Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805019550/ci6598sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805019550/ci6598Isup2.hkl |
CCDC reference: 277227
Key indicators
- Single-crystal X-ray study
- T = 297 K
- Mean (C-C) = 0.003 Å
- R factor = 0.041
- wR factor = 0.113
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H9A .. H12B .. 1.99 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N1 .. 6.38 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N2 .. 5.81 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N3 .. 5.48 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N4 .. 6.61 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N6 .. 5.67 su PLAT417_ALERT_2_C Short Inter D-H..H-D H9B .. H10B .. 2.14 Ang. PLAT731_ALERT_1_C Bond Calc 0.88(6), Rep 0.89(2) ...... 3.00 su-Rat O9 -H9B 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(7), Rep 0.86(2) ...... 3.50 su-Rat O9 -H9A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.88(6), Rep 0.89(2) ...... 3.00 su-Rat O9 -H9B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(7), Rep 0.86(2) ...... 3.50 su-Rat O9 -H9A 1.555 1.555
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Fe(C12H8N2)3](C4O4)·8H2O | F(000) = 1776 |
Mr = 852.63 | Dx = 1.454 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5187 reflections |
a = 10.9285 (6) Å | θ = 1.7–27.8° |
b = 21.3431 (7) Å | µ = 0.46 mm−1 |
c = 16.8988 (8) Å | T = 297 K |
β = 98.804 (4)° | Plate, red |
V = 3895.4 (3) Å3 | 0.31 × 0.25 × 0.19 mm |
Z = 4 |
Stoe IPDS-2 diffractometer | 8612 independent reflections |
Radiation source: fine-focus sealed tube | 5723 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 6.67 pixels mm-1 | θmax = 27.2°, θmin = 1.6° |
ω scans | h = −13→14 |
Absorption correction: integration (X-RED32; Stoe & Cie, 2002) | k = −27→27 |
Tmin = 0.734, Tmax = 0.932 | l = −21→21 |
42766 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.113 | w = 1/[σ2(Fo2) + (0.0679P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.96 | (Δ/σ)max = 0.001 |
8612 reflections | Δρmax = 0.28 e Å−3 |
583 parameters | Δρmin = −0.40 e Å−3 |
25 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0023 (3) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
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 | ||
C1 | 0.3344 (2) | 0.22086 (11) | 0.94575 (13) | 0.0491 (5) | |
H1 | 0.2886 | 0.2517 | 0.9156 | 0.059* | |
C2 | 0.3111 (2) | 0.20920 (13) | 1.02306 (14) | 0.0611 (6) | |
H2 | 0.2497 | 0.2316 | 1.0433 | 0.073* | |
C3 | 0.3775 (3) | 0.16530 (14) | 1.06872 (15) | 0.0685 (7) | |
H3 | 0.3615 | 0.1571 | 1.1202 | 0.082* | |
C4 | 0.4711 (2) | 0.13215 (12) | 1.03793 (14) | 0.0601 (6) | |
C5 | 0.5492 (3) | 0.08535 (15) | 1.08055 (17) | 0.0821 (9) | |
H5 | 0.5400 | 0.0758 | 1.1330 | 0.098* | |
C6 | 0.6353 (3) | 0.05505 (15) | 1.04633 (17) | 0.0822 (9) | |
H6 | 0.6854 | 0.0254 | 1.0759 | 0.099* | |
C7 | 0.6518 (2) | 0.06738 (11) | 0.96529 (15) | 0.0578 (6) | |
C8 | 0.7405 (2) | 0.03784 (12) | 0.92542 (17) | 0.0663 (7) | |
H8 | 0.7928 | 0.0073 | 0.9512 | 0.080* | |
C9 | 0.7483 (2) | 0.05457 (11) | 0.84895 (15) | 0.0585 (6) | |
H9 | 0.8070 | 0.0358 | 0.8222 | 0.070* | |
C10 | 0.66867 (19) | 0.09996 (10) | 0.81014 (14) | 0.0493 (5) | |
