Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768199015761/zh0020sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768199015761/zh0020sup2.hkl |
Data collection: Rigaku/AFC Diffractometer Control Software; cell refinement: Rigaku/AFC Diffractometer Control Software; data reduction: TEXSAN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Al477.44Cr63.42Fe51.42 | Dx = 3.518 Mg m−3 |
Mr = 19051.3 | Mo Kα radiation, λ = 0.71069 Å |
Hexagonal, P63/m | Cell parameters from 23 reflections |
Hall symbol: -P 6c | θ = 9–23.5° |
a = 40.68 (7) Å | µ = 5.03 mm−1 |
c = 12.546 (1) Å | T = 293 K |
V = 17983 (8) Å3 | Needle, grey |
Z = 2 | 0.6 × 0.12 × 0.1 mm |
F(000) = 18433 |
Rigaku AFC5R diffractometer | Rint = 0.086 |
Graphite monochromator | θmax = 26.0°, θmin = 1.5° |
ω–2θ scans | h = 0→50 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→50 |
Tmin = 0.481, Tmax = 0.593 | l = 0→15 |
12684 measured reflections | 3 standard reflections every 500 reflections |
12273 independent reflections | intensity decay: 0.6% |
3854 reflections with I > 2σ(I) |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.075 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.207 | Calculated w = 1/[σ2(Fo2) + (0.0778P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
5453 reflections | Δρmax = 1.61 e Å−3 |
474 parameters | Δρmin = −1.30 e Å−3 |
Al477.44Cr63.42Fe51.42 | Z = 2 |
Mr = 19051.3 | Mo Kα radiation |
Hexagonal, P63/m | µ = 5.03 mm−1 |
a = 40.68 (7) Å | T = 293 K |
c = 12.546 (1) Å | 0.6 × 0.12 × 0.1 mm |
V = 17983 (8) Å3 |
Rigaku AFC5R diffractometer | 3854 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.086 |
Tmin = 0.481, Tmax = 0.593 | 3 standard reflections every 500 reflections |
12684 measured reflections | intensity decay: 0.6% |
12273 independent reflections |
R[F2 > 2σ(F2)] = 0.075 | 474 parameters |
wR(F2) = 0.207 | 0 restraints |
S = 1.09 | Δρmax = 1.61 e Å−3 |
5453 reflections | Δρmin = −1.30 e Å−3 |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Al1 | 0.0000 | 0.0000 | 0.2500 | 0.003 (10)* | 0.47 |
Cr1 | 0.0000 | 0.0000 | 0.2500 | 0.003 (10)* | 0.015 |
Fe1 | 0.0000 | 0.0000 | 0.2500 | 0.003 (10)* | 0.015 |
Al2 | 0.0000 | 0.0000 | 0.1099 (18) | 0.001 (4)* | 0.50 |
Al3 | 0.6667 | 0.3333 | 0.0426 (9) | 0.005 (2)* | |
