Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270111026758/ga3164sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270111026758/ga3164Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270111026758/ga3164IIsup3.hkl |
CCDC references: 813661; 813662
For related literature, see: Allen (2002); Blann et al. (2005); Bollmann et al. (2004); Busi et al. (2006); Evans et al. (1992); Gilbertson et al. (2007); Maithufi (2010); Merkel et al. (2005); Mikhailine et al. (2008); Ondrejkovičová & Vrábel (2002); Overett et al. (2005); Pohl et al. (1995); Spek (2009).
The Ph2PN(Et)PPh2 ligand was prepared as described previously (Bollmann et al., 2004), while FeBr2 (98%) and acetonitrile were both purchased from Aldrich and used as received.
The compounds were prepared by dissolving FeBr2 (20 mg, 9.27 × 10 -5 mol) and Ph2PN(Et)PPh2 (38 mg, 9.27 × 10 -5 mol) in acetonitrile (10 ml) with stirring under an inert atmosphere. The reaction medium was stirred at room temperature until complete dissolution of the FeBr2.
Crystals suitable for X-ray diffraction were obtained by slow evaporation of the acetonitrile solvent from the reaction mixture under aerobic conditions. Visual inspection of the crystals under a microscope indicated the presence of orange and red crystals. Representatives of each were selected by hand and used for crystallographic studies. The crystals of (I) were prismatic and orange in colour, while those for (II) were red, slightly larger, and with a rectangular cross-section.
1H and 31P NMR analyses (CD2Cl2) of (I) and (II) were identical, with only broad singlets obtained in the 1H spectra due to the unfavourable NMR characteristics of iron. 1H NMR (δ, p.p.m.): 0.7–3.2 (12H), 3.6–4.7 (4H), 6.6–7.9 (24H), 7.9–9.9 (16H); 31P NMR (δ, p.p.m.): 103.83.
The intensity data (2450 frames) were collected with an exposure time of 8 s per frame (frame width 0.30°) for (I) and 5 s per frame for (II). All non-methyl H atoms were placed in geometrically idealized positions, with C—H = 0.98 for CH (alkyl), 0.93 for CH (aryl) and 0.97 Å for CH2, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C). The methyl H atoms were constrained to an ideal geometry with C—H = 0.96 Å and with Uiso(H) = 1.5Ueq(C), but were allowed to rotate freely about the adjacent C—C bond.
The disorder of the ethyl C atoms in cation 2 of (II) was modelled over two sites, with the occupancies initially as free variables summing to unity. Values of 0.511 (14) and 0.489 (14) were obtained, and since these values do not differ significantly from 0.5 they were subsequently fixed at 0.5 for the final refinement. The disorder of the Br atoms in the anions of (II) was modelled using a combination of geometric (all Fe—Br distances) and ellipsoid restraints. For the Fe4-based anion, two site major/minor occupancies (summing to 1.0) sufficed, but the disorder at the Fe3-based anion could only be modelled with multiple sites. No evidence was found to suggest that a mixture of anions, such as [FeBr4]2-, exists in this structure.
The minimum and maximum residual electron densities for (II) are located 0.61 Å from Br43 and 1.2 Å from Br46, respectively. The location of the maximum residual electron-density peak does not fit the geometry of any expected disorder or impurity.
For both compounds, data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
[Fe(C2H3N)2(C26H25NP2)2][FeBr4] | Z = 4 |
Mr = 1340.27 | F(000) = 2688 |
Triclinic, P1 | Dx = 1.647 Mg m−3 |
Hall symbol: -p 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.4596 (10) Å | Cell parameters from 9884 reflections |
b = 21.834 (2) Å | θ = 2.9–26.9° |
c = 23.905 (2) Å | µ = 3.65 mm−1 |
α = 114.399 (1)° | T = 100 K |
β = 96.285 (1)° | Shard, orange |
γ = 90.388 (1)° | 0.40 × 0.20 × 0.08 mm |
V = 5405.4 (8) Å3 |
Bruker APEX CCD area-detector diffractometer | 21891 independent reflections |
Radiation source: fine-focus sealed tube | 16724 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
ω scans | θmax = 26.4°, θmin = 4.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | h = −14→14 |
Tmin = 0.323, Tmax = 0.771 | k = −27→27 |
59375 measured reflections | l = −29→29 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.030P)2] where P = (Fo2 + 2Fc2)/3 |
21891 reflections | (Δ/σ)max = 0.001 |
1272 parameters | Δρmax = 0.61 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Fe(C2H3N)2(C26H25NP2)2][FeBr4] | γ = 90.388 (1)° |
Mr = 1340.27 | V = 5405.4 (8) Å3 |
Triclinic, P1 | Z = 4 |
a = 11.4596 (10) Å | Mo Kα radiation |
b = 21.834 (2) Å | µ = 3.65 mm−1 |
c = 23.905 (2) Å | T = 100 K |
α = 114.399 (1)° | 0.40 × 0.20 × 0.08 mm |
β = 96.285 (1)° |
Bruker APEX CCD area-detector diffractometer | 21891 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | 16724 reflections with I > 2σ(I) |
Tmin = 0.323, Tmax = 0.771 | Rint = 0.038 |
59375 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.61 e Å−3 |
21891 reflections | Δρmin = −0.41 e Å−3 |
1272 parameters |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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 | ||
Fe1 | 0.0000 | 0.0000 | 0.5000 | 0.01002 (12) | |
P11 | 0.09864 (6) | 0.09333 (3) | 0.57266 (3) | 0.01109 (15) | |
P12 | −0.12432 (6) | 0.08623 (3) | 0.52924 (3) | 0.01100 (15) | |
N11 | 0.04766 (18) | 0.02116 (10) | 0.43581 (10) | 0.0105 (5) | |
C11 | 0.0823 (2) | 0.02665 (13) | 0.39498 (13) | 0.0142 (6) | |
C12 | 0.1284 (3) | 0.03190 (15) | 0.34293 (13) | 0.0223 (7) | |
H12A | 0.1903 | 0.0667 | 0.3579 | 0.033* | |
H12B | 0.0666 | 0.0427 | 0.3186 | 0.033* | |
H12C | 0.1588 | −0.0102 | 0.3179 | 0.033* | |
N101 | −0.01344 (19) | 0.14435 (10) | 0.57390 (10) | 0.0120 (5) | |
C101 | −0.0090 (2) | 0.21843 (13) | 0.61239 (13) | 0.0166 (6) | |
H10A | 0.0727 | 0.2350 | 0.6248 | 0.020* | |
H10B | −0.0444 | 0.2266 | 0.6497 | 0.020* | |
C102 | −0.0705 (3) | 0.25769 (14) | 0.58033 (14) | 0.0237 (7) | |
H10C | −0.0330 | 0.2523 | 0.5447 | 0.036* | |
H10D | −0.0666 | 0.3045 | 0.6083 | 0.036* | |
H10E | −0.1513 | 0.2414 | 0.5675 | 0.036* | |
C111 | 0.2268 (2) | 0.13467 (13) | 0.56167 (12) | 0.0132 (6) | |
C112 | 0.3372 (2) | 0.13989 (14) | 0.59547 (13) | 0.0161 (6) | |
H112 | 0.3452 | 0.1242 | 0.6263 | 0.019* | |
C113 | 0.4347 (3) | 0.16827 (14) | 0.58331 (14) | 0.0208 (7) | |
H113 | 0.5074 | 0.1723 | 0.6065 | 0.025* | |
C114 | 0.4233 (2) | 0.19045 (14) | 0.53661 (14) | 0.0189 (7) | |
H114 | 0.4888 | 0.2091 | 0.5282 | 0.023* | |
C115 | 0.3152 (2) | 0.18516 (14) | 0.50228 (13) | 0.0185 (6) | |
H115 | 0.3083 | 0.1996 | 0.4706 | 0.022* | |
C116 | 0.2178 (2) | 0.15837 (13) | 0.51532 (13) | 0.0162 (6) | |
H116 | 0.1450 | 0.1560 | 0.4929 | 0.019* | |
C121 | 0.1291 (2) | 0.09122 (13) | 0.64842 (12) | 0.0118 (6) | |
C122 | 0.2040 (2) | 0.04332 (13) | 0.65444 (13) | 0.0157 (6) | |
H122 | 0.2471 | 0.0187 | 0.6225 | 0.019* | |
C123 | 0.2140 (2) | 0.03245 (14) | 0.70767 (13) | 0.0185 (7) | |
H123 | 0.2647 | 0.0010 | 0.7116 | 0.022* | |
C124 | 0.1488 (2) | 0.06834 (14) | 0.75541 (13) | 0.0198 (7) | |
H124 | 0.1536 | 0.0599 | 0.7907 | 0.024* | |
C125 | 0.0766 (2) | 0.11662 (15) | 0.75021 (13) | 0.0199 (7) | |
H125 | 0.0349 | 0.1418 | 0.7827 | 0.024* | |
C126 | 0.0658 (2) | 0.12789 (14) | 0.69664 (13) | 0.0165 (6) | |
H126 | 0.0161 | 0.1600 | 0.6932 | 0.020* | |
C131 | −0.2035 (2) | 0.11398 (13) | 0.47436 (12) | 0.0125 (6) | |
C132 | −0.1417 (2) | 0.13198 (13) | 0.43524 (13) | 0.0164 (6) | |
H132 | −0.0599 | 0.1353 | 0.4412 | 0.020* | |
C133 | −0.2008 (2) | 0.14481 (13) | 0.38805 (13) | 0.0171 (6) | |
H133 | −0.1586 | 0.1567 | 0.3626 | 0.021* | |
C134 | −0.3223 (3) | 0.14008 (14) | 0.37840 (13) | 0.0187 (7) | |
H134 | −0.3618 | 0.1483 | 0.3463 | 0.022* | |
C135 | −0.3849 (3) | 0.12300 (14) | 0.41667 (13) | 0.0199 (7) | |
H135 | −0.4667 | 0.1200 | 0.4104 | 0.024* | |
C136 | −0.3260 (2) | 0.11013 (13) | 0.46472 (13) | 0.0146 (6) | |
H136 | −0.3687 | 0.0989 | 0.4904 | 0.017* | |
C141 | −0.2357 (2) | 0.08254 (13) | 0.57660 (13) | 0.0140 (6) | |
C142 | −0.3124 (2) | 0.02479 (14) | 0.55378 (13) | 0.0170 (6) | |
H142 | −0.3075 | −0.0090 | 0.5146 | 0.020* | |
C143 | −0.3951 (2) | 0.01772 (15) | 0.58894 (14) | 0.0219 (7) | |
H143 | −0.4461 | −0.0205 | 0.5732 | 0.026* | |
C144 | −0.4023 (3) | 0.06760 (16) | 0.64797 (14) | 0.0239 (7) | |
H144 | −0.4571 | 0.0624 | 0.6719 | 0.029* | |
C145 | −0.3277 (2) | 0.12482 (15) | 0.67068 (14) | 0.0215 (7) | |
H145 | −0.3326 | 0.1584 | 0.7099 | 0.026* | |
C146 | −0.2453 (2) | 0.13245 (14) | 0.63518 (13) | 0.0170 (6) | |
H146 | −0.1961 | 0.1714 | 0.6507 | 0.020* | |
Fe2 | 0.50602 (3) | 0.248965 (18) | 0.000936 (17) | 0.01030 (8) | |
P21 | 0.69823 (6) | 0.22895 (3) | −0.00399 (3) | 0.01100 (15) | |
P22 | 0.53051 (6) | 0.17546 (3) | −0.09745 (3) | 0.01112 (15) | |
P23 | 0.48086 (6) | 0.31801 (3) | 0.10036 (3) | 0.01172 (15) | |
P24 | 0.31276 (6) | 0.26934 (3) | 0.00627 (3) | 0.01185 (15) | |
N21 | 0.52837 (18) | 0.32102 (11) | −0.02288 (10) | 0.0114 (5) | |
C21 | 0.5437 (2) | 0.36151 (14) | −0.03963 (13) | 0.0173 (6) | |
C22 | 0.5662 (3) | 0.41500 (15) | −0.05963 (16) | 0.0331 (8) | |
H22A | 0.5789 | 0.4574 | −0.0241 | 0.050* | |
H22B | 0.4997 | 0.4168 | −0.0870 | 0.050* | |
H22C | 0.6348 | 0.4059 | −0.0809 | 0.050* | |
N22 | 0.48622 (18) | 0.17682 (11) | 0.02471 (10) | 0.0124 (5) | |
C23 | 0.4758 (2) | 0.13631 (14) | 0.04233 (13) | 0.0156 (6) | |
C24 | 0.4617 (3) | 0.08467 (15) | 0.06547 (15) | 0.0270 (8) | |
H24A | 0.4042 | 0.0976 | 0.0941 | 0.041* | |
H24B | 0.5355 | 0.0800 | 0.0861 | 0.041* | |
H24C | 0.4359 | 0.0425 | 0.0314 | 0.041* | |
N201 | 0.67902 (18) | 0.17727 (10) | −0.08060 (10) | 0.0111 (5) | |
C201 | 0.7664 (2) | 0.13067 (14) | −0.11441 (13) | 0.0176 (6) | |
H20A | 0.7453 | 0.0859 | −0.1183 | 0.021* | |
H20B | 0.8428 | 0.1446 | −0.0898 | 0.021* | |
C202 | 0.7770 (2) | 0.12696 (14) | −0.17853 (12) | 0.0182 (6) | |
H20C | 0.7005 | 0.1177 | −0.2021 | 0.027* | |
H20D | 0.8272 | 0.0917 | −0.1991 | 0.027* | |
H20E | 0.8100 | 0.1692 | −0.1749 | 0.027* | |
N202 | 0.33143 (18) | 0.31186 (11) | 0.08457 (10) | 0.0122 (5) | |
C203 | 0.2475 (2) | 0.35048 (14) | 0.12842 (12) | 0.0162 (6) | |
H20F | 0.2600 | 0.3980 | 0.1381 | 0.019* | |
H20G | 0.2653 | 0.3449 | 0.1666 | 0.019* | |
C204 | 0.1193 (2) | 0.32956 (15) | 0.10424 (13) | 0.0205 (7) | |
H20H | 0.1037 | 0.3276 | 0.0632 | 0.031* | |
H20I | 0.0710 | 0.3618 | 0.1310 | 0.031* | |
H20J | 0.1019 | 0.2860 | 0.1032 | 0.031* | |
C211 | 0.8003 (2) | 0.29889 (13) | 0.00768 (13) | 0.0122 (6) | |
C212 | 0.8540 (2) | 0.30178 (14) | −0.04105 (13) | 0.0164 (6) | |
H212 | 0.8452 | 0.2652 | −0.0795 | 0.020* | |
C213 | 0.9203 (2) | 0.35891 (14) | −0.03225 (13) | 0.0187 (7) | |
H213 | 0.9554 | 0.3607 | −0.0649 | 0.022* | |
C214 | 0.9347 (2) | 0.41368 (14) | 0.02516 (13) | 0.0170 (6) | |
H214 | 0.9797 | 0.4519 | 0.0310 | 0.020* | |
C215 | 0.8820 (2) | 0.41128 (13) | 0.07372 (13) | 0.0158 (6) | |
H215 | 0.8918 | 0.4478 | 0.1122 | 0.019* | |
C216 | 0.8147 (2) | 0.35439 (13) | 0.06480 (13) | 0.0132 (6) | |
H216 | 0.7786 | 0.3532 | 0.0974 | 0.016* | |
C221 | 0.7714 (2) | 0.17933 (13) | 0.03261 (12) | 0.0135 (6) | |
C222 | 0.7399 (2) | 0.11016 (13) | 0.00896 (13) | 0.0153 (6) | |
H222 | 0.6844 | 0.0905 | −0.0258 | 0.018* | |
C223 | 0.7909 (2) | 0.07108 (14) | 0.03707 (13) | 0.0190 (7) | |
H223 | 0.7722 | 0.0250 | 0.0201 | 0.023* | |
C224 | 0.8703 (2) | 0.10069 (14) | 0.09067 (13) | 0.0196 (7) | |
H224 | 0.9027 | 0.0747 | 0.1103 | 0.024* | |
C225 | 0.9007 (2) | 0.16858 (14) | 0.11456 (13) | 0.0205 (7) | |
H225 | 0.9538 | 0.1883 | 0.1503 | 0.025* | |
C226 | 0.8527 (2) | 0.20770 (14) | 0.08563 (13) | 0.0172 (6) | |
H226 | 0.8750 | 0.2534 | 0.1018 | 0.021* | |
C231 | 0.5039 (2) | 0.20225 (13) | −0.15999 (12) | 0.0124 (6) | |
C232 | 0.5808 (2) | 0.24839 (13) | −0.16557 (12) | 0.0148 (6) | |
H232 | 0.6518 | 0.2618 | −0.1398 | 0.018* | |
C233 | 0.5536 (3) | 0.27474 (14) | −0.20894 (13) | 0.0190 (7) | |
H233 | 0.6067 | 0.3047 | −0.2129 | 0.023* | |
C234 | 0.4460 (3) | 0.25592 (14) | −0.24643 (13) | 0.0201 (7) | |
H234 | 0.4261 | 0.2740 | −0.2751 | 0.024* | |
