The title compound, [Gd(C4H9NO)4(H2O)3][Fe(CN)6]·2H2O, is a bimetallic complex containing two isolated metal complexes. The Fe atom is bonded to six cyano ligands forming an almost ideal octahedron. One of the cyano groups is also connected through a hydrogen bond to a water molecule bonded to the Ga atom. Aside from three water molecules, gadolinium is also coordinated by four dimethylacetamide molecules, two of which show various degrees of structural disorder. The asymmetric unit also includes two solvent water molecules, which take part in hydrogen bonding, forming an extended network.
Supporting information
CCDC reference: 608347
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.003 Å
- Disorder in main residue
- R factor = 0.028
- wR factor = 0.070
- Data-to-parameter ratio = 35.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 5
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.89 Ratio
PLAT301_ALERT_3_B Main Residue Disorder ......................... 27.00 Perc.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.36
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.17 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Gd1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N30
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N40
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C30
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C40
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N40A
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C30A
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C40A
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C32
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
12 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
11 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEX2 (Bruker–Nonius, 2004); cell refinement: SAINT-Plus; data reduction: SAINT-Plus (Bruker–Nonius, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XSHELL (Bruker, 2000); software used to prepare material for publication: enCIFer (Version 1.1; Allen et al., 2004) and WinGX (Farrugia,
1999)'.
Triaquatetrakis(dimethylacetamide-
κO)gadolinium(III)
hexacyanoferrate(III) dihydrate
top
Crystal data top
[Gd(C4H9NO)4(H2O)3][Fe(CN)6]·2H2O | F(000) = 3280 |
Mr = 807.77 | Dx = 1.556 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 8587 reflections |
a = 16.0883 (3) Å | θ = 4.6–68.7° |
b = 19.2620 (4) Å | µ = 2.39 mm−1 |
c = 22.2566 (4) Å | T = 100 K |
V = 6897.2 (2) Å3 | Block, yellow |
Z = 8 | 0.25 × 0.15 × 0.10 mm |
Data collection top
Bruker X8 APEX-II diffractometer | 14850 independent reflections |
Radiation source: fine-focus sealed tube | 11939 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 83.33 pixels mm-1 | θmax = 35.4°, θmin = 1.9° |