Cr4 | 0.03193 (15) | 0.90723 (14) | 0.2500 | 0.0037 (11)* | |
Cr5 | 0.18049 (15) | 0.85053 (15) | 0.2500 | 0.0050 (12)* | |
Cr6 | 0.33670 (14) | 0.02076 (15) | 0.2500 | 0.0061 (12)* | |
Cr7 | 0.59667 (14) | 0.15519 (14) | 0.2500 | 0.0042 (12)* | |
Cr8 | 0.75065 (15) | 0.09767 (15) | 0.2500 | 0.0084 (12)* | |
Cr9 | 0.84274 (15) | 0.21868 (14) | 0.2500 | 0.0049 (13)* | |
Cr10 | 0.94010 (16) | 0.18129 (15) | 0.2500 | 0.0060 (12)* | |
Cr11 | 0.99335 (14) | 0.15933 (14) | 0.2500 | 0.0028 (11)* | |
Cr12 | 0.03669 (15) | 0.75047 (15) | 0.2500 | 0.0089 (12)* | 0.5 |
Fe12 | 0.03669 (15) | 0.75047 (15) | 0.2500 | 0.0089 (12)* | 0.5 |
Cr13 | 0.06812 (15) | 0.66065 (15) | 0.2500 | 0.0081 (12)* | 0.5 |
Fe13 | 0.06812 (15) | 0.66065 (15) | 0.2500 | 0.0081 (12)* | 0.5 |
Cr14 | 0.12878 (15) | 0.87186 (15) | 0.2500 | 0.0090 (12)* | 0.5 |
Fe14 | 0.12878 (15) | 0.87186 (15) | 0.2500 | 0.0090 (12)* | 0.5 |
Cr15 | 0.14507 (19) | 0.71979 (18) | 0.2500 | 0.010 (2)* | 0.3 |
Fe15 | 0.14507 (19) | 0.71979 (18) | 0.2500 | 0.010 (2)* | 0.3 |
Al15 | 0.14507 (19) | 0.71979 (18) | 0.2500 | 0.010 (2)* | 0.4 |
Cr16 | 0.27105 (17) | 0.52623 (17) | 0.2500 | 0.008 (2)* | 0.31 |
Fe16 | 0.27105 (17) | 0.52623 (17) | 0.2500 | 0.008 (2)* | 0.31 |
Al16 | 0.27105 (17) | 0.52623 (17) | 0.2500 | 0.008 (2)* | 0.38 |
Cr17 | 0.27959 (16) | 0.81464 (16) | 0.2500 | 0.0100 (12)* | 0.5 |
Fe17 | 0.27959 (16) | 0.81464 (16) | 0.2500 | 0.0100 (12)* | 0.5 |
Cr18 | 0.31882 (15) | 0.94934 (15) | 0.2500 | 0.0093 (12)* | 0.5 |
Fe18 | 0.31882 (15) | 0.94934 (15) | 0.2500 | 0.0093 (12)* | 0.5 |
Cr19 | 0.37904 (16) | 0.77809 (17) | 0.2500 | 0.010 (2)* | 0.405 |
Fe19 | 0.37904 (16) | 0.77809 (17) | 0.2500 | 0.010 (2)* | 0.405 |
Al19 | 0.37904 (16) | 0.77809 (17) | 0.2500 | 0.010 (2)* | 0.19 |
Cr20 | 0.46032 (14) | 1.05536 (14) | 0.2500 | 0.0080 (11)* | 0.5 |
Fe20 | 0.46032 (14) | 1.05536 (14) | 0.2500 | 0.0080 (11)* | 0.5 |
Cr21 | 0.49307 (14) | 0.96621 (14) | 0.2500 | 0.0056 (12)* | 0.5 |
Fe21 | 0.49307 (14) | 0.96621 (14) | 0.2500 | 0.0056 (12)* | 0.5 |
Cr22 | 0.62837 (15) | 0.06518 (15) | 0.2500 | 0.0078 (11)* | 0.5 |
Fe22 | 0.62837 (15) | 0.06518 (15) | 0.2500 | 0.0078 (11)* | 0.5 |
Cr23 | 0.80862 (14) | 0.30749 (14) | 0.2500 | 0.0089 (12)* | 0.5 |