H10 | 0.6754 | 0.1104 | 0.7576 | 0.059* | |
C11 | 0.57649 (19) | 0.11274 (10) | 0.92268 (12) | 0.0452 (5) | |
C12 | 0.48709 (19) | 0.14546 (10) | 0.95944 (12) | 0.0458 (5) | |
C13 | 0.22761 (18) | 0.26333 (10) | 0.73763 (13) | 0.0483 (5) | |
H13 | 0.1899 | 0.2249 | 0.7241 | 0.058* | |
C14 | 0.1583 (2) | 0.31764 (11) | 0.72133 (15) | 0.0559 (6) | |
H14 | 0.0761 | 0.3149 | 0.6971 | 0.067* | |
C15 | 0.2093 (2) | 0.37477 (11) | 0.74042 (14) | 0.0531 (5) | |
H15 | 0.1625 | 0.4111 | 0.7305 | 0.064* | |
C16 | 0.33425 (19) | 0.37784 (9) | 0.77533 (12) | 0.0445 (4) | |
C17 | 0.4003 (2) | 0.43505 (10) | 0.79635 (14) | 0.0555 (5) | |
H17 | 0.3583 | 0.4730 | 0.7897 | 0.067* | |
C18 | 0.5213 (2) | 0.43477 (10) | 0.82536 (15) | 0.0561 (6) | |
H18 | 0.5621 | 0.4727 | 0.8370 | 0.067* | |
C19 | 0.5897 (2) | 0.37743 (10) | 0.83892 (12) | 0.0471 (5) | |
C20 | 0.7159 (2) | 0.37344 (11) | 0.87166 (14) | 0.0543 (5) | |
H20 | 0.7624 | 0.4096 | 0.8841 | 0.065* | |
C21 | 0.7686 (2) | 0.31586 (12) | 0.88477 (15) | 0.0590 (6) | |
H21 | 0.8517 | 0.3126 | 0.9068 | 0.071* | |
C22 | 0.69939 (18) | 0.26209 (11) | 0.86547 (13) | 0.0498 (5) | |
H22 | 0.7381 | 0.2234 | 0.8745 | 0.060* | |
C23 | 0.52638 (17) | 0.32112 (9) | 0.82152 (11) | 0.0386 (4) | |
C24 | 0.39834 (18) | 0.32152 (9) | 0.78847 (11) | 0.0385 (4) | |
C25 | 0.58742 (19) | 0.21882 (11) | 0.66050 (13) | 0.0499 (5) | |
H25 | 0.6365 | 0.2485 | 0.6907 | 0.060* | |
C26 | 0.6063 (2) | 0.20793 (13) | 0.58212 (14) | 0.0619 (6) | |
H26 | 0.6672 | 0.2299 | 0.5608 | 0.074* | |
C27 | 0.5354 (3) | 0.16508 (14) | 0.53695 (15) | 0.0677 (7) | |
H27 | 0.5487 | 0.1571 | 0.4848 | 0.081* | |
C28 | 0.4420 (2) | 0.13279 (11) | 0.56859 (13) | 0.0556 (6) | |
C29 | 0.3584 (3) | 0.08803 (13) | 0.52634 (15) | 0.0693 (7) | |
H29 | 0.3657 | 0.0782 | 0.4736 | 0.083* | |
C30 | 0.2698 (2) | 0.05979 (12) | 0.56079 (15) | 0.0630 (6) | |
H30 | 0.2158 | 0.0318 | 0.5312 | 0.076* | |
C31 | 0.2576 (2) | 0.07231 (9) | 0.64215 (14) | 0.0491 (5) | |
C32 | 0.1694 (2) | 0.04452 (10) | 0.68286 (16) | 0.0587 (6) | |
H32 | 0.1130 | 0.0158 | 0.6569 | 0.070* | |
C33 | 0.1668 (2) | 0.05979 (11) | 0.76071 (17) | 0.0617 (6) | |
H33 | 0.1080 | 0.0417 | 0.7881 | 0.074* | |
C34 | 0.2520 (2) | 0.10245 (10) | 0.79951 (15) | 0.0530 (5) | |
H34 | 0.2491 | 0.1119 | 0.8529 | 0.064* | |
C35 | 0.33943 (18) | 0.11517 (9) | 0.68519 (12) | 0.0420 (4) | |
C36 | 0.42994 (18) | 0.14625 (9) | 0.64790 (12) | 0.0432 (4) | |
C37 | 0.8632 (2) | 0.08495 (11) | 0.63575 (15) | 0.0561 (6) | |
C38 | 0.8991 (2) | 0.14814 (11) | 0.66219 (14) | 0.0576 (6) | |
C39 | 0.9576 (2) | 0.15746 (11) | 0.59251 (14) | 0.0562 (5) | |
C40 | 0.91917 (19) | 0.09514 (10) | 0.56355 (13) | 0.0477 (5) | |
N1 | 0.41973 (15) | 0.18965 (8) | 0.91332 (10) | 0.0420 (4) | |
N2 | 0.50220 (15) | 0.18863 (8) | 0.69413 (10) | 0.0408 (4) | |
N3 | 0.33754 (15) | 0.13031 (7) | 0.76332 (10) | 0.0419 (4) | |
N4 | 0.57940 (14) | 0.26340 (7) | 0.83441 (9) | 0.0397 (4) | |
N5 | 0.58338 (15) | 0.12883 (7) | 0.84551 (10) | 0.0411 (4) | |
N6 | 0.34573 (14) | 0.26396 (7) | 0.77179 (9) | 0.0387 (3) | |
O1 | 0.8115 (2) | 0.03966 (9) | 0.66285 (13) | 0.0851 (6) | |
O2 | 0.92904 (16) | 0.06266 (7) | 0.50370 (10) | 0.0609 (4) | |
