coors quite quiet prep slept through thought next day we knocked off and the rest in brooklyn used like baseballs embrace or end or embrace or accept i've already is blurry apparently in the desert though thought through depends how much my opinion can contextualize fire and conversation embrace or re create it roll it before being work or a little cinematic How can i keep your thoughts in check i'd like your opinion before "getting fucked" when both circumstances glitch and hiccup apparently cameras don't like to be hit with rocks or baseballs or anyway good luck on monday the next day heart throb
Structure determination of tris(acetylacetonate) iron(III)
A red crystal of tris(acetylacetonate) iron(III), synthesized from 0.012 g iron(II) oxide isolated from a sample of dirt collected at Superior Dry Lake, Mojave Desert, California, with the dimensions of 0.10 mm x 0.48 mm x 0.48 mm, was mounted on a Mitegen Micromount and automatically centered on a Bruker SMART X2S benchtop crystallographic system. Intensity measurements were performed using monochromated (doubly curved silicon crystal) Mo-K
α-radiation (0.71073 Å) from a sealed microfocus tube. Generator settings were 50 kV, 1 mA. Data collection temperature was 27°C. Data were acquired using three sets of Omega scans at different Phi settings. The frame width was 0.5° with an exposure time of 60.0 s.
| Run |
Omega (start) |
Omega (end) |
Phi |
Frames |
| 1 |
-20.0 |
160.0 |
0.0 |
360 |
| 2 |
-20.0 |
130.0 |
60.0 |
300 |
| 3 |
-20.0 |
100.0 |
120.0 |
240 |
| 4 |
-20.0 |
70.0 |
180.0 |
180 |
| 5 |
-20.0 |
40.0 |
240.0 |
120 |
| 6 |
-20.0 |
10.0 |
300.0 |
60 |
APEX2 software was used for preliminary determination of the unit cell. Determination of integrated intensities and unit cell refinement were performed using SAINT. The integration of the data yielded a total of 20346 reflections to a maximum θ angle of 21.70° ( 0.96 Å resolution).
The constants for the orthorhombic unit cell are a = 13.573(4) Å, b = 15.482(3) Å, c = 16.590(4) Å, V = 3486.2(15) Å
3. They are based upon the refinement of the XYZ-centroids of 2044 reflections above 20.0 I/σ(I) with 2.45° ≤ θ ≤ 18.68°.
Data were corrected for absorption effects with SADABS using the multiscan technique. The ratio of minimum to maximum apparent transmission is 80.1:100. The average residual for symmetry equivalent reflections is R
int = 10.61% and R
σ = 4.12%. XPREP determined the space group to be P b c a, with Z = 8 for the formula unit, C
15H
21FeO
6.
The structure was solved with XS and subsequent structure refinements were performed with XL. The final anisotropic full-matrix least-squares refinement on F
o2 with 205 variables converged at R
1 = 3.90% for the observed data and wR
2 = 11.54% for all data. The goodness-of-fit was 1.011. The largest peak on the final difference electron density synthesis was 0.21 e
-/Å
3 and the deepest hole was -0.20 e
-/Å
3 with an RMS deviation of 0.04 e
-/Å
3. On the basis of the final model, the calculated density is 1.346 g/cm
3 and F(000) = 1480.
APEX2 Version 2009.9 (Bruker AXS Inc.)
SAINT Version 7.68A (Bruker AXS Inc., 2009)
SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)
XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)
XS Version 2008/1 (George M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
XL Version 2008/4 (George M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
|
Table 1. Crystal data and structure refinement for tris(acetylacetonate) iron(III).
|
| Identification code
| tris(acetylacetonate) iron(III) |
| Empirical formula
| C15 H21 Fe O6 |
| Formula weight
| 353.17 |
| Temperature
| 300(2) K |
| Wavelength
| 0.71073 Å |
| Crystal system
| Orthorhombic |
| Space group
| P b c a |
| Unit cell dimensions
| a = 13.573(4) Å |
α = 90° |
|
| b = 15.482(3) Å |
β = 90° |
|
| c = 16.590(4) Å
| γ = 90° |
| Volume
| 3486.2(15) Å3
|
| Z
| 8 |
| Density (calculated)
| 1.346 Mg/cm3
|
| Absorption coefficient
| 0.888 mm-1
|
| F(000)
| 1480 |
| Crystal size
| 0.10 x 0.48 x 0.48 mm3
|
| Theta range for data collection
| 2.34 to 21.70° |
| Index ranges
| -14<=h<=14, -12<=k<=12, -14<=l<=15 |
| Reflections collected
| 20346 |
| Independent reflections
| 1412 [R(int) = 0.1061] |
| Completeness to theta = 21.70°
| 68.6% |
| Absorption correction
| Multiscan |
| Max. and min. transmission
| 0.9569 and 0.7669 |
| Refinement method
| Full-matrix least-squares on F2
|
| Data / restraints / parameters
| 1412 / 0 / 205 |
| Goodness-of-fit on F2
| 1.011 |
| Final R indices [I>2sigma(I)]
| R1 = 0.0390, wR2 = 0.0993 |
| R indices (all data)
| R1 = 0.0682, wR2 = 0.1154 |
| Largest diff. peak and hole
| 0.206 and -0.203 |
R
int = Σ|
Fo2 -
Fo2(mean)| / Σ[
Fo2]
R
1 = Σ||
Fo| - |
Fc|| / Σ|
Fo|
GOOF = S = {Σ[
w(
Fo2 -
Fc2)
2] / (n - p)}
1/2
wR
2 = {Σ[
w(
Fo2 -
Fc2)
2] / Σ[
w(
Fo2)
2]}
1/2
w = 1 / [σ(
Fo2) + (a
P)
2 + b
P] where
P is [2
Fc2 + Max(
Fo2, 0)] / 3
|
Table 2. Atomic coordinates (x104) and equivalent isotropic
displacement parameters (Å2x103) for tris(acetylacetonate) iron(III).