Fe23 | 0.80862 (14) | 0.30749 (14) | 0.2500 | 0.0089 (12)* | 0.5 |
Cr24 | 0.84853 (14) | 0.06002 (14) | 0.2500 | 0.0083 (11)* | 0.5 |
Fe24 | 0.84853 (14) | 0.06002 (14) | 0.2500 | 0.0083 (11)* | 0.5 |
Cr25 | 0.9647 (2) | 0.0358 (2) | 0.2500 | 0.019 (3)* | 0.24 |
Fe25 | 0.9647 (2) | 0.0358 (2) | 0.2500 | 0.019 (3)* | 0.24 |
Al25 | 0.9647 (2) | 0.0358 (2) | 0.2500 | 0.019 (3)* | 0.52 |
Al26 | 0.0567 (3) | 0.5951 (3) | 0.2500 | 0.007 (2)* | |
Al27 | 0.0722 (3) | 0.8798 (3) | 0.2500 | 0.011 (2)* | |
Al28 | 0.0881 (3) | 0.7318 (3) | 0.2500 | 0.004 (2)* | |
Al29 | 0.0962 (3) | 0.9616 (3) | 0.2500 | 0.024 (3)* | |
Al30 | 0.1081 (3) | 0.8020 (3) | 0.2500 | 0.002 (2)* | |
Al31 | 0.1538 (3) | 0.9409 (3) | 0.2500 | 0.015 (3)* | |
Al32 | 0.2147 (5) | 0.7549 (5) | 0.2500 | 0.040 (6)* | 0.84 |
Al33 | 0.2234 (3) | 0.8253 (3) | 0.2500 | 0.012 (2)* | |
Al34 | 0.2475 (3) | 0.9053 (3) | 0.2500 | 0.007 (2)* | |
Al35 | 0.3039 (3) | 0.8842 (3) | 0.2500 | 0.013 (2)* | |
Al36 | 0.3120 (3) | 0.7186 (3) | 0.2500 | 0.0043 (19)* | |
Al37 | 0.3896 (3) | 1.0029 (3) | 0.2500 | 0.010 (2)* | |
Al38 | 0.4117 (3) | 0.9089 (3) | 0.2500 | 0.020 (4)* | 0.83 |
Cr38 | 0.4117 (3) | 0.9089 (3) | 0.2500 | 0.020 (4)* | 0.085 |
Fe38 | 0.4117 (3) | 0.9089 (3) | 0.2500 | 0.020 (4)* | 0.085 |
Al39 | 0.4298 (3) | 0.7613 (3) | 0.2500 | 0.027 (4)* | 0.76 |
Cr39 | 0.4298 (3) | 0.7613 (3) | 0.2500 | 0.027 (4)* | 0.12 |
Fe39 | 0.4298 (3) | 0.7613 (3) | 0.2500 | 0.027 (4)* | 0.12 |
Al40 | 0.4412 (3) | 0.9843 (3) | 0.2500 | 0.006 (2)* | |
Al41 | 0.4606 (3) | 0.8424 (3) | 0.2500 | 0.016 (2)* | |
Al42 | 0.4614 (4) | 0.6740 (4) | 0.2500 | 0.037 (4)* | |
Al43 | 0.5321 (3) | 0.0969 (3) | 0.2500 | 0.011 (2)* | |
Al44 | 0.5459 (3) | 0.1706 (3) | 0.2500 | 0.011 (2)* | |
Al45 | 0.5583 (3) | 0.0238 (3) | 0.2500 | 0.005 (2)* | |
Al46 | 0.6207 (3) | 0.0018 (3) | 0.2500 | 0.005 (2)* | |
Al47 | 0.6476 (3) | 0.1361 (3) | 0.2500 | 0.012 (2)* | |
Al48 | 0.6680 (3) | 0.2091 (3) | 0.2500 | 0.013 (2)* | |
Al49 | 0.6991 (3) | 0.1178 (3) | 0.2500 | 0.010 (3)* | 0.87 |
Cr49 | 0.6991 (3) | 0.1178 (3) | 0.2500 | 0.010 (3)* | 0.065 |
Fe49 | 0.6991 (3) | 0.1178 (3) | 0.2500 | 0.010 (3)* | 0.065 |
Al50 | 0.7159 (3) | 0.3462 (3) | 0.2500 | 0.010 (2)* | |
Al51 | 0.7259 (3) | 0.0290 (3) | 0.2500 | 0.011 (2)* | |