O3 | 1.0200 (2) | 0.20095 (8) | 0.56762 (13) | 0.0839 (6) | |
O4 | 0.8848 (2) | 0.18132 (9) | 0.72229 (12) | 0.0810 (6) | |
O5 | 1.0081 (2) | −0.03433 (10) | 0.89716 (15) | 0.0931 (7) | |
O6 | 1.0955 (2) | −0.08269 (9) | 0.76703 (12) | 0.0777 (5) | |
O7 | 1.06292 (19) | 0.06723 (8) | 0.37953 (11) | 0.0666 (5) | |
O8 | 1.10008 (19) | 0.19476 (8) | 0.42302 (13) | 0.0708 (5) | |
O9 | 0.8793 (4) | 0.30815 (16) | 0.5277 (2) | 0.1258 (10) | |
O10 | 0.8240 (2) | 0.30343 (10) | 0.68316 (16) | 0.0877 (6) | |
O11 | 1.0097 (3) | 0.18597 (10) | 0.87431 (16) | 0.1172 (10) | |
O12 | 0.0861 (3) | 0.08040 (12) | 0.96385 (16) | 0.1091 (8) | |
Fe1 | 0.46192 (2) | 0.194212 (12) | 0.803680 (16) | 0.03605 (9) | |
H5A | 0.992 (2) | −0.0607 (10) | 0.9312 (12) | 0.054* | |
H5B | 1.040 (2) | −0.0554 (10) | 0.8636 (11) | 0.054* | |
H6A | 1.0504 (19) | −0.0846 (11) | 0.7204 (11) | 0.054* | |
H6B | 1.124 (2) | −0.1216 (8) | 0.7751 (13) | 0.054* | |
H7A | 1.110 (2) | 0.0390 (10) | 0.3715 (14) | 0.054* | |
H7B | 1.030 (2) | 0.0628 (11) | 0.4200 (12) | 0.054* | |
H8A | 1.080 (2) | 0.1943 (10) | 0.4694 (10) | 0.054* | |
H8B | 1.093 (2) | 0.1591 (8) | 0.4048 (13) | 0.054* | |
H10A | 0.858 (2) | 0.2701 (9) | 0.7012 (13) | 0.054* | |
H10B | 0.829 (2) | 0.3083 (11) | 0.6337 (10) | 0.054* | |
H11A | 0.975 (2) | 0.1864 (10) | 0.8248 (10) | 0.054* | |
H11B | 1.041 (2) | 0.2204 (9) | 0.8838 (13) | 0.054* | |
H12A | 0.061 (2) | 0.0489 (8) | 0.9377 (14) | 0.054* | |
H12B | 0.0242 (19) | 0.1070 (9) | 0.9524 (15) | 0.054* | |
H9B | 0.940 (5) | 0.282 (3) | 0.545 (5) | 0.31 (5)* | |
H9A | 0.915 (6) | 0.334 (3) | 0.500 (4) | 0.26 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0499 (12) | 0.0571 (12) | 0.0422 (12) | 0.0022 (9) | 0.0129 (9) | −0.0061 (10) |
C2 | 0.0598 (14) | 0.0823 (16) | 0.0446 (13) | 0.0055 (12) | 0.0186 (11) | −0.0081 (12) |
C3 | 0.0754 (17) | 0.0943 (19) | 0.0397 (13) | 0.0024 (15) | 0.0214 (12) | 0.0042 (13) |
C4 | 0.0682 (15) | 0.0743 (15) | 0.0387 (12) | 0.0024 (12) | 0.0107 (11) | 0.0070 (11) |
C5 | 0.098 (2) | 0.103 (2) | 0.0472 (15) | 0.0227 (18) | 0.0174 (14) | 0.0277 (15) |
C6 | 0.096 (2) | 0.092 (2) | 0.0576 (17) | 0.0272 (17) | 0.0099 (15) | 0.0292 (15) |
C7 | 0.0593 (14) | 0.0605 (13) | 0.0523 (14) | 0.0135 (11) | 0.0042 (11) | 0.0122 (11) |
C8 | 0.0654 (15) | 0.0611 (14) | 0.0703 (18) | 0.0193 (12) | 0.0031 (13) | 0.0109 (13) |
C9 | 0.0539 (13) | 0.0602 (14) | 0.0617 (16) | 0.0146 (11) | 0.0098 (11) | −0.0041 (12) |
C10 | 0.0484 (12) | 0.0504 (11) | 0.0501 (13) | 0.0083 (9) | 0.0105 (9) | −0.0046 (10) |
C11 | 0.0466 (11) | 0.0487 (11) | 0.0399 (11) | 0.0015 (9) | 0.0055 (8) | 0.0016 (9) |
C12 | 0.0483 (11) | 0.0515 (11) | 0.0377 (11) | −0.0004 (9) | 0.0066 (9) | 0.0020 (9) |
C13 | 0.0376 (10) | 0.0549 (12) | 0.0511 (13) | −0.0003 (9) | 0.0030 (9) | 0.0004 (10) |
C14 | 0.0371 (11) | 0.0676 (15) | 0.0612 (15) | 0.0073 (10) | 0.0022 (10) | 0.0046 (11) |
C15 | 0.0504 (12) | 0.0562 (13) | 0.0535 (14) | 0.0113 (10) | 0.0106 (10) | 0.0061 (10) |
C16 | 0.0505 (11) | 0.0465 (11) | 0.0375 (11) | 0.0058 (9) | 0.0094 (9) | 0.0028 (9) |
C17 | 0.0697 (15) | 0.0414 (11) | 0.0560 (14) | 0.0022 (10) | 0.0117 (11) | 0.0004 (10) |