φ and ω scans | h = −25→25 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −30→30 |
Tmin = 0.61, Tmax = 0.79 | l = −34→36 |
147578 measured reflections | |
Refinement top
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.070 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.28 | w = 1/[σ2(Fo2) + (0.0232P)2 + 1.8917P] where P = (Fo2 + 2Fc2)/3 |
14850 reflections | (Δ/σ)max = 0.003 |
423 parameters | Δρmax = 2.21 e Å−3 |
15 restraints | Δρmin = −0.93 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe2 | 0.208971 (13) | 0.311700 (11) | 0.401257 (9) | 0.01688 (4) | |
C1 | 0.12596 (10) | 0.26303 (9) | 0.35316 (8) | 0.0235 (3) | |
C2 | 0.12083 (10) | 0.36744 (9) | 0.43716 (7) | 0.0236 (3) | |
C3 | 0.20538 (10) | 0.24575 (9) | 0.46772 (8) | 0.0244 (3) | |
C4 | 0.28539 (10) | 0.36600 (8) | 0.44935 (7) | 0.0219 (3) | |
C5 | 0.21815 (11) | 0.37751 (8) | 0.33595 (7) | 0.0229 (3) | |
C6 | 0.30006 (10) | 0.26089 (8) | 0.36218 (7) | 0.0215 (3) | |
N1 | 0.07604 (10) | 0.23791 (9) | 0.32300 (7) | 0.0329 (3) | |
N2 | 0.07020 (11) | 0.40236 (9) | 0.45783 (8) | 0.0349 (3) | |
N3 | 0.20622 (11) | 0.20830 (9) | 0.50825 (8) | 0.0353 (4) | |
N4 | 0.32747 (10) | 0.39966 (9) | 0.47924 (7) | 0.0321 (3) | |
N5 | 0.22562 (12) | 0.41493 (8) | 0.29594 (7) | 0.0348 (4) | |
N6 | 0.35374 (10) | 0.23447 (8) | 0.33652 (7) | 0.0302 (3) | |
Gd1 | 0.372106 (5) | 0.074475 (4) | 0.174648 (3) | 0.01797 (2) | |
O1 | 0.35170 (9) | 0.01903 (7) | 0.07888 (5) | 0.0290 (3) | |
H1A | 0.3489 (13) | 0.0474 (9) | 0.0429 (6) | 0.035* | |
H1B | 0.3141 (11) | −0.0199 (7) | 0.0740 (8) | 0.035* | |
O2 | 0.28536 (11) | −0.02567 (7) | 0.18610 (6) | 0.0370 (3) | |
H2A | 0.2773 (15) | −0.0493 (9) | 0.2241 (4) | 0.044* | |
H2B | 0.2709 (16) | −0.0572 (8) | 0.1538 (6) | 0.044* | |
O3 | 0.44073 (8) | 0.16670 (7) | 0.22916 (6) | 0.0322 (3) | |
H3A | 0.4234 (12) | 0.1885 (9) | 0.2663 (5) | 0.039* | |
H3B | 0.4863 (10) | 0.1928 (9) | 0.2120 (8) | 0.039* | |
O10 | 0.47628 (9) | 0.00122 (8) | 0.19967 (7) | 0.0374 (3) | |
N10 | 0.53399 (10) | −0.07714 (9) | 0.25999 (8) | 0.0348 (4) | |
C10 | 0.51860 (11) | −0.05295 (10) | 0.20616 (8) | 0.0274 (3) | |
C11 | 0.55375 (17) | −0.08887 (13) | 0.15250 (10) | 0.0474 (5) | |
H11A | 0.5269 | −0.0719 | 0.1169 | 0.071* | |
H11B | 0.5446 | −0.1380 | 0.1560 | 0.071* | |
H11C | 0.6123 | −0.0799 | 0.1501 | 0.071* | |
C12 | 0.4989 (2) | −0.04156 (19) | 0.31243 (11) | 0.0652 (8) | |
H12A | 0.4827 | 0.0046 | 0.3013 | 0.098* | |
H12B | 0.5400 | −0.0394 | 0.3437 | 0.098* | |
H12C | 0.4513 | −0.0667 | 0.3266 | 0.098* | |
C13 | 0.58444 (15) | −0.13872 (12) | 0.27198 (12) | 0.0493 (6) | |
H13A | 0.5491 | −0.1761 | 0.2848 | 0.074* | |
