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The crystal of barium penta­cyano­nitro­syl­ferrate trihydrate {barium nitro­prusside trihydrate, Ba[Fe(CN)5(NO)]·3H2O} has been studied by neutron diffraction at 20 K. The study was performed to characterize the structural phase generated by the phase transition undergone by the crystals at 80 K, at which temperature the unit-cell volume doubles. This crystal phase still exists at 20 K. The crystal structure, in space group P1, is completely ordered. The positional changes of the water mol­ecules in the present structure with respect to those of the compound at 105 K are presented.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104000599/sq1146sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104000599/sq1146Isup2.hkl
Contains datablock I

Comment top

At room temperature, barium nitroprusside crystallizes as a trihydrate. The crystals of barium nitroprusside trihydrate, (I), undergo four phase transitions when the temperature decreases. The first neutron diffraction study of (I) detected the two phase transitions occurring at 112 K and 130 K (Navaza et al., 1990). The comparison between the neutron structures at 140 K and 295 K (Navaza et al., 1992) confirmed the phase transition observed at 233 K by differential thermal analysis and 14N NQR experiments (Güida, 1992; Murgich et al., 1990). Recently, a new neutron diffraction study of (I) gave evidence of a fourth phase transition, at 80 K. At this temperature, commensurate superlattice reflections (h±1/2 k l) appear, suggesting a doubling of the a cell parameter of the room temperature crystal cell (Chevrier et al., 2003). To determine the crystal phase below this transition temperature, a neutron diffraction data set, including superlattice reflections with a resolution of 1.2 Å, has been measured on a single-crystal at 20 K. At this temperature, the three unit-cell angles are not 90° within the standard uncertainty. The crystal cell volume is exactly double that at 105 K. \sch

In this structure, of space group P1, molecules of (I) occupy eight independent sites, labelled 1–8 in Fig. 1. The principal structural differences between the crystal models refined at 20 K and 105 K are related to the positions of the water molecules. Table 1 presents distances and angles concerning these molecules.

In all the sites, water molecule W2, bonded to one Ba atom in a trigonal coordination, has atoms N3, N4, N5 and N6 as possible acceptors of weak hydrogen bonds. These contacts connect the nitroprusside anions along the [010] direction. The average H21···N3, H21···N4, H22···N5 and H22···N6 distances [2.84 (13), 2.52 (15), 2.71 (15) and 2.63 (13) Å, respectively] are equivalent to those found at 105 K, but the shortening of H21···N4 in sites 1 and 3 [2.27 (3) and 2.34 (3) Å, respectively, at 20 K, and 2.63 and 2.45 Å, respectively, at 105 K] indicates that the contact forces between W2 and these N atoms are significantly strengthened, pointing to a hydrogen bond in these sites.

In sites 1, 2, 3 and 8, small positional variations are observed in water molecule W3. The molecular plane rotates about 10° and the molecule is displaced by about 0.1 Å from its position at 105 K (Fig. 2 b and c). By contrast, in sites 4, 5, 6 and 7, W3 rotates about 80° around the O3—H32 direction and moves about 0.6 Å, introducing significant changes in the hydrogen-bond system (Fig. 2a and d). As at 105 K, W3 forms hydrogen bonds with N atoms of the same nitroprusside anion. In all sites, W3 forms a hydrogen bond with atom N2 via atom H32. In sites 3, 5, 6 and 8, W3 acts as a donor to atom N3, and in the other sites as a donor to atom N6 via atom H31. W3 is also coordinated to one Ba atom. Its tetragonal coordination is completed by accepting from W4 the strongest hydrogen bond of the structure [average distances and angle O4···O3 2.85 (3) Å, H42···O3 2.08 (4) Å and O4—H42···O3 137 (5)°].

In sites 1,2,3 and 8, W4 keeps the same orientation as in the structure at 105 K. The molecular plane rotates by less than 6° and the centre of gravity of the molecules is displaced by about 0.2 Å (Fig. 2 b and c). However, in all other sites W4 moves to take a pseudocentrosymmetric position with respect to that occupied at 105 K, the molecular plane rotates by 170° around the b axis and the molecule is displaced by about 0.9 Å along the [010] direction (Fig. 2a and d). In all sites, W4 acts as a hydrogen-bond donor to W3 via atom H42. In sites 1, 2, 4 and 7, W4 is also a hydrogen-bond donor to atom N4 [average distances and angle 2.98 (4) Å, 2.18 (6) Å and 140 (4)°] and in all other sites to atom N5 [average distances and angle 2.98 (2) Å, 2.14 (3) Å and 145 (3)°] via atom H41. W4 is shared between two Ba atoms, giving a distorted tetrahedral coordination [average Ba—O4—Ba angles 160.3 (1)°].

In conclusion, this study shows unambiguously the positional redistribution of water molecules in (I) at 20 K which, breaking the translational symmetry satisfied at 105 K, induces the doubling of the a cell parameter.

Experimental top

Compound (I) was obtained by stirring together stoichiometric quantities of silver nitroprusside (prepared by precipitation from stoichiometric amounts of sodium nitroprusside and silver nitrate solutions) and barium chloride solution. Silver chloride was separated from the solution by filtration and the liquid was concentrated in a vacuum rotary evaporator at room temperature, producing crystals of (I). Large single crystals were grown from small crystals by spontaneous concentration of saturated aqueous solutions kept in a thermostat slightly above room temperature, using the hanging seed method.