Al52 | 0.7355 (3) | 0.2554 (3) | 0.2500 | 0.020 (3)* | |
Al53 | 0.7708 (3) | 0.1682 (3) | 0.2500 | 0.014 (3)* | 0.92 |
Cr53 | 0.7708 (3) | 0.1682 (3) | 0.2500 | 0.014 (3)* | 0.04 |
Fe53 | 0.7708 (3) | 0.1682 (3) | 0.2500 | 0.014 (3)* | 0.04 |
Al54 | 0.7828 (3) | 0.0071 (3) | 0.2500 | 0.008 (2)* | |
Al55 | 0.7909 (3) | 0.2372 (3) | 0.2500 | 0.011 (2)* | |
Al56 | 0.8048 (3) | 0.0856 (3) | 0.2500 | 0.011 (2)* | |
Al57 | 0.8804 (3) | 0.3484 (3) | 0.2500 | 0.004 (2)* | |
Al58 | 0.8834 (3) | 0.1897 (3) | 0.2500 | 0.007 (2)* | |
Al59 | 0.9010 (3) | 0.0398 (3) | 0.2500 | 0.013 (2)* | |
Al60 | 0.9088 (3) | 0.2744 (3) | 0.2500 | 0.011 (2)* | |
Al61 | 0.9207 (3) | 0.1107 (3) | 0.2500 | 0.010 (2)* | |
Al62 | 0.9656 (3) | 0.2497 (3) | 0.2500 | 0.006 (2)* | |
Fe63 | 0.14240 (8) | 0.61874 (8) | 0.0633 (3) | 0.0044 (6)* | |
Fe64 | 0.70289 (9) | 0.23518 (8) | 0.0733 (3) | 0.0087 (7)* | |
Fe65 | 0.73475 (8) | 0.35062 (8) | 0.0534 (2) | 0.0051 (6)* | |
Cr66 | 0.73951 (9) | 0.12994 (9) | 0.0766 (3) | 0.0031 (7)* | |
Cr67 | 0.07945 (9) | 0.76160 (9) | 0.0748 (3) | 0.0077 (7)* | 0.5 |
Fe67 | 0.07945 (9) | 0.76160 (9) | 0.0748 (3) | 0.0077 (7)* | 0.5 |
Cr68 | 0.39138 (10) | 0.89074 (10) | 0.0530 (3) | 0.0060 (11)* | 0.405 |
Fe68 | 0.39138 (10) | 0.89074 (10) | 0.0530 (3) | 0.0060 (11)* | 0.405 |
Al68 | 0.39138 (10) | 0.89074 (10) | 0.0530 (3) | 0.0060 (11)* | 0.19 |
Cr69 | 0.42939 (9) | 1.01312 (9) | 0.0754 (3) | 0.0060 (7)* | 0.5 |
Fe69 | 0.42939 (9) | 1.01312 (9) | 0.0754 (3) | 0.0060 (7)* | 0.5 |
Cr70 | 0.89035 (9) | 0.07075 (9) | 0.0751 (3) | 0.0075 (8)* | 0.5 |
Fe70 | 0.89035 (9) | 0.07075 (9) | 0.0751 (3) | 0.0075 (8)* | 0.5 |
Cr71 | 0.98087 (16) | 0.04531 (16) | 0.0464 (5) | 0.0241 (18)* | 0.235 |
Fe71 | 0.98087 (16) | 0.04531 (16) | 0.0464 (5) | 0.0241 (18)* | 0.235 |
Al71 | 0.98087 (16) | 0.04531 (16) | 0.0464 (5) | 0.0241 (18)* | 0.53 |
Al72 | 0.0028 (2) | 0.8395 (2) | 0.1365 (6) | 0.0115 (17)* | |
Al73 | 0.00492 (19) | 0.2216 (2) | 0.1341 (6) | 0.0087 (16)* | |
Al74 | 0.00535 (18) | 0.74239 (18) | 0.0569 (6) | 0.0090 (15)* | |
Al75 | 0.02462 (19) | 0.16719 (19) | 0.0693 (6) | 0.0133 (17)* | |
Al76 | 0.02517 (19) | 0.68767 (19) | 0.1361 (6) | 0.0063 (15)* | |
Al77 | 0.0326 (2) | 0.9590 (2) | 0.1458 (7) | 0.0240 (19)* | |