C235 | 0.3691 (3) | 0.21032 (14) | −0.24091 (13) | 0.0216 (7) | |
H235 | 0.2973 | 0.1978 | −0.2660 | 0.026* | |
C236 | 0.3973 (2) | 0.18309 (13) | −0.19873 (12) | 0.0163 (6) | |
H236 | 0.3451 | 0.1519 | −0.1961 | 0.020* | |
C241 | 0.4700 (2) | 0.08856 (13) | −0.13117 (12) | 0.0127 (6) | |
C242 | 0.3688 (2) | 0.07395 (13) | −0.11078 (13) | 0.0153 (6) | |
H242 | 0.3370 | 0.1078 | −0.0787 | 0.018* | |
C243 | 0.3144 (3) | 0.00978 (14) | −0.13748 (13) | 0.0190 (7) | |
H243 | 0.2454 | 0.0013 | −0.1241 | 0.023* | |
C244 | 0.3624 (3) | −0.04169 (14) | −0.18404 (13) | 0.0204 (7) | |
H244 | 0.3263 | −0.0848 | −0.2016 | 0.025* | |
C245 | 0.4648 (3) | −0.02873 (15) | −0.20446 (14) | 0.0252 (7) | |
H245 | 0.4983 | −0.0632 | −0.2353 | 0.030* | |
C246 | 0.5167 (3) | 0.03596 (14) | −0.17847 (13) | 0.0216 (7) | |
H246 | 0.5844 | 0.0446 | −0.1929 | 0.026* | |
C251 | 0.5210 (2) | 0.40765 (13) | 0.14406 (13) | 0.0139 (6) | |
C252 | 0.5835 (2) | 0.44441 (14) | 0.12056 (13) | 0.0159 (6) | |
H252 | 0.6091 | 0.4228 | 0.0819 | 0.019* | |
C253 | 0.6084 (3) | 0.51314 (14) | 0.15420 (14) | 0.0217 (7) | |
H253 | 0.6540 | 0.5368 | 0.1390 | 0.026* | |
C254 | 0.5654 (3) | 0.54637 (15) | 0.21015 (14) | 0.0262 (8) | |
H254 | 0.5787 | 0.5928 | 0.2316 | 0.031* | |
C255 | 0.5027 (3) | 0.51089 (15) | 0.23445 (14) | 0.0239 (7) | |
H255 | 0.4738 | 0.5333 | 0.2722 | 0.029* | |
C256 | 0.4830 (2) | 0.44182 (14) | 0.20242 (13) | 0.0197 (7) | |
H256 | 0.4441 | 0.4177 | 0.2198 | 0.024* | |
C261 | 0.5212 (2) | 0.28541 (13) | 0.15845 (12) | 0.0128 (6) | |
C262 | 0.4421 (2) | 0.25201 (14) | 0.17754 (13) | 0.0166 (6) | |
H262 | 0.3626 | 0.2480 | 0.1628 | 0.020* | |
C263 | 0.4816 (3) | 0.22439 (14) | 0.21885 (13) | 0.0210 (7) | |
H263 | 0.4281 | 0.2032 | 0.2326 | 0.025* | |
C264 | 0.6003 (3) | 0.22844 (14) | 0.23954 (13) | 0.0189 (7) | |
H264 | 0.6265 | 0.2093 | 0.2666 | 0.023* | |
C265 | 0.6801 (3) | 0.26102 (14) | 0.21990 (13) | 0.0206 (7) | |
H265 | 0.7599 | 0.2634 | 0.2335 | 0.025* | |
C266 | 0.6406 (2) | 0.29001 (14) | 0.18001 (13) | 0.0186 (6) | |
H266 | 0.6940 | 0.3126 | 0.1675 | 0.022* | |
C271 | 0.2569 (2) | 0.32389 (13) | −0.02969 (13) | 0.0130 (6) | |
C272 | 0.2371 (2) | 0.29953 (14) | −0.09384 (13) | 0.0177 (6) | |
H272 | 0.2500 | 0.2548 | −0.1181 | 0.021* | |
C273 | 0.1983 (2) | 0.34117 (15) | −0.12202 (14) | 0.0212 (7) | |
H273 | 0.1835 | 0.3239 | −0.1649 | 0.025* | |
C274 | 0.1815 (2) | 0.40816 (15) | −0.08658 (14) | 0.0209 (7) | |
H274 | 0.1537 | 0.4358 | −0.1054 | 0.025* | |
C275 | 0.2064 (2) | 0.43389 (14) | −0.02248 (14) | 0.0187 (7) | |
H275 | 0.1978 | 0.4793 | 0.0014 | 0.022* | |
C276 | 0.2439 (2) | 0.39247 (13) | 0.00594 (13) | 0.0155 (6) | |
H276 | 0.2605 | 0.4102 | 0.0488 | 0.019* | |
C281 | 0.2015 (2) | 0.20132 (13) | −0.01218 (13) | 0.0134 (6) | |
C282 | 0.1988 (2) | 0.17082 (13) | 0.02896 (13) | 0.0167 (6) | |
H282 | 0.2467 | 0.1887 | 0.0667 | 0.020* | |
C283 | 0.1252 (2) | 0.11410 (14) | 0.01408 (14) | 0.0211 (7) | |
H283 | 0.1225 | 0.0951 | 0.0424 | 0.025* | |
C284 | 0.0557 (2) | 0.08550 (14) | −0.04279 (14) | 0.0216 (7) | |
H284 | 0.0076 | 0.0470 | −0.0531 | 0.026* | |
C285 | 0.0589 (2) | 0.11509 (14) | −0.08404 (14) | 0.0206 (7) | |
H285 | 0.0132 | 0.0958 | −0.1224 | 0.025* | |
C286 | 0.1293 (2) | 0.17295 (14) | −0.06889 (13) | 0.0175 (6) | |
H286 | 0.1285 | 0.1930 | −0.0965 | 0.021* | |
Fe3 | 0.0000 | 0.5000 | 0.5000 | 0.01026 (12) | |
P31 | 0.13162 (6) | 0.41734 (3) | 0.47439 (3) | 0.01135 (15) | |
P32 | −0.09047 (6) | 0.40397 (3) | 0.42608 (3) | 0.01146 (15) | |
N31 | −0.04992 (19) | 0.47972 (10) | 0.56434 (10) | 0.0128 (5) | |
C31 | −0.0871 (2) | 0.47510 (13) | 0.60493 (13) | 0.0147 (6) | |
C32 | −0.1353 (3) | 0.46982 (15) | 0.65658 (13) | 0.0220 (7) | |
H32A | −0.1704 | 0.5110 | 0.6799 | 0.033* | |
H32B | −0.0735 | 0.4618 | 0.6828 | 0.033* | |
H32C | −0.1939 | 0.4332 | 0.6412 | 0.033* | |
N301 | 0.02723 (19) | 0.35708 (10) | 0.42620 (10) | 0.0126 (5) | |
C301 | 0.0306 (2) | 0.28344 (13) | 0.38746 (13) | 0.0157 (6) | |
H30A | 0.0764 | 0.2771 | 0.3538 | 0.019* | |
H30B | −0.0489 | 0.2653 | 0.3693 | 0.019* | |
C302 | 0.0817 (3) | 0.24451 (14) | 0.42202 (14) | 0.0286 (8) | |
H30C | 0.1620 | 0.2603 | 0.4382 | 0.043* | |
H30D | 0.0788 | 0.1976 | 0.3946 | 0.043* | |
H30E | 0.0373 | 0.2506 | 0.4556 | 0.043* | |
C311 | 0.2112 (2) | 0.38754 (13) | 0.52800 (12) | 0.0135 (6) | |
C312 | 0.3327 (2) | 0.38225 (13) | 0.53121 (13) | 0.0159 (6) | |
H312 | 0.3737 | 0.3900 | 0.5030 | 0.019* | |
C313 | 0.3934 (3) | 0.36547 (14) | 0.57625 (13) | 0.0204 (7) | |
H313 | 0.4746 | 0.3628 | 0.5783 | 0.024* | |
C314 | 0.3334 (3) | 0.35287 (14) | 0.61776 (13) | 0.0205 (7) | |
H314 | 0.3741 | 0.3417 | 0.6478 | 0.025* | |
C315 | 0.2115 (3) | 0.35695 (13) | 0.61453 (13) | 0.0195 (7) | |
H315 | 0.1707 | 0.3480 | 0.6421 | 0.023* | |
C316 | 0.1517 (3) | 0.37442 (13) | 0.57027 (13) | 0.0171 (6) | |
H316 | 0.0706 | 0.3775 | 0.5686 | 0.021* | |
C321 | 0.2470 (2) | 0.42692 (13) | 0.43155 (13) | 0.0135 (6) | |
C322 | 0.3197 (2) | 0.48593 (14) | 0.45919 (13) | 0.0168 (6) | |
H322 | 0.3087 | 0.5177 | 0.4984 | 0.020* | |
C323 | 0.4080 (3) | 0.49762 (15) | 0.42892 (14) | 0.0225 (7) | |
H323 | 0.4561 | 0.5370 | 0.4479 | 0.027* | |
C324 | 0.4246 (3) | 0.45050 (15) | 0.37028 (14) | 0.0234 (7) | |
H324 | 0.4835 | 0.4584 | 0.3498 | 0.028* | |
C325 | 0.3537 (3) | 0.39209 (16) | 0.34257 (14) | 0.0245 (7) | |
H325 | 0.3648 | 0.3605 | 0.3033 | 0.029* | |
C326 | 0.2653 (2) | 0.38028 (14) | 0.37312 (13) | 0.0189 (7) | |
H326 | 0.2180 | 0.3406 | 0.3541 | 0.023* | |
C331 | −0.2162 (2) | 0.35804 (13) | 0.43402 (12) | 0.0128 (6) | |
C332 | −0.2111 (2) | 0.33939 (13) | 0.48369 (13) | 0.0166 (6) | |
H332 | −0.1411 | 0.3468 | 0.5098 | 0.020* | |
C333 | −0.3086 (2) | 0.31019 (14) | 0.49441 (13) | 0.0187 (6) | |
H333 | −0.3047 | 0.2992 | 0.5282 | 0.022* | |
C334 | −0.4122 (2) | 0.29738 (14) | 0.45458 (14) | 0.0194 (7) | |
H334 | −0.4778 | 0.2774 | 0.4616 | 0.023* | |
C335 | −0.4187 (2) | 0.31405 (14) | 0.40467 (13) | 0.0192 (7) | |
H335 | −0.4883 | 0.3049 | 0.3779 | 0.023* | |
C336 | −0.3216 (2) | 0.34448 (14) | 0.39428 (13) | 0.0178 (6) | |
H336 | −0.3266 | 0.3559 | 0.3607 | 0.021* | |
C341 | −0.1216 (2) | 0.40599 (13) | 0.35065 (12) | 0.0131 (6) | |
C342 | −0.2027 (2) | 0.45080 (14) | 0.34391 (13) | 0.0181 (6) | |
H342 | −0.2487 | 0.4731 | 0.3753 | 0.022* | |
C343 | −0.2147 (3) | 0.46196 (14) | 0.29051 (14) | 0.0226 (7) | |
H343 | −0.2684 | 0.4920 | 0.2863 | 0.027* | |
C344 | −0.1469 (3) | 0.42843 (15) | 0.24351 (14) | 0.0249 (7) | |
H344 | −0.1542 | 0.4364 | 0.2080 | 0.030* | |
C345 | −0.0685 (3) | 0.38327 (15) | 0.24940 (14) | 0.0230 (7) | |
H345 | −0.0245 | 0.3602 | 0.2174 | 0.028* | |
C346 | −0.0547 (2) | 0.37177 (14) | 0.30276 (13) | 0.0164 (6) | |
H346 | −0.0012 | 0.3414 | 0.3065 | 0.020* | |
Fe4 | 0.14631 (4) | 0.63246 (2) | 0.232917 (19) | 0.01662 (9) | |
Br41 | 0.10956 (3) | 0.732653 (14) | 0.212627 (13) | 0.01975 (7) | |
Br42 | −0.05024 (3) | 0.597971 (16) | 0.246892 (14) | 0.02454 (8) | |
Br43 | 0.30617 (3) | 0.665945 (16) | 0.321454 (14) | 0.02432 (8) | |
Br44 | 0.21358 (3) | 0.540478 (16) | 0.145070 (15) | 0.03289 (9) | |
Fe5 | 0.16724 (3) | 0.14210 (2) | 0.237383 (19) | 0.01592 (9) | |
Br51 | 0.16129 (2) | 0.249260 (14) | 0.225475 (13) | 0.01683 (7) | |
Br52 | −0.03289 (3) | 0.115160 (16) | 0.252091 (14) | 0.02229 (7) | |
Br53 | 0.21409 (3) | 0.051224 (15) | 0.141635 (14) | 0.02397 (8) | |
Br54 | 0.32399 (3) | 0.159690 (16) | 0.323658 (14) | 0.02511 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0109 (3) | 0.0098 (3) | 0.0095 (3) | 0.0004 (2) | 0.0010 (2) | 0.0043 (2) |
P11 | 0.0120 (4) | 0.0107 (3) | 0.0102 (4) | −0.0002 (3) | 0.0004 (3) | 0.0042 (3) |
P12 | 0.0119 (4) | 0.0102 (3) | 0.0102 (4) | 0.0004 (3) | 0.0008 (3) | 0.0037 (3) |
N11 | 0.0100 (12) | 0.0069 (11) | 0.0125 (13) | −0.0025 (9) | −0.0010 (10) | 0.0025 (10) |
C11 | 0.0122 (14) | 0.0117 (14) | 0.0153 (16) | −0.0006 (11) | −0.0010 (12) | 0.0028 (12) |
C12 | 0.0275 (18) | 0.0265 (17) | 0.0172 (16) | 0.0010 (14) | 0.0068 (14) | 0.0124 (14) |
N101 | 0.0129 (12) | 0.0089 (11) | 0.0125 (12) | 0.0002 (9) | −0.0015 (10) | 0.0035 (10) |
C101 | 0.0185 (15) | 0.0094 (14) | 0.0193 (16) | 0.0004 (12) | 0.0009 (13) | 0.0036 (12) |
C102 | 0.0334 (19) | 0.0150 (15) | 0.0206 (17) | 0.0059 (14) | 0.0037 (14) | 0.0051 (13) |
C111 | 0.0149 (15) | 0.0082 (13) | 0.0120 (15) | −0.0016 (11) | 0.0008 (12) | 0.0001 (11) |
C112 | 0.0165 (15) | 0.0186 (15) | 0.0162 (16) | 0.0014 (12) | 0.0020 (12) | 0.0100 (13) |
C113 | 0.0142 (15) | 0.0248 (17) | 0.0228 (17) | 0.0020 (13) | 0.0000 (13) | 0.0100 (14) |
C114 | 0.0127 (15) | 0.0187 (15) | 0.0266 (18) | 0.0000 (12) | 0.0063 (13) | 0.0099 (14) |
C115 | 0.0211 (16) | 0.0194 (15) | 0.0207 (17) | 0.0024 (13) | 0.0056 (13) | 0.0134 (13) |
C116 | 0.0137 (15) | 0.0164 (15) | 0.0172 (16) | −0.0004 (12) | −0.0009 (12) | 0.0065 (13) |
C121 | 0.0120 (14) | 0.0128 (14) | 0.0101 (14) | −0.0038 (11) | −0.0044 (11) | 0.0058 (11) |
C122 | 0.0187 (15) | 0.0110 (14) | 0.0131 (15) | −0.0009 (12) | −0.0002 (12) | 0.0012 (12) |
C123 | 0.0178 (16) | 0.0180 (15) | 0.0193 (16) | −0.0005 (12) | −0.0079 (13) | 0.0098 (13) |
C124 | 0.0224 (16) | 0.0249 (16) | 0.0139 (16) | −0.0070 (13) | −0.0046 (13) | 0.0117 (13) |
C125 | 0.0154 (15) | 0.0314 (17) | 0.0154 (16) | 0.0008 (13) | 0.0013 (13) | 0.0124 (14) |
C126 | 0.0131 (15) | 0.0193 (15) | 0.0179 (16) | 0.0002 (12) | 0.0008 (12) | 0.0089 (13) |
C131 | 0.0163 (15) | 0.0089 (13) | 0.0098 (14) | 0.0025 (11) | −0.0008 (12) | 0.0020 (11) |
C132 | 0.0168 (15) | 0.0137 (14) | 0.0183 (16) | 0.0026 (12) | 0.0021 (12) | 0.0063 (12) |
C133 | 0.0237 (17) | 0.0152 (15) | 0.0133 (15) | 0.0036 (12) | 0.0048 (13) | 0.0061 (12) |
C134 | 0.0275 (17) | 0.0177 (15) | 0.0103 (15) | 0.0035 (13) | −0.0027 (13) | 0.0065 (12) |
C135 | 0.0170 (16) | 0.0174 (15) | 0.0227 (17) | 0.0005 (12) | −0.0021 (13) | 0.0069 (13) |
C136 | 0.0153 (15) | 0.0147 (14) | 0.0148 (15) | −0.0005 (12) | 0.0022 (12) | 0.0072 (12) |
C141 | 0.0130 (14) | 0.0167 (14) | 0.0157 (15) | 0.0040 (12) | 0.0008 (12) | 0.0103 (12) |
C142 | 0.0155 (15) | 0.0183 (15) | 0.0172 (16) | 0.0014 (12) | 0.0049 (12) | 0.0065 (13) |
C143 | 0.0150 (16) | 0.0237 (17) | 0.0323 (19) | −0.0007 (13) | 0.0058 (14) | 0.0162 (15) |
C144 | 0.0188 (16) | 0.0386 (19) | 0.0254 (18) | 0.0105 (14) | 0.0124 (14) | 0.0218 (16) |
C145 | 0.0210 (17) | 0.0285 (17) | 0.0154 (16) | 0.0092 (14) | 0.0048 (13) | 0.0087 (14) |
C146 | 0.0165 (15) | 0.0190 (15) | 0.0140 (15) | 0.0034 (12) | 0.0017 (12) | 0.0053 (13) |
Fe2 | 0.0102 (2) | 0.01134 (19) | 0.0103 (2) | 0.00068 (16) | 0.00200 (16) | 0.00533 (16) |
P21 | 0.0102 (4) | 0.0119 (4) | 0.0109 (4) | 0.0003 (3) | 0.0011 (3) | 0.0049 (3) |
P22 | 0.0103 (4) | 0.0121 (4) | 0.0109 (4) | 0.0000 (3) | 0.0015 (3) | 0.0046 (3) |
P23 | 0.0121 (4) | 0.0123 (4) | 0.0111 (4) | 0.0008 (3) | 0.0026 (3) | 0.0050 (3) |
P24 | 0.0109 (4) | 0.0142 (4) | 0.0117 (4) | 0.0020 (3) | 0.0026 (3) | 0.0063 (3) |
N21 | 0.0085 (11) | 0.0145 (12) | 0.0100 (12) | 0.0008 (9) | 0.0014 (9) | 0.0038 (10) |
C21 | 0.0185 (16) | 0.0175 (15) | 0.0146 (16) | 0.0011 (12) | 0.0017 (12) | 0.0054 (13) |
C22 | 0.049 (2) | 0.0244 (18) | 0.034 (2) | −0.0040 (16) | 0.0037 (17) | 0.0215 (16) |
N22 | 0.0079 (12) | 0.0172 (12) | 0.0130 (13) | 0.0006 (10) | 0.0022 (9) | 0.0069 (10) |
C23 | 0.0130 (15) | 0.0179 (15) | 0.0145 (15) | 0.0007 (12) | 0.0023 (12) | 0.0050 (13) |
C24 | 0.0359 (19) | 0.0230 (17) | 0.0323 (19) | 0.0049 (15) | 0.0098 (16) | 0.0203 (15) |
N201 | 0.0093 (11) | 0.0132 (12) | 0.0100 (12) | −0.0002 (9) | 0.0009 (9) | 0.0040 (10) |
C201 | 0.0145 (15) | 0.0217 (16) | 0.0168 (16) | 0.0053 (12) | 0.0032 (12) | 0.0078 (13) |
C202 | 0.0205 (16) | 0.0185 (15) | 0.0160 (16) | 0.0053 (13) | 0.0079 (13) | 0.0063 (13) |
N202 | 0.0107 (12) | 0.0172 (12) | 0.0092 (12) | 0.0020 (10) | 0.0022 (9) | 0.0057 (10) |
C203 | 0.0203 (16) | 0.0155 (15) | 0.0123 (15) | 0.0054 (12) | 0.0051 (12) | 0.0046 (12) |
C204 | 0.0157 (15) | 0.0298 (17) | 0.0190 (17) | 0.0068 (13) | 0.0072 (13) | 0.0118 (14) |