C18 | 0.0670 (15) | 0.0417 (11) | 0.0593 (14) | −0.0084 (10) | 0.0081 (11) | −0.0011 (10) |
C19 | 0.0542 (12) | 0.0473 (11) | 0.0397 (12) | −0.0097 (9) | 0.0067 (9) | −0.0011 (9) |
C20 | 0.0529 (13) | 0.0567 (13) | 0.0520 (14) | −0.0168 (10) | 0.0040 (10) | −0.0047 (10) |
C21 | 0.0429 (12) | 0.0729 (16) | 0.0581 (15) | −0.0110 (11) | −0.0015 (10) | −0.0053 (12) |
C22 | 0.0378 (10) | 0.0560 (12) | 0.0533 (13) | −0.0013 (9) | −0.0004 (9) | −0.0029 (10) |
C23 | 0.0399 (10) | 0.0450 (10) | 0.0313 (10) | −0.0028 (8) | 0.0066 (8) | −0.0020 (8) |
C24 | 0.0420 (10) | 0.0435 (10) | 0.0305 (10) | 0.0012 (8) | 0.0073 (8) | 0.0000 (7) |
C25 | 0.0463 (11) | 0.0626 (13) | 0.0418 (12) | −0.0029 (10) | 0.0100 (9) | 0.0062 (10) |
C26 | 0.0595 (14) | 0.0845 (17) | 0.0446 (13) | 0.0006 (13) | 0.0172 (11) | 0.0099 (12) |
C27 | 0.0775 (17) | 0.0931 (19) | 0.0349 (12) | 0.0075 (15) | 0.0159 (12) | 0.0021 (13) |
C28 | 0.0660 (15) | 0.0652 (14) | 0.0341 (12) | 0.0066 (11) | 0.0028 (10) | −0.0015 (10) |
C29 | 0.0893 (19) | 0.0733 (16) | 0.0406 (13) | 0.0024 (14) | −0.0049 (13) | −0.0143 (12) |
C30 | 0.0743 (17) | 0.0577 (13) | 0.0495 (14) | −0.0010 (12) | −0.0146 (12) | −0.0094 (11) |
C31 | 0.0516 (12) | 0.0393 (10) | 0.0515 (13) | 0.0051 (9) | −0.0074 (9) | −0.0024 (9) |
C32 | 0.0527 (13) | 0.0426 (11) | 0.0757 (18) | −0.0058 (9) | −0.0060 (12) | −0.0037 (11) |
C33 | 0.0570 (14) | 0.0502 (12) | 0.0789 (18) | −0.0144 (11) | 0.0137 (12) | 0.0008 (12) |
C34 | 0.0538 (13) | 0.0490 (12) | 0.0582 (14) | −0.0092 (10) | 0.0151 (10) | −0.0002 (10) |
C35 | 0.0450 (11) | 0.0376 (9) | 0.0416 (11) | 0.0051 (8) | 0.0000 (8) | −0.0015 (8) |
C36 | 0.0456 (11) | 0.0471 (10) | 0.0353 (11) | 0.0043 (8) | 0.0013 (8) | 0.0004 (8) |
C37 | 0.0596 (14) | 0.0550 (13) | 0.0554 (14) | 0.0064 (10) | 0.0143 (11) | 0.0030 (11) |
C38 | 0.0661 (15) | 0.0578 (13) | 0.0472 (13) | 0.0091 (11) | 0.0036 (11) | −0.0006 (11) |
C39 | 0.0620 (14) | 0.0526 (13) | 0.0529 (14) | −0.0009 (10) | 0.0049 (11) | 0.0003 (10) |
C40 | 0.0475 (11) | 0.0463 (11) | 0.0486 (12) | 0.0040 (9) | 0.0053 (9) | 0.0024 (9) |
N1 | 0.0415 (9) | 0.0462 (9) | 0.0381 (9) | −0.0006 (7) | 0.0058 (7) | −0.0032 (7) |
N2 | 0.0387 (8) | 0.0459 (9) | 0.0376 (9) | 0.0013 (7) | 0.0054 (7) | 0.0017 (7) |
N3 | 0.0430 (9) | 0.0409 (8) | 0.0420 (10) | −0.0006 (7) | 0.0068 (7) | −0.0007 (7) |
N4 | 0.0389 (8) | 0.0448 (8) | 0.0350 (9) | 0.0004 (7) | 0.0041 (7) | −0.0003 (7) |
N5 | 0.0432 (9) | 0.0434 (9) | 0.0373 (9) | 0.0011 (7) | 0.0079 (7) | −0.0013 (7) |
N6 | 0.0367 (8) | 0.0436 (8) | 0.0355 (9) | −0.0028 (7) | 0.0045 (6) | −0.0018 (7) |
O1 | 0.1122 (16) | 0.0663 (11) | 0.0884 (15) | −0.0131 (11) | 0.0528 (13) | 0.0028 (10) |
O2 | 0.0709 (11) | 0.0558 (9) | 0.0574 (10) | 0.0011 (8) | 0.0144 (8) | −0.0070 (8) |
O3 | 0.1099 (16) | 0.0608 (11) | 0.0865 (15) | −0.0258 (10) | 0.0326 (12) | −0.0070 (10) |
O4 | 0.1127 (16) | 0.0756 (12) | 0.0556 (11) | 0.0096 (11) | 0.0156 (11) | −0.0126 (9) |
O5 | 0.1196 (19) | 0.0806 (15) | 0.0850 (17) | 0.0105 (13) | 0.0342 (14) | −0.0044 (12) |
O6 | 0.1090 (16) | 0.0534 (10) | 0.0704 (13) | 0.0032 (10) | 0.0124 (11) | 0.0011 (9) |
O7 | 0.0891 (14) | 0.0585 (10) | 0.0544 (11) | −0.0093 (9) | 0.0180 (9) | 0.0011 (9) |