Refinement top

The crystal of (I), enclosed in a vanadium container under atmospheric conditions, was cooled directly to 20 K at a cooling rate of 3 K min−1. The experimental conditions for cooling prevented the collection of a complete set of diffracted reflections. The structure of (I) at 20 K was solved in three steps. In the first step, the crystal structure of (I) at 140 K, placed in one half of the 20 K unit cell, was refined in space group P1 using the intensities of the data without the commensurate superlattice reflections. An average model was refined in this `half cell'. High residual peaks were found on the difference Fourier maps around water positions W3 and W4. In the second step, the difference Fourier maps were also calculated in the same `half cell' but without the contributions of W3 and W4. Eight possible positions for water molecules W3 and W4 were detected. In the last step, 85 acceptable models of (I) at 20 K were built into the 20 K unit cell, via combination of the possible positions of W3 and W4, and refined using all data. The criterion used to choose the final model was the best convergence of refinements in space group P1. High correlations and the low ratio of the refined parameters to the number of independent reflections obliged us to refine all atoms isotropically and to constrain the isotropic displacements of all atoms occupying pseudosymmetrical positions (Ba, Fe, C, nitrosyl N, nitrosyl O, cyanide N, water O2, water O3 and water O4) to be identical. The H—O and H—H distances of the water molecules were restrained to 0.963 and 1.511 Å, respectively. The absolute value of the largest residual peak was less than 17% of the peak associated with a removed C atom.

Computing details top

Data collection: 4c-edi (Person et al., 1995); cell refinement: 4c-edi; data reduction: COLL5 (Lehmann & Larsen, 1974); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: CAMERON (Pearce et al., 2000); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A perspective view of the unit-cell contents of (I) at 20 K. For the sake of clarity, only selected labels are included. The eight independent nitroprusside anions occupy sites differentiated by the last number in the label. Dotted lines represent possible hydrogen bonds.
[Figure 2] Fig. 2. Unit-cell sections along the [100] direction, showing the differences between the W3 and W4 positions in the 20 and 105 K structures of (I). (a) x = 0, (b) x = 1/4, (c) x = 1/2, (d) x = 3/4.
barium pentacyanonitrosylferrate trihydrate top
Crystal data top
Ba[Fe(CN)5(NO)]·3H2OZ = 8
Mr = 407.32F(000) = 839.55
Triclinic, P1Dx = 2.131 Mg m3
Hall symbol: P 1Neutron radiation, λ = 1.54800 Å
a = 37.91 (7) ÅCell parameters from 32 reflections
b = 7.694 (7) Åθ = 15.6–24.2°
c = 8.705 (9) ŵ = 0.16 mm1
α = 90.03 (1)°T = 20 K
β = 90.086 (7)°Parallepiped, brown-red
γ = 90.146 (2)°5.5 × 2.5 × 1.5 mm
V = 2539 (6) Å3
Data collection top
Four-circle
diffractometer, 6T2 Orphee reactor
2676 reflections with I > 2σ(I)
Radiation source: Orphee reactorRint = 0.012
Er filters monochromatorθmax = 55.0°, θmin = 4.7°
ω 3<2θ<50 ωθ 50<2θ<80 ω–2θ 80<2θ<110 scansh = 3612
Absorption correction: numerical