H13B | 0.6240 | −0.1285 | 0.3030 | 0.074* | |
H13C | 0.6133 | −0.1520 | 0.2360 | 0.074* | |
O20 | 0.45277 (9) | 0.13228 (7) | 0.10736 (5) | 0.0323 (3) | |
C20 | 0.47564 (12) | 0.15377 (12) | 0.05680 (9) | 0.0262 (5) | 0.863 (5) |
N20 | 0.45662 (12) | 0.21685 (10) | 0.03935 (8) | 0.0310 (5) | 0.863 (5) |
N20A | 0.4925 (7) | 0.1772 (6) | 0.0212 (5) | 0.025 (3)* | 0.137 (5) |
C20A | 0.4492 (8) | 0.1856 (7) | 0.0696 (6) | 0.021 (3)* | 0.137 (5) |
C21 | 0.52479 (13) | 0.10784 (13) | 0.01430 (10) | 0.0417 (6) | 0.863 (5) |
H21A | 0.5337 | 0.0633 | 0.0326 | 0.063* | 0.863 (5) |
H21B | 0.5774 | 0.1291 | 0.0058 | 0.063* | 0.863 (5) |
H21C | 0.4943 | 0.1020 | −0.0224 | 0.063* | 0.863 (5) |
C23A | 0.52479 (13) | 0.10784 (13) | 0.01430 (10) | 0.042* | 0.137 (5) |
H23D | 0.5097 | 0.0805 | 0.0487 | 0.063* | 0.137 (5) |
H23E | 0.5842 | 0.1097 | 0.0110 | 0.063* | 0.137 (5) |
H23F | 0.5019 | 0.0872 | −0.0213 | 0.063* | 0.137 (5) |
C22 | 0.47850 (19) | 0.24163 (15) | −0.02123 (10) | 0.0584 (9) | 0.863 (5) |
H22A | 0.5379 | 0.2419 | −0.0256 | 0.088* | 0.863 (5) |
H22B | 0.4574 | 0.2878 | −0.0268 | 0.088* | 0.863 (5) |
H22C | 0.4545 | 0.2113 | −0.0508 | 0.088* | 0.863 (5) |
C22A | 0.47850 (19) | 0.24163 (15) | −0.02123 (10) | 0.058* | 0.137 (5) |
H22D | 0.4221 | 0.2574 | −0.0175 | 0.088* | 0.137 (5) |
H22E | 0.4891 | 0.2284 | −0.0621 | 0.088* | 0.137 (5) |
H22F | 0.5157 | 0.2783 | −0.0099 | 0.088* | 0.137 (5) |
C23 | 0.40672 (15) | 0.26048 (12) | 0.07840 (11) | 0.0439 (6) | 0.863 (5) |
H23A | 0.3508 | 0.2625 | 0.0634 | 0.066* | 0.863 (5) |
H23B | 0.4299 | 0.3064 | 0.0794 | 0.066* | 0.863 (5) |
H23C | 0.4065 | 0.2414 | 0.1182 | 0.066* | 0.863 (5) |
C21A | 0.40672 (15) | 0.26048 (12) | 0.07840 (11) | 0.044* | 0.137 (5) |
H21D | 0.4488 | 0.2943 | 0.0873 | 0.066* | 0.137 (5) |
H21E | 0.3678 | 0.2584 | 0.1110 | 0.066* | 0.137 (5) |
H21F | 0.3782 | 0.2734 | 0.0422 | 0.066* | 0.137 (5) |
O30 | 0.32424 (9) | 0.07773 (7) | 0.27171 (6) | 0.0314 (3) | |
N30 | 0.27527 (19) | 0.07357 (15) | 0.36485 (14) | 0.0386 (8)* | 0.616 (5) |
C30 | 0.2612 (2) | 0.07658 (15) | 0.30634 (15) | 0.0267 (6)* | 0.616 (5) |
N30A | 0.2143 (4) | 0.0776 (3) | 0.3300 (2) | 0.0465 (15)* | 0.384 (5) |
C30A | 0.2922 (3) | 0.0737 (2) | 0.3227 (2) | 0.0242 (10)* | 0.384 (5) |
C31 | 0.17085 (19) | 0.08003 (14) | 0.28123 (14) | 0.0574 (11)* | 0.616 (5) |
H31A | 0.1345 | 0.0537 | 0.3068 | 0.086* | 0.616 (5) |
H31B | 0.1697 | 0.0610 | 0.2414 | 0.086* | 0.616 (5) |
H31C | 0.1527 | 0.1275 | 0.2801 | 0.086* | 0.616 (5) |
C33A | 0.17085 (19) | 0.08003 (14) | 0.28123 (14) | 0.057* | 0.384 (5) |
H33D | 0.1785 | 0.1243 | 0.2622 | 0.086* | 0.384 (5) |
H33E | 0.1131 | 0.0738 | 0.2908 | 0.086* | 0.384 (5) |