C211 | 0.0079 (13) | 0.0129 (14) | 0.0178 (15) | 0.0001 (11) | −0.0033 (11) | 0.0096 (12) |
C212 | 0.0125 (14) | 0.0210 (15) | 0.0151 (15) | −0.0005 (12) | 0.0011 (12) | 0.0072 (13) |
C213 | 0.0145 (15) | 0.0244 (16) | 0.0201 (17) | −0.0016 (13) | 0.0043 (13) | 0.0116 (14) |
C214 | 0.0134 (15) | 0.0139 (14) | 0.0250 (17) | −0.0026 (12) | −0.0011 (13) | 0.0106 (13) |
C215 | 0.0133 (14) | 0.0116 (14) | 0.0190 (16) | 0.0015 (11) | −0.0006 (12) | 0.0036 (12) |
C216 | 0.0122 (14) | 0.0142 (14) | 0.0147 (15) | 0.0003 (11) | 0.0036 (12) | 0.0069 (12) |
C221 | 0.0111 (14) | 0.0168 (14) | 0.0145 (15) | 0.0008 (11) | 0.0024 (12) | 0.0083 (12) |
C222 | 0.0146 (15) | 0.0160 (15) | 0.0130 (15) | 0.0005 (12) | 0.0011 (12) | 0.0039 (12) |
C223 | 0.0187 (16) | 0.0180 (15) | 0.0207 (17) | 0.0004 (13) | 0.0042 (13) | 0.0082 (13) |
C224 | 0.0177 (16) | 0.0240 (16) | 0.0215 (17) | 0.0032 (13) | 0.0011 (13) | 0.0142 (14) |
C225 | 0.0165 (16) | 0.0269 (17) | 0.0174 (16) | −0.0030 (13) | −0.0060 (13) | 0.0105 (14) |
C226 | 0.0160 (15) | 0.0165 (15) | 0.0178 (16) | −0.0028 (12) | 0.0013 (12) | 0.0060 (13) |
C231 | 0.0156 (15) | 0.0110 (14) | 0.0092 (14) | 0.0034 (11) | 0.0034 (11) | 0.0022 (11) |
C232 | 0.0137 (15) | 0.0175 (15) | 0.0121 (15) | 0.0015 (12) | 0.0014 (12) | 0.0052 (12) |
C233 | 0.0225 (16) | 0.0164 (15) | 0.0192 (16) | 0.0028 (13) | 0.0062 (13) | 0.0077 (13) |
C234 | 0.0305 (18) | 0.0177 (15) | 0.0128 (16) | 0.0043 (13) | 0.0014 (13) | 0.0074 (13) |
C235 | 0.0245 (17) | 0.0212 (16) | 0.0139 (16) | 0.0018 (13) | −0.0067 (13) | 0.0042 (13) |
C236 | 0.0169 (15) | 0.0153 (15) | 0.0131 (15) | −0.0029 (12) | −0.0002 (12) | 0.0027 (12) |
C241 | 0.0131 (14) | 0.0111 (14) | 0.0136 (15) | 0.0001 (11) | −0.0005 (12) | 0.0055 (12) |
C242 | 0.0176 (15) | 0.0145 (14) | 0.0143 (15) | 0.0011 (12) | 0.0019 (12) | 0.0064 (12) |
C243 | 0.0183 (16) | 0.0193 (15) | 0.0222 (17) | −0.0013 (13) | 0.0023 (13) | 0.0116 (13) |
C244 | 0.0236 (17) | 0.0128 (15) | 0.0210 (17) | −0.0031 (13) | −0.0063 (13) | 0.0054 (13) |
C245 | 0.0199 (17) | 0.0209 (16) | 0.0254 (18) | 0.0020 (13) | 0.0018 (14) | 0.0004 (14) |
C246 | 0.0185 (16) | 0.0210 (16) | 0.0214 (17) | −0.0036 (13) | 0.0064 (13) | 0.0041 (14) |
C251 | 0.0130 (14) | 0.0117 (14) | 0.0160 (15) | 0.0010 (11) | −0.0016 (12) | 0.0057 (12) |
C252 | 0.0154 (15) | 0.0169 (15) | 0.0159 (16) | 0.0002 (12) | 0.0022 (12) | 0.0072 (12) |
C253 | 0.0267 (17) | 0.0180 (16) | 0.0229 (17) | −0.0033 (13) | −0.0003 (14) | 0.0119 (14) |
C254 | 0.0328 (19) | 0.0148 (16) | 0.0249 (18) | 0.0001 (14) | −0.0056 (15) | 0.0043 (14) |
C255 | 0.0268 (18) | 0.0229 (17) | 0.0164 (17) | 0.0056 (14) | 0.0021 (14) | 0.0025 (14) |
C256 | 0.0192 (16) | 0.0225 (16) | 0.0176 (16) | 0.0020 (13) | 0.0050 (13) | 0.0080 (13) |
C261 | 0.0140 (14) | 0.0127 (14) | 0.0084 (14) | 0.0017 (11) | 0.0001 (11) | 0.0016 (11) |
C262 | 0.0144 (15) | 0.0224 (16) | 0.0160 (16) | 0.0026 (12) | 0.0020 (12) | 0.0111 (13) |
C263 | 0.0227 (17) | 0.0228 (16) | 0.0218 (17) | −0.0002 (13) | 0.0053 (13) | 0.0128 (14) |
C264 | 0.0281 (17) | 0.0174 (15) | 0.0141 (16) | 0.0024 (13) | −0.0001 (13) | 0.0100 (13) |
C265 | 0.0179 (16) | 0.0252 (17) | 0.0188 (17) | −0.0013 (13) | −0.0033 (13) | 0.0108 (14) |
C266 | 0.0186 (16) | 0.0196 (15) | 0.0179 (16) | −0.0020 (13) | 0.0011 (13) | 0.0082 (13) |
C271 | 0.0070 (13) | 0.0166 (14) | 0.0190 (16) | 0.0026 (11) | 0.0028 (11) | 0.0105 (12) |
C272 | 0.0202 (16) | 0.0183 (15) | 0.0161 (16) | 0.0048 (13) | 0.0037 (13) | 0.0082 (13) |
C273 | 0.0220 (17) | 0.0296 (18) | 0.0148 (16) | 0.0005 (14) | 0.0008 (13) | 0.0125 (14) |
C274 | 0.0172 (16) | 0.0274 (17) | 0.0258 (18) | 0.0024 (13) | 0.0020 (13) | 0.0189 (15) |
C275 | 0.0178 (16) | 0.0149 (15) | 0.0268 (18) | 0.0035 (12) | 0.0076 (13) | 0.0109 (13) |
C276 | 0.0132 (15) | 0.0196 (15) | 0.0142 (15) | −0.0009 (12) | 0.0004 (12) | 0.0078 (13) |
C281 | 0.0101 (14) | 0.0158 (14) | 0.0148 (15) | 0.0025 (11) | 0.0046 (12) | 0.0059 (12) |
C282 | 0.0133 (15) | 0.0168 (15) | 0.0202 (16) | 0.0015 (12) | 0.0007 (12) | 0.0083 (13) |
C283 | 0.0167 (16) | 0.0203 (16) | 0.0311 (19) | 0.0043 (13) | 0.0067 (14) | 0.0145 (14) |
C284 | 0.0127 (15) | 0.0162 (15) | 0.0330 (19) | 0.0006 (12) | 0.0071 (14) | 0.0063 (14) |
C285 | 0.0111 (15) | 0.0227 (16) | 0.0206 (17) | 0.0031 (12) | 0.0014 (13) | 0.0018 (13) |
C286 | 0.0139 (15) | 0.0201 (15) | 0.0187 (16) | 0.0043 (12) | 0.0043 (12) | 0.0077 (13) |
Fe3 | 0.0108 (3) | 0.0100 (3) | 0.0105 (3) | −0.0001 (2) | 0.0010 (2) | 0.0048 (2) |
P31 | 0.0116 (4) | 0.0112 (3) | 0.0110 (4) | −0.0006 (3) | 0.0011 (3) | 0.0045 (3) |
P32 | 0.0114 (4) | 0.0115 (3) | 0.0116 (4) | −0.0005 (3) | 0.0009 (3) | 0.0051 (3) |
N31 | 0.0128 (12) | 0.0096 (12) | 0.0160 (13) | −0.0012 (9) | −0.0018 (10) | 0.0062 (10) |
C31 | 0.0129 (15) | 0.0114 (14) | 0.0192 (16) | −0.0005 (11) | −0.0006 (12) | 0.0065 (12) |
C32 | 0.0235 (17) | 0.0287 (17) | 0.0203 (17) | 0.0010 (14) | 0.0061 (14) | 0.0157 (14) |
N301 | 0.0141 (12) | 0.0100 (11) | 0.0122 (12) | 0.0004 (9) | −0.0006 (10) | 0.0037 (10) |
C301 | 0.0181 (15) | 0.0103 (14) | 0.0162 (16) | −0.0009 (12) | 0.0020 (12) | 0.0031 (12) |
C302 | 0.047 (2) | 0.0147 (16) | 0.0212 (18) | 0.0060 (15) | 0.0004 (16) | 0.0058 (14) |
C311 | 0.0172 (15) | 0.0120 (14) | 0.0086 (14) | −0.0003 (12) | −0.0015 (12) | 0.0025 (11) |
C312 | 0.0159 (15) | 0.0177 (15) | 0.0142 (15) | −0.0020 (12) | 0.0002 (12) | 0.0073 (12) |
C313 | 0.0159 (16) | 0.0217 (16) | 0.0224 (17) | 0.0013 (13) | −0.0009 (13) | 0.0088 (14) |
C314 | 0.0277 (17) | 0.0157 (15) | 0.0183 (16) | 0.0036 (13) | −0.0044 (13) | 0.0089 (13) |
C315 | 0.0274 (17) | 0.0163 (15) | 0.0175 (16) | 0.0032 (13) | 0.0074 (13) | 0.0085 (13) |
C316 | 0.0196 (16) | 0.0148 (15) | 0.0182 (16) | 0.0035 (12) | 0.0060 (13) | 0.0072 (13) |
C321 | 0.0125 (14) | 0.0161 (14) | 0.0147 (15) | 0.0034 (12) | 0.0014 (12) | 0.0091 (12) |
C322 | 0.0177 (15) | 0.0151 (15) | 0.0159 (16) | 0.0002 (12) | 0.0023 (12) | 0.0046 (12) |
C323 | 0.0174 (16) | 0.0257 (17) | 0.0260 (18) | −0.0047 (13) | 0.0010 (14) | 0.0127 (14) |
C324 | 0.0154 (16) | 0.0351 (19) | 0.0266 (18) | 0.0009 (14) | 0.0081 (14) | 0.0184 (16) |
C325 | 0.0179 (16) | 0.0377 (19) | 0.0153 (16) | 0.0038 (14) | 0.0049 (13) | 0.0077 (15) |
C326 | 0.0168 (16) | 0.0202 (16) | 0.0159 (16) | −0.0030 (12) | −0.0002 (13) | 0.0044 (13) |
C331 | 0.0143 (14) | 0.0077 (13) | 0.0145 (15) | −0.0002 (11) | 0.0024 (12) | 0.0025 (11) |
C332 | 0.0151 (15) | 0.0160 (15) | 0.0172 (16) | 0.0004 (12) | −0.0020 (12) | 0.0064 (13) |
C333 | 0.0229 (16) | 0.0167 (15) | 0.0198 (16) | 0.0003 (13) | 0.0047 (13) | 0.0103 (13) |
C334 | 0.0146 (15) | 0.0159 (15) | 0.0294 (18) | 0.0000 (12) | 0.0066 (13) | 0.0103 (14) |
C335 | 0.0117 (15) | 0.0206 (16) | 0.0218 (17) | −0.0016 (12) | −0.0025 (13) | 0.0066 (13) |
C336 | 0.0174 (15) | 0.0198 (15) | 0.0163 (16) | 0.0009 (12) | 0.0002 (13) | 0.0081 (13) |
C341 | 0.0127 (14) | 0.0136 (14) | 0.0133 (15) | −0.0054 (11) | −0.0025 (12) | 0.0069 (12) |
C342 | 0.0169 (15) | 0.0165 (15) | 0.0166 (16) | −0.0011 (12) | −0.0008 (12) | 0.0033 (13) |
C343 | 0.0273 (18) | 0.0169 (15) | 0.0205 (17) | −0.0025 (13) | −0.0108 (14) | 0.0082 (13) |
C344 | 0.039 (2) | 0.0221 (17) | 0.0151 (17) | −0.0074 (15) | −0.0047 (14) | 0.0111 (14) |
C345 | 0.0273 (18) | 0.0249 (17) | 0.0165 (17) | −0.0037 (14) | 0.0044 (14) | 0.0080 (14) |
C346 | 0.0137 (15) | 0.0201 (15) | 0.0169 (16) | −0.0022 (12) | −0.0003 (12) | 0.0098 (13) |
Fe4 | 0.0196 (2) | 0.0150 (2) | 0.0156 (2) | 0.00046 (17) | 0.00424 (18) | 0.00618 (18) |
Br41 | 0.02573 (17) | 0.01523 (15) | 0.01923 (16) | 0.00135 (12) | 0.00420 (13) | 0.00777 (12) |
Br42 | 0.02170 (17) | 0.03379 (18) | 0.02361 (17) | −0.00469 (14) | 0.00257 (13) | 0.01754 (15) |
Br43 | 0.02348 (17) | 0.03017 (18) | 0.02137 (17) | −0.00340 (14) | −0.00050 (13) | 0.01365 (14) |
Br44 | 0.0464 (2) | 0.02217 (17) | 0.02545 (19) | 0.01064 (15) | 0.01292 (16) | 0.00312 (15) |
Fe5 | 0.0157 (2) | 0.0174 (2) | 0.0149 (2) | −0.00073 (17) | 0.00152 (17) | 0.00711 (18) |
Br51 | 0.01698 (15) | 0.01555 (14) | 0.01768 (16) | 0.00025 (12) | 0.00260 (12) | 0.00655 (12) |
Br52 | 0.01755 (16) | 0.03281 (18) | 0.01856 (16) | −0.00492 (13) | 0.00183 (13) | 0.01293 (14) |
Br53 | 0.02957 (18) | 0.01813 (15) | 0.02158 (17) | 0.00578 (13) | 0.00572 (14) | 0.00496 (13) |
Br54 | 0.01952 (16) | 0.03858 (19) | 0.02197 (17) | −0.00576 (14) | −0.00288 (13) | 0.01876 (15) |
Fe1—N11i | 1.906 (2) | C233—H233 | 0.9300 |
Fe1—N11 | 1.906 (2) | C234—C235 | 1.381 (4) |
Fe1—P11 | 2.2499 (7) | C234—H234 | 0.9300 |
Fe1—P11i | 2.2499 (7) | C235—C236 | 1.379 (4) |
Fe1—P12 | 2.2870 (7) | C235—H235 | 0.9300 |
Fe1—P12i | 2.2870 (7) | C236—H236 | 0.9300 |
P11—N101 | 1.701 (2) | C241—C242 | 1.390 (4) |
P11—C111 | 1.818 (3) | C241—C246 | 1.397 (4) |
P11—C121 | 1.826 (3) | C242—C243 | 1.386 (4) |
P12—N101 | 1.711 (2) | C242—H242 | 0.9300 |
P12—C141 | 1.818 (3) | C243—C244 | 1.383 (4) |
P12—C131 | 1.821 (3) | C243—H243 | 0.9300 |
N11—C11 | 1.143 (3) | C244—C245 | 1.389 (4) |
C11—C12 | 1.449 (4) | C244—H244 | 0.9300 |
C12—H12A | 0.9600 | C245—C246 | 1.385 (4) |
C12—H12B | 0.9600 | C245—H245 | 0.9300 |
C12—H12C | 0.9600 | C246—H246 | 0.9300 |
N101—C101 | 1.492 (3) | C251—C252 | 1.388 (4) |
C101—C102 | 1.501 (4) | C251—C256 | 1.403 (4) |
C101—H10A | 0.9700 | C252—C253 | 1.388 (4) |
C101—H10B | 0.9700 | C252—H252 | 0.9300 |
C102—H10C | 0.9600 | C253—C254 | 1.380 (4) |
C102—H10D | 0.9600 | C253—H253 | 0.9300 |
C102—H10E | 0.9600 | C254—C255 | 1.382 (4) |
C111—C116 | 1.398 (4) | C254—H254 | 0.9300 |
C111—C112 | 1.401 (4) | C255—C256 | 1.384 (4) |
C112—C113 | 1.389 (4) | C255—H255 | 0.9300 |
C112—H112 | 0.9300 | C256—H256 | 0.9300 |
C113—C114 | 1.383 (4) | C261—C262 | 1.385 (4) |
C113—H113 | 0.9300 | C261—C266 | 1.396 (4) |
C114—C115 | 1.385 (4) | C262—C263 | 1.394 (4) |
C114—H114 | 0.9300 | C262—H262 | 0.9300 |
C115—C116 | 1.379 (4) | C263—C264 | 1.384 (4) |
C115—H115 | 0.9300 | C263—H263 | 0.9300 |
C116—H116 | 0.9300 | C264—C265 | 1.387 (4) |
C121—C126 | 1.387 (4) | C264—H264 | 0.9300 |
C121—C122 | 1.400 (4) | C265—C266 | 1.386 (4) |
C122—C123 | 1.381 (4) | C265—H265 | 0.9300 |
C122—H122 | 0.9300 | C266—H266 | 0.9300 |
C123—C124 | 1.390 (4) | C271—C272 | 1.391 (4) |
C123—H123 | 0.9300 | C271—C276 | 1.403 (4) |
C124—C125 | 1.381 (4) | C272—C273 | 1.387 (4) |
C124—H124 | 0.9300 | C272—H272 | 0.9300 |
C125—C126 | 1.393 (4) | C273—C274 | 1.382 (4) |
C125—H125 | 0.9300 | C273—H273 | 0.9300 |
C126—H126 | 0.9300 | C274—C275 | 1.391 (4) |
C131—C136 | 1.393 (4) | C274—H274 | 0.9300 |
C131—C132 | 1.406 (4) | C275—C276 | 1.383 (4) |
C132—C133 | 1.381 (4) | C275—H275 | 0.9300 |
C132—H132 | 0.9300 | C276—H276 | 0.9300 |
C133—C134 | 1.382 (4) | C281—C286 | 1.400 (4) |
C133—H133 | 0.9300 | C281—C282 | 1.400 (4) |
C134—C135 | 1.383 (4) | C282—C283 | 1.388 (4) |
C134—H134 | 0.9300 | C282—H282 | 0.9300 |
C135—C136 | 1.398 (4) | C283—C284 | 1.388 (4) |
C135—H135 | 0.9300 | C283—H283 | 0.9300 |
C136—H136 | 0.9300 | C284—C285 | 1.388 (4) |
C141—C146 | 1.391 (4) | C284—H284 | 0.9300 |
C141—C142 | 1.405 (4) | C285—C286 | 1.386 (4) |
C142—C143 | 1.381 (4) | C285—H285 | 0.9300 |
C142—H142 | 0.9300 | C286—H286 | 0.9300 |
C143—C144 | 1.393 (4) | Fe3—N31ii | 1.908 (2) |
C143—H143 | 0.9300 | Fe3—N31 | 1.908 (2) |
C144—C145 | 1.383 (4) | Fe3—P32 | 2.2588 (7) |
C144—H144 | 0.9300 | Fe3—P32ii | 2.2588 (7) |
C145—C146 | 1.389 (4) | Fe3—P31 | 2.2877 (7) |
C145—H145 | 0.9300 | Fe3—P31ii | 2.2877 (7) |
C146—H146 | 0.9300 | P31—N301 | 1.707 (2) |
Fe2—N22 | 1.902 (2) | P31—C321 | 1.819 (3) |
Fe2—N21 | 1.906 (2) | P31—C311 | 1.827 (3) |
Fe2—P21 | 2.2547 (8) | P31—P32 | 2.6389 (10) |
Fe2—P24 | 2.2687 (8) | P32—N301 | 1.699 (2) |
Fe2—P23 | 2.2805 (8) | P32—C341 | 1.818 (3) |
Fe2—P22 | 2.2842 (8) | P32—C331 | 1.820 (3) |
P21—N201 | 1.696 (2) | N31—C31 | 1.142 (3) |
P21—C221 | 1.810 (3) | C31—C32 | 1.452 (4) |
P21—C211 | 1.825 (3) | C32—H32A | 0.9600 |
P21—P22 | 2.6311 (10) | C32—H32B | 0.9600 |
P22—N201 | 1.702 (2) | C32—H32C | 0.9600 |
P22—C231 | 1.815 (3) | N301—C301 | 1.491 (3) |