O8 | 0.0801 (12) | 0.0551 (10) | 0.0804 (14) | −0.0135 (9) | 0.0223 (10) | −0.0007 (10) |
O9 | 0.175 (3) | 0.108 (2) | 0.100 (2) | 0.001 (2) | 0.036 (2) | 0.0071 (16) |
O10 | 0.1004 (17) | 0.0679 (12) | 0.0972 (17) | −0.0174 (11) | 0.0222 (14) | −0.0086 (12) |
O11 | 0.187 (3) | 0.0608 (12) | 0.0837 (17) | 0.0043 (14) | −0.0429 (17) | −0.0050 (12) |
O12 | 0.142 (2) | 0.0836 (16) | 0.0943 (19) | −0.0146 (15) | −0.0042 (17) | 0.0058 (14) |
Fe1 | 0.03569 (14) | 0.03935 (14) | 0.03331 (15) | −0.00076 (12) | 0.00589 (10) | −0.00136 (12) |
C1—N1 | 1.330 (3) | C26—C27 | 1.356 (4) |
C1—C2 | 1.391 (3) | C26—H26 | 0.93 |
C1—H1 | 0.93 | C27—C28 | 1.403 (4) |
C2—C3 | 1.353 (4) | C27—H27 | 0.93 |
C2—H2 | 0.93 | C28—C36 | 1.396 (3) |
C3—C4 | 1.407 (4) | C28—C29 | 1.434 (3) |
C3—H3 | 0.93 | C29—C30 | 1.347 (4) |
C4—C12 | 1.393 (3) | C29—H29 | 0.93 |
C4—C5 | 1.434 (4) | C30—C31 | 1.427 (3) |
C5—C6 | 1.344 (4) | C30—H30 | 0.93 |
C5—H5 | 0.93 | C31—C32 | 1.399 (3) |
C6—C7 | 1.433 (4) | C31—C35 | 1.402 (3) |
C6—H6 | 0.93 | C32—C33 | 1.360 (4) |
C7—C11 | 1.397 (3) | C32—H32 | 0.93 |
C7—C8 | 1.411 (3) | C33—C34 | 1.393 (3) |
C8—C9 | 1.356 (4) | C33—H33 | 0.93 |
C8—H8 | 0.93 | C34—N3 | 1.333 (3) |
C9—C10 | 1.397 (3) | C34—H34 | 0.93 |
C9—H9 | 0.93 | C35—N3 | 1.363 (3) |
C10—N5 | 1.333 (2) | C35—C36 | 1.416 (3) |
C10—H10 | 0.93 | C36—N2 | 1.365 (3) |
C11—N5 | 1.362 (3) | C37—O1 | 1.242 (3) |
C11—C12 | 1.419 (3) | C37—C38 | 1.456 (3) |
C12—N1 | 1.365 (3) | C37—C40 | 1.462 (3) |
C13—N6 | 1.331 (2) | C38—O4 | 1.267 (3) |
C13—C14 | 1.389 (3) | C38—C39 | 1.437 (3) |
C13—H13 | 0.93 | C39—O3 | 1.262 (3) |
C14—C15 | 1.359 (3) | C39—C40 | 1.457 (3) |
C14—H14 | 0.93 | C40—O2 | 1.244 (3) |
C15—C16 | 1.403 (3) | N1—Fe1 | 1.9791 (16) |
C15—H15 | 0.93 | N2—Fe1 | 1.9710 (16) |
C16—C24 | 1.392 (3) | N3—Fe1 | 1.9721 (16) |
C16—C17 | 1.435 (3) | N4—Fe1 | 1.9735 (16) |
C17—C18 | 1.338 (3) | N5—Fe1 | 1.9803 (16) |
C17—H17 | 0.93 | N6—Fe1 | 1.9773 (16) |
C18—C19 | 1.434 (3) | O5—H5A | 0.840 (15) |
C18—H18 | 0.93 | O5—H5B | 0.843 (15) |
C19—C23 | 1.396 (3) | O6—H6A | 0.864 (15) |
C19—C20 | 1.407 (3) | O6—H6B | 0.891 (15) |
C20—C21 | 1.361 (3) | O7—H7A | 0.817 (15) |
C20—H20 | 0.93 | O7—H7B | 0.824 (15) |
C21—C22 | 1.386 (3) | O8—H8A | 0.847 (15) |
C21—H21 | 0.93 | O8—H8B | 0.820 (15) |
C22—N4 | 1.336 (2) | O9—H9B | 0.89 (2) |
C22—H22 | 0.93 | O9—H9A | 0.86 (2) |
C23—N4 | 1.365 (2) | O10—H10A | 0.837 (15) |
C23—C24 | 1.425 (3) | O10—H10B | 0.851 (15) |
C24—N6 | 1.367 (2) | O11—H11A | 0.865 (16) |
C25—N2 | 1.329 (3) | O11—H11B | 0.817 (15) |
C25—C26 | 1.391 (3) | O12—H12A | 0.828 (15) |
C25—H25 | 0.93 | O12—H12B | 0.882 (15) |
N1—C1—C2 | 122.6 (2) | C36—C28—C27 | 116.5 (2) |
N1—C1—H1 | 118.7 | C36—C28—C29 | 117.9 (2) |
C2—C1—H1 | 118.7 | C27—C28—C29 | 125.6 (2) |
C3—C2—C1 | 120.0 (2) | C30—C29—C28 | 121.9 (2) |
C3—C2—H2 | 120.0 | C30—C29—H29 | 119.1 |
C1—C2—H2 | 120.0 | C28—C29—H29 | 119.1 |
C2—C3—C4 | 119.6 (2) | C29—C30—C31 | 120.8 (2) |
C2—C3—H3 | 120.2 | C29—C30—H30 | 119.6 |
C4—C3—H3 | 120.2 | C31—C30—H30 | 119.6 |
C12—C4—C3 | 117.0 (2) | C32—C31—C35 | 117.0 (2) |
C12—C4—C5 | 118.0 (2) | C32—C31—C30 | 124.6 (2) |
C3—C4—C5 | 125.1 (2) | C35—C31—C30 | 118.4 (2) |
C6—C5—C4 | 121.4 (2) | C33—C32—C31 | 119.5 (2) |