H33F | 0.1886 | 0.0438 | 0.2545 | 0.086* | 0.384 (5) |
C32 | 0.2112 (4) | 0.0669 (3) | 0.4096 (3) | 0.0688 (15)* | 0.616 (5) |
H32A | 0.1577 | 0.0691 | 0.3906 | 0.103* | 0.616 (5) |
H32B | 0.2161 | 0.1039 | 0.4382 | 0.103* | 0.616 (5) |
H32C | 0.2170 | 0.0231 | 0.4298 | 0.103* | 0.616 (5) |
C32A | 0.1756 (6) | 0.0756 (5) | 0.3922 (4) | 0.069* | 0.384 (5) |
H32D | 0.1657 | 0.0283 | 0.4036 | 0.103* | 0.384 (5) |
H32E | 0.1238 | 0.1005 | 0.3917 | 0.103* | 0.384 (5) |
H32F | 0.2127 | 0.0969 | 0.4205 | 0.103* | 0.384 (5) |
C33 | 0.3549 (2) | 0.07107 (17) | 0.38548 (17) | 0.0696 (14)* | 0.616 (5) |
H33A | 0.3688 | 0.0241 | 0.3957 | 0.104* | 0.616 (5) |
H33B | 0.3599 | 0.0999 | 0.4205 | 0.104* | 0.616 (5) |
H33C | 0.3920 | 0.0875 | 0.3548 | 0.104* | 0.616 (5) |
C31A | 0.3549 (2) | 0.07107 (17) | 0.38548 (17) | 0.070* | 0.384 (5) |
H31D | 0.4118 | 0.0776 | 0.3738 | 0.104* | 0.384 (5) |
H31E | 0.3489 | 0.0269 | 0.4049 | 0.104* | 0.384 (5) |
H31F | 0.3388 | 0.1073 | 0.4127 | 0.104* | 0.384 (5) |
O40 | 0.26367 (9) | 0.14411 (7) | 0.15078 (7) | 0.0357 (3) | |
N40 | 0.17207 (13) | 0.22774 (11) | 0.16812 (8) | 0.0318 (5) | 0.847 (5) |
C40 | 0.19217 (14) | 0.16846 (12) | 0.14340 (10) | 0.0298 (5) | 0.847 (5) |
N40A | 0.1368 (6) | 0.1888 (6) | 0.1485 (5) | 0.029 (3)* | 0.153 (5) |
C40A | 0.2139 (7) | 0.1955 (6) | 0.1652 (5) | 0.019 (2)* | 0.153 (5) |
C41 | 0.1284 (2) | 0.12905 (17) | 0.10645 (16) | 0.0741 (12) | 0.847 (5) |
H41A | 0.1512 | 0.0852 | 0.0943 | 0.111* | 0.847 (5) |
H41B | 0.1141 | 0.1557 | 0.0715 | 0.111* | 0.847 (5) |
H41C | 0.0794 | 0.1213 | 0.1302 | 0.111* | 0.847 (5) |
C43A | 0.1284 (2) | 0.12905 (17) | 0.10645 (16) | 0.074* | 0.153 (5) |
H43D | 0.1281 | 0.1457 | 0.0658 | 0.111* | 0.153 (5) |
H43E | 0.0773 | 0.1050 | 0.1145 | 0.111* | 0.153 (5) |
H43F | 0.1743 | 0.0979 | 0.1119 | 0.111* | 0.153 (5) |
C42 | 0.08994 (19) | 0.26042 (18) | 0.16108 (13) | 0.0659 (11) | 0.847 (5) |
H42A | 0.0935 | 0.2973 | 0.1321 | 0.099* | 0.847 (5) |
H42B | 0.0721 | 0.2789 | 0.1990 | 0.099* | 0.847 (5) |
H42C | 0.0506 | 0.2264 | 0.1475 | 0.099* | 0.847 (5) |
C42A | 0.08994 (19) | 0.26042 (18) | 0.16108 (13) | 0.066* | 0.153 (5) |
H42D | 0.1176 | 0.2848 | 0.1930 | 0.099* | 0.153 (5) |
H42E | 0.0335 | 0.2512 | 0.1725 | 0.099* | 0.153 (5) |
H42F | 0.0906 | 0.2884 | 0.1254 | 0.099* | 0.153 (5) |
C43 | 0.23525 (17) | 0.26515 (13) | 0.20157 (11) | 0.0506 (7) | 0.847 (5) |
H43A | 0.2852 | 0.2379 | 0.2031 | 0.076* | 0.847 (5) |
H43B | 0.2158 | 0.2737 | 0.2417 | 0.076* | 0.847 (5) |
H43C | 0.2466 | 0.3086 | 0.1820 | 0.076* | 0.847 (5) |
C41A | 0.23525 (17) | 0.26515 (13) | 0.20157 (11) | 0.051* | 0.153 (5) |
H41D | 0.2371 | 0.3037 | 0.1742 | 0.076* | 0.153 (5) |
H41E | 0.2883 | 0.2602 | 0.2209 | 0.076* | 0.153 (5) |