(CRYSTAL SHAPE; local program)
k = 88
Tmin = 0.498, Tmax = 0.794l = 99
3218 measured reflections2 standard reflections every 100 reflections
3021 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.068All H-atom parameters refined
wR(F2) = 0.072 w = 1/[σ2(Fo2)]
S = 3.24(Δ/σ)max < 0.001
3021 reflectionsΔρmax = 1.06 e Å3
565 parametersΔρmin = 0.83 e Å3
72 restraintsExtinction correction: SHELXL93 (Sheldrick, 1993), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00058 (2)
Crystal data top
Ba[Fe(CN)5(NO)]·3H2Oγ = 90.146 (2)°
Mr = 407.32V = 2539 (6) Å3
Triclinic, P1Z = 8
a = 37.91 (7) ÅNeutron radiation, λ = 1.54800 Å
b = 7.694 (7) ŵ = 0.16 mm1
c = 8.705 (9) ÅT = 20 K
α = 90.03 (1)°5.5 × 2.5 × 1.5 mm
β = 90.086 (7)°
Data collection top
Four-circle
diffractometer, 6T2 Orphee reactor
2676 reflections with I > 2σ(I)
Absorption correction: numerical
(CRYSTAL SHAPE; local program)
Rint = 0.012
Tmin = 0.498, Tmax = 0.794θmax = 55.0°
3218 measured reflections2 standard reflections every 100 reflections
3021 independent reflections intensity decay: none
Refinement top
R[F2 > 2σ(F2)] = 0.06872 restraints
wR(F2) = 0.072All H-atom parameters refined
S = 3.24Δρmax = 1.06 e Å3
3021 reflectionsΔρmin = 0.83 e Å3
565 parameters
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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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
xyzUiso*/Ueq
Ba10.2011 (9)0.919 (4)0.248 (4)0.0015 (9)*
Ba20.3025 (9)0.076 (4)0.750 (4)0.0015 (9)*
Ba30.0494 (9)0.929 (4)0.747 (4)0.0015 (9)*
Ba40.4470 (9)0.088 (4)0.245 (4)0.0015 (9)*
Ba50.7006 (10)0.944 (4)0.241 (4)0.0015 (9)*
Ba60.8037 (8)0.078 (4)0.740 (3)0.0015 (9)*
Ba70.5498 (10)0.944 (4)0.742 (4)0.0015 (9)*
Ba80.9484 (10)0.082 (4)0.247 (4)0.0015 (9)*
Fe10.3317 (7)0.589 (3)0.249 (3)0.0001 (5)*
Fe20.1690 (7)0.4194 (3)0.754 (3)0.0001 (5)*
Fe30.4178 (7)0.5984 (3)0.7457 (3)0.0001 (5)*
Fe40.0807 (7)0.424 (3)0.250 (3)0.0001 (5)*
Fe50.8330 (7)0.590 (3)0.250 (3)0.0001 (5)*
Fe60.6684 (7)0.436 (3)0.744 (3)0.0001 (5)*
Fe70.9185 (7)0.584 (3)0.750 (3)0.0001 (5)*
Fe80.5823 (7)0.435 (3)0.246 (3)0.0001 (5)*
O10.4058 (9)0.571 (4)0.233 (3)0.0074 (11)*
O20.0946 (10)0.472 (4)0.751 (4)0.0074 (11)*
O30.3440 (10)0.545 (4)0.748 (4)0.0074 (11)*
O40.1559 (10)0.462 (420.239 (4)0.0074 (11)*
O50.9066 (10)0.551 (4)0.251 (4)0.0074 (11)*
O60.5953 (10)0.472 (4)0.734 (3)0.0074 (11)*
O70.8442 (8)0.573 (3)0.727 (3)0.0074 (11)*
O80.6550 (11)0.478 (4)0.238 (4)0.0074 (11)*
N110.3754 (7)0.565 (3)0.246 (3)0.0016 (5)*
N120.1244 (7)0.435 (3)0.754 (3)0.0016 (5)*
N130.3741 (7)0.565 (3)0.757 (3)0.0016 (5)*
N140.1254 (7)0.446 (3)0.252 (3)0.0016 (5)*
N150.8751 (7)0.559 (3)0.255 (3)0.0016 (5)*
N160.6229 (7)0.459 (3)0.747 (3)0.0016 (5)*
N170.8727 (7)0.568 (3)0.741 (3)0.0016 (5)*
N180.6241 (7)0.463 (3)0.246 (3)0.0016 (5)*
N210.2499 (6)0.653 (3)0.265 (2)0.0072 (3)*
N220.2485 (8)0.359 (3)0.756 (3)0.0072 (3)*
N230.4995 (7)0.658 (3)0.728 (3)0.0072 (3)*
N240.0006 (7)0.365 (3)0.239 (3)0.0072 (3)*
N250.7489 (7)0.660 (3)0.237 (3)0.0072 (3)*
N260.7482 (7)0.355 (3)0.746 (3)0.0072 (3)*
N270.9986 (7)0.662 (3)0.745 (3)0.0072 (3)*
N280.4999 (7)0.357 (3)0.234 (3)0.0072 (3)*
N310.3216 (6)0.314 (3)0.501 (3)0.0072 (3)*
N320.1808 (7)0.697 (3)1.008 (3)0.0072 (3)*