|
|
U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
|
|
| x
| y
| z
| U(eq) |
| Fe1 |
8572(1) |
7688(1) |
2539(1) |
52(1) |
| O1 |
9336(3) |
8521(3) |
1795(3) |
68(1) |
| O2 |
9556(3) |
6743(3) |
2499(3) |
65(1) |
| O3 |
7981(3) |
6955(3) |
1673(2) |
67(1) |
| O4 |
7522(3) |
8671(3) |
2486(3) |
66(1) |
| O5 |
9052(3) |
8391(3) |
3495(3) |
68(1) |
| O6 |
7979(2) |
6805(3) |
3326(3) |
64(1) |
| C1 |
9983(6) |
8373(5) |
1481(4) |
65(2) |
| C2 |
10289(5) |
9186(5) |
909(4) |
110(3) |
| C3 |
10474(4) |
7567(6) |
1629(4) |
76(2) |
| C4 |
10260(5) |
6787(5) |
2109(4) |
61(2) |
| C5 |
10854(4) |
5918(5) |
2207(5) |
95(3) |
| C6 |
7244(6) |
7122(6) |
1354(4) |
74(2) |
| C7 |
6942(5) |
6359(6) |
769(5) |
123(3) |
| C8 |
6756(5) |
7942(6) |
1509(5) |
84(2) |
| C9 |
6955(5) |
8677(5) |
2035(5) |
64(2) |
| C10 |
6393(4) |
9566(5) |
2114(5) |
98(3) |
| C11 |
9036(4) |
8145(6) |
4230(5) |
71(2) |
| C12 |
9503(5) |
8826(5) |
4800(4) |
114(3) |
| C13 |
8604(5) |
7335(6) |
4528(5) |
83(2) |
| C14 |
8099(4) |
6716(5) |
4075(5) |
67(2) |
| C15 |
7607(5) |
5882(5) |
4481(4) |
104(3) |
|
Table 3. Bond lengths (Å) and angles (°) for tris(acetylacetonate) iron(III).
|
| Fe1-O2 |
1.982(4) |
| Fe1-O4 |
1.996(4) |
| Fe1-O3 |
1.999(4) |
| Fe1-O1 |
2.001(4) |
| Fe1-O5 |
2.035(5) |
| Fe1-O6 |
2.054(4) |
| O1-C1 |
1.150(7) |
| O2-C4 |
1.157(7) |
| O3-C6 |
1.162(7) |
| O4-C9 |
1.174(7) |
| O5-C11 |
1.279(8) |
| O6-C14 |
1.261(7) |
| C1-C3 |
1.443(9) |
| C1-C2 |
1.632(9) |
| C3-C4 |
1.475(9) |
| C4-C5 |
1.577(9) |
| C6-C8 |
1.454(10) |
| C6-C7 |
1.582(9) |
| C8-C9 |
1.459(9) |
| C9-C10 |
1.579(9) |
| C11-C13 |
1.469(10) |
| C11-C12 |
1.552(9) |
| C13-C14 |
1.397(9) |
| C14-C15 |
1.603(9) |
| O2-Fe1-O4 |
174.05(19) |
| O2-Fe1-O3 |
80.03(18) |
| O4-Fe1-O3 |
98.18(19) |
| O2-Fe1-O1 |
98.70(19) |
| O4-Fe1-O1 |
76.83(18) |
| O3-Fe1-O1 |
95.89(18) |
| O2-Fe1-O5 |
102.60(17) |
| O4-Fe1-O5 |
80.64(18) |
| O3-Fe1-O5 |
174.24(17) |
| O1-Fe1-O5 |
89.34(19) |
| O2-Fe1-O6 |
78.11(17) |
| O4-Fe1-O6 |
106.43(16) |
| O3-Fe1-O6 |
85.51(18) |
| O1-Fe1-O6 |
176.27(16) |
| O5-Fe1-O6 |
89.4(2) |
| C1-O1-Fe1 |
122.9(5) |
| C4-O2-Fe1 |
122.2(5) |
| C6-O3-Fe1 |
123.1(5) |
| C9-O4-Fe1 |
122.1(5) |
| C11-O5-Fe1 |
125.0(4) |
| C14-O6-Fe1 |
130.4(5) |
Table 4. Anisotropic displacement parameters (Å2x103)
for tris(acetylacetonate) iron(III).