H41F | 0.1932 | 0.2733 | 0.2314 | 0.076* | 0.153 (5) |
O98 | −0.09462 (10) | 0.46485 (9) | 0.46164 (8) | 0.0449 (4) | |
H98A | −0.0993 (13) | 0.5038 (9) | 0.4889 (10) | 0.054* | |
H98B | −0.0376 (5) | 0.4489 (12) | 0.4607 (11) | 0.054* | |
O99 | 0.24239 (9) | −0.09196 (7) | 0.07917 (6) | 0.0330 (3) | |
H99A | 0.2613 (11) | −0.1328 (7) | 0.0579 (8) | 0.040* | |
H99B | 0.1902 (8) | −0.0764 (9) | 0.0623 (9) | 0.040* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe2 | 0.01826 (9) | 0.01633 (9) | 0.01604 (9) | −0.00011 (7) | −0.00166 (7) | 0.00056 (7) |
C1 | 0.0230 (7) | 0.0251 (8) | 0.0226 (7) | −0.0014 (6) | −0.0006 (6) | −0.0001 (6) |
C2 | 0.0253 (7) | 0.0255 (7) | 0.0201 (7) | 0.0002 (6) | −0.0013 (6) | 0.0021 (6) |
C3 | 0.0241 (7) | 0.0235 (7) | 0.0257 (7) | −0.0019 (6) | −0.0020 (6) | 0.0023 (6) |
C4 | 0.0224 (7) | 0.0236 (7) | 0.0196 (6) | 0.0014 (6) | 0.0003 (5) | −0.0007 (5) |
C5 | 0.0287 (8) | 0.0195 (7) | 0.0206 (7) | 0.0030 (6) | −0.0009 (6) | −0.0017 (5) |
C6 | 0.0240 (7) | 0.0186 (7) | 0.0220 (7) | −0.0011 (5) | −0.0039 (6) | −0.0003 (5) |
N1 | 0.0290 (7) | 0.0361 (9) | 0.0336 (8) | −0.0074 (6) | −0.0052 (6) | −0.0030 (6) |
N2 | 0.0337 (8) | 0.0373 (9) | 0.0338 (8) | 0.0086 (7) | 0.0032 (7) | −0.0014 (7) |
N3 | 0.0382 (8) | 0.0340 (8) | 0.0336 (8) | −0.0052 (7) | −0.0061 (7) | 0.0118 (7) |
N4 | 0.0328 (8) | 0.0340 (8) | 0.0296 (7) | −0.0025 (6) | −0.0056 (6) | −0.0068 (6) |
N5 | 0.0520 (10) | 0.0267 (8) | 0.0257 (7) | 0.0060 (7) | 0.0006 (7) | 0.0049 (6) |
N6 | 0.0297 (7) | 0.0271 (8) | 0.0337 (8) | 0.0027 (6) | 0.0021 (6) | −0.0025 (6) |
Gd1 | 0.02136 (4) | 0.01686 (4) | 0.01568 (4) | 0.00018 (2) | 0.00109 (2) | 0.00168 (2) |
O1 | 0.0434 (7) | 0.0260 (6) | 0.0175 (5) | −0.0077 (5) | −0.0020 (5) | 0.0018 (4) |
O2 | 0.0633 (10) | 0.0293 (7) | 0.0185 (5) | −0.0208 (7) | 0.0000 (6) | 0.0019 (5) |
O3 | 0.0354 (7) | 0.0337 (7) | 0.0277 (6) | −0.0146 (5) | 0.0090 (5) | −0.0078 (5) |
O10 | 0.0375 (7) | 0.0386 (8) | 0.0362 (7) | 0.0164 (6) | −0.0024 (6) | 0.0065 (6) |
N10 | 0.0316 (8) | 0.0407 (9) | 0.0320 (8) | 0.0063 (7) | 0.0033 (7) | 0.0097 (7) |
C10 | 0.0233 (7) | 0.0292 (8) | 0.0298 (8) | 0.0006 (6) | −0.0009 (6) | 0.0006 (7) |
C11 | 0.0603 (15) | 0.0503 (13) | 0.0315 (10) | 0.0112 (11) | 0.0041 (10) | −0.0097 (9) |
C12 | 0.0737 (19) | 0.096 (2) | 0.0261 (10) | 0.0233 (18) | 0.0084 (12) | 0.0005 (13) |
C13 | 0.0471 (12) | 0.0414 (12) | 0.0593 (15) | 0.0113 (10) | −0.0009 (11) | 0.0238 (11) |
O20 | 0.0405 (7) | 0.0345 (7) | 0.0219 (6) | −0.0124 (6) | 0.0036 (5) | 0.0045 (5) |
C20 | 0.0240 (9) | 0.0342 (11) | 0.0205 (9) | −0.0105 (8) | −0.0012 (7) | 0.0014 (7) |
N20 | 0.0338 (9) | 0.0360 (10) | 0.0232 (8) | −0.0096 (8) | −0.0047 (7) | 0.0069 (7) |