N330.4369 (6)0.313 (3)0.992 (3)0.0072 (3)*
N340.0686 (7)0.701 (3)0.506 (3)0.0072 (3)*
N350.8142 (7)0.312 (3)0.488 (3)0.0072 (3)*
N360.6834 (7)0.728 (3)0.983 (3)0.0072 (3)*
N370.9294 (6)0.320 (3)1.006 (3)0.0072 (3)*
N380.5659 (7)0.726 (3)0.487 (3)0.0072 (3)*
N410.3317 (7)0.873 (3)0.499 (3)0.0072 (3)*
N420.1703 (7)0.133 (3)0.989 (3)0.0072 (3)*
N430.4221 (7)0.872 (3)1.000 (3)0.0072 (3)*
N440.0813 (7)0.127 (3)0.489 (3)0.0072 (3)*
N450.8292 (7)0.865 (3)0.507 (3)0.0072 (3)*
N460.6708 (7)0.163 (3)1.009 (3)0.0072 (3)*
N470.9203 (7)0.883 (3)0.995 (3)0.0072 (3)*
N480.5781 (7)0.153 (3)0.502 (3)0.0072 (3)*
N510.3288 (7)0.870 (3)0.016 (3)0.0072 (3)*
N520.1731 (7)0.153 (3)0.481 (3)0.0072 (3)*
N530.4201 (7)0.867 (3)0.486 (3)0.0072 (3)*
N540.0791 (7)0.161 (3)0.023 (3)0.0072 (3)*
N550.8295 (7)0.880 (3)0.011 (3)0.0072 (3)*
N560.6700 (7)0.133 (3)0.501 (3)0.0072 (3)*
N570.9217 (7)0.866 (3)0.482 (3)0.0072 (3)*
N580.5801 (7)0.138 (3)0.004 (3)0.0072 (3)*
N610.3115 (6)0.303 (3)0.011 (3)0.0072 (3)*
N620.1865 (7)0.727 (3)0.513 (3)0.0072 (3)*
N630.4309 (7)0.311 (3)0.495 (3)0.0072 (3)*
N640.0646 (7)0.728 (3)0.014 (3)0.0072 (3)*
N650.8182 (7)0.309 (3)0.006 (3)0.0072 (3)*
N660.6832 (7)0.711 (3)0.490 (3)0.0072 (3)*
N670.9382 (6)0.302 (3)0.512 (3)0.0072 (3)*
N680.5679 (7)0.718 (3)0.000 (3)0.0072 (3)*
C210.2821 (9)0.6200 (4)0.244 (3)0.0032 (4)*
C220.2200 (10)0.387 (4)0.745 (3)0.0032 (4)*
C230.4706 (8)0.618 (3)0.739 (3)0.0032 (4)*
C240.0326 (8)0.379 (3)0.256 (3)0.0032 (4)*
C250.7817 (8)0.641 (3)0.231 (3)0.0032 (4)*
C260.7193 (8)0.393 (4)0.730 (3)0.0032 (4)*
C270.9683 (9)0.631 (4)0.758 (3)0.0032 (4)*
C280.5303 (9)0.387 (4)0.242 (3)0.0032 (4)*
C310.3258 (7)0.410 (4)0.406 (3)0.0032 (4)*
C320.1745 (7)0.594 (3)0.913 (3)0.0032 (4)*
C330.4304 (8)0.412 (4)0.897 (3)0.0032 (4)*
C340.0739 (7)0.594 (3)0.417 (3)0.0032 (4)*
C350.8219 (8)0.405 (4)0.390 (3)0.0032 (4)*
C360.6786 (8)0.613 (4)0.888 (3)0.0032 (4)*
C370.9255 (8)0.426 (3)0.907 (3)0.0032 (4)*
C380.5724 (8)0.612 (4)0.397 (3)0.0032 (4)*
C410.3309 (8)0.778 (4)0.399 (3)0.0032 (4)*
C420.1697 (8)0.244 (4)0.904 (3)0.0032 (4)*
C430.4190 (8)0.776 (4)0.897 (3)0.0032 (4)*
C440.0820 (8)0.249 (4)0.394 (3)0.0032 (4)*
C450.8302 (9)0.770 (4)0.410 (3)0.0032 (4)*
C460.6690 (8)0.259 (4)0.911 (3)0.0032 (4)*
C470.9174 (8)0.775 (4)0.897 (3)0.0032 (4)*
C480.5820 (8)0.259 (4)0.399 (3)0.0032 (4)*
C510.3307 (8)0.761 (4)0.088 (3)0.0032 (4)*
C520.1696 (8)0.263 (4)0.582 (3)0.0032 (4)*
C530.4192 (8)0.772 (4)0.578 (3)0.0032 (4)*
C540.0805 (8)0.261 (4)0.077 (3)0.0032 (4)*
C550.8320 (8)0.770 (4)0.092 (3)0.0032 (4)*
C560.6672 (8)0.254 (4)0.591 (3)0.0032 (4)*
C570.9199 (8)0.764 (4)0.579 (3)0.0032 (4)*
C580.5803 (9)0.258 (4)0.083 (3)0.0032 (4)*
C610.3206 (8)0.414 (4)0.096 (3)0.0032 (4)*
C620.1787 (8)0.602 (4)0.595 (3)0.0032 (4)*
C630.4287 (8)0.410 (4)0.594 (3)0.0032 (4)*
C640.0723 (8)0.607 (4)0.101 (3)0.0032 (4)*
C650.8226 (8)0.409 (4)0.087 (3)0.0032 (4)*
C660.6781 (8)0.594 (4)0.582 (3)0.0032 (4)*
C670.9279 (8)0.413 (4)0.601 (3)0.0032 (4)*
C680.5734 (8)0.614 (4)0.083 (3)0.0032 (4)*
O210.1257 (8)0.903 (4)0.247 (3)0.0076 (8)*
O220.3730 (8)0.114 (4)0.754 (3)0.0076 (8)*
O230.1249 (7)0.891 (4)0.752 (3)0.0076 (8)*
O240.3771 (8)0.113 (4)0.240 (3)0.0076 (8)*