P22—C241 | 1.824 (3) | C301—C302 | 1.493 (4) |
P23—N202 | 1.705 (2) | C301—H30A | 0.9700 |
P23—C251 | 1.824 (3) | C301—H30B | 0.9700 |
P23—C261 | 1.825 (3) | C302—H30C | 0.9600 |
P23—P24 | 2.6360 (10) | C302—H30D | 0.9600 |
P24—N202 | 1.699 (2) | C302—H30E | 0.9600 |
P24—C271 | 1.817 (3) | C311—C312 | 1.395 (4) |
P24—C281 | 1.826 (3) | C311—C316 | 1.398 (4) |
N21—C21 | 1.131 (3) | C312—C313 | 1.393 (4) |
C21—C22 | 1.464 (4) | C312—H312 | 0.9300 |
C22—H22A | 0.9600 | C313—C314 | 1.380 (4) |
C22—H22B | 0.9600 | C313—H313 | 0.9300 |
C22—H22C | 0.9600 | C314—C315 | 1.396 (4) |
N22—C23 | 1.136 (3) | C314—H314 | 0.9300 |
C23—C24 | 1.461 (4) | C315—C316 | 1.383 (4) |
C24—H24A | 0.9600 | C315—H315 | 0.9300 |
C24—H24B | 0.9600 | C316—H316 | 0.9300 |
C24—H24C | 0.9600 | C321—C326 | 1.387 (4) |
N201—C201 | 1.484 (3) | C321—C322 | 1.397 (4) |
C201—C202 | 1.520 (4) | C322—C323 | 1.386 (4) |
C201—H20A | 0.9700 | C322—H322 | 0.9300 |
C201—H20B | 0.9700 | C323—C324 | 1.389 (4) |
C202—H20C | 0.9600 | C323—H323 | 0.9300 |
C202—H20D | 0.9600 | C324—C325 | 1.377 (4) |
C202—H20E | 0.9600 | C324—H324 | 0.9300 |
N202—C203 | 1.495 (3) | C325—C326 | 1.392 (4) |
C203—C204 | 1.512 (4) | C325—H325 | 0.9300 |
C203—H20F | 0.9700 | C326—H326 | 0.9300 |
C203—H20G | 0.9700 | C331—C336 | 1.400 (4) |
C204—H20H | 0.9600 | C331—C332 | 1.401 (4) |
C204—H20I | 0.9600 | C332—C333 | 1.381 (4) |
C204—H20J | 0.9600 | C332—H332 | 0.9300 |
C211—C216 | 1.393 (4) | C333—C334 | 1.387 (4) |
C211—C212 | 1.399 (4) | C333—H333 | 0.9300 |
C212—C213 | 1.383 (4) | C334—C335 | 1.379 (4) |
C212—H212 | 0.9300 | C334—H334 | 0.9300 |
C213—C214 | 1.390 (4) | C335—C336 | 1.389 (4) |
C213—H213 | 0.9300 | C335—H335 | 0.9300 |
C214—C215 | 1.385 (4) | C336—H336 | 0.9300 |
C214—H214 | 0.9300 | C341—C346 | 1.396 (4) |
C215—C216 | 1.384 (4) | C341—C342 | 1.399 (4) |
C215—H215 | 0.9300 | C342—C343 | 1.388 (4) |
C216—H216 | 0.9300 | C342—H342 | 0.9300 |
C221—C226 | 1.394 (4) | C343—C344 | 1.386 (4) |
C221—C222 | 1.405 (4) | C343—H343 | 0.9300 |
C222—C223 | 1.384 (4) | C344—C345 | 1.377 (4) |
C222—H222 | 0.9300 | C344—H344 | 0.9300 |
C223—C224 | 1.393 (4) | C345—C346 | 1.391 (4) |
C223—H223 | 0.9300 | C345—H345 | 0.9300 |
C224—C225 | 1.377 (4) | C346—H346 | 0.9300 |
C224—H224 | 0.9300 | Fe4—Br44 | 2.4348 (5) |
C225—C226 | 1.386 (4) | Fe4—Br41 | 2.4583 (5) |
C225—H225 | 0.9300 | Fe4—Br42 | 2.4701 (5) |
C226—H226 | 0.9300 | Fe4—Br43 | 2.4948 (5) |
C231—C232 | 1.391 (4) | Fe5—Br53 | 2.4485 (5) |
C231—C236 | 1.397 (4) | Fe5—Br52 | 2.4614 (5) |
C232—C233 | 1.388 (4) | Fe5—Br51 | 2.4716 (5) |
C232—H232 | 0.9300 | Fe5—Br54 | 2.4805 (5) |
C233—C234 | 1.392 (4) | ||
N11i—Fe1—N11 | 180.000 (1) | C225—C226—C221 | 120.7 (3) |
N11i—Fe1—P11 | 89.05 (6) | C225—C226—H226 | 119.6 |
N11—Fe1—P11 | 90.95 (6) | C221—C226—H226 | 119.7 |
N11i—Fe1—P11i | 90.95 (6) | C232—C231—C236 | 118.6 (3) |
N11—Fe1—P11i | 89.05 (6) | C232—C231—P22 | 121.3 (2) |
P11—Fe1—P11i | 180.00 (3) | C236—C231—P22 | 119.5 (2) |
N11i—Fe1—P12 | 87.31 (7) | C233—C232—C231 | 121.2 (3) |
N11—Fe1—P12 | 92.69 (7) | C233—C232—H232 | 119.4 |
P11—Fe1—P12 | 70.82 (3) | C231—C232—H232 | 119.4 |
P11i—Fe1—P12 | 109.18 (3) | C232—C233—C234 | 119.4 (3) |
N11i—Fe1—P12i | 92.69 (7) | C232—C233—H233 | 120.3 |
N11—Fe1—P12i | 87.31 (7) | C234—C233—H233 | 120.3 |
P11—Fe1—P12i | 109.18 (3) | C235—C234—C233 | 119.7 (3) |
P11i—Fe1—P12i | 70.82 (3) | C235—C234—H234 | 120.2 |
P12—Fe1—P12i | 180.000 (1) | C233—C234—H234 | 120.2 |
N101—P11—C111 | 105.46 (12) | C236—C235—C234 | 120.9 (3) |
N101—P11—C121 | 109.35 (12) | C236—C235—H235 | 119.5 |
C111—P11—C121 | 106.96 (12) | C234—C235—H235 | 119.5 |
N101—P11—Fe1 | 94.42 (8) | C235—C236—C231 | 120.2 (3) |
C111—P11—Fe1 | 124.95 (9) | C235—C236—H236 | 119.9 |
C121—P11—Fe1 | 113.83 (9) | C231—C236—H236 | 119.9 |
N101—P12—C141 | 110.11 (12) | C242—C241—C246 | 117.7 (2) |
N101—P12—C131 | 110.15 (11) | C242—C241—P22 | 118.5 (2) |
C141—P12—C131 | 103.43 (12) | C246—C241—P22 | 123.7 (2) |
N101—P12—Fe1 | 92.84 (8) | C243—C242—C241 | 121.1 (3) |
C141—P12—Fe1 | 117.03 (9) | C243—C242—H242 | 119.4 |
C131—P12—Fe1 | 122.62 (9) | C241—C242—H242 | 119.4 |
C11—N11—Fe1 | 171.8 (2) | C244—C243—C242 | 120.2 (3) |
N11—C11—C12 | 178.3 (3) | C244—C243—H243 | 119.9 |
C11—C12—H12A | 109.5 | C242—C243—H243 | 119.9 |
C11—C12—H12B | 109.5 | C243—C244—C245 | 119.8 (3) |
H12A—C12—H12B | 109.5 | C243—C244—H244 | 120.1 |
C11—C12—H12C | 109.5 | C245—C244—H244 | 120.1 |
H12A—C12—H12C | 109.5 | C246—C245—C244 | 119.5 (3) |
H12B—C12—H12C | 109.5 | C246—C245—H245 | 120.3 |
C101—N101—P11 | 125.24 (17) | C244—C245—H245 | 120.3 |
C101—N101—P12 | 133.48 (18) | C245—C246—C241 | 121.6 (3) |
P11—N101—P12 | 100.82 (11) | C245—C246—H246 | 119.2 |
N101—C101—C102 | 114.1 (2) | C241—C246—H246 | 119.2 |
N101—C101—H10A | 108.7 | C252—C251—C256 | 118.3 (3) |
C102—C101—H10A | 108.7 | C252—C251—P23 | 122.4 (2) |
N101—C101—H10B | 108.7 | C256—C251—P23 | 119.2 (2) |
C102—C101—H10B | 108.7 | C251—C252—C253 | 120.7 (3) |
H10A—C101—H10B | 107.6 | C251—C252—H252 | 119.6 |
C101—C102—H10C | 109.5 | C253—C252—H252 | 119.6 |
C101—C102—H10D | 109.5 | C254—C253—C252 | 120.0 (3) |
H10C—C102—H10D | 109.5 | C254—C253—H253 | 120.0 |
C101—C102—H10E | 109.5 | C252—C253—H253 | 120.0 |
H10C—C102—H10E | 109.5 | C253—C254—C255 | 120.2 (3) |
H10D—C102—H10E | 109.5 | C253—C254—H254 | 119.9 |
C116—C111—C112 | 118.3 (3) | C255—C254—H254 | 119.9 |
C116—C111—P11 | 119.4 (2) | C254—C255—C256 | 119.7 (3) |
C112—C111—P11 | 122.2 (2) | C254—C255—H255 | 120.1 |
C113—C112—C111 | 120.6 (3) | C256—C255—H255 | 120.1 |
C113—C112—H112 | 119.7 | C255—C256—C251 | 120.8 (3) |
C111—C112—H112 | 119.7 | C255—C256—H256 | 119.6 |
C114—C113—C112 | 119.7 (3) | C251—C256—H256 | 119.6 |
C114—C113—H113 | 120.2 | C262—C261—C266 | 119.5 (3) |
C112—C113—H113 | 120.2 | C262—C261—P23 | 123.6 (2) |
C113—C114—C115 | 120.5 (3) | C266—C261—P23 | 116.7 (2) |
C113—C114—H114 | 119.7 | C261—C262—C263 | 120.0 (3) |
C115—C114—H114 | 119.7 | C261—C262—H262 | 120.0 |
C116—C115—C114 | 119.7 (3) | C263—C262—H262 | 120.0 |
C116—C115—H115 | 120.1 | C264—C263—C262 | 120.3 (3) |
C114—C115—H115 | 120.1 | C264—C263—H263 | 119.9 |
C115—C116—C111 | 121.1 (3) | C262—C263—H263 | 119.9 |
C115—C116—H116 | 119.5 | C263—C264—C265 | 120.0 (3) |
C111—C116—H116 | 119.5 | C263—C264—H264 | 120.0 |
C126—C121—C122 | 119.3 (2) | C265—C264—H264 | 120.0 |
C126—C121—P11 | 121.4 (2) | C266—C265—C264 | 119.9 (3) |
C122—C121—P11 | 118.5 (2) | C266—C265—H265 | 120.1 |
C123—C122—C121 | 120.3 (3) | C264—C265—H265 | 120.1 |
C123—C122—H122 | 119.9 | C265—C266—C261 | 120.4 (3) |
C121—C122—H122 | 119.9 | C265—C266—H266 | 119.8 |
C122—C123—C124 | 120.3 (3) | C261—C266—H266 | 119.8 |
C122—C123—H123 | 119.9 | C272—C271—C276 | 118.6 (2) |
C124—C123—H123 | 119.9 | C272—C271—P24 | 120.1 (2) |
C125—C124—C123 | 119.6 (3) | C276—C271—P24 | 121.0 (2) |
C125—C124—H124 | 120.2 | C273—C272—C271 | 120.8 (3) |
C123—C124—H124 | 120.2 | C273—C272—H272 | 119.6 |
C124—C125—C126 | 120.5 (3) | C271—C272—H272 | 119.6 |
C124—C125—H125 | 119.8 | C274—C273—C272 | 120.3 (3) |
C126—C125—H125 | 119.8 | C274—C273—H273 | 119.9 |
C121—C126—C125 | 120.0 (3) | C272—C273—H273 | 119.9 |
C121—C126—H126 | 120.0 | C273—C274—C275 | 119.5 (3) |
C125—C126—H126 | 120.0 | C273—C274—H274 | 120.3 |
C136—C131—C132 | 118.3 (2) | C275—C274—H274 | 120.3 |
C136—C131—P12 | 121.3 (2) | C276—C275—C274 | 120.5 (3) |
C132—C131—P12 | 119.9 (2) | C276—C275—H275 | 119.7 |
C133—C132—C131 | 120.8 (3) | C274—C275—H275 | 119.7 |
C133—C132—H132 | 119.6 | C275—C276—C271 | 120.2 (3) |
C131—C132—H132 | 119.6 | C275—C276—H276 | 119.9 |
C132—C133—C134 | 120.4 (3) | C271—C276—H276 | 119.9 |
C132—C133—H133 | 119.8 | C286—C281—C282 | 118.5 (3) |
C134—C133—H133 | 119.8 | C286—C281—P24 | 122.8 (2) |
C133—C134—C135 | 119.7 (3) | C282—C281—P24 | 118.2 (2) |
C133—C134—H134 | 120.2 | C283—C282—C281 | 120.7 (3) |
C135—C134—H134 | 120.2 | C283—C282—H282 | 119.6 |
C134—C135—C136 | 120.4 (3) | C281—C282—H282 | 119.6 |
C134—C135—H135 | 119.8 | C282—C283—C284 | 120.4 (3) |
C136—C135—H135 | 119.8 | C282—C283—H283 | 119.8 |
C131—C136—C135 | 120.4 (3) | C284—C283—H283 | 119.8 |
C131—C136—H136 | 119.8 | C285—C284—C283 | 119.2 (3) |
C135—C136—H136 | 119.8 | C285—C284—H284 | 120.4 |
C146—C141—C142 | 118.5 (3) | C283—C284—H284 | 120.4 |
C146—C141—P12 | 123.5 (2) | C286—C285—C284 | 120.9 (3) |
C142—C141—P12 | 118.0 (2) | C286—C285—H285 | 119.5 |
C143—C142—C141 | 120.6 (3) | C284—C285—H285 | 119.5 |
C143—C142—H142 | 119.7 | C285—C286—C281 | 120.3 (3) |
C141—C142—H142 | 119.7 | C285—C286—H286 | 119.9 |
C142—C143—C144 | 120.2 (3) | C281—C286—H286 | 119.9 |
C142—C143—H143 | 119.9 | N31ii—Fe3—N31 | 180.000 (1) |
C144—C143—H143 | 119.9 | N31ii—Fe3—P32 | 88.21 (7) |
C145—C144—C143 | 119.6 (3) | N31—Fe3—P32 | 91.79 (7) |
C145—C144—H144 | 120.2 | N31ii—Fe3—P32ii | 91.79 (7) |
C143—C144—H144 | 120.2 | N31—Fe3—P32ii | 88.21 (7) |
C144—C145—C146 | 120.4 (3) | P32—Fe3—P32ii | 180.00 (3) |
C144—C145—H145 | 119.8 | N31ii—Fe3—P31 | 86.52 (7) |
C146—C145—H145 | 119.8 | N31—Fe3—P31 | 93.48 (7) |
C145—C146—C141 | 120.7 (3) | P32—Fe3—P31 | 70.96 (3) |
C145—C146—H146 | 119.6 | P32ii—Fe3—P31 | 109.04 (3) |
C141—C146—H146 | 119.6 | N31ii—Fe3—P31ii | 93.48 (7) |
N22—Fe2—N21 | 179.12 (9) | N31—Fe3—P31ii | 86.52 (7) |
N22—Fe2—P21 | 89.60 (7) | P32—Fe3—P31ii | 109.04 (3) |
N21—Fe2—P21 | 89.53 (7) | P32ii—Fe3—P31ii | 70.96 (3) |
N22—Fe2—P24 | 90.39 (7) | P31—Fe3—P31ii | 180.00 (4) |
N21—Fe2—P24 | 90.49 (7) | N301—P31—C321 | 110.51 (12) |
P21—Fe2—P24 | 179.79 (4) | N301—P31—C311 | 109.44 (11) |
N22—Fe2—P23 | 85.89 (7) | C321—P31—C311 | 102.30 (12) |
N21—Fe2—P23 | 94.35 (7) | N301—P31—Fe3 | 92.83 (8) |
P21—Fe2—P23 | 108.97 (3) | C321—P31—Fe3 | 115.69 (9) |
P24—Fe2—P23 | 70.82 (3) | C311—P31—Fe3 | 125.43 (9) |
N22—Fe2—P22 | 91.34 (7) | N301—P32—C341 | 109.48 (12) |
N21—Fe2—P22 | 88.42 (7) | N301—P32—C331 | 106.19 (11) |
P21—Fe2—P22 | 70.85 (3) | C341—P32—C331 | 105.83 (12) |
P24—Fe2—P22 | 109.36 (3) | N301—P32—Fe3 | 94.06 (8) |
P23—Fe2—P22 | 177.23 (3) | C341—P32—Fe3 | 113.76 (9) |
N201—P21—C221 | 104.76 (12) | C331—P32—Fe3 | 125.85 (9) |
N201—P21—C211 | 107.95 (12) | C331—P32—P31 | 130.73 (9) |
C221—P21—C211 | 107.53 (12) | Fe3—P32—P31 | 55.03 (2) |
N201—P21—Fe2 | 94.40 (8) | C31—N31—Fe3 | 171.2 (2) |
C221—P21—Fe2 | 121.62 (9) | N31—C31—C32 | 179.3 (3) |
C211—P21—Fe2 | 117.96 (9) | C31—C32—H32A | 109.5 |
N201—P22—C231 | 106.64 (12) | C31—C32—H32B | 109.5 |
N201—P22—C241 | 109.74 (11) | H32A—C32—H32B | 109.5 |
C231—P22—C241 | 104.20 (12) | C31—C32—H32C | 109.5 |
N201—P22—Fe2 | 93.20 (8) | H32A—C32—H32C | 109.5 |
C231—P22—Fe2 | 119.35 (9) | H32B—C32—H32C | 109.5 |
C241—P22—Fe2 | 122.05 (9) | C301—N301—P32 | 125.11 (18) |
N202—P23—C251 | 105.73 (12) | C301—N301—P31 | 133.09 (18) |
N202—P23—C261 | 108.43 (12) | P32—N301—P31 | 101.56 (11) |
C251—P23—C261 | 101.65 (12) | N301—C301—C302 | 114.1 (2) |
N202—P23—Fe2 | 93.13 (8) | N301—C301—H30A | 108.7 |
C251—P23—Fe2 | 129.41 (10) | C302—C301—H30A | 108.7 |
C261—P23—Fe2 | 116.33 (9) | N301—C301—H30B | 108.7 |
N202—P23—P24 | 39.16 (7) | C302—C301—H30B | 108.7 |
C251—P23—P24 | 123.81 (9) | H30A—C301—H30B | 107.6 |
C261—P23—P24 | 127.22 (9) | C301—C302—H30C | 109.5 |
Fe2—P23—P24 | 54.38 (2) | C301—C302—H30D | 109.5 |
N202—P24—C271 | 110.43 (12) | H30C—C302—H30D | 109.5 |
N202—P24—C281 | 106.44 (12) | C301—C302—H30E | 109.5 |
C271—P24—C281 | 108.10 (12) | H30C—C302—H30E | 109.5 |
N202—P24—Fe2 | 93.71 (8) | H30D—C302—H30E | 109.5 |
C271—P24—Fe2 | 115.17 (9) | C312—C311—C316 | 118.4 (2) |
C281—P24—Fe2 | 121.39 (9) | C312—C311—P31 | 121.4 (2) |
N202—P24—P23 | 39.33 (7) | C316—C311—P31 | 120.0 (2) |
C271—P24—P23 | 118.72 (9) | C313—C312—C311 | 120.6 (3) |
C281—P24—P23 | 128.81 (9) | C313—C312—H312 | 119.7 |
Fe2—P24—P23 | 54.80 (2) | C311—C312—H312 | 119.7 |
C21—N21—Fe2 | 176.5 (2) | C314—C313—C312 | 120.3 (3) |
N21—C21—C22 | 178.2 (3) | C314—C313—H313 | 119.9 |
C21—C22—H22A | 109.5 | C312—C313—H313 | 119.9 |
C21—C22—H22B | 109.5 | C313—C314—C315 | 119.8 (3) |
H22A—C22—H22B | 109.5 | C313—C314—H314 | 120.1 |