C21 | 0.0313 (11) | 0.0531 (15) | 0.0406 (13) | −0.0029 (10) | 0.0037 (10) | −0.0131 (11) |
C22 | 0.079 (2) | 0.0699 (19) | 0.0259 (11) | −0.0341 (17) | −0.0137 (13) | 0.0263 (12) |
C23 | 0.0439 (14) | 0.0381 (13) | 0.0497 (15) | 0.0012 (10) | −0.0004 (12) | −0.0015 (11) |
O30 | 0.0386 (7) | 0.0324 (7) | 0.0231 (6) | −0.0088 (5) | 0.0106 (5) | −0.0039 (5) |
O40 | 0.0360 (7) | 0.0323 (7) | 0.0387 (7) | 0.0121 (6) | −0.0044 (6) | 0.0013 (6) |
N40 | 0.0311 (10) | 0.0342 (11) | 0.0301 (9) | 0.0085 (8) | −0.0038 (7) | −0.0024 (7) |
C40 | 0.0328 (11) | 0.0288 (11) | 0.0277 (10) | 0.0018 (8) | −0.0065 (8) | 0.0014 (8) |
C41 | 0.079 (2) | 0.057 (2) | 0.086 (3) | −0.0052 (17) | −0.051 (2) | −0.0223 (19) |
C42 | 0.0552 (18) | 0.090 (3) | 0.0529 (17) | 0.0501 (19) | −0.0023 (15) | 0.0004 (17) |
C43 | 0.0562 (17) | 0.0445 (15) | 0.0510 (16) | −0.0076 (13) | −0.0081 (14) | −0.0181 (13) |
O98 | 0.0320 (7) | 0.0485 (9) | 0.0541 (10) | 0.0056 (7) | −0.0052 (7) | −0.0123 (8) |
O99 | 0.0381 (7) | 0.0303 (6) | 0.0306 (6) | −0.0032 (6) | −0.0039 (6) | −0.0094 (5) |
Geometric parameters (Å, º) top
Fe2—C5 | 1.9342 (16) | C21—H21C | 0.9600 |
Fe2—C4 | 1.9369 (16) | C22—H22A | 0.9600 |
Fe2—C2 | 1.9499 (17) | C22—H22B | 0.9600 |
Fe2—C3 | 1.9506 (17) | C22—H22C | 0.9600 |
Fe2—C1 | 1.9514 (16) | C23—H23A | 0.9600 |
Fe2—C6 | 1.9652 (16) | C23—H23B | 0.9600 |
C1—N1 | 1.153 (2) | C23—H23C | 0.9600 |
C2—N2 | 1.152 (2) | O30—C30A | 1.248 (5) |
C3—N3 | 1.155 (2) | O30—C30 | 1.274 (3) |
C4—N4 | 1.149 (2) | N30—C30 | 1.323 (5) |
C5—N5 | 1.152 (2) | N30—C33 | 1.361 (5) |
C6—N6 | 1.154 (2) | N30—C32 | 1.439 (6) |
Gd1—O10 | 2.2606 (13) | C30—C31 | 1.558 (5) |
Gd1—O40 | 2.2639 (13) | N30A—C30A | 1.266 (8) |
Gd1—O20 | 2.2730 (12) | N30A—C32A | 1.519 (11) |
Gd1—O30 | 2.2942 (12) | C31—H31A | 0.9600 |
Gd1—O2 | 2.3945 (13) | C31—H31B | 0.9600 |
Gd1—O1 | 2.4065 (12) | C31—H31C | 0.9600 |
Gd1—O3 | 2.4180 (12) | C32—H32A | 0.9600 |
O1—H1A | 0.971 (13) | C32—H32B | 0.9600 |
O1—H1B | 0.969 (13) | C32—H32C | 0.9600 |
O2—H2A | 0.969 (13) | C32A—H32D | 0.9600 |
O2—H2B | 0.969 (13) | C32A—H32E | 0.9600 |
O3—H3A | 0.968 (13) | C32A—H32F | 0.9600 |
O3—H3B | 0.969 (13) | C33—H33A | 0.9600 |
O10—C10 | 1.254 (2) | C33—H33B | 0.9600 |
N10—C10 | 1.309 (2) | C33—H33C | 0.9600 |
N10—C13 | 1.462 (3) | O40—C40 | 1.253 (3) |
N10—C12 | 1.466 (3) | O40—C40A | 1.314 (11) |
C10—C11 | 1.492 (3) | N40—C40 | 1.308 (3) |
C11—H11A | 0.9600 | N40—C43 | 1.451 (3) |
C11—H11B | 0.9600 | N40—C42 | 1.472 (3) |
C11—H11C | 0.9600 | C40—C41 | 1.519 (3) |
C12—H12A | 0.9600 | N40A—C40A | 1.301 (15) |
C12—H12B | 0.9600 | C41—H41A | 0.9600 |
C12—H12C | 0.9600 | C41—H41B | 0.9600 |
C13—H13A | 0.9600 | C41—H41C | 0.9600 |