C6—C5—H5 | 119.3 | C33—C32—H32 | 120.3 |
C4—C5—H5 | 119.3 | C31—C32—H32 | 120.3 |
C5—C6—C7 | 121.4 (2) | C32—C33—C34 | 120.0 (2) |
C5—C6—H6 | 119.3 | C32—C33—H33 | 120.0 |
C7—C6—H6 | 119.3 | C34—C33—H33 | 120.0 |
C11—C7—C8 | 117.2 (2) | N3—C34—C33 | 122.8 (2) |
C11—C7—C6 | 118.0 (2) | N3—C34—H34 | 118.6 |
C8—C7—C6 | 124.8 (2) | C33—C34—H34 | 118.6 |
C9—C8—C7 | 119.1 (2) | N3—C35—C31 | 123.66 (19) |
C9—C8—H8 | 120.5 | N3—C35—C36 | 115.81 (18) |
C7—C8—H8 | 120.5 | C31—C35—C36 | 120.53 (19) |
C8—C9—C10 | 120.3 (2) | N2—C36—C28 | 123.7 (2) |
C8—C9—H9 | 119.9 | N2—C36—C35 | 115.97 (17) |
C10—C9—H9 | 119.9 | C28—C36—C35 | 120.4 (2) |
N5—C10—C9 | 122.6 (2) | O1—C37—C38 | 136.4 (2) |
N5—C10—H10 | 118.7 | O1—C37—C40 | 134.1 (2) |
C9—C10—H10 | 118.7 | C38—C37—C40 | 89.48 (18) |
N5—C11—C7 | 123.64 (19) | O4—C38—C39 | 134.8 (2) |
N5—C11—C12 | 115.96 (18) | O4—C38—C37 | 134.7 (2) |
C7—C11—C12 | 120.40 (19) | C39—C38—C37 | 90.54 (19) |
N1—C12—C4 | 123.3 (2) | O3—C39—C38 | 134.9 (2) |
N1—C12—C11 | 115.93 (18) | O3—C39—C40 | 134.6 (2) |
C4—C12—C11 | 120.7 (2) | C38—C39—C40 | 90.44 (19) |
N6—C13—C14 | 122.7 (2) | O2—C40—C39 | 136.5 (2) |
N6—C13—H13 | 118.6 | O2—C40—C37 | 134.0 (2) |
C14—C13—H13 | 118.6 | C39—C40—C37 | 89.50 (18) |
C15—C14—C13 | 120.7 (2) | C1—N1—C12 | 117.48 (18) |
C15—C14—H14 | 119.7 | C1—N1—Fe1 | 129.75 (15) |
C13—C14—H14 | 119.7 | C12—N1—Fe1 | 112.71 (13) |
C14—C15—C16 | 118.6 (2) | C25—N2—C36 | 117.28 (18) |
C14—C15—H15 | 120.7 | C25—N2—Fe1 | 130.09 (15) |
C16—C15—H15 | 120.7 | C36—N2—Fe1 | 112.63 (13) |
C24—C16—C15 | 117.40 (19) | C34—N3—C35 | 117.04 (18) |
C24—C16—C17 | 118.26 (19) | C34—N3—Fe1 | 130.13 (15) |
C15—C16—C17 | 124.3 (2) | C35—N3—Fe1 | 112.78 (13) |
C18—C17—C16 | 121.2 (2) | C22—N4—C23 | 116.67 (17) |
C18—C17—H17 | 119.4 | C22—N4—Fe1 | 130.36 (14) |
C16—C17—H17 | 119.4 | C23—N4—Fe1 | 112.97 (12) |
C17—C18—C19 | 121.6 (2) | C10—N5—C11 | 117.24 (18) |
C17—C18—H18 | 119.2 | C10—N5—Fe1 | 129.97 (15) |
C19—C18—H18 | 119.2 | C11—N5—Fe1 | 112.78 (13) |
C23—C19—C20 | 117.09 (19) | C13—N6—C24 | 116.60 (17) |
C23—C19—C18 | 118.12 (19) | C13—N6—Fe1 | 130.57 (14) |
C20—C19—C18 | 124.7 (2) | C24—N6—Fe1 | 112.83 (12) |
C21—C20—C19 | 118.9 (2) | H5A—O5—H5B | 105 (2) |
C21—C20—H20 | 120.5 | H6A—O6—H6B | 103.7 (18) |
C19—C20—H20 | 120.5 | H7A—O7—H7B | 115 (2) |
C20—C21—C22 | 120.5 (2) | H8A—O8—H8B | 108.2 (19) |
C20—C21—H21 | 119.8 | H9B—O9—H9A | 102 (3) |
C22—C21—H21 | 119.8 | H10A—O10—H10B | 112 (2) |
N4—C22—C21 | 122.9 (2) | H11A—O11—H11B | 106.9 (19) |
N4—C22—H22 | 118.6 | H12A—O12—H12B | 103 (2) |
C21—C22—H22 | 118.6 | N2—Fe1—N3 | 82.80 (7) |
N4—C23—C19 | 123.98 (18) | N2—Fe1—N4 | 93.58 (7) |
N4—C23—C24 | 115.81 (16) | N3—Fe1—N4 | 174.11 (7) |
C19—C23—C24 | 120.22 (18) | N2—Fe1—N6 | 90.91 (7) |
N6—C24—C16 | 123.89 (18) | N3—Fe1—N6 | 92.67 (6) |
N6—C24—C23 | 115.61 (16) | N4—Fe1—N6 | 82.71 (6) |
C16—C24—C23 | 120.50 (18) | N2—Fe1—N1 | 173.69 (7) |
N2—C25—C26 | 122.8 (2) | N3—Fe1—N1 | 92.45 (7) |
N2—C25—H25 | 118.6 | N4—Fe1—N1 | 91.48 (7) |
C26—C25—H25 | 118.6 | N6—Fe1—N1 | 93.46 (7) |
C27—C26—C25 | 119.6 (2) | N2—Fe1—N5 | 93.37 (7) |
C27—C26—H26 | 120.2 | N3—Fe1—N5 | 91.43 (7) |
C25—C26—H26 | 120.2 | N4—Fe1—N5 | 93.43 (7) |