C21—C22—H22C | 109.5 | C315—C314—H314 | 120.1 |
H22A—C22—H22C | 109.5 | C316—C315—C314 | 119.8 (3) |
H22B—C22—H22C | 109.5 | C316—C315—H315 | 120.1 |
C23—N22—Fe2 | 176.1 (2) | C314—C315—H315 | 120.1 |
N22—C23—C24 | 179.4 (3) | C315—C316—C311 | 121.1 (3) |
C23—C24—H24A | 109.5 | C315—C316—H316 | 119.5 |
C23—C24—H24B | 109.5 | C311—C316—H316 | 119.5 |
H24A—C24—H24B | 109.5 | C326—C321—C322 | 118.4 (3) |
C23—C24—H24C | 109.5 | C326—C321—P31 | 124.2 (2) |
H24A—C24—H24C | 109.5 | C322—C321—P31 | 117.3 (2) |
H24B—C24—H24C | 109.5 | C323—C322—C321 | 120.8 (3) |
C201—N201—P21 | 125.14 (17) | C323—C322—H322 | 119.6 |
C201—N201—P22 | 130.45 (18) | C321—C322—H322 | 119.6 |
P21—N201—P22 | 101.49 (12) | C322—C323—C324 | 120.0 (3) |
N201—C201—C202 | 115.0 (2) | C322—C323—H323 | 120.0 |
N201—C201—H20A | 108.5 | C324—C323—H323 | 120.0 |
C202—C201—H20A | 108.5 | C325—C324—C323 | 119.8 (3) |
N201—C201—H20B | 108.5 | C325—C324—H324 | 120.1 |
C202—C201—H20B | 108.5 | C323—C324—H324 | 120.1 |
H20A—C201—H20B | 107.5 | C324—C325—C326 | 120.2 (3) |
C201—C202—H20C | 109.5 | C324—C325—H325 | 119.9 |
C201—C202—H20D | 109.5 | C326—C325—H325 | 119.9 |
H20C—C202—H20D | 109.5 | C321—C326—C325 | 120.8 (3) |
C201—C202—H20E | 109.5 | C321—C326—H326 | 119.6 |
H20C—C202—H20E | 109.5 | C325—C326—H326 | 119.6 |
H20D—C202—H20E | 109.5 | C336—C331—C332 | 118.4 (3) |
C203—N202—P24 | 130.88 (17) | C336—C331—P32 | 122.0 (2) |
C203—N202—P23 | 125.86 (17) | C332—C331—P32 | 119.5 (2) |
P24—N202—P23 | 101.52 (12) | C333—C332—C331 | 120.9 (3) |
N202—C203—C204 | 114.4 (2) | C333—C332—H332 | 119.5 |
N202—C203—H20F | 108.7 | C331—C332—H332 | 119.5 |
C204—C203—H20F | 108.7 | C332—C333—C334 | 119.7 (3) |
N202—C203—H20G | 108.7 | C332—C333—H333 | 120.1 |
C204—C203—H20G | 108.7 | C334—C333—H333 | 120.1 |
H20F—C203—H20G | 107.6 | C335—C334—C333 | 120.4 (3) |
C203—C204—H20H | 109.5 | C335—C334—H334 | 119.8 |
C203—C204—H20I | 109.5 | C333—C334—H334 | 119.8 |
H20H—C204—H20I | 109.5 | C334—C335—C336 | 120.1 (3) |
C203—C204—H20J | 109.5 | C334—C335—H335 | 119.9 |
H20H—C204—H20J | 109.5 | C336—C335—H335 | 119.9 |
H20I—C204—H20J | 109.5 | C335—C336—C331 | 120.4 (3) |
C216—C211—C212 | 118.9 (2) | C335—C336—H336 | 119.8 |
C216—C211—P21 | 119.0 (2) | C331—C336—H336 | 119.8 |
C212—C211—P21 | 121.7 (2) | C346—C341—C342 | 119.4 (3) |
C213—C212—C211 | 120.2 (3) | C346—C341—P32 | 121.5 (2) |
C213—C212—H212 | 119.9 | C342—C341—P32 | 118.4 (2) |
C211—C212—H212 | 119.9 | C343—C342—C341 | 120.1 (3) |
C212—C213—C214 | 120.3 (3) | C343—C342—H342 | 119.9 |
C212—C213—H213 | 119.9 | C341—C342—H342 | 119.9 |
C214—C213—H213 | 119.9 | C344—C343—C342 | 120.1 (3) |
C215—C214—C213 | 120.0 (3) | C344—C343—H343 | 119.9 |
C215—C214—H214 | 120.0 | C342—C343—H343 | 119.9 |
C213—C214—H214 | 120.0 | C345—C344—C343 | 120.0 (3) |
C216—C215—C214 | 119.8 (3) | C345—C344—H344 | 120.0 |
C216—C215—H215 | 120.1 | C343—C344—H344 | 120.0 |
C214—C215—H215 | 120.1 | C344—C345—C346 | 120.7 (3) |
C215—C216—C211 | 120.9 (3) | C344—C345—H345 | 119.6 |
C215—C216—H216 | 119.6 | C346—C345—H345 | 119.6 |
C211—C216—H216 | 119.6 | C345—C346—C341 | 119.6 (3) |
C226—C221—C222 | 118.5 (3) | C345—C346—H346 | 120.2 |
C226—C221—P21 | 122.6 (2) | C341—C346—H346 | 120.2 |
C222—C221—P21 | 118.8 (2) | Br44—Fe4—Br41 | 112.36 (2) |
C223—C222—C221 | 120.4 (3) | Br44—Fe4—Br42 | 108.159 (19) |
C223—C222—H222 | 119.8 | Br41—Fe4—Br42 | 103.198 (18) |
C221—C222—H222 | 119.8 | Br44—Fe4—Br43 | 107.70 (2) |
C222—C223—C224 | 120.1 (3) | Br41—Fe4—Br43 | 107.016 (18) |
C222—C223—H223 | 119.9 | Br42—Fe4—Br43 | 118.46 (2) |
C224—C223—H223 | 119.9 | Br53—Fe5—Br52 | 106.989 (18) |
C225—C224—C223 | 119.8 (3) | Br53—Fe5—Br51 | 109.886 (19) |
C225—C224—H224 | 120.1 | Br52—Fe5—Br51 | 106.833 (18) |
C223—C224—H224 | 120.1 | Br53—Fe5—Br54 | 110.360 (19) |
C224—C225—C226 | 120.4 (3) | Br52—Fe5—Br54 | 116.388 (19) |
C224—C225—H225 | 119.8 | Br51—Fe5—Br54 | 106.252 (18) |
C226—C225—H225 | 119.8 | ||
Fe1—P11—C111—C112 | −116.7 (2) | Fe2—P23—C251—C252 | −5.2 (3) |
Fe1—P11—C111—C116 | 59.1 (2) | Fe2—P23—C251—C256 | 171.75 (17) |
Fe1—P11—C121—C122 | 64.9 (2) | Fe2—P23—C261—C262 | −93.9 (2) |
Fe1—P11—C121—C126 | −104.5 (2) | Fe2—P23—C261—C266 | 80.4 (2) |
Fe1—P12—C131—C132 | −54.0 (2) | Fe2—P24—C271—C272 | 74.3 (2) |
Fe1—P12—C131—C136 | 118.1 (2) | Fe2—P24—C271—C276 | −99.4 (2) |
Fe1—P12—C141—C142 | −55.8 (2) | Fe2—P24—C281—C282 | 70.5 (2) |
Fe1—P12—C141—C146 | 121.2 (2) | Fe2—P24—C281—C286 | −101.3 (2) |
Fe2—P21—C211—C212 | −109.0 (2) | Fe3—P31—C311—C312 | −130.0 (2) |
Fe2—P21—C211—C216 | 63.6 (2) | Fe3—P31—C311—C316 | 45.1 (3) |
Fe2—P21—C221—C222 | 67.9 (2) | Fe3—P31—C321—C322 | 58.2 (2) |
Fe2—P21—C221—C226 | −108.2 (2) | Fe3—P31—C321—C326 | −120.4 (2) |
Fe2—P22—C231—C232 | 71.8 (2) | Fe3—P32—C331—C332 | −53.1 (2) |
Fe2—P22—C231—C236 | −99.9 (2) | Fe3—P32—C331—C336 | 122.6 (2) |
Fe2—P22—C241—C242 | 28.5 (3) | Fe3—P32—C341—C342 | −65.9 (2) |
Fe2—P22—C241—C246 | −154.3 (2) | Fe3—P32—C341—C346 | 104.5 (2) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C32—H32B···Br42ii | 0.96 | 2.80 | 3.718 (3) | 160 |
C315—H315···Br42ii | 0.93 | 2.93 | 3.746 (3) | 147 |
C276—H276···Br44 | 0.93 | 2.93 | 3.607 (3) | 131 |
C202—H20E···Br41iii | 0.96 | 2.83 | 3.741 (3) | 159 |
C225—H225···Br51iv | 0.93 | 2.77 | 3.658 (3) | 159 |
C262—H262···Br51 | 0.93 | 2.88 | 3.540 (3) | 129 |
C326—H326···Br51 | 0.93 | 2.89 | 3.571 (3) | 131 |
C12—H12B···Br52 | 0.96 | 2.83 | 3.724 (3) | 154 |
C201—H20A···Br53v | 0.97 | 2.86 | 3.762 (3) | 155 |
C24—H24A···Br53 | 0.96 | 2.92 | 3.755 (3) | 146 |
C242—H242···Cg14 | 0.93 | 2.78 | 3.553 (3) | 142 |
Symmetry codes: (ii) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z; (iv) x+1, y, z; (v) −x+1, −y, −z. |
[Fe(C2H3N)2(C26H25NP2)2][Fe2Br6O] | F(000) = 3104 |
Mr = 1571.94 | Dx = 1.743 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9916 reflections |
a = 18.928 (5) Å | θ = 2.2–27.3° |
b = 18.352 (4) Å | µ = 4.87 mm−1 |
c = 17.243 (4) Å | T = 100 K |
β = 90.365 (3)° | Plate, red |
V = 5989 (3) Å3 | 0.55 × 0.24 × 0.22 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 13071 independent reflections |
Radiation source: fine-focus sealed tube | 10694 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
ω scans | θmax = 27.1°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | h = −24→23 |
Tmin = 0.175, Tmax = 0.413 | k = −22→23 |
64539 measured reflections | l = −22→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0393P)2 + 17.460P] where P = (Fo2 + 2Fc2)/3 |
13071 reflections | (Δ/σ)max = 0.004 |
758 parameters | Δρmax = 3.18 e Å−3 |
49 restraints | Δρmin = −1.08 e Å−3 |
[Fe(C2H3N)2(C26H25NP2)2][Fe2Br6O] | V = 5989 (3) Å3 |
Mr = 1571.94 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 18.928 (5) Å | µ = 4.87 mm−1 |
b = 18.352 (4) Å | T = 100 K |
c = 17.243 (4) Å | 0.55 × 0.24 × 0.22 mm |
β = 90.365 (3)° |
Bruker APEXII CCD area-detector diffractometer | 13071 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | 10694 reflections with I > 2σ(I) |
Tmin = 0.175, Tmax = 0.413 | Rint = 0.038 |
64539 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 49 restraints |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0393P)2 + 17.460P] where P = (Fo2 + 2Fc2)/3 |
13071 reflections | Δρmax = 3.18 e Å−3 |
758 parameters | Δρmin = −1.08 e Å−3 |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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) | |
Fe1 | 0.5000 | 0.0000 | 1.0000 | 0.01014 (13) | |
P12 | 0.56645 (4) | 0.04259 (4) | 1.10119 (5) | 0.01188 (17) | |
P11 | 0.53319 (4) | −0.09495 (4) | 1.07553 (5) | 0.01136 (16) | |
N11 | 0.41664 (15) | 0.00619 (15) | 1.05991 (16) | 0.0131 (6) | |
C11 | 0.3695 (2) | 0.0056 (2) | 1.1003 (2) | 0.0226 (8) | |
C12 | 0.3103 (3) | 0.0053 (3) | 1.1541 (3) | 0.0536 (15) | |
H12A | 0.3268 | 0.0188 | 1.2048 | 0.080* | |
H12B | 0.2901 | −0.0426 | 1.1559 | 0.080* | |
H12C | 0.2752 | 0.0395 | 1.1368 | 0.080* | |
N101 | 0.58636 (15) | −0.04306 (14) | 1.13331 (16) | 0.0133 (6) | |
C101 | 0.62703 (19) | −0.06177 (19) | 1.2050 (2) | 0.0201 (8) | |
H10A | 0.5981 | −0.0510 | 1.2498 | 0.024* | |
H10B | 0.6687 | −0.0311 | 1.2078 | 0.024* | |
C102 | 0.6498 (2) | −0.14064 (19) | 1.2088 (2) | 0.0231 (8) | |
H10C | 0.6092 | −0.1715 | 1.2029 | 0.035* | |
H10D | 0.6719 | −0.1500 | 1.2581 | 0.035* | |
H10E | 0.6827 | −0.1505 | 1.1680 | 0.035* | |
C111 | 0.58560 (18) | −0.16878 (18) | 1.03474 (19) | 0.0143 (7) | |
C112 | 0.55556 (19) | −0.23711 (18) | 1.0192 (2) | 0.0168 (7) | |
H112 | 0.5104 | −0.2478 | 1.0368 | 0.020* | |
C113 | 0.5932 (2) | −0.28874 (19) | 0.9776 (2) | 0.0219 (8) | |
H113 | 0.5729 | −0.3338 | 0.9671 | 0.026* | |
C114 | 0.6607 (2) | −0.2737 (2) | 0.9516 (2) | 0.0229 (8) | |
H114 | 0.6853 | −0.3086 | 0.9235 | 0.028* | |
C115 | 0.6913 (2) | −0.2072 (2) | 0.9674 (2) | 0.0217 (8) | |
H115 | 0.7368 | −0.1974 | 0.9504 | 0.026* | |
C116 | 0.65440 (19) | −0.15468 (19) | 1.0085 (2) | 0.0184 (7) | |
H116 | 0.6754 | −0.1098 | 1.0188 | 0.022* | |
C121 | 0.46495 (18) | −0.13735 (17) | 1.13365 (19) | 0.0140 (7) | |
C122 | 0.40902 (18) | −0.17262 (19) | 1.0953 (2) | 0.0180 (7) | |
H122 | 0.4085 | −0.1748 | 1.0414 | 0.022* | |
C123 | 0.3548 (2) | −0.2041 (2) | 1.1368 (2) | 0.0225 (8) | |
H123 | 0.3183 | −0.2279 | 1.1107 | 0.027* | |
C124 | 0.3545 (2) | −0.2004 (2) | 1.2167 (2) | 0.0270 (9) | |
H124 | 0.3186 | −0.2229 | 1.2444 | 0.032* | |
C125 | 0.4071 (2) | −0.1636 (2) | 1.2554 (2) | 0.0272 (9) | |
H125 | 0.4059 | −0.1599 | 1.3092 | 0.033* | |
C126 | 0.4623 (2) | −0.1317 (2) | 1.2142 (2) | 0.0213 (8) | |
H126 | 0.4976 | −0.1065 | 1.2407 | 0.026* | |
C131 | 0.65150 (18) | 0.08776 (18) | 1.09073 (19) | 0.0148 (7) | |
C132 | 0.71268 (19) | 0.04872 (19) | 1.0730 (2) | 0.0187 (7) | |
H132 | 0.7106 | −0.0018 | 1.0687 | 0.022* | |
C133 | 0.7765 (2) | 0.0842 (2) | 1.0615 (2) | 0.0242 (8) | |
H133 | 0.8170 | 0.0576 | 1.0505 | 0.029* | |
C134 | 0.7796 (2) | 0.1597 (2) | 1.0667 (2) | 0.0259 (8) | |
H134 | 0.8221 | 0.1837 | 1.0580 | 0.031* | |
C135 | 0.7198 (2) | 0.1992 (2) | 1.0846 (2) | 0.0212 (8) | |
H135 | 0.7223 | 0.2497 | 1.0885 | 0.025* | |
C136 | 0.65596 (19) | 0.16376 (19) | 1.0969 (2) | 0.0176 (7) | |
H136 | 0.6159 | 0.1906 | 1.1093 | 0.021* | |
C141 | 0.52630 (18) | 0.09546 (17) | 1.17818 (19) | 0.0145 (7) | |
C142 | 0.4678 (2) | 0.13852 (19) | 1.1615 (2) | 0.0200 (7) | |
H142 | 0.4489 | 0.1381 | 1.1116 | 0.024* | |
C143 | 0.4372 (2) | 0.1822 (2) | 1.2178 (2) | 0.0219 (8) | |
H143 | 0.3986 | 0.2115 | 1.2054 | 0.026* | |
C144 | 0.4644 (2) | 0.1817 (2) | 1.2922 (2) | 0.0231 (8) | |
H144 | 0.4429 | 0.2092 | 1.3307 | 0.028* | |
C145 | 0.5236 (2) | 0.1403 (2) | 1.3097 (2) | 0.0274 (9) | |
H145 | 0.5421 | 0.1408 | 1.3597 | 0.033* | |
C146 | 0.5551 (2) | 0.0984 (2) | 1.2531 (2) | 0.0219 (8) | |
H146 | 0.5957 | 0.0720 | 1.2649 | 0.026* | |
Fe2 | 0.0000 | 0.5000 | 1.0000 | 0.01327 (14) | |
P21 | −0.06981 (4) | 0.40074 (5) | 0.98158 (5) | 0.01386 (17) | |
P22 | 0.07000 (4) | 0.39978 (5) | 0.98305 (5) | 0.01414 (17) | |
N21 | −0.00206 (15) | 0.52075 (15) | 0.89202 (18) | 0.0165 (6) | |
C21 | −0.00811 (19) | 0.54028 (19) | 0.8293 (2) | 0.0203 (8) | |
C22 | −0.0168 (2) | 0.5655 (2) | 0.7501 (2) | 0.0307 (9) | |
H22A | −0.0449 | 0.5312 | 0.7215 | 0.046* | |
H22B | 0.0287 | 0.5701 | 0.7264 | 0.046* | |
H22C | −0.0399 | 0.6121 | 0.7501 | 0.046* | |
N201 | −0.00051 (15) | 0.34486 (15) | 0.96243 (17) | 0.0148 (6) | |
C20A | 0.0048 (7) | 0.2765 (8) | 0.9170 (7) | 0.017 (3) | 0.50 |
H20A | 0.0518 | 0.2564 | 0.9237 | 0.021* | 0.50 |
H20B | −0.0017 | 0.2878 | 0.8624 | 0.021* | 0.50 |
C20B | −0.0082 (8) | 0.2648 (8) | 0.9415 (8) | 0.023 (3) | 0.50 |
H20C | 0.0192 | 0.2358 | 0.9779 | 0.028* | 0.50 |
H20D | −0.0574 | 0.2507 | 0.9466 | 0.028* | 0.50 |
C202 | −0.0495 (4) | 0.2193 (4) | 0.9407 (4) | 0.0222 (16) | 0.50 |
H20E | −0.0404 | 0.2043 | 0.9932 | 0.033* | 0.50 |
H20F | −0.0460 | 0.1779 | 0.9069 | 0.033* | 0.50 |
H20G | −0.0961 | 0.2397 | 0.9369 | 0.033* | 0.50 |
C203 | 0.0154 (6) | 0.2485 (5) | 0.8620 (5) | 0.047 (3) | 0.50 |
H20H | −0.0047 | 0.2834 | 0.8268 | 0.070* | 0.50 |