C13—H13B | 0.9600 | C42—H42A | 0.9600 |
C13—H13C | 0.9600 | C42—H42B | 0.9600 |
O20—C20 | 1.254 (2) | C42—H42C | 0.9600 |
O20—C20A | 1.329 (12) | C43—H43A | 0.9600 |
C20—N20 | 1.312 (3) | C43—H43B | 0.9600 |
C20—C21 | 1.517 (3) | C43—H43C | 0.9600 |
N20—C23 | 1.451 (3) | O98—H98A | 0.968 (13) |
N20—C22 | 1.473 (3) | O98—H98B | 0.968 (13) |
N20A—C20A | 1.293 (17) | O99—H99A | 0.968 (13) |
C21—H21A | 0.9600 | O99—H99B | 0.967 (13) |
C21—H21B | 0.9600 | | |
| | | |
C5—Fe2—C4 | 90.74 (7) | C23—N20—C22 | 119.5 (2) |
C5—Fe2—C2 | 90.15 (7) | N20A—C20A—O20 | 114.1 (11) |
C4—Fe2—C2 | 86.43 (7) | C20—C21—H21A | 109.5 |
C5—Fe2—C3 | 177.28 (7) | C20—C21—H21B | 109.5 |
C4—Fe2—C3 | 87.21 (7) | H21A—C21—H21B | 109.5 |
C2—Fe2—C3 | 91.51 (7) | C20—C21—H21C | 109.5 |
C5—Fe2—C1 | 87.42 (7) | H21A—C21—H21C | 109.5 |
C4—Fe2—C1 | 175.55 (7) | H21B—C21—H21C | 109.5 |
C2—Fe2—C1 | 89.52 (7) | N20—C22—H22A | 109.5 |
C3—Fe2—C1 | 94.75 (7) | N20—C22—H22B | 109.5 |
C5—Fe2—C6 | 86.38 (7) | H22A—C22—H22B | 109.5 |
C4—Fe2—C6 | 92.30 (7) | N20—C22—H22C | 109.5 |
C2—Fe2—C6 | 176.29 (7) | H22A—C22—H22C | 109.5 |
C3—Fe2—C6 | 91.91 (7) | H22B—C22—H22C | 109.5 |
C1—Fe2—C6 | 91.62 (7) | N20—C23—H23A | 109.5 |
N1—C1—Fe2 | 175.95 (17) | N20—C23—H23B | 109.5 |
N2—C2—Fe2 | 177.70 (17) | H23A—C23—H23B | 109.5 |
N3—C3—Fe2 | 176.90 (16) | N20—C23—H23C | 109.5 |
N4—C4—Fe2 | 176.68 (15) | H23A—C23—H23C | 109.5 |
N5—C5—Fe2 | 177.35 (16) | H23B—C23—H23C | 109.5 |
N6—C6—Fe2 | 175.56 (15) | C30A—O30—Gd1 | 173.0 (2) |
O10—Gd1—O40 | 177.44 (6) | C30—O30—Gd1 | 146.75 (18) |
O10—Gd1—O20 | 92.57 (5) | C30—N30—C33 | 119.7 (3) |
O40—Gd1—O20 | 89.72 (5) | C30—N30—C32 | 124.2 (4) |
O10—Gd1—O30 | 91.95 (5) | C33—N30—C32 | 115.9 (4) |
O40—Gd1—O30 | 86.91 (5) | O30—C30—N30 | 117.4 (3) |
O20—Gd1—O30 | 143.00 (5) | O30—C30—C31 | 121.7 (3) |
O10—Gd1—O2 | 84.43 (6) | N30—C30—C31 | 121.0 (3) |
O40—Gd1—O2 | 93.05 (6) | C30A—N30A—C32A | 121.4 (6) |
O20—Gd1—O2 | 142.89 (5) | O30—C30A—N30A | 121.4 (5) |
O30—Gd1—O2 | 74.11 (4) | C30—C31—H31A | 109.5 |
O10—Gd1—O1 | 92.42 (5) | C30—C31—H31B | 109.5 |
O40—Gd1—O1 | 87.13 (5) | H31A—C31—H31B | 109.5 |
O20—Gd1—O1 | 73.25 (4) | C30—C31—H31C | 109.5 |
O30—Gd1—O1 | 143.16 (5) | H31A—C31—H31C | 109.5 |
O2—Gd1—O1 | 69.96 (4) | H31B—C31—H31C | 109.5 |
O10—Gd1—O3 | 89.80 (5) | N30—C32—H32A | 109.5 |
O40—Gd1—O3 | 91.97 (5) | N30—C32—H32B | 109.5 |
O20—Gd1—O3 | 73.14 (4) | H32A—C32—H32B | 109.5 |
O30—Gd1—O3 | 70.17 (4) | N30—C32—H32C | 109.5 |
O2—Gd1—O3 | 143.57 (4) | H32A—C32—H32C | 109.5 |
O1—Gd1—O3 | 146.38 (4) | H32B—C32—H32C | 109.5 |
Gd1—O1—H1A | 119.2 (12) | N30A—C32A—H32D | 109.5 |
Gd1—O1—H1B | 121.8 (11) | N30A—C32A—H32E | 109.5 |
H1A—O1—H1B | 108.3 (13) | H32D—C32A—H32E | 109.5 |