C26—C27—C28 | 120.2 (2) | N6—Fe1—N5 | 174.41 (7) |
C26—C27—H27 | 119.9 | N1—Fe1—N5 | 82.57 (7) |
C28—C27—H27 | 119.9 | ||
N1—C1—C2—C3 | 1.0 (4) | C38—C37—C40—O2 | −178.8 (3) |
C1—C2—C3—C4 | 0.7 (4) | O1—C37—C40—C39 | −175.9 (3) |
C2—C3—C4—C12 | −2.1 (4) | C38—C37—C40—C39 | 1.71 (18) |
C2—C3—C4—C5 | 179.0 (3) | C2—C1—N1—C12 | −1.1 (3) |
C12—C4—C5—C6 | 0.0 (5) | C2—C1—N1—Fe1 | 175.80 (17) |
C3—C4—C5—C6 | 178.9 (3) | C4—C12—N1—C1 | −0.4 (3) |
C4—C5—C6—C7 | −1.0 (5) | C11—C12—N1—C1 | 179.48 (19) |
C5—C6—C7—C11 | 0.9 (5) | C4—C12—N1—Fe1 | −177.87 (18) |
C5—C6—C7—C8 | 179.6 (3) | C11—C12—N1—Fe1 | 2.0 (2) |
C11—C7—C8—C9 | 0.0 (4) | C26—C25—N2—C36 | −1.3 (3) |
C6—C7—C8—C9 | −178.7 (3) | C26—C25—N2—Fe1 | 178.06 (17) |
C7—C8—C9—C10 | −0.7 (4) | C28—C36—N2—C25 | 0.8 (3) |
C8—C9—C10—N5 | 0.5 (4) | C35—C36—N2—C25 | −179.56 (18) |
C8—C7—C11—N5 | 1.0 (4) | C28—C36—N2—Fe1 | −178.68 (17) |
C6—C7—C11—N5 | 179.8 (2) | C35—C36—N2—Fe1 | 1.0 (2) |
C8—C7—C11—C12 | −178.5 (2) | C33—C34—N3—C35 | −0.3 (3) |
C6—C7—C11—C12 | 0.3 (4) | C33—C34—N3—Fe1 | 177.02 (17) |
C3—C4—C12—N1 | 2.0 (4) | C31—C35—N3—C34 | −0.3 (3) |
C5—C4—C12—N1 | −179.0 (2) | C36—C35—N3—C34 | 179.01 (18) |
C3—C4—C12—C11 | −177.9 (2) | C31—C35—N3—Fe1 | −178.07 (15) |
C5—C4—C12—C11 | 1.1 (4) | C36—C35—N3—Fe1 | 1.2 (2) |
N5—C11—C12—N1 | −0.7 (3) | C21—C22—N4—C23 | 0.5 (3) |
C7—C11—C12—N1 | 178.8 (2) | C21—C22—N4—Fe1 | −179.08 (17) |
N5—C11—C12—C4 | 179.2 (2) | C19—C23—N4—C22 | −0.1 (3) |
C7—C11—C12—C4 | −1.3 (3) | C24—C23—N4—C22 | −179.93 (17) |
N6—C13—C14—C15 | −0.3 (4) | C19—C23—N4—Fe1 | 179.50 (15) |
C13—C14—C15—C16 | 1.4 (3) | C24—C23—N4—Fe1 | −0.3 (2) |
C14—C15—C16—C24 | −0.2 (3) | C9—C10—N5—C11 | 0.5 (3) |
C14—C15—C16—C17 | 178.2 (2) | C9—C10—N5—Fe1 | 179.64 (16) |
C24—C16—C17—C18 | 2.2 (3) | C7—C11—N5—C10 | −1.2 (3) |
C15—C16—C17—C18 | −176.2 (2) | C12—C11—N5—C10 | 178.35 (18) |
C16—C17—C18—C19 | −1.8 (4) | C7—C11—N5—Fe1 | 179.49 (18) |
C17—C18—C19—C23 | −0.5 (3) | C12—C11—N5—Fe1 | −1.0 (2) |
C17—C18—C19—C20 | −177.8 (2) | C14—C13—N6—C24 | −1.9 (3) |
C23—C19—C20—C21 | −0.2 (3) | C14—C13—N6—Fe1 | 178.08 (16) |
C18—C19—C20—C21 | 177.1 (2) | C16—C24—N6—C13 | 3.2 (3) |
C19—C20—C21—C22 | 0.6 (4) | C23—C24—N6—C13 | −177.15 (17) |
C20—C21—C22—N4 | −0.7 (4) | C16—C24—N6—Fe1 | −176.78 (15) |
C20—C19—C23—N4 | 0.0 (3) | C23—C24—N6—Fe1 | 2.9 (2) |
C18—C19—C23—N4 | −177.52 (18) | C25—N2—Fe1—N3 | −179.60 (19) |
C20—C19—C23—C24 | 179.81 (18) | C36—N2—Fe1—N3 | −0.26 (13) |
C18—C19—C23—C24 | 2.3 (3) | C25—N2—Fe1—N4 | 5.07 (19) |
C15—C16—C24—N6 | −2.2 (3) | C36—N2—Fe1—N4 | −175.59 (13) |
C17—C16—C24—N6 | 179.31 (18) | C25—N2—Fe1—N6 | 87.82 (19) |
C15—C16—C24—C23 | 178.15 (18) | C36—N2—Fe1—N6 | −92.83 (13) |
C17—C16—C24—C23 | −0.4 (3) | C25—N2—Fe1—N5 | −88.58 (19) |
N4—C23—C24—N6 | −1.8 (2) | C36—N2—Fe1—N5 | 90.76 (13) |
C19—C23—C24—N6 | 178.45 (17) | C34—N3—Fe1—N2 | −177.9 (2) |
N4—C23—C24—C16 | 177.94 (17) | C35—N3—Fe1—N2 | −0.54 (13) |
C19—C23—C24—C16 | −1.9 (3) | C34—N3—Fe1—N6 | −87.36 (19) |
N2—C25—C26—C27 | 0.3 (4) | C35—N3—Fe1—N6 | 90.04 (13) |
C25—C26—C27—C28 | 1.2 (4) | C34—N3—Fe1—N1 | 6.23 (19) |
C26—C27—C28—C36 | −1.6 (4) | C35—N3—Fe1—N1 | −176.38 (13) |
C26—C27—C28—C29 | 177.9 (2) | C34—N3—Fe1—N5 | 88.85 (19) |