H20I | 0.0001 | 0.2004 | 0.8477 | 0.070* | 0.50 |
H20J | 0.0660 | 0.2510 | 0.8599 | 0.070* | 0.50 |
C211 | −0.13224 (18) | 0.38791 (18) | 0.9024 (2) | 0.0152 (7) | |
C212 | −0.20471 (19) | 0.37592 (19) | 0.9142 (2) | 0.0190 (7) | |
H212 | −0.2218 | 0.3710 | 0.9643 | 0.023* | |
C213 | −0.25088 (19) | 0.37137 (19) | 0.8518 (2) | 0.0206 (8) | |
H213 | −0.2987 | 0.3631 | 0.8604 | 0.025* | |
C214 | −0.22640 (19) | 0.3791 (2) | 0.7765 (2) | 0.0223 (8) | |
H214 | −0.2578 | 0.3772 | 0.7348 | 0.027* | |
C215 | −0.15475 (19) | 0.3897 (2) | 0.7637 (2) | 0.0207 (8) | |
H215 | −0.1380 | 0.3938 | 0.7133 | 0.025* | |
C216 | −0.10802 (19) | 0.39419 (19) | 0.8258 (2) | 0.0179 (7) | |
H216 | −0.0602 | 0.4015 | 0.8167 | 0.021* | |
C221 | −0.11514 (19) | 0.37032 (19) | 1.0686 (2) | 0.0184 (7) | |
C222 | −0.1700 (2) | 0.4129 (2) | 1.0982 (2) | 0.0240 (8) | |
H222 | −0.1866 | 0.4527 | 1.0701 | 0.029* | |
C223 | −0.1998 (2) | 0.3963 (3) | 1.1690 (3) | 0.0340 (10) | |
H223 | −0.2370 | 0.4242 | 1.1878 | 0.041* | |
C224 | −0.1742 (2) | 0.3379 (2) | 1.2120 (2) | 0.0337 (10) | |
H224 | −0.1939 | 0.3271 | 1.2600 | 0.040* | |
C225 | −0.1199 (2) | 0.2959 (2) | 1.1840 (2) | 0.0301 (9) | |
H225 | −0.1031 | 0.2566 | 1.2130 | 0.036* | |
C226 | −0.0898 (2) | 0.3119 (2) | 1.1124 (2) | 0.0230 (8) | |
H226 | −0.0528 | 0.2836 | 1.0938 | 0.028* | |
C231 | 0.13568 (18) | 0.38267 (19) | 0.9082 (2) | 0.0187 (7) | |
C232 | 0.1242 (2) | 0.4041 (2) | 0.8322 (2) | 0.0250 (8) | |
H232 | 0.0827 | 0.4286 | 0.8193 | 0.030* | |
C233 | 0.1733 (2) | 0.3898 (2) | 0.7752 (2) | 0.0278 (9) | |
H233 | 0.1648 | 0.4045 | 0.7243 | 0.033* | |
C234 | 0.2347 (2) | 0.3537 (3) | 0.7937 (3) | 0.0382 (11) | |
H234 | 0.2680 | 0.3442 | 0.7556 | 0.046* | |
C235 | 0.2469 (3) | 0.3318 (4) | 0.8689 (3) | 0.066 (2) | |
H235 | 0.2883 | 0.3070 | 0.8814 | 0.079* | |
C236 | 0.1978 (2) | 0.3466 (3) | 0.9260 (3) | 0.0494 (14) | |
H236 | 0.2067 | 0.3321 | 0.9768 | 0.059* | |
C241 | 0.11373 (18) | 0.36635 (19) | 1.0703 (2) | 0.0166 (7) | |
C242 | 0.15970 (19) | 0.41359 (19) | 1.1095 (2) | 0.0202 (7) | |
H242 | 0.1695 | 0.4592 | 1.0886 | 0.024* | |
C243 | 0.1907 (2) | 0.3929 (2) | 1.1791 (2) | 0.0273 (9) | |
H243 | 0.2210 | 0.4247 | 1.2051 | 0.033* | |
C244 | 0.1766 (2) | 0.3249 (3) | 1.2100 (3) | 0.0349 (10) | |
H244 | 0.1969 | 0.3112 | 1.2571 | 0.042* | |
C245 | 0.1326 (2) | 0.2774 (3) | 1.1710 (3) | 0.0423 (12) | |
H245 | 0.1237 | 0.2314 | 1.1915 | 0.051* | |
C246 | 0.1013 (2) | 0.2980 (2) | 1.1012 (3) | 0.0306 (9) | |
H246 | 0.0719 | 0.2655 | 1.0751 | 0.037* | |
Fe3 | 0.41163 (3) | 0.52266 (3) | 0.98284 (3) | 0.01799 (11) | |
O1 | 0.5000 | 0.5000 | 1.0000 | 0.0503 (14) | |
Br31 | 0.39313 (2) | 0.651012 (19) | 0.98317 (2) | 0.02250 (9) | |
Br32 | 0.3389 (4) | 0.4712 (3) | 1.0794 (6) | 0.0326 (9) | 0.63 (4) |
Br34 | 0.3519 (8) | 0.4744 (5) | 1.0917 (5) | 0.0270 (13) | 0.37 (4) |
Br35 | 0.372 (2) | 0.4754 (9) | 0.8646 (10) | 0.049 (4) | 0.36 (3) |
Br36 | 0.3537 (10) | 0.4780 (9) | 0.8699 (9) | 0.041 (2) | 0.28 (3) |
Br33 | 0.3887 (6) | 0.4873 (7) | 0.8547 (5) | 0.0348 (13) | 0.36 (3) |
Fe4 | 0.06461 (3) | 0.45461 (3) | 0.55308 (3) | 0.02737 (13) | |
O2 | 0.0000 | 0.5000 | 0.5000 | 0.0497 (13) | |
Br41 | 0.13996 (5) | 0.38726 (6) | 0.47044 (8) | 0.0432 (3) | 0.967 (5) |
Br44 | 0.1243 (15) | 0.4060 (16) | 0.4449 (18) | 0.0444 (12) | 0.033 (5) |
Br42 | 0.00698 (4) | 0.37757 (2) | 0.64378 (6) | 0.0300 (2) | 0.979 (3) |
Br45 | −0.0143 (18) | 0.3775 (12) | 0.615 (3) | 0.0313 (12) | 0.021 (3) |
Br43 | 0.13436 (12) | 0.53934 (15) | 0.62243 (9) | 0.0396 (4) | 0.779 (9) |
Br46 | 0.1183 (4) | 0.5613 (4) | 0.6108 (4) | 0.0416 (8) | 0.221 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0118 (3) | 0.0088 (3) | 0.0098 (3) | 0.0007 (2) | −0.0012 (2) | −0.0011 (2) |
P12 | 0.0148 (4) | 0.0097 (4) | 0.0111 (4) | 0.0001 (3) | −0.0027 (3) | −0.0011 (3) |
P11 | 0.0137 (4) | 0.0092 (4) | 0.0112 (4) | 0.0001 (3) | −0.0023 (3) | −0.0007 (3) |
N11 | 0.0145 (14) | 0.0124 (13) | 0.0125 (13) | 0.0024 (11) | −0.0032 (11) | −0.0009 (11) |
C11 | 0.026 (2) | 0.0207 (18) | 0.0216 (19) | 0.0069 (15) | −0.0002 (16) | 0.0015 (15) |
C12 | 0.044 (3) | 0.065 (4) | 0.053 (3) | 0.020 (3) | 0.035 (3) | 0.013 (3) |
N101 | 0.0169 (14) | 0.0085 (13) | 0.0144 (14) | −0.0001 (11) | −0.0056 (11) | −0.0010 (11) |
C101 | 0.0227 (19) | 0.0173 (17) | 0.0202 (18) | −0.0038 (14) | −0.0129 (15) | 0.0026 (14) |
C102 | 0.026 (2) | 0.0174 (18) | 0.026 (2) | 0.0028 (15) | −0.0138 (16) | 0.0016 (15) |
C111 | 0.0184 (17) | 0.0126 (16) | 0.0118 (15) | 0.0040 (13) | −0.0048 (13) | 0.0001 (12) |
C112 | 0.0196 (18) | 0.0138 (16) | 0.0171 (17) | 0.0007 (13) | −0.0044 (14) | 0.0011 (13) |
C113 | 0.030 (2) | 0.0128 (17) | 0.0228 (19) | 0.0011 (15) | −0.0043 (16) | −0.0036 (14) |
C114 | 0.028 (2) | 0.0177 (18) | 0.0227 (19) | 0.0101 (15) | −0.0012 (15) | −0.0036 (15) |
C115 | 0.0183 (18) | 0.0242 (19) | 0.0227 (19) | 0.0060 (15) | 0.0008 (15) | 0.0010 (15) |
C116 | 0.0203 (18) | 0.0140 (16) | 0.0208 (18) | 0.0008 (14) | −0.0046 (14) | 0.0038 (14) |
C121 | 0.0160 (16) | 0.0105 (15) | 0.0155 (16) | 0.0040 (13) | 0.0013 (13) | 0.0004 (12) |
C122 | 0.0204 (18) | 0.0156 (16) | 0.0179 (17) | −0.0004 (14) | −0.0010 (14) | 0.0015 (13) |
C123 | 0.0192 (18) | 0.0192 (18) | 0.029 (2) | −0.0034 (14) | −0.0002 (15) | 0.0016 (15) |
C124 | 0.0209 (19) | 0.027 (2) | 0.033 (2) | −0.0002 (16) | 0.0108 (16) | 0.0057 (17) |
C125 | 0.030 (2) | 0.035 (2) | 0.0167 (18) | 0.0023 (17) | 0.0053 (16) | −0.0005 (16) |
C126 | 0.0228 (19) | 0.0236 (19) | 0.0176 (18) | 0.0011 (15) | −0.0014 (14) | −0.0034 (15) |
C131 | 0.0197 (17) | 0.0147 (16) | 0.0099 (15) | −0.0033 (13) | −0.0038 (13) | −0.0005 (12) |
C132 | 0.0230 (19) | 0.0148 (16) | 0.0184 (17) | −0.0027 (14) | −0.0029 (14) | −0.0053 (14) |
C133 | 0.0210 (19) | 0.029 (2) | 0.0221 (19) | −0.0031 (16) | −0.0003 (15) | −0.0083 (16) |
C134 | 0.025 (2) | 0.032 (2) | 0.0208 (19) | −0.0124 (17) | −0.0012 (15) | −0.0002 (16) |
C135 | 0.028 (2) | 0.0158 (17) | 0.0192 (18) | −0.0083 (15) | −0.0067 (15) | 0.0013 (14) |
C136 | 0.0206 (18) | 0.0165 (17) | 0.0156 (17) | −0.0025 (14) | −0.0069 (14) | −0.0003 (13) |
C141 | 0.0199 (17) | 0.0109 (15) | 0.0126 (16) | −0.0027 (13) | −0.0004 (13) | −0.0023 (12) |
C142 | 0.030 (2) | 0.0159 (17) | 0.0142 (17) | 0.0025 (15) | −0.0061 (14) | −0.0025 (13) |
C143 | 0.028 (2) | 0.0160 (17) | 0.0213 (18) | 0.0070 (15) | −0.0031 (15) | −0.0029 (14) |
C144 | 0.036 (2) | 0.0182 (18) | 0.0154 (17) | 0.0040 (16) | 0.0043 (15) | −0.0043 (14) |
C145 | 0.042 (2) | 0.027 (2) | 0.0139 (18) | 0.0039 (18) | −0.0045 (16) | −0.0051 (15) |
C146 | 0.026 (2) | 0.0206 (18) | 0.0185 (18) | 0.0036 (15) | −0.0072 (15) | −0.0010 (14) |
Fe2 | 0.0113 (3) | 0.0111 (3) | 0.0174 (3) | −0.0002 (3) | −0.0029 (3) | −0.0010 (3) |
P21 | 0.0118 (4) | 0.0123 (4) | 0.0174 (4) | −0.0010 (3) | −0.0029 (3) | −0.0015 (3) |
P22 | 0.0116 (4) | 0.0123 (4) | 0.0185 (4) | 0.0007 (3) | −0.0031 (3) | −0.0007 (3) |
N21 | 0.0137 (14) | 0.0118 (13) | 0.0240 (17) | −0.0003 (11) | −0.0006 (12) | −0.0023 (12) |
C21 | 0.0217 (19) | 0.0144 (17) | 0.025 (2) | −0.0005 (14) | −0.0034 (15) | −0.0017 (15) |
C22 | 0.039 (2) | 0.031 (2) | 0.022 (2) | 0.0006 (18) | −0.0016 (17) | 0.0050 (17) |
N201 | 0.0139 (14) | 0.0106 (13) | 0.0200 (15) | 0.0012 (11) | −0.0033 (11) | −0.0027 (11) |
C20A | 0.015 (5) | 0.011 (5) | 0.025 (7) | −0.009 (4) | −0.002 (5) | 0.001 (5) |
C20B | 0.028 (7) | 0.006 (6) | 0.035 (8) | −0.001 (5) | 0.002 (5) | 0.002 (5) |
C202 | 0.023 (4) | 0.016 (4) | 0.028 (4) | −0.003 (3) | 0.004 (3) | −0.004 (3) |
C203 | 0.078 (8) | 0.030 (5) | 0.032 (5) | 0.001 (5) | −0.005 (5) | −0.015 (4) |
C211 | 0.0146 (16) | 0.0112 (15) | 0.0198 (17) | −0.0007 (13) | −0.0047 (13) | −0.0014 (13) |
C212 | 0.0189 (18) | 0.0148 (17) | 0.0232 (19) | −0.0013 (14) | −0.0006 (14) | −0.0004 (14) |
C213 | 0.0135 (17) | 0.0171 (17) | 0.031 (2) | 0.0003 (14) | −0.0044 (15) | −0.0035 (15) |
C214 | 0.0199 (18) | 0.0203 (18) | 0.026 (2) | 0.0007 (15) | −0.0084 (15) | −0.0047 (15) |
C215 | 0.0208 (18) | 0.0208 (18) | 0.0205 (18) | −0.0001 (14) | −0.0015 (15) | −0.0052 (14) |
C216 | 0.0165 (17) | 0.0162 (17) | 0.0211 (18) | −0.0024 (14) | −0.0002 (14) | −0.0045 (14) |
C221 | 0.0175 (17) | 0.0188 (17) | 0.0188 (18) | −0.0081 (14) | −0.0007 (14) | −0.0050 (14) |
C222 | 0.0194 (19) | 0.0235 (19) | 0.029 (2) | −0.0054 (15) | 0.0005 (15) | −0.0060 (16) |
C223 | 0.027 (2) | 0.043 (3) | 0.033 (2) | −0.0124 (19) | 0.0108 (18) | −0.015 (2) |
C224 | 0.037 (2) | 0.041 (3) | 0.023 (2) | −0.024 (2) | 0.0075 (18) | −0.0044 (18) |
C225 | 0.039 (2) | 0.030 (2) | 0.022 (2) | −0.0135 (18) | −0.0033 (17) | 0.0035 (17) |
C226 | 0.026 (2) | 0.0197 (18) | 0.0234 (19) | −0.0074 (15) | −0.0014 (15) | −0.0023 (15) |
C231 | 0.0144 (17) | 0.0179 (17) | 0.0238 (19) | −0.0014 (14) | 0.0006 (14) | −0.0038 (14) |
C232 | 0.0215 (19) | 0.026 (2) | 0.027 (2) | 0.0091 (16) | −0.0015 (16) | 0.0011 (16) |
C233 | 0.029 (2) | 0.031 (2) | 0.024 (2) | −0.0012 (17) | 0.0033 (16) | 0.0007 (17) |
C234 | 0.021 (2) | 0.064 (3) | 0.030 (2) | 0.003 (2) | 0.0047 (17) | −0.006 (2) |
C235 | 0.031 (3) | 0.130 (6) | 0.037 (3) | 0.042 (3) | 0.005 (2) | 0.001 (3) |
C236 | 0.031 (2) | 0.089 (4) | 0.028 (2) | 0.032 (3) | 0.0018 (19) | 0.007 (2) |
C241 | 0.0118 (16) | 0.0158 (16) | 0.0220 (18) | 0.0018 (13) | −0.0025 (13) | −0.0001 (14) |
C242 | 0.0174 (18) | 0.0153 (17) | 0.028 (2) | 0.0013 (14) | −0.0049 (15) | 0.0013 (14) |
C243 | 0.0205 (19) | 0.031 (2) | 0.030 (2) | 0.0011 (16) | −0.0096 (16) | −0.0037 (17) |
C244 | 0.025 (2) | 0.047 (3) | 0.032 (2) | −0.0043 (19) | −0.0127 (18) | 0.017 (2) |
C245 | 0.032 (2) | 0.038 (3) | 0.057 (3) | −0.013 (2) | −0.017 (2) | 0.029 (2) |
C246 | 0.026 (2) | 0.025 (2) | 0.041 (2) | −0.0060 (17) | −0.0136 (18) | 0.0083 (18) |
Fe3 | 0.0153 (2) | 0.0163 (2) | 0.0224 (3) | 0.00231 (19) | −0.0015 (2) | 0.0013 (2) |
O1 | 0.019 (2) | 0.054 (3) | 0.078 (4) | 0.009 (2) | 0.000 (2) | 0.029 (3) |
Br31 | 0.0340 (2) | 0.01457 (17) | 0.01885 (18) | −0.00344 (15) | −0.00553 (15) | 0.00132 (13) |
Br32 | 0.0329 (15) | 0.0154 (7) | 0.050 (2) | −0.0010 (7) | 0.0179 (13) | 0.0008 (12) |
Br34 | 0.044 (3) | 0.0155 (10) | 0.0213 (19) | −0.0044 (16) | 0.0108 (15) | 0.0011 (8) |
Br35 | 0.090 (13) | 0.027 (3) | 0.032 (3) | 0.008 (6) | −0.009 (5) | −0.013 (2) |
Br36 | 0.061 (5) | 0.029 (2) | 0.033 (3) | 0.013 (2) | −0.031 (4) | −0.016 (2) |
Br33 | 0.048 (2) | 0.024 (2) | 0.0329 (17) | 0.0028 (15) | 0.0029 (13) | −0.0109 (14) |
Fe4 | 0.0275 (3) | 0.0260 (3) | 0.0287 (3) | −0.0009 (2) | −0.0005 (2) | 0.0040 (2) |
O2 | 0.059 (3) | 0.047 (3) | 0.043 (3) | 0.012 (2) | −0.009 (2) | 0.007 (2) |
Br41 | 0.0389 (3) | 0.0323 (3) | 0.0587 (5) | 0.0010 (3) | 0.0184 (3) | −0.0028 (4) |
Br44 | 0.042 (2) | 0.032 (2) | 0.059 (2) | 0.002 (2) | 0.015 (2) | −0.004 (2) |
Br42 | 0.0270 (3) | 0.0263 (2) | 0.0367 (4) | 0.00007 (18) | 0.0064 (3) | 0.00691 (19) |
Br45 | 0.027 (2) | 0.029 (2) | 0.038 (2) | 0.000 (2) | 0.005 (2) | 0.006 (2) |
Br43 | 0.0405 (7) | 0.0445 (8) | 0.0338 (5) | −0.0182 (6) | 0.0000 (4) | −0.0034 (5) |
Br46 | 0.0409 (17) | 0.0459 (18) | 0.0381 (15) | −0.0127 (14) | 0.0097 (12) | −0.0080 (14) |
Fe1—N11i | 1.895 (3) | C21—C22 | 1.451 (5) |
Fe1—N11 | 1.895 (3) | C22—H22A | 0.9600 |
Fe1—P11 | 2.2620 (9) | C22—H22B | 0.9600 |
Fe1—P11i | 2.2620 (9) | C22—H22C | 0.9600 |
Fe1—P12i | 2.2824 (9) | N201—C20A | 1.482 (15) |
Fe1—P12 | 2.2824 (9) | N201—C20B | 1.520 (15) |
P12—N101 | 1.708 (3) | C20A—C202 | 1.526 (13) |
P12—C141 | 1.815 (3) | C20A—H20A | 0.9700 |
P12—C131 | 1.821 (4) | C20A—H20B | 0.9700 |
P11—N101 | 1.703 (3) | C20B—C203 | 1.475 (16) |
P11—C121 | 1.815 (3) | C20B—H20C | 0.9700 |
P11—C111 | 1.823 (3) | C20B—H20D | 0.9700 |
N11—C11 | 1.135 (5) | C202—H20E | 0.9600 |
C11—C12 | 1.459 (6) | C202—H20F | 0.9600 |
C12—H12A | 0.9600 | C202—H20G | 0.9600 |
C12—H12B | 0.9600 | C203—H20H | 0.9600 |
C12—H12C | 0.9600 | C203—H20I | 0.9600 |
N101—C101 | 1.492 (4) | C203—H20J | 0.9600 |
C101—C102 | 1.511 (5) | C211—C212 | 1.405 (5) |
C101—H10A | 0.9700 | C211—C216 | 1.406 (5) |