Al78 | 0.04435 (19) | 0.63116 (19) | 0.0694 (6) | 0.0107 (15)* | |
Al79 | 0.05941 (19) | 0.9144 (2) | 0.0651 (6) | 0.0141 (16)* | |
Al80 | 0.0613 (2) | 0.8159 (2) | 0.1347 (6) | 0.0081 (16)* | |
Al81 | 0.09837 (18) | 0.70722 (19) | 0.0614 (6) | 0.0086 (14)* | |
Al82 | 0.1180 (2) | 0.6554 (2) | 0.1371 (6) | 0.0120 (16)* | |
Al83 | 0.11879 (18) | 0.89340 (18) | 0.0705 (5) | 0.0066 (14)* | |
Al84 | 0.13639 (19) | 0.83721 (19) | 0.0647 (6) | 0.0108 (15)* | |
Al85 | 0.1531 (2) | 0.78225 (19) | 0.1377 (7) | 0.0116 (17)* | |
Al86 | 0.16097 (19) | 0.56140 (19) | 0.1375 (6) | 0.0075 (15)* | |
Al87 | 0.1641 (2) | 0.4319 (2) | 0.0717 (7) | 0.0201 (18)* | |
Al88 | 0.17214 (14) | 0.73356 (14) | 0.0587 (5) | 0.0114 (17)* | 0.71 |
Cr88 | 0.17214 (14) | 0.73356 (14) | 0.0587 (5) | 0.0114 (17)* | 0.145 |
Fe88 | 0.17214 (14) | 0.73356 (14) | 0.0587 (5) | 0.0114 (17)* | 0.145 |
Al89 | 0.1939 (2) | 0.9138 (2) | 0.1328 (6) | 0.0068 (15)* | |
Al90 | 0.1959 (2) | 0.6898 (2) | 0.1335 (6) | 0.0108 (16)* | |
Al91 | 0.2077 (2) | 0.6312 (2) | 0.0557 (6) | 0.0165 (16)* | |
Al92 | 0.21199 (18) | 0.85803 (18) | 0.0677 (6) | 0.0083 (14)* | |
Al93 | 0.27552 (19) | 0.97233 (19) | 0.1327 (6) | 0.0081 (16)* | |
Al94 | 0.29474 (18) | 0.91707 (18) | 0.0670 (6) | 0.0088 (14)* | |
Al95 | 0.33166 (18) | 1.04641 (17) | 0.0702 (6) | 0.0073 (14)* | |
Al96 | 0.3370 (2) | 0.8499 (2) | 0.1370 (7) | 0.018 (3)* | 0.87 |
Al97 | 0.35193 (18) | 0.99159 (18) | 0.0641 (6) | 0.0082 (14)* | |
Al98 | 0.3655 (2) | 0.7136 (2) | 0.1311 (6) | 0.0130 (17)* | |
Al99 | 0.3731 (2) | 0.9386 (2) | 0.1358 (5) | 0.0099 (16)* | |
Al100 | 0.40795 (19) | 1.06524 (19) | 0.1359 (6) | 0.0062 (15)* | |
Al101 | 0.41792 (17) | 0.65273 (17) | 0.0537 (6) | 0.0070 (14)* | |
Al102 | 0.43661 (18) | 0.72931 (18) | 0.0562 (6) | 0.0102 (15)* | |
Al103 | 0.44743 (18) | 0.95708 (18) | 0.0581 (7) | 0.0115 (16)* | |
Al104 | 0.4674 (2) | 0.9068 (2) | 0.1327 (6) | 0.0113 (16)* | |
Al105 | 0.48329 (18) | 1.08619 (18) | 0.0552 (6) | 0.0077 (14)* | |
Al106 | 0.4982 (3) | 0.7256 (3) | 0.0922 (8) | 0.022 (3)* | 0.84 |
Al107 | 0.5017 (2) | 1.03015 (19) | 0.1359 (6) | 0.0063 (15)* | |
Al108 | 0.52460 (18) | 0.97830 (18) | 0.0694 (6) | 0.0074 (14)* | |
Al109 | 0.56637 (18) | 0.13897 (18) | 0.0605 (6) | 0.0102 (15)* | |