|
|
The anisotropic displacement factor exponent takes the form:
-2π2[ h2 a*2 U11 + … + 2 h k a* b* U12 ]
|
|
| U11
| U22
| U33
| U23
| U13
| U12
|
| Fe1 |
35(1) |
70(1) |
50(1) |
1(1) |
1(1) |
-6(1) |
| O1 |
45(2) |
97(4) |
62(3) |
17(3) |
17(3) |
0(3) |
| O2 |
33(2) |
78(4) |
84(3) |
14(3) |
14(3) |
-5(2) |
| O3 |
47(2) |
90(4) |
63(3) |
-15(3) |
-15(3) |
3(3) |
| O4 |
38(2) |
83(4) |
75(3) |
-15(3) |
-15(3) |
5(2) |
| O5 |
47(2) |
100(4) |
55(3) |
7(3) |
7(3) |
-26(2) |
| O6 |
39(2) |
92(4) |
62(4) |
6(3) |
6(3) |
-17(2) |
| C1 |
61(5) |
85(7) |
50(5) |
-1(5) |
-1(5) |
-24(5) |
| C2 |
85(5) |
156(8) |
89(6) |
27(6) |
27(6) |
-15(6) |
| C3 |
41(4) |
101(7) |
84(6) |
-3(6) |
-3(6) |
-1(5) |
| C4 |
36(4) |
71(6) |
76(5) |
-7(5) |
-7(5) |
-9(4) |
| C5 |
37(3) |
97(7) |
152(8) |
-11(6) |
-11(6) |
-2(4) |
| C6 |
61(5) |
106(8) |
55(5) |
-14(5) |
-14(5) |
-22(5) |
| C7 |
80(5) |
178(10) |
111(7) |
-61(7) |
-61(7) |
-9(6) |
| C8 |
59(4) |
106(7) |
88(6) |
-15(6) |
-15(6) |
14(5) |
| C9 |
43(4) |
70(6) |
79(6) |
17(5) |
17(5) |
3(5) |
| C10 |
58(4) |
93(7) |
144(7) |
13(6) |
13(6) |
29(5) |
| C11 |
46(4) |
101(7) |
66(6) |
-11(6) |
-11(6) |
3(4) |
| C12 |
83(5) |
183(10) |
76(6) |
-24(6) |
-24(6) |
-14(6) |
| C13 |
64(4) |
130(9) |
53(5) |
17(6) |
17(6) |
-10(5) |
| C14 |
38(4) |
94(7) |
70(6) |
17(6) |
17(6) |
8(4) |
| C15 |
77(5) |
132(8) |
102(7) |
46(6) |
46(6) |
-10(5) |
|
Table 5. Hydrogen coordinates (x104) and isotropic displacement
parameters (Å2x103) for tris(acetylacetonate) iron(III).
|
|
| x
| y
| z
| U(eq) |
| H2A |
9906 |
9174 |
422 |
165 |
| H2B |
10979 |
9143 |
778 |
165 |
| H2C |
10169 |
9717 |
1190 |
165 |
| H3 |
11075 |
7531 |
1360 |
91 |
| H5A |
10710 |
5668 |
2724 |
143 |
| H5B |
11547 |
6035 |
2170 |
143 |
| H5C |
10666 |
5522 |
1789 |
143 |
| H7A |
7330 |
6389 |
286 |
185 |
| H7B |
6256 |
6410 |
634 |
185 |
| H7C |
7055 |
5816 |
1033 |
185 |
| H8 |
6189 |
8015 |
1202 |
101 |
| H10A |
6093 |
9604 |
2637 |
147 |
| H10B |
5893 |
9602 |
1706 |
147 |
| H10C |
6852 |
10033 |
2047 |
147 |
| H12A |
10205 |
8754 |
4806 |
171 |
| H12B |
9248 |
8750 |
5335 |
171 |
| H12C |
9344 |
9395 |
4610 |
171 |
| H13 |
8675 |
7222 |
5075 |
99 |
| H15A |
6958 |
6024 |
4669 |
156 |
| H15B |
8003 |
5695 |
4927 |
156 |
| H15C |
7564 |
5426 |
4090 |
156 |