O250.6258 (8)0.886 (4)0.241 (3)0.0076 (8)*
O260.8738 (8)0.124 (4)0.733 (3)0.0076 (8)*
O270.6228 (7)0.898 (4)0.743 (3)0.0076 (8)*
O280.8758 (8)0.122 (4)0.252 (3)0.0076 (8)*
O310.2396 (8)0.261 (3)0.208 (3)0.0082 (10)*
O320.2619 (8)0.764 (3)0.708 (3)0.0082 (10)*
O380.4898 (7)0.759 (3)0.274 (3)0.0082 (10)*
O330.5123 (8)0.254 (3)0.778 (3)0.0082 (10)*
O371.0117 (8)0.259 (3)0.711 (3)0.0082 (10)*
O350.7391 (7)0.262 (3)0.273 (3)0.0082 (10)*
O360.7600 (8)0.763 (3)0.771 (3)0.0082 (10)*
O340.9903 (7)0.760 (3)0.212 (3)0.0082 (10)*
O410.2408 (7)0.978 (3)0.959 (3)0.0083 (10)*
O460.7423 (7)0.991 (3)0.535 (3)0.0083 (10)*
O471.0085 (8)0.984 (3)0.457 (3)0.0083 (10)*
O480.5086 (7)0.986 (3)0.031 (3)0.0083 (10)*
O420.2586 (7)1.031 (3)0.458 (3)0.0083 (10)*
O430.4921 (7)1.022 (3)0.536 (3)0.0083 (10)*
O440.9921 (7)1.025 (3)0.954 (3)0.0083 (10)*
O450.7571 (7)1.019 (3)0.036 (3)0.0083 (10)*
H2110.1151 (9)0.957 (5)0.335 (3)0.021 (2)*
H2120.3888 (11)0.086 (6)0.838 (3)0.021 (2)*
H2130.1365 (10)0.939 (5)0.841 (3)0.021 (2)*
H2140.3629 (11)0.087 (6)0.329 (3)0.021 (2)*
H2150.6096 (10)0.928 (5)0.318 (3)0.021 (2)*
H2160.8910 (9)0.139 (5)0.814 (3)0.021 (2)*
H2170.6390 (10)0.955 (5)0.813 (3)0.021 (2)*
H2180.8614 (10)0.066 (5)0.329 (3)0.021 (2)*
H2210.1122 (11)0.951 (5)0.163 (3)0.021 (2)*
H2220.3888 (9)0.135 (5)0.670 (3)0.021 (2)*
H2230.1432 (9)0.890 (5)0.675 (3)0.021 (2)*
H2240.3599 (10)0.133 (6)0.160 (4)0.021 (2)*
H2250.6129 (10)0.902 (5)0.146 (3)0.021 (2)*
H2260.8881 (9)0.115 (5)0.642 (3)0.021 (2)*
H2270.6356 (9)0.895 (5)0.648 (3)0.021 (2)*
H2280.8614 (11)0.119 (6)0.161 (3)0.021 (2)*
H3110.2538 (9)0.261 (4)0.117 (3)0.0225 (15)*
H3120.2470 (9)0.756 (4)0.618 (3)0.0225 (15)*
H3180.5108 (7)0.758 (4)0.337 (3)0.0225 (15)*
H3130.4975 (9)0.259 (4)0.867 (3)0.0225 (15)*
H3210.2325 (10)0.380 (3)0.218 (4)0.0225 (15)*
H3220.2701 (9)0.646 (3)0.720 (4)0.0225 (15)*
H3271.0124 (11)0.381 (3)0.738 (4)0.0225 (15)*
H3280.4837 (10)0.637 (3)0.267 (5)0.0225 (15)*
H3250.7383 (10)0.383 (3)0.245 (4)0.0225 (15)*
H3260.7629 (10)0.645 (4)0.737 (4)0.0225 (15)*
H3230.5161 (13)0.374 (3)0.753 (5)0.0225 (15)*
H3240.9846 (11)0.638 (3)0.222 (5)0.0225 (15)*
H3170.9976 (8)0.258 (4)0.618 (3)0.0225 (15)*
H3150.7591 (8)0.255 (4)0.340 (3)0.0225 (15)*
H3160.7406 (8)0.757 (4)0.842 (3)0.0225 (15)*
H3141.0097 (8)0.760 (4)0.141 (4)0.0225 (15)*
H4110.2203 (9)1.038 (4)0.921 (5)0.0251 (14)*
H4160.7219 (9)1.061 (4)0.557 (4)0.0251 (14)*
H4171.0111 (11)0.881 (4)0.396 (4)0.0251 (14)*
H4180.5112 (10)0.871 (3)0.071 (4)0.0251 (14)*
H4210.2402 (11)0.868 (3)0.906 (5)0.0251 (14)*
H4260.7371 (10)0.882 (3)0.582 (4)0.0251 (14)*
H4271.0268 (9)1.059 (4)0.418 (4)0.0251 (14)*
H4280.5294 (10)1.046 (4)0.067 (5)0.0251 (14)*
H4120.2795 (9)0.979 (4)0.415 (4)0.0251 (14)*
H4130.4694 (8)0.976 (4)0.565 (4)0.0251 (14)*
H4140.9709 (9)0.966 (5)0.924 (5)0.0251 (14)*
H4150.7780 (9)0.959 (4)0.069 (5)0.0251 (14)*
H4220.2570 (10)1.142 (4)0.407 (4)0.0251 (14)*
H4230.4916 (10)1.139 (3)0.578 (4)0.0251 (14)*
H4240.9912 (10)1.132 (3)0.897 (4)0.0251 (14)*
H4250.7600 (11)1.134 (3)0.079 (5)0.0251 (14)*
Geometric parameters (Å, º) top
Ba1—O212.86 (3)N55—C551.24 (3)
Ba1—O41i2.96 (3)N56—C561.23 (3)
Ba1—O422.97 (3)N57—C571.15 (2)
Ba1—O31ii3.03 (2)N58—C581.20 (3)
Ba2—O222.69 (4)N61—C611.18 (3)