C101—H10B | 0.9700 | C212—C213 | 1.384 (5) |
C102—H10C | 0.9600 | C212—H212 | 0.9300 |
C102—H10D | 0.9600 | C213—C214 | 1.389 (5) |
C102—H10E | 0.9600 | C213—H213 | 0.9300 |
C111—C112 | 1.402 (5) | C214—C215 | 1.389 (5) |
C111—C116 | 1.405 (5) | C214—H214 | 0.9300 |
C112—C113 | 1.388 (5) | C215—C216 | 1.387 (5) |
C112—H112 | 0.9300 | C215—H215 | 0.9300 |
C113—C114 | 1.384 (5) | C216—H216 | 0.9300 |
C113—H113 | 0.9300 | C221—C226 | 1.395 (5) |
C114—C115 | 1.378 (5) | C221—C222 | 1.400 (5) |
C114—H114 | 0.9300 | C222—C223 | 1.382 (6) |
C115—C116 | 1.387 (5) | C222—H222 | 0.9300 |
C115—H115 | 0.9300 | C223—C224 | 1.389 (7) |
C116—H116 | 0.9300 | C223—H223 | 0.9300 |
C121—C126 | 1.394 (5) | C224—C225 | 1.375 (6) |
C121—C122 | 1.403 (5) | C224—H224 | 0.9300 |
C122—C123 | 1.382 (5) | C225—C226 | 1.395 (5) |
C122—H122 | 0.9300 | C225—H225 | 0.9300 |
C123—C124 | 1.379 (6) | C226—H226 | 0.9300 |
C123—H123 | 0.9300 | C231—C236 | 1.381 (6) |
C124—C125 | 1.373 (6) | C231—C232 | 1.384 (5) |
C124—H124 | 0.9300 | C232—C233 | 1.383 (6) |
C125—C126 | 1.396 (5) | C232—H232 | 0.9300 |
C125—H125 | 0.9300 | C233—C234 | 1.374 (6) |
C126—H126 | 0.9300 | C233—H233 | 0.9300 |
C131—C132 | 1.397 (5) | C234—C235 | 1.375 (7) |
C131—C136 | 1.401 (5) | C234—H234 | 0.9300 |
C132—C133 | 1.387 (5) | C235—C236 | 1.386 (6) |
C132—H132 | 0.9300 | C235—H235 | 0.9300 |
C133—C134 | 1.390 (6) | C236—H236 | 0.9300 |
C133—H133 | 0.9300 | C241—C246 | 1.384 (5) |
C134—C135 | 1.381 (6) | C241—C242 | 1.399 (5) |
C134—H134 | 0.9300 | C242—C243 | 1.387 (5) |
C135—C136 | 1.390 (5) | C242—H242 | 0.9300 |
C135—H135 | 0.9300 | C243—C244 | 1.384 (6) |
C136—H136 | 0.9300 | C243—H243 | 0.9300 |
C141—C142 | 1.388 (5) | C244—C245 | 1.378 (6) |
C141—C146 | 1.401 (5) | C244—H244 | 0.9300 |
C142—C143 | 1.389 (5) | C245—C246 | 1.390 (6) |
C142—H142 | 0.9300 | C245—H245 | 0.9300 |
C143—C144 | 1.379 (5) | C246—H246 | 0.9300 |
C143—H143 | 0.9300 | Fe3—O1 | 1.7469 (6) |
C144—C145 | 1.385 (6) | Fe3—Br35 | 2.334 (10) |
C144—H144 | 0.9300 | Fe3—Br33 | 2.341 (8) |
C145—C146 | 1.380 (5) | Fe3—Br32 | 2.364 (5) |
C145—H145 | 0.9300 | Fe3—Br34 | 2.369 (8) |
C146—H146 | 0.9300 | Fe3—Br36 | 2.375 (8) |
Fe2—N21ii | 1.901 (3) | Fe3—Br31 | 2.3814 (8) |
Fe2—N21 | 1.901 (3) | O1—Fe3iii | 1.7469 (6) |
Fe2—P21 | 2.2715 (9) | Fe4—O2 | 1.7358 (6) |
Fe2—P21ii | 2.2715 (9) | Fe4—Br45 | 2.320 (13) |
Fe2—P22ii | 2.2866 (9) | Fe4—Br43 | 2.3604 (14) |
Fe2—P22 | 2.2866 (9) | Fe4—Br44 | 2.362 (13) |
P21—N201 | 1.699 (3) | Fe4—Br41 | 2.3703 (9) |
P21—C211 | 1.815 (3) | Fe4—Br42 | 2.3782 (8) |
P21—C221 | 1.820 (4) | Fe4—Br46 | 2.417 (5) |
P21—P22 | 2.6463 (14) | O2—Fe4iv | 1.7358 (6) |
P22—N201 | 1.708 (3) | Br41—Br44 | 0.63 (4) |
P22—C241 | 1.820 (4) | Br42—Br45 | 0.64 (5) |
P22—C231 | 1.825 (4) | Br43—Br46 | 0.543 (8) |
N21—C21 | 1.144 (5) | ||
N11i—Fe1—N11 | 180.0 | H22A—C22—H22B | 109.5 |
N11i—Fe1—P11 | 92.21 (8) | C21—C22—H22C | 109.5 |
N11—Fe1—P11 | 87.79 (8) | H22A—C22—H22C | 109.5 |
N11i—Fe1—P11i | 87.79 (8) | H22B—C22—H22C | 109.5 |
N11—Fe1—P11i | 92.21 (8) | C20A—N201—C20B | 20.5 (5) |
P11—Fe1—P11i | 180.000 (1) | C20A—N201—P21 | 131.9 (6) |
N11i—Fe1—P12i | 91.11 (9) | C20B—N201—P21 | 123.8 (6) |
N11—Fe1—P12i | 88.89 (9) | C20A—N201—P22 | 123.6 (5) |
P11—Fe1—P12i | 109.03 (3) | C20B—N201—P22 | 133.9 (6) |
P11i—Fe1—P12i | 70.97 (3) | P21—N201—P22 | 101.92 (15) |
N11i—Fe1—P12 | 88.89 (9) | N201—C20A—C202 | 113.1 (9) |
N11—Fe1—P12 | 91.11 (9) | N201—C20A—H20A | 109.0 |
P11—Fe1—P12 | 70.97 (3) | C202—C20A—H20A | 109.0 |
P11i—Fe1—P12 | 109.03 (3) | N201—C20A—H20B | 109.0 |
P12i—Fe1—P12 | 180.0 | C202—C20A—H20B | 109.0 |
N101—P12—C141 | 110.33 (15) | H20A—C20A—H20B | 107.8 |
N101—P12—C131 | 104.94 (15) | C203—C20B—N201 | 112.8 (9) |
C141—P12—C131 | 101.75 (15) | C203—C20B—H20C | 109.0 |
N101—P12—Fe1 | 92.99 (10) | N201—C20B—H20C | 109.0 |
C141—P12—Fe1 | 120.73 (12) | C203—C20B—H20D | 109.0 |
C131—P12—Fe1 | 124.30 (11) | N201—C20B—H20D | 109.0 |
N101—P12—P11 | 39.26 (9) | H20C—C20B—H20D | 107.8 |
C141—P12—P11 | 122.25 (11) | C20A—C202—H20E | 109.5 |
C131—P12—P11 | 128.99 (12) | C20A—C202—H20F | 109.5 |
Fe1—P12—P11 | 54.15 (2) | H20E—C202—H20F | 109.5 |
N101—P11—C121 | 109.67 (15) | C20A—C202—H20G | 109.5 |
N101—P11—C111 | 108.69 (15) | H20E—C202—H20G | 109.5 |
C121—P11—C111 | 106.58 (15) | H20F—C202—H20G | 109.5 |
N101—P11—Fe1 | 93.84 (10) | C20B—C203—H20H | 109.5 |
C121—P11—Fe1 | 116.88 (11) | C20B—C203—H20I | 109.5 |
C111—P11—Fe1 | 120.01 (11) | H20H—C203—H20I | 109.5 |
C11—N11—Fe1 | 173.9 (3) | C20B—C203—H20J | 109.5 |
N11—C11—C12 | 178.3 (5) | H20H—C203—H20J | 109.5 |
C11—C12—H12A | 109.5 | H20I—C203—H20J | 109.5 |
C11—C12—H12B | 109.5 | C212—C211—C216 | 118.2 (3) |
H12A—C12—H12B | 109.5 | C212—C211—P21 | 122.9 (3) |
C11—C12—H12C | 109.5 | C216—C211—P21 | 118.8 (3) |
H12A—C12—H12C | 109.5 | C213—C212—C211 | 120.7 (3) |
H12B—C12—H12C | 109.5 | C213—C212—H212 | 119.7 |
C101—N101—P11 | 131.0 (2) | C211—C212—H212 | 119.7 |
C101—N101—P12 | 126.3 (2) | C212—C213—C214 | 120.5 (3) |
P11—N101—P12 | 101.34 (14) | C212—C213—H213 | 119.7 |
N101—C101—C102 | 113.7 (3) | C214—C213—H213 | 119.7 |
N101—C101—H10A | 108.8 | C215—C214—C213 | 119.6 (3) |
C102—C101—H10A | 108.8 | C215—C214—H214 | 120.2 |
N101—C101—H10B | 108.8 | C213—C214—H214 | 120.2 |
C102—C101—H10B | 108.8 | C216—C215—C214 | 120.3 (3) |
H10A—C101—H10B | 107.7 | C216—C215—H215 | 119.8 |
C101—C102—H10C | 109.5 | C214—C215—H215 | 119.8 |
C101—C102—H10D | 109.5 | C215—C216—C211 | 120.7 (3) |
H10C—C102—H10D | 109.5 | C215—C216—H216 | 119.7 |
C101—C102—H10E | 109.5 | C211—C216—H216 | 119.7 |
H10C—C102—H10E | 109.5 | C226—C221—C222 | 119.0 (3) |
H10D—C102—H10E | 109.5 | C226—C221—P21 | 121.3 (3) |
C112—C111—C116 | 118.6 (3) | C222—C221—P21 | 119.0 (3) |
C112—C111—P11 | 121.2 (3) | C223—C222—C221 | 120.5 (4) |
C116—C111—P11 | 119.7 (3) | C223—C222—H222 | 119.7 |
C113—C112—C111 | 120.0 (3) | C221—C222—H222 | 119.7 |
C113—C112—H112 | 120.0 | C222—C223—C224 | 120.0 (4) |
C111—C112—H112 | 120.0 | C222—C223—H223 | 120.0 |
C114—C113—C112 | 120.6 (3) | C224—C223—H223 | 120.0 |
C114—C113—H113 | 119.7 | C225—C224—C223 | 120.3 (4) |
C112—C113—H113 | 119.7 | C225—C224—H224 | 119.9 |
C115—C114—C113 | 120.0 (3) | C223—C224—H224 | 119.9 |
C115—C114—H114 | 120.0 | C224—C225—C226 | 120.2 (4) |
C113—C114—H114 | 120.0 | C224—C225—H225 | 119.9 |
C114—C115—C116 | 120.3 (3) | C226—C225—H225 | 119.9 |
C114—C115—H115 | 119.9 | C225—C226—C221 | 120.0 (4) |
C116—C115—H115 | 119.9 | C225—C226—H226 | 120.0 |
C115—C116—C111 | 120.5 (3) | C221—C226—H226 | 120.0 |
C115—C116—H116 | 119.8 | C236—C231—C232 | 118.3 (4) |
C111—C116—H116 | 119.8 | C236—C231—P22 | 120.5 (3) |
C126—C121—C122 | 118.1 (3) | C232—C231—P22 | 121.1 (3) |
C126—C121—P11 | 123.3 (3) | C233—C232—C231 | 121.2 (4) |
C122—C121—P11 | 118.4 (3) | C233—C232—H232 | 119.4 |
C123—C122—C121 | 120.7 (3) | C231—C232—H232 | 119.4 |
C123—C122—H122 | 119.7 | C234—C233—C232 | 119.8 (4) |
C121—C122—H122 | 119.7 | C234—C233—H233 | 120.1 |
C124—C123—C122 | 120.2 (4) | C232—C233—H233 | 120.1 |
C124—C123—H123 | 119.9 | C233—C234—C235 | 119.8 (4) |
C122—C123—H123 | 119.9 | C233—C234—H234 | 120.1 |
C125—C124—C123 | 120.2 (4) | C235—C234—H234 | 120.1 |
C125—C124—H124 | 119.9 | C234—C235—C236 | 120.2 (4) |
C123—C124—H124 | 119.9 | C234—C235—H235 | 119.9 |
C124—C125—C126 | 120.1 (4) | C236—C235—H235 | 119.9 |
C124—C125—H125 | 120.0 | C231—C236—C235 | 120.7 (4) |
C126—C125—H125 | 120.0 | C231—C236—H236 | 119.7 |
C121—C126—C125 | 120.5 (3) | C235—C236—H236 | 119.7 |
C121—C126—H126 | 119.7 | C246—C241—C242 | 118.9 (3) |
C125—C126—H126 | 119.7 | C246—C241—P22 | 123.2 (3) |
C132—C131—C136 | 118.5 (3) | C242—C241—P22 | 117.9 (3) |
C132—C131—P12 | 121.5 (3) | C243—C242—C241 | 120.4 (3) |
C136—C131—P12 | 119.9 (3) | C243—C242—H242 | 119.8 |
C133—C132—C131 | 120.9 (3) | C241—C242—H242 | 119.8 |
C133—C132—H132 | 119.5 | C244—C243—C242 | 119.9 (4) |
C131—C132—H132 | 119.5 | C244—C243—H243 | 120.0 |
C132—C133—C134 | 119.7 (4) | C242—C243—H243 | 120.0 |
C132—C133—H133 | 120.2 | C245—C244—C243 | 120.0 (4) |
C134—C133—H133 | 120.2 | C245—C244—H244 | 120.0 |
C135—C134—C133 | 120.3 (4) | C243—C244—H244 | 120.0 |
C135—C134—H134 | 119.9 | C244—C245—C246 | 120.3 (4) |
C133—C134—H134 | 119.9 | C244—C245—H245 | 119.9 |
C134—C135—C136 | 120.1 (3) | C246—C245—H245 | 119.9 |
C134—C135—H135 | 119.9 | C241—C246—C245 | 120.5 (4) |
C136—C135—H135 | 119.9 | C241—C246—H246 | 119.8 |
C135—C136—C131 | 120.4 (3) | C245—C246—H246 | 119.8 |
C135—C136—H136 | 119.8 | O1—Fe3—Br35 | 111.1 (10) |
C131—C136—H136 | 119.8 | O1—Fe3—Br33 | 105.4 (3) |
C142—C141—C146 | 118.3 (3) | Br35—Fe3—Br33 | 10.2 (8) |
C142—C141—P12 | 119.3 (3) | O1—Fe3—Br32 | 110.3 (2) |
C146—C141—P12 | 122.2 (3) | Br35—Fe3—Br32 | 106.4 (11) |
C141—C142—C143 | 121.3 (3) | Br33—Fe3—Br32 | 116.6 (4) |
C141—C142—H142 | 119.3 | O1—Fe3—Br34 | 103.8 (4) |
C143—C142—H142 | 119.3 | Br35—Fe3—Br34 | 113.7 (11) |
C144—C143—C142 | 119.4 (3) | Br33—Fe3—Br34 | 123.9 (4) |
C144—C143—H143 | 120.3 | Br32—Fe3—Br34 | 8.0 (3) |
C142—C143—H143 | 120.3 | O1—Fe3—Br36 | 119.6 (4) |
C143—C144—C145 | 120.2 (3) | Br35—Fe3—Br36 | 8.8 (11) |
C143—C144—H144 | 119.9 | Br33—Fe3—Br36 | 17.9 (7) |
C145—C144—H144 | 119.9 | Br32—Fe3—Br36 | 99.9 (7) |
C146—C145—C144 | 120.3 (3) | Br34—Fe3—Br36 | 107.5 (7) |
C146—C145—H145 | 119.9 | O1—Fe3—Br31 | 112.06 (3) |
C144—C145—H145 | 119.9 | Br35—Fe3—Br31 | 108.9 (4) |
C145—C146—C141 | 120.4 (3) | Br33—Fe3—Br31 | 104.5 (3) |
C145—C146—H146 | 119.8 | Br32—Fe3—Br31 | 107.90 (15) |
C141—C146—H146 | 119.8 | Br34—Fe3—Br31 | 107.3 (2) |
N21ii—Fe2—N21 | 180.000 (1) | Br36—Fe3—Br31 | 106.0 (4) |
N21ii—Fe2—P21 | 89.12 (9) | Fe3iii—O1—Fe3 | 180.0 |
N21—Fe2—P21 | 90.88 (9) | O2—Fe4—Br45 | 94.6 (12) |
N21ii—Fe2—P21ii | 90.88 (9) | O2—Fe4—Br43 | 109.93 (9) |
N21—Fe2—P21ii | 89.12 (9) | Br45—Fe4—Br43 | 122.0 (12) |
P21—Fe2—P21ii | 180.000 (1) | O2—Fe4—Br44 | 95.9 (11) |
N21ii—Fe2—P22ii | 92.54 (9) | Br45—Fe4—Br44 | 116.3 (10) |
N21—Fe2—P22ii | 87.46 (9) | Br43—Fe4—Br44 | 112.4 (6) |
P21—Fe2—P22ii | 109.02 (4) | O2—Fe4—Br41 | 110.97 (5) |
P21ii—Fe2—P22ii | 70.98 (4) | Br45—Fe4—Br41 | 110.4 (6) |
N21ii—Fe2—P22 | 87.46 (9) | Br43—Fe4—Br41 | 108.14 (7) |
N21—Fe2—P22 | 92.54 (9) | Br44—Fe4—Br41 | 15.3 (10) |
P21—Fe2—P22 | 70.98 (4) | O2—Fe4—Br42 | 107.91 (4) |
P21ii—Fe2—P22 | 109.02 (4) | Br45—Fe4—Br42 | 15.6 (13) |
P22ii—Fe2—P22 | 180.00 (4) | Br43—Fe4—Br42 | 108.42 (6) |
N201—P21—C211 | 105.98 (15) | Br44—Fe4—Br42 | 121.2 (7) |
N201—P21—C221 | 110.09 (16) | Br41—Fe4—Br42 | 111.45 (4) |
C211—P21—C221 | 105.76 (16) | O2—Fe4—Br46 | 97.0 (3) |
N201—P21—Fe2 | 93.56 (10) | Br45—Fe4—Br46 | 125.2 (10) |
C211—P21—Fe2 | 125.78 (11) | Br43—Fe4—Br46 | 12.98 (18) |
C221—P21—Fe2 | 114.05 (11) | Br44—Fe4—Br46 | 115.4 (5) |
N201—P22—C241 | 108.90 (15) | Br41—Fe4—Br46 | 114.63 (15) |
N201—P22—C231 | 106.63 (15) | Br42—Fe4—Br46 | 113.85 (17) |
C241—P22—C231 | 102.63 (16) | Fe4—O2—Fe4iv | 180.0 |
N201—P22—Fe2 | 92.79 (10) | Br44—Br41—Fe4 | 81.6 (12) |
C241—P22—Fe2 | 115.23 (12) | Br41—Br44—Fe4 | 83.1 (14) |
C231—P22—Fe2 | 128.81 (12) | Br45—Br42—Fe4 | 77.0 (12) |
C21—N21—Fe2 | 171.8 (3) | Br42—Br45—Fe4 | 87.4 (16) |
N21—C21—C22 | 179.2 (4) | Br46—Br43—Fe4 | 89.5 (6) |
C21—C22—H22A | 109.5 | Br43—Br46—Fe4 | 77.6 (6) |
C21—C22—H22B | 109.5 | ||
Fe1—P11—C111—C112 | −106.4 (3) | Fe2—P21—C211—C212 | −121.4 (3) |
Fe1—P11—C111—C116 | 64.8 (3) | Fe2—P21—C211—C216 | 54.9 (3) |
Fe1—P11—C121—C122 | 64.6 (3) | Fe2—P21—C221—C222 | 70.7 (3) |
Fe1—P11—C121—C126 | −110.2 (3) | Fe2—P21—C221—C226 | −99.7 (3) |
Fe1—P12—C131—C132 | −74.8 (3) | Fe2—P22—C231—C232 | −38.9 (4) |
Fe1—P12—C131—C136 | 102.1 (3) | Fe2—P22—C231—C236 | 142.3 (4) |
Fe1—P12—C141—C142 | −30.1 (3) | Fe2—P22—C241—C242 | −59.9 (3) |
Fe1—P12—C141—C146 | 154.4 (3) | Fe2—P22—C241—C246 | 117.3 (3) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y+1, −z+2; (iii) −x+1, −y+1, −z+2; (iv) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C22—H22B···Br43 (major site) | 0.96 | 2.75 | 3.653 (5) | 157 |
C142—H142···Cg11v | 0.93 | 2.73 | 3.517 (4) | 143 |