Gd1—O2—H2A | 123.3 (12) | N30A—C32A—H32F | 109.5 |
Gd1—O2—H2B | 124.4 (12) | H32D—C32A—H32F | 109.5 |
H2A—O2—H2B | 108.8 (13) | H32E—C32A—H32F | 109.5 |
Gd1—O3—H3A | 128.0 (11) | N30—C33—H33A | 109.5 |
Gd1—O3—H3B | 122.0 (11) | N30—C33—H33B | 109.5 |
H3A—O3—H3B | 109.3 (13) | H33A—C33—H33B | 109.5 |
C10—O10—Gd1 | 161.83 (14) | N30—C33—H33C | 109.5 |
C10—N10—C13 | 124.13 (19) | H33A—C33—H33C | 109.5 |
C10—N10—C12 | 119.29 (19) | H33B—C33—H33C | 109.5 |
C13—N10—C12 | 116.6 (2) | C40—O40—Gd1 | 163.74 (15) |
O10—C10—N10 | 120.29 (18) | C40A—O40—Gd1 | 149.2 (5) |
O10—C10—C11 | 119.96 (18) | C40—N40—C43 | 118.4 (2) |
N10—C10—C11 | 119.73 (18) | C40—N40—C42 | 123.4 (2) |
C10—C11—H11A | 109.5 | C43—N40—C42 | 118.1 (2) |
C10—C11—H11B | 109.5 | O40—C40—N40 | 119.9 (2) |
H11A—C11—H11B | 109.5 | O40—C40—C41 | 120.3 (2) |
C10—C11—H11C | 109.5 | N40—C40—C41 | 119.8 (2) |
H11A—C11—H11C | 109.5 | N40A—C40A—O40 | 115.8 (10) |
H11B—C11—H11C | 109.5 | C40—C41—H41A | 109.5 |
N10—C12—H12A | 109.5 | C40—C41—H41B | 109.5 |
N10—C12—H12B | 109.5 | H41A—C41—H41B | 109.5 |
H12A—C12—H12B | 109.5 | C40—C41—H41C | 109.5 |
N10—C12—H12C | 109.5 | H41A—C41—H41C | 109.5 |
H12A—C12—H12C | 109.5 | H41B—C41—H41C | 109.5 |
H12B—C12—H12C | 109.5 | N40—C42—H42A | 109.5 |
N10—C13—H13A | 109.5 | N40—C42—H42B | 109.5 |
N10—C13—H13B | 109.5 | H42A—C42—H42B | 109.5 |
H13A—C13—H13B | 109.5 | N40—C42—H42C | 109.5 |
N10—C13—H13C | 109.5 | H42A—C42—H42C | 109.5 |
H13A—C13—H13C | 109.5 | H42B—C42—H42C | 109.5 |
H13B—C13—H13C | 109.5 | N40—C43—H43A | 109.5 |
C20—O20—Gd1 | 156.97 (13) | N40—C43—H43B | 109.5 |
C20A—O20—Gd1 | 140.5 (6) | H43A—C43—H43B | 109.5 |
O20—C20—N20 | 120.2 (2) | N40—C43—H43C | 109.5 |
O20—C20—C21 | 121.3 (2) | H43A—C43—H43C | 109.5 |
N20—C20—C21 | 118.49 (19) | H43B—C43—H43C | 109.5 |
C20—N20—C23 | 119.21 (18) | H98A—O98—H98B | 109.5 (13) |
C20—N20—C22 | 121.0 (2) | H99A—O99—H99B | 109.6 (13) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···O99 | 0.97 (1) | 1.81 (1) | 2.7682 (19) | 170 (2) |
O1—H1A···N4i | 0.97 (1) | 1.78 (1) | 2.743 (2) | 171 (2) |
O2—H2A···N5ii | 0.97 (1) | 1.74 (1) | 2.705 (2) | 172 (2) |
O2—H2B···O99 | 0.97 (1) | 1.85 (1) | 2.7878 (18) | 162 (2) |
O3—H3A···N6 | 0.97 (1) | 2.12 (1) | 3.061 (2) | 165 (2) |
O3—H3B···N1iii | 0.97 (1) | 1.86 (1) | 2.823 (2) | 177 (2) |
O98—H98B···N2 | 0.97 (1) | 1.95 (1) | 2.913 (2) | 171 (2) |
O98—H98A···N2iv | 0.97 (1) | 2.21 (2) | 3.148 (2) | 162 (2) |
O99—H99B···O98v | 0.97 (1) | 1.81 (1) | 2.770 (2) | 171 (2) |
O99—H99A···N3vi | 0.97 (1) | 1.90 (1) | 2.863 (2) | 174 (2) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1/2, y−1/2, z; (iii) x+1/2, y, −z+1/2; (iv) −x, −y+1, −z+1; (v) −x, y−1/2, −z+1/2; (vi) −x+1/2, −y, z−1/2. |