Ba2—O32iii2.87 (4)N62—C621.23 (3)
Ba2—O42iii3.06 (4)N63—C631.15 (3)
Ba2—O41iii3.06 (4)N64—C641.23 (2)
Ba3—O232.88 (4)N65—C651.13 (3)
Ba3—O44iv2.92 (4)N66—C661.22 (2)
Ba3—O37v2.94 (3)N67—C671.22 (3)
Ba3—O47iv2.99 (4)N68—C681.10 (2)
Ba4—O242.66 (4)O21—H2110.965 (6)
Ba4—O38iii3.02 (3)O21—H2210.967 (6)
Ba4—O48iii3.09 (4)O22—H2120.965 (6)
Ba4—O43iii3.10 (4)O22—H2220.964 (6)
Ba5—O452.85 (3)O23—H2130.964 (6)
Ba5—O35ii2.86 (3)O23—H2230.963 (6)
Ba5—O252.87 (4)O24—H2140.963 (6)
Ba5—O463.02 (4)O24—H2240.964 (6)
Ba6—O262.68 (4)O25—H2150.964 (6)
Ba6—O36iii2.94 (3)O25—H2250.965 (6)
Ba6—O46iii3.00 (4)O26—H2160.965 (7)
Ba7—O272.79 (4)O26—H2260.963 (6)
Ba7—O33ii2.80 (3)O27—H2170.964 (7)
Ba7—O432.89 (4)O27—H2270.964 (6)
Ba7—O48vi2.98 (4)O28—H2180.963 (6)
Ba8—O282.77 (4)O28—H2280.964 (6)
Ba8—O34iii2.96 (3)O31—O42iii2.89 (3)
Ba8—O47iii3.02 (4)O31—Ba1iii3.03 (2)
Ba8—O44vii3.07 (4)O31—O41vii3.07 (2)
Fe1—N111.67 (3)O31—H3110.964 (6)
Fe1—C211.90 (3)O31—H3210.963 (6)
Fe1—C511.93 (3)O32—O412.85 (2)
Fe1—C611.94 (3)O32—Ba2ii2.87 (4)
Fe1—C411.95 (3)O32—O423.00 (2)
Fe1—C311.96 (3)O32—H3120.965 (6)
Fe2—N121.70 (2)O32—H3220.965 (6)
Fe2—C421.88 (3)O32—H4212.08 (4)
Fe2—C521.92 (3)O38—O482.84 (3)
Fe2—C321.94 (3)O38—Ba4ii3.02 (3)
Fe2—C221.95 (4)O38—O433.05 (3)
Fe3—N131.68 (3)O38—H3180.965 (7)
Fe3—C431.90 (3)O38—H3280.963 (6)
Fe3—C531.98 (3)O38—H4182.13 (3)
Fe3—C632.00 (3)O33—Ba7iii2.80 (3)
Fe4—N141.70 (3)O33—O43iii2.86 (3)
Fe4—C441.84 (3)O33—O48viii3.02 (3)
Fe4—C241.85 (3)O33—H3130.965 (6)
Fe4—C641.95 (3)O33—H3230.963 (6)
Fe4—C541.96 (3)O37—O44iii2.88 (3)
Fe4—C341.97 (3)O37—Ba3ix2.94 (3)
Fe5—N151.62 (3)O37—O47iii3.06 (2)
Fe5—C351.92 (3)O37—H3270.964 (6)
Fe5—C551.95 (3)O37—H3170.965 (6)
Fe5—C451.96 (3)O35—Ba5iii2.86 (3)
Fe5—C251.99 (3)O35—O45iii2.86 (3)
Fe6—N161.74 (3)O35—O46iii3.09 (3)
Fe6—C361.89 (3)O35—H3250.963 (6)
Fe6—C661.90 (3)O35—H3150.963 (7)
Fe6—C561.93 (3)O36—O462.78 (3)
Fe6—C261.96 (3)O36—Ba6ii2.94 (3)
Fe6—C461.99 (3)O36—O45vi3.04 (2)
Fe7—N171.74 (3)O36—H3260.964 (6)
Fe7—C371.85 (3)O36—H3160.963 (6)
Fe7—C671.88 (3)O36—H4262.07 (4)
Fe7—C271.92 (3)O34—O472.83 (3)
Fe7—C471.94 (3)O34—Ba8ii2.96 (3)
Fe8—N181.60 (3)O34—O44i3.04 (3)
Fe8—C481.90 (3)O34—H3240.964 (6)
Fe8—C381.94 (3)O34—H3140.964 (6)
Fe8—C581.96 (3)O34—H4172.01 (4)
Fe8—C682.00 (3)O41—Ba1vi2.96 (3)
Fe8—C282.00 (3)O41—Ba2ii3.06 (4)
O1—N111.16 (3)O41—O31x3.07 (2)
O2—N121.17 (3)O41—H4110.964 (7)
O3—N131.15 (3)O41—H4210.962 (6)
O4—N141.17 (3)O46—Ba6ii3.00 (4)
O5—N151.19 (3)O46—O35ii3.09 (3)
O6—N161.06 (3)O46—H4160.964 (7)
O7—N171.09 (2)O46—H4260.961 (6)
O8—N181.18 (3)O47—Ba3xi2.99 (4)
N21—C211.26 (3)O47—Ba8ii3.02 (4)
N22—C221.11 (3)O47—O37ii3.06 (2)
N23—C231.14 (2)O47—H4170.965 (6)
N24—C241.23 (3)O47—H4270.964 (7)
N25—C251.25 (3)O48—Ba7i2.98 (4)
N26—C261.14 (2)O48—O33xii3.02 (3)
N27—C271.18 (3)O48—Ba4ii3.09 (4)
N28—C281.17 (3)O48—H4180.962 (6)
N31—C311.12 (2)O48—H4280.963 (6)
N32—C321.16 (2)O42—O31ii2.89 (3)
N33—C331.15 (2)O42—Ba2ii3.06 (4)
N34—C341.15 (2)O42—H4120.963 (7)
N35—C351.15 (2)O42—H4220.961 (6)
N36—C361.22 (2)O43—O33ii2.86 (3)
N37—C371.20 (2)O43—Ba4ii3.10 (4)
N38—C381.20 (3)O43—H4130.964 (7)
N41—C411.15 (2)O43—H4230.966 (6)
N42—C421.13 (2)O44—O37ii2.88 (3)
N43—C431.17 (3)O44—Ba3xi2.92 (4)