C214—H214···Cg10 | 0.93 | 2.73 | 3.571 (4) | 151 |
Symmetry code: (v) −x+1, −y+1, −z+1. |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | [Fe(C2H3N)2(C26H25NP2)2][FeBr4] | [Fe(C2H3N)2(C26H25NP2)2][Fe2Br6O] |
Mr | 1340.27 | 1571.94 |
Crystal system, space group | Triclinic, P1 | Monoclinic, P21/c |
Temperature (K) | 100 | 100 |
a, b, c (Å) | 11.4596 (10), 21.834 (2), 23.905 (2) | 18.928 (5), 18.352 (4), 17.243 (4) |
α, β, γ (°) | 114.399 (1), 96.285 (1), 90.388 (1) | 90, 90.365 (3), 90 |
V (Å3) | 5405.4 (8) | 5989 (3) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 3.65 | 4.87 |
Crystal size (mm) | 0.40 × 0.20 × 0.08 | 0.55 × 0.24 × 0.22 |
Data collection | ||
Diffractometer | Bruker APEX CCD area-detector diffractometer | Bruker APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2009) | Multi-scan (SADABS; Bruker, 2009) |
Tmin, Tmax | 0.323, 0.771 | 0.175, 0.413 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 59375, 21891, 16724 | 64539, 13071, 10694 |
Rint | 0.038 | 0.038 |
(sin θ/λ)max (Å−1) | 0.625 | 0.641 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.074, 1.00 | 0.039, 0.097, 1.04 |
No. of reflections | 21891 | 13071 |
No. of parameters | 1272 | 758 |
No. of restraints | 0 | 49 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.030P)2] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0393P)2 + 17.460P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.61, −0.41 | 3.18, −1.08 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Berndt, 1999).
D—H···A | D—H | H···A | D···A | D—H···A |
C32—H32B···Br42i | 0.96 | 2.80 | 3.718 (3) | 160.0 |
C315—H315···Br42i | 0.93 | 2.93 | 3.746 (3) | 147.4 |
C276—H276···Br44 | 0.93 | 2.93 | 3.607 (3) | 131.2 |
C202—H20E···Br41ii | 0.96 | 2.83 | 3.741 (3) | 158.6 |
C225—H225···Br51iii | 0.93 | 2.77 | 3.658 (3) | 159.1 |
C262—H262···Br51 | 0.93 | 2.88 | 3.540 (3) | 129.1 |
C326—H326···Br51 | 0.93 | 2.89 | 3.571 (3) | 131.4 |
C12—H12B···Br52 | 0.96 | 2.83 | 3.724 (3) | 154.4 |
C201—H20A···Br53iv | 0.97 | 2.86 | 3.762 (3) | 155.1 |
C24—H24A···Br53 | 0.96 | 2.92 | 3.755 (3) | 146.0 |
C242—H242···Cg14 | 0.93 | 2.78 | 3.553 (3) | 142 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z; (iii) x+1, y, z; (iv) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C22—H22B···Br43 (major site) | 0.96 | 2.75 | 3.653 (5) | 156.6 |
C142—H142···Cg11i | 0.93 | 2.73 | 3.517 (4) | 143 |
C214—H214···Cg10 | 0.93 | 2.73 | 3.571 (4) | 151 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Bond/angle | (I) n=1 | (I) n=2 | (I) n=3 | (II) n=1 | (II) n=2 |
Fen-Nn1 | 1.906 (2) | 1.906 (2) | 1.908 (2) | 1.895 (3) | 1.901 (3) |
Fen-Pn1 | 2.2499 (7) | 2.2547 (8) | 2.2877 (7) | 2.2620 (9) | 2.2715 (9) |
Fen-Pn2 | 2.2870 (7) | 2.2842 (8) | 2.2588 (7) | 2.2824 (9) | 2.2866 (9) |
Pn1-Nn01 | 1.701 (2) | 1.696 (2) | 1.707 (2) | 1.703 (3) | 1.699 (3) |
Pn1-Fen-Pn2 | 70.82 (3) | 70.85 (3) | 70.96 (3) | 70.97 (3) | 70.98 (4) |
P21-Fe2-P23 | 108.97 (3) | ||||
P21-Fe2-P24 | 179.79 (4) | ||||
P22-Fe2-P23 | 177.23 (3) | ||||
P22-Fe2-P24 | 109.36 (3) | ||||
Fen-Pn1-Cn11-Cn12 | -116.7 (2) | -109.0 (2) | -130.0 (2) | -106.4 (3) | -121.4 (3) |
Fen-Pn1-Cn21-Cn22 | 64.9 (2) | 67.9 (2) | 58.2 (2) | 64.6 (3) | 70.7 (3) |
Fen-Pn2-Cn31-Cn32 | -54.0 (2) | 71.8 (2) | -53.1 (2) | -74.8 (3) | -38.9 (4) |
Fen-Pn2-Cn41-Cn42 | -55.8 (2) | 28.5 (3) | -65.9 (2) | -30.1 (3) | -59.9 (3) |
Symmetry code: (i) -x, -y, 1 - z. |
Bond/angle | (I) n=4 | (I) n=5 | (II) n=3 | (II) n=4 |
Fen-Brn1 | 2.4583 (5) | 2.4716 (5) | 2.3814 (8) | 2.3703 (9) |
Fen-Brn2 | 2.4701 (5) | 2.4614 (5) | 2.364 (5) | 2.3782 (8) |
Fen-Brn3 | 2.4948 (5) | 2.4485 (5) | 2.341 (8) | 2.3604 (14) |
Fen-Brn4 | 2.4348 (5) | 2.4805 (5) | ||
Fen-O1/O2 | 1.7469 (6) | 1.7358 (6) |
* Only the Fe—Br bonds involving the highest-occupancy disordered atoms Br are given (see text). |
P-P | Fe-P (Å) | P-Fe-P (°) | Fe-N (Å) | Reference |
Me2P(CH2)2PMe2 | 2.267 (4) | 84.8 (2) | 1.905 (7) | (a) |
Me2P(CH2)2PMe2 | 2.259 (2) | 85.17 (6) | 1.917 (5) | (b) |
Et2P(CH2)2PEt2 | 2.2784 (11) | 84.88 (3) | 1.896 (2) | (c) |
Ph2P(CH2)2PPh2 | 2.33 (6) | 83.20 (4) | 1.913 (95) | (d) |
Ph2P(CH=CH)PPh2 | 2.321 (3) | 82.57 (9) | 1.916 (10) | (e) |
{MeO(CH2)3}2P(CH2)2P{(CH2)3OMe}2 | 2.2926 (6) | 84.26 (2) | 1.9188 (19) | (f) |
{HO(CH2)3}2P(CH2)2P{(CH2)3OH}2 | 2.2967 (4) | 84.187 (16) | 1.9077 (14) | (g) |
Ph2P(C6H4)PPh2 | 2.340 (1) | 81.1 (1) | 1.894 (4) | (h) |
Ph2P(CH2)PPh2 | 2.275 (6) | 73.1 (2) | 1.889 (11) | (i) |
Ph2PN(Et)PPh2 | 2.2715 (8) | 70.86 (3) | 1.906 (2) | (j) |
Ph2PN(Et)PPh2 | 2.2757 (9) | 70.98 (4) | 1.898 (3) | (k) |
* Since all the P—P ligands are symmetrical, only average Fe—P bond distances are reported in all cases. References: (a) Barron et al. (1987); (b) George et al. (1997); (c) Martins et al. (1998); (d) Blake et al. (1992); (e) Williams (1988); (f) Gilbertson et al. (2007); (g) Gohdes et al. (2009); (h) Barclay et al. (1988); (i) Bechlars et al. (2008); (j) this work, (I); (k) this work, (II). |
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The bis(diphenylphosphanyl)amine ligands (PNP), used together with Cr(acac)3 as the metal source, have been extensively studied and used successfully for selective olefin oligomerization, with high activities and selectivities reported for the trimerization and tetramerization of ethylene (Bollmann et al., 2004; Blann et al., 2005; Overett et al., 2005). As part of our general interest (Maithufi, 2010) in bidentate phosphine ligands containing the PNP bridging unit, we additionally obtained crystals of the two title iron complexes, (I) and (II), which are reported here.
Upon solving the crystal structures for the two sets of crystals, it was found that the cations in both compounds correspond to [Fe(MeCN)2(Ph2PN(Et)PPh2)2]2+, while the anions are different, with [FeBr4]2- in the orange crystals of (I) and [Br3FeOFeBr3]2- in the red crystals of (II). The molecular structures of representative cations and the anions, with the associated numbering schemes, are shown in Figs. 1–5, and selected geometric parameters are presented in Tables 3 and 4 for the cations and anions, respectively.
The chemical formula for (I) was determined to be [Fe(MeCN)2(Ph2PN(Et)PPh2)2].[FeBr4] in crystals containing three independent cations, with cations 1 and 3 situated on inversion centres while cation 2 occupies a general position. Both anions, required to balance the charge, are located on general positions. Except for the two coordinated MeCN molecules in each of the cations, no additional solvent molecules were detected in the structure. The cations in (I) are distorted octahedral molecules, with two Ph2PN(Et)PPh2 ligands, coordinated in a bidentate fashion to the FeII metal centre, occupying the equatorial plane, and two MeCN molecules in the apical positions (Figs. 1 and 2). Since the Ph2PN(Et)PPh2 ligands form a four-membered chelate upon coordination, the P—Fe—P angles deviate significantly from the ideal 90°, with values ranging from 70.82 (3) to 70.96 (3)° observed in the three crystallographically independent molecules (Table 3). In all cases, one of the Fe—P bond distances is significantly longer than the other, at ca 2.28 versus ca 2.25 Å, with individual values ranging from 2.2499 (7) to 2.2877 (7) Å. The Fe—N bonds to the acetonitrile are identical with an average of 1.906 (2) Å, while the C—N—Fe angles deviate significantly from 180°, ranging from 171.2 (2) to 176.1 (2)°.
The anions in (I) consist of FeII cations surrounded by four bromide anions in a distorted tetrahedral arrangement (Fig. 3). The Fe—Br bond distances vary to a larger degree than the bond distances of equivalent sets found in the cations, corresponding to their greater degree of freedom. Nevertheless, all distances are still within normal limits for bonds of this nature, ranging from 2.4348 (5) to 2.4948 (5) Å (Mikhailine et al., 2008; Pohl et al., 1995) (Table 4).
The chemical formula for the red crystals, (II), was determined as [Fe(MeCN)2(Ph2PN(Et)PPh2)2].[Br3FeOFeBr3]. There are two independent cations present in the structure, with each molecule being accompanied by a [Br3FeOFeBr3]2- anion. All molecules are situated on special positions. The anions result, presumably, from partial air oxidation of the FeII used in the synthesis to the FeIII oxidation state associated with this anion. The ethyl substituent in cation 2 is disordered over two positions, with initial refined occupancies of 0.505 (14) and 0.495 (14), respectively. Since these values do not differ significantly they were subsequently fixed at 0.50 for the final refinement. In addition, the Br atoms in the anions are also disordered over multiple positions (see Experimental); these were refined with the occupancies as variables summing to unity for each Br atom. The large maximum and minimum final difference Fourier electron densities are situated close to two such disordered atom, Br46 and Br43, respectively.
The geometry of the cations in (II) is very similar to that in (I), as shown by the Fe—P bond distances, the average Fe—N bond distance and the average P—Fe—P bite angles (Table 3). Since the cation compositions in the two structures are chemically equivalent, geometric differences are expected to be due to packing effects in the respective crystal latices (Tables 1 and 2). There are significant differences in the orientation of the phenyl rings of the various cations in both structures, as shown by the relevant torsion angles (Table 3). The [Br3FeOFeBr3]2- anion in (II) consists of a linear Fe—O—Fe core, with each FeIII cation surrounded by three Br- anions to complete a distorted tetrahedral arrangement around Fe. The average Fe—O bond distance of 1.7414 (6) Å indicates the single-order nature of this bond (Table 4). Both the final Fe—Br and Fe—O bond distances are within the typical range for these anions (Evans et al., 1992; Merkel et al., 2005; Busi et al., 2006).
From the data presented in Table 5 for representative [Fe(MeCN)2(P—P)2]2+ cations, only one other structure was found where the bidentate bisphosphine ligand (Ph2PCH2PPh2) forms a four-membered chelate (Gilbertson et al., 2007). The values obtained for the P—Fe—P bite angle of the Ph2PN(Et)PPh2 ligand, reported in this study, represent the smallest bite angles reported to date for bidentate phosphine ligands in complexes of this nature. The average Fe—P bond distances listed in Table 5 range from 2.259 (2) to 2.340 (1) Å and the values obtained during the current study fall well within this range, irrespective of the P—Fe—P angle deviating significantly from the ideal 90° required for optimal orbital overlap. The Fe—N bond distances have a narrow range of 1.889 (11)–1.9188 (19) Å.
Weak intermolecular C—H···.Br interactions are present in the two structures (Tables 1 and 2), particularly in (I). In addition, some significant C—H···π interactions of less than 3Å are also observed; these were evaluated using PLATON (Spek, 2009). In Table 1, the phenyl group centroid Cg14 is that for atoms C281–C286, and in Table 2 Cg11 is for C111–C116 and Cg10 for C131–C136.
The [FeBr4]2- anion is significantly less common than the FeIII version, [FeBr4]-. A general search of the Cambridge Structural Database (CSD, Version 5.31, August 2010 update; Allen, 2002) for the FeBr4 fragment (no charge specified) yielded 93 hits, with only five corresponding to FeII. In addition, this report represents only the fourth crystallographic description of the [Br3FeOFeBr3]2- anion found in the open literature. In the FeIII anion, the bond distances are significantly shorter, at 2.24–2.34 Å, and may be used as a basis for distinguishing between the FeII and FeIII oxidation states in these molecules (Ondrejkovičová & Vrábel,2002). Here, the average Fe—Br bond distance of 2.364 (14) Å in the [Br3FeOFeBr3]2- anion is significantly shorter than the average of 2.4650 (6) Å determined for the Fe—Br bonds for FeII in [FeBr4]2-, but slightly longer than those found for FeIII in [FeBr4]-.