Al110 | 0.5870 (2) | 0.0899 (2) | 0.1357 (6) | 0.0136 (17)* | |
Al111 | 0.60568 (19) | 0.03463 (19) | 0.0692 (6) | 0.0121 (15)* | |
Al112 | 0.61537 (19) | 0.21344 (19) | 0.1374 (6) | 0.0088 (16)* | |
Al113 | 0.64393 (19) | 0.16902 (18) | 0.0623 (6) | 0.0116 (15)* | |
Al114 | 0.66306 (19) | 0.10882 (19) | 0.0598 (6) | 0.0115 (15)* | |
Al115 | 0.68393 (19) | 0.28295 (19) | 0.1195 (5) | 0.0069 (14)* | |
Al116 | 0.6846 (2) | 0.0569 (2) | 0.1367 (6) | 0.0092 (15)* | |
Al117 | 0.7194 (2) | 0.1849 (2) | 0.1306 (6) | 0.0075 (16)* | |
Al118 | 0.75885 (18) | 0.07369 (18) | 0.0572 (6) | 0.0105 (15)* | |
Al119 | 0.76254 (18) | 0.31908 (18) | 0.1378 (6) | 0.0076 (15)* | |
Al120 | 0.77458 (17) | 0.26177 (17) | 0.0657 (6) | 0.0062 (14)* | |
Al121 | 0.79724 (19) | 0.20399 (19) | 0.0641 (6) | 0.0100 (15)* | |
Al122 | 0.8140 (2) | 0.1486 (2) | 0.1390 (6) | 0.0109 (17)* | |
Al123 | 0.81693 (19) | 0.05171 (19) | 0.0574 (6) | 0.0122 (15)* | |
Al124 | 0.83502 (19) | 0.33443 (19) | 0.0656 (6) | 0.0114 (15)* | |
Al125 | 0.8548 (2) | 0.2817 (2) | 0.1369 (6) | 0.0111 (16)* | |
Al126 | 0.8731 (2) | 0.1260 (2) | 0.1361 (6) | 0.0095 (16)* | |
Al127 | 0.87326 (17) | 0.22510 (18) | 0.0701 (6) | 0.0067 (14)* | |
Al128 | 0.90992 (19) | 0.01769 (19) | 0.0560 (6) | 0.0125 (15)* | |
Al129 | 0.93007 (19) | 0.20256 (19) | 0.0696 (6) | 0.0108 (15)* | |
Al130 | 0.94878 (19) | 0.14683 (19) | 0.0656 (6) | 0.0099 (15)* | |
Al131 | 0.9664 (2) | 0.0919 (2) | 0.1375 (6) | 0.0152 (17)* |
Experimental details
Crystal data | |
Chemical formula | Al477.44Cr63.42Fe51.42 |
Mr | 19051.3 |
Crystal system, space group | Hexagonal, P63/m |
Temperature (K) | 293 |
a, c (Å) | 40.68 (7), 12.546 (1) |
V (Å3) | 17983 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 5.03 |
Crystal size (mm) | 0.6 × 0.12 × 0.1 |
Data collection | |
Diffractometer | Rigaku AFC5R diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.481, 0.593 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12684, 12273, 3854 |
Rint | 0.086 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.075, 0.207, 1.09 |
No. of reflections | 5453 |
No. of parameters | 474 |
Δρmax, Δρmin (e Å−3) | 1.61, −1.30 |
Computer programs: Rigaku/AFC Diffractometer Control Software, TEXSAN, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).