N44—C441.25 (2)O44—O34vi3.04 (3)
N45—C451.12 (3)O44—Ba8x3.07 (4)
N46—C461.13 (2)O44—H4140.963 (7)
N47—C471.20 (3)O44—H4240.961 (6)
N48—C481.22 (3)O45—O35ii2.86 (3)
N51—C511.24 (3)O45—O36i3.04 (2)
N52—C521.23 (2)O45—H4150.963 (7)
N53—C531.08 (2)O45—H4250.962 (6)
N54—C541.16 (2)
O21—Ba1—O41i120.8 (8)Ba1iii—O31—H311111.2 (19)
O21—Ba1—O42138.2 (8)O41vii—O31—H31153.5 (19)
O41i—Ba1—O4296.0 (7)O42iii—O31—H321126 (2)
O21—Ba1—O31ii121.0 (8)Ba1iii—O31—H321133 (2)
O41i—Ba1—O31ii61.7 (6)O41vii—O31—H321138 (2)
O42—Ba1—O31ii57.7 (6)H311—O31—H321103.3 (10)
O22—Ba2—O32iii128.5 (13)O41—O32—Ba2ii64.7 (8)
O22—Ba2—O42iii124.4 (11)O41—O32—O4298.7 (7)
O32iii—Ba2—O42iii60.6 (8)Ba2ii—O32—O4262.8 (8)
O22—Ba2—O41iii141.0 (12)O41—O32—H312119.7 (19)
O32iii—Ba2—O41iii57.4 (8)Ba2ii—O32—H312118 (2)
O42iii—Ba2—O41iii93.0 (10)O42—O32—H31255.5 (19)
O23—Ba3—O44iv139.3 (11)O41—O32—H322123 (2)
O23—Ba3—O37v125.2 (12)Ba2ii—O32—H322127 (2)
O44iv—Ba3—O37v58.9 (8)O42—O32—H322138 (2)
O23—Ba3—O47iv122.8 (10)H312—O32—H322102.6 (10)
O44iv—Ba3—O47iv95.7 (9)O41—O32—H42113.4 (9)
O37v—Ba3—O47iv62.1 (7)Ba2ii—O32—H42177.6 (12)
O24—Ba4—O38iii126.8 (13)O42—O32—H421108.9 (11)
O24—Ba4—O48iii139.9 (12)H312—O32—H421118 (2)
O38iii—Ba4—O48iii55.4 (7)H322—O32—H421113 (2)
O24—Ba4—O43iii124.9 (11)O48—O38—Ba4ii63.5 (7)
O38iii—Ba4—O43iii59.8 (7)O48—O38—O4398.1 (7)
O48iii—Ba4—O43iii92.0 (9)Ba4ii—O38—O4361.4 (7)
O45—Ba5—O35ii60.2 (8)O48—O38—H318103 (2)
O45—Ba5—O25140.8 (11)Ba4ii—O38—H318119.7 (18)
O35ii—Ba5—O25129.5 (11)O43—O38—H31863.9 (17)
O45—Ba5—O4696.4 (9)O48—O38—H328128 (2)
O35ii—Ba5—O4663.4 (8)Ba4ii—O38—H328133 (2)
O25—Ba5—O46122.3 (10)O43—O38—H328134 (2)
O26—Ba6—O36iii131.8 (12)H318—O38—H328103.2 (10)
O26—Ba6—O46iii141.5 (11)O48—O38—H41815.2 (7)
O36iii—Ba6—O46iii55.8 (8)Ba4ii—O38—H41878.2 (10)
O27—Ba7—O33ii127.8 (13)O43—O38—H418110.0 (10)
O27—Ba7—O43141.3 (11)H318—O38—H41899 (2)
O33ii—Ba7—O4360.3 (8)H328—O38—H418115 (3)
O27—Ba7—O48vi122.1 (11)Ba7iii—O33—O43iii61.5 (8)
O33ii—Ba7—O48vi62.9 (7)Ba7iii—O33—O48viii61.5 (8)
O43—Ba7—O48vi95.9 (10)O43iii—O33—O48viii95.7 (7)
O28—Ba8—O34iii129.1 (13)Ba7iii—O33—H313115 (2)
O28—Ba8—O47iii140.1 (11)O43iii—O33—H313118 (2)
O34iii—Ba8—O47iii56.4 (8)O48viii—O33—H31353.7 (19)
O28—Ba8—O44vii124.6 (12)Ba7iii—O33—H323136 (3)
O34iii—Ba8—O44vii60.4 (7)O43iii—O33—H323118 (3)
O47iii—Ba8—O44vii93.4 (10)O48viii—O33—H323146 (3)
N11—Fe1—C21177.9 (13)H313—O33—H323103.2 (10)
N11—Fe1—C5195.0 (12)O44iii—O37—Ba3ix60.3 (8)
C21—Fe1—C5183.0 (12)O44iii—O37—O47iii95.1 (7)
N11—Fe1—C6197.4 (12)Ba3ix—O37—O47iii59.8 (7)
C21—Fe1—C6182.0 (12)O44iii—O37—H327116 (2)
C51—Fe1—C6188.4 (12)Ba3ix—O37—H327143 (2)
N11—Fe1—C4196.4 (13)O47iii—O37—H327148 (2)
C21—Fe1—C4184.2 (11)O44iii—O37—H317118 (2)
C51—Fe1—C4188.4 (12)Ba3ix—O37—H317110.7 (18)
C61—Fe1—C41166.1 (15)O47iii—O37—H31751.2 (17)
N11—Fe1—C3192.6 (11)H327—O37—H317102.8 (10)
C21—Fe1—C3189.4 (11)Ba5iii—O35—O45iii59.7 (7)
C51—Fe1—C31172.0 (15)Ba5iii—O35—O46iii61.0 (8)
C61—Fe1—C3188.2 (12)O45iii—O35—O46iii94.6 (7)
C41—Fe1—C3193.1 (11)Ba5iii—O35—H325142 (2)
N12—Fe2—C4293.9 (11)O45iii—O35—H325117 (2)
N12—Fe2—C5293.4 (11)O46iii—O35—H325147 (2)
C42—Fe2—C5295.2 (11)Ba5iii—O35—H315114.3 (19)
N12—Fe2—C3293.2 (10)O45iii—O35—H315102 (2)
C42—Fe2—C3290.3 (10)O46iii—O35—H31558.5 (18)
