | 3.74 (5) |
Si—O4 | 1.60 (4) | 1.60 (4) | 1.60 (4) |
Si—O4xviii | 3.98 (4) | 3.98 (4) | 3.98 (4) |
Si—O4xix | 3.75 (4) | 3.75 (4) | 3.75 (4) |
Si—O4xx | 3.75 (4) | 3.75 (4) | 3.75 (4) |
Symmetry codes: (i) x1, x2−1, x3, x4, x5; (ii) x1, x2+1, x3, x4, x5; (iii) −x1, x2−1/2, −x3+2, −x5, −x4; (iv) −x1, x2+1/2, −x3+2, −x5, −x4; (v) −x1+1/2, −x2+1, x3−1/2, x5, x4; (vi) −x1+1/2, −x2+1, x3+1/2, x5, x4; (vii) −x1+1/2, −x2+2, x3−1/2, x5, x4; (viii) −x1+1/2, −x2+2, x3+1/2, x5, x4; (ix) x1−1/2, −x2+3/2, −x3+3/2, −x4, −x5; (x) x1−1/2, x2, −x3+3/2, −x5, −x4; (xi) x1, −x2+3/2, x3, x5, x4; (xii) −x1+1/2, x2−1/2, x3−1/2, x4, x5; (xiii) −x1+1/2, x2−1/2, x3+1/2, x4, x5; (xiv) −x1+1/2, x2+1/2, x3−1/2, x4, x5; (xv) −x1+1/2, x2+1/2, x3+1/2, x4, x5; (xvi) x1−1/2, −x2+1/2, −x3+3/2, −x4, −x5; (xvii) x1−1/2, x2+1, −x3+3/2, −x5, −x4; (xviii) x1, x2, x3+1, x4, x5; (xix) −x1+1, x2−1/2, −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, x2−1/2, −x3+1, −x5, −x4; (xxvii) −x1+1, x2+1/2, −x3+1, −x5, −x4. |
Experimental details
(I) | (II) | (III) | |
Crystal data | |||
Chemical formula | B3.041O10.479Si0.959Sr4 | B3.376O10.312Si0.624Sr4 | B3.704O10.148Si0.296Sr4 |
Mr | 577.9 | 569.5 | 561.2 |
Crystal system, space group | Orthorhombic, Pnma | Orthorhombic, Pnma† | Orthorhombic, Pnma‡ |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 12.2774, 3.9006, 5.4091 | ? | ? |
V (Å3) | 259.04 | 90, 90, 90 | 90, 90, 90 |
Z | 1 | 254.55 (9) | 251.18 |
Radiation type | Mo Kα | ? | ? |
µ (mm−1) | 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 |
Rint | 0.107 | 0.054 | 0.087 |
(sin θ/λ)max (Å−1) | 0.964 | 0.685 | 0.686 |
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 reflections | 1031 | 1403 | 1431 |
No. of parameters | 29 | 35 | 35 |
Δρmax, Δρmin (e Å−3) | 3.58, −5.05 | 0.94, −1.19 | 1.09, −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.