C36—C28—C29—C30 | 0.6 (4) | C35—N3—Fe1—N5 | −93.76 (14) |
C27—C28—C29—C30 | −178.9 (3) | C22—N4—Fe1—N2 | −88.52 (18) |
C28—C29—C30—C31 | −1.6 (4) | C23—N4—Fe1—N2 | 91.91 (13) |
C29—C30—C31—C32 | −179.1 (2) | C22—N4—Fe1—N6 | −178.98 (19) |
C29—C30—C31—C35 | 0.6 (3) | C23—N4—Fe1—N6 | 1.45 (13) |
C35—C31—C32—C33 | −0.1 (3) | C22—N4—Fe1—N1 | 87.72 (18) |
C30—C31—C32—C33 | 179.7 (2) | C23—N4—Fe1—N1 | −91.85 (13) |
C31—C32—C33—C34 | −0.5 (4) | C22—N4—Fe1—N5 | 5.08 (19) |
C32—C33—C34—N3 | 0.7 (4) | C23—N4—Fe1—N5 | −174.49 (13) |
C32—C31—C35—N3 | 0.5 (3) | C13—N6—Fe1—N2 | 84.18 (18) |
C30—C31—C35—N3 | −179.27 (19) | C24—N6—Fe1—N2 | −95.88 (13) |
C32—C31—C35—C36 | −178.80 (19) | C13—N6—Fe1—N3 | 1.34 (19) |
C30—C31—C35—C36 | 1.4 (3) | C24—N6—Fe1—N3 | −178.71 (13) |
C27—C28—C36—N2 | 0.7 (3) | C13—N6—Fe1—N4 | 177.67 (19) |
C29—C28—C36—N2 | −178.9 (2) | C24—N6—Fe1—N4 | −2.38 (12) |
C27—C28—C36—C35 | −179.0 (2) | C13—N6—Fe1—N1 | −91.27 (18) |
C29—C28—C36—C35 | 1.4 (3) | C24—N6—Fe1—N1 | 88.67 (13) |
N3—C35—C36—N2 | −1.5 (3) | C1—N1—Fe1—N3 | −87.91 (18) |
C31—C35—C36—N2 | 177.82 (17) | C12—N1—Fe1—N3 | 89.14 (14) |
N3—C35—C36—C28 | 178.19 (18) | C1—N1—Fe1—N4 | 87.70 (18) |
C31—C35—C36—C28 | −2.5 (3) | C12—N1—Fe1—N4 | −95.25 (14) |
O1—C37—C38—O4 | −4.1 (5) | C1—N1—Fe1—N6 | 4.91 (19) |
C40—C37—C38—O4 | 178.4 (3) | C12—N1—Fe1—N6 | −178.03 (14) |
O1—C37—C38—C39 | 175.8 (3) | C1—N1—Fe1—N5 | −179.04 (19) |
C40—C37—C38—C39 | −1.73 (18) | C12—N1—Fe1—N5 | −1.98 (13) |
O4—C38—C39—O3 | 3.5 (5) | C10—N5—Fe1—N2 | 7.25 (19) |
C37—C38—C39—O3 | −176.3 (3) | C11—N5—Fe1—N2 | −173.54 (14) |
O4—C38—C39—C40 | −178.4 (3) | C10—N5—Fe1—N3 | 90.11 (18) |
C37—C38—C39—C40 | 1.74 (18) | C11—N5—Fe1—N3 | −90.67 (14) |
O3—C39—C40—O2 | −3.1 (5) | C10—N5—Fe1—N4 | −86.55 (18) |
C38—C39—C40—O2 | 178.8 (3) | C11—N5—Fe1—N4 | 92.66 (14) |
O3—C39—C40—C37 | 176.4 (3) | C10—N5—Fe1—N1 | −177.60 (19) |
C38—C39—C40—C37 | −1.73 (18) | C11—N5—Fe1—N1 | 1.61 (14) |
O1—C37—C40—O2 | 3.6 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O12i | 0.84 (2) | 2.13 (2) | 2.878 (4) | 149 (2) |
O5—H5B···O6 | 0.84 (2) | 1.91 (2) | 2.731 (3) | 163 (2) |
O6—H6A···O7ii | 0.86 (2) | 1.97 (2) | 2.816 (3) | 166 (2) |
O6—H6B···O10iii | 0.89 (2) | 1.81 (2) | 2.677 (3) | 166 (2) |
O7—H7A···O1ii | 0.82 (2) | 2.01 (2) | 2.811 (3) | 166 (3) |
O7—H7B···O2 | 0.82 (2) | 1.92 (2) | 2.737 (2) | 169 (2) |
O8—H8A···O3 | 0.85 (2) | 1.88 (2) | 2.722 (3) | 173 (2) |
O8—H8B···O7 | 0.82 (2) | 2.02 (2) | 2.832 (3) | 169 (2) |
O9—H9B···O3 | 0.89 (2) | 1.94 (3) | 2.782 (4) | 157 (7) |
O9—H9A···O11iv | 0.86 (2) | 2.53 (6) | 3.147 (5) | 129 (6) |
O10—H10A···O4 | 0.84 (2) | 1.94 (2) | 2.745 (3) | 160 (2) |
O10—H10B···O9 | 0.85 (2) | 1.95 (2) | 2.786 (4) | 165 (2) |
O11—H11A···O4 | 0.87 (2) | 1.86 (2) | 2.720 (3) | 173 (2) |
O11—H11B···O8v | 0.82 (2) | 2.00 (2) | 2.808 (3) | 170 (2) |
O12—H12A···O5vi | 0.83 (2) | 1.96 (2) | 2.775 (4) | 168 (2) |
O12—H12B···O11vi | 0.88 (2) | 2.13 (2) | 2.771 (3) | 129 (2) |
C20—H20···O2v | 0.93 | 2.57 | 3.267 (3) | 132 |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+2, −y, −z+1; (iii) −x+2, y−1/2, −z+3/2; (iv) x, −y+1/2, z−1/2; (v) x, −y+1/2, z+1/2; (vi) x−1, y, z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register