C52—Fe2—C32171.2 (12)H325—O35—H315103.5 (11)
N12—Fe2—C22176.0 (12)O46—O36—Ba6ii63.2 (8)
C42—Fe2—C2285.6 (12)O46—O36—O45vi98.3 (7)
C52—Fe2—C2282.7 (11)Ba6ii—O36—O45vi63.8 (7)
C32—Fe2—C2290.8 (11)O46—O36—H326114 (2)
N13—Fe3—C4395.2 (11)Ba6ii—O36—H326134 (2)
N13—Fe3—C5399.9 (12)O45vi—O36—H326148 (2)
C43—Fe3—C5391.5 (11)O46—O36—H316109 (2)
N13—Fe3—C6397.7 (12)Ba6ii—O36—H316122.0 (19)
C43—Fe3—C63166.6 (15)O45vi—O36—H31661.0 (18)
C53—Fe3—C6389.9 (11)H326—O36—H316103.4 (11)
N14—Fe4—C4492.3 (12)O46—O36—H42615.3 (8)
N14—Fe4—C24174.6 (13)Ba6ii—O36—H42678.5 (11)
C44—Fe4—C2482.7 (11)O45vi—O36—H426107.6 (11)
N14—Fe4—C6495.6 (11)H326—O36—H426103 (3)
C44—Fe4—C64172.1 (15)H316—O36—H426102 (2)
C24—Fe4—C6489.4 (11)O47—O34—Ba8ii62.8 (8)
N14—Fe4—C5494.0 (11)O47—O34—O44i98.1 (7)
C44—Fe4—C5493.2 (11)Ba8ii—O34—O44i61.6 (8)
C24—Fe4—C5484.4 (11)O47—O34—H324125 (3)
C64—Fe4—C5487.2 (10)Ba8ii—O34—H324133 (2)
N14—Fe4—C3493.6 (11)O44i—O34—H324136 (3)
C44—Fe4—C3489.3 (10)O47—O34—H314108 (2)
C24—Fe4—C3488.3 (11)Ba8ii—O34—H314119 (2)
C64—Fe4—C3489.2 (10)O44i—O34—H31460.4 (19)
C54—Fe4—C34171.9 (13)H324—O34—H314103.2 (10)
N15—Fe5—C3595.1 (11)O47—O34—H41712.3 (10)
N15—Fe5—C5598.1 (12)Ba8ii—O34—H41775.1 (12)
C35—Fe5—C55165.7 (15)O44i—O34—H417105.6 (11)
N15—Fe5—C4598.1 (13)H324—O34—H417118 (3)
C35—Fe5—C4593.5 (11)H314—O34—H417103 (2)
C55—Fe5—C4590.0 (12)O32—O41—Ba1vi134.8 (8)
N15—Fe5—C25175.6 (13)O32—O41—Ba2ii57.9 (8)
C35—Fe5—C2589.3 (11)Ba1vi—O41—Ba2ii158.7 (9)
C55—Fe5—C2577.5 (11)O32—O41—O31x162.6 (9)
C45—Fe5—C2582.2 (11)Ba1vi—O41—O31x60.2 (6)
N16—Fe6—C3696.6 (11)Ba2ii—O41—O31x105.0 (8)
N16—Fe6—C6697.8 (11)O32—O41—H411104 (2)
C36—Fe6—C6689.6 (11)Ba1vi—O41—H41188 (3)
N16—Fe6—C5693.7 (12)Ba2ii—O41—H411107 (3)
C36—Fe6—C56169.6 (14)O31x—O41—H41184 (2)
C66—Fe6—C5687.5 (10)O32—O41—H42130 (3)
N16—Fe6—C26175.4 (13)Ba1vi—O41—H421105 (3)
C36—Fe6—C2688.0 (11)Ba2ii—O41—H42187 (3)
C66—Fe6—C2682.6 (11)O31x—O41—H421164 (3)
C56—Fe6—C2681.7 (11)H411—O41—H421103.5 (10)
N16—Fe6—C4694.1 (11)O36—O46—Ba6ii61.0 (8)
C36—Fe6—C4690.4 (10)O36—O46—Ba5132.4 (10)
C66—Fe6—C46168.0 (14)Ba6ii—O46—Ba5158.7 (9)
C56—Fe6—C4690.4 (11)O36—O46—O35ii168.1 (10)
C26—Fe6—C4685.4 (11)Ba6ii—O46—O35ii108.6 (8)
N17—Fe7—C3797.4 (11)Ba5—O46—O35ii55.7 (7)
N17—Fe7—C6796.3 (12)O36—O46—H416113 (2)
C37—Fe7—C6791.0 (11)Ba6ii—O46—H416112 (3)
N17—Fe7—C27173.5 (13)Ba5—O46—H41680 (3)
C37—Fe7—C2787.4 (12)O35ii—O46—H41675.0 (18)
C67—Fe7—C2788.1 (12)O36—O46—H42635 (2)
N17—Fe7—C4793.5 (11)Ba6ii—O46—H42696 (3)
C37—Fe7—C4790.9 (10)Ba5—O46—H42699 (3)
C67—Fe7—C47169.6 (14)O35ii—O46—H426155 (3)
C27—Fe7—C4781.8 (11)H416—O46—H426103.7 (10)
N18—Fe8—C4895.8 (12)O34—O47—Ba3xi132.4 (9)
N18—Fe8—C3895.6 (12)O34—O47—Ba8ii60.8 (8)
C48—Fe8—C3891.1 (11)Ba3xi—O47—Ba8ii159.8 (10)
N18—Fe8—C5897.6 (12)O34—O47—O37ii167.3 (10)
C48—Fe8—C5890.9 (12)Ba3xi—O47—O37ii58.1 (7)
C38—Fe8—C58166.4 (15)Ba8ii—O47—O37ii107.1 (8)
N18—Fe8—C6894.3 (11)O34—O47—H41726 (3)
C48—Fe8—C68169.9 (14)Ba3xi—O47—H417107 (3)
C38—Fe8—C6887.9 (11)Ba8ii—O47—H41787 (3)
C58—Fe8—C6887.8 (11)O37ii—O47—H417165 (3)
N18—Fe8—C28177.0 (14)O34—O47—H427105.7 (19)
C48—Fe8—C2882.8 (12)Ba3xi—O47—H42791 (2)
C38—Fe8—C2887.1 (12)Ba8ii—O47—H427100 (3)
C58—Fe8—C2879.9 (12)O37ii—O47—H42779.4 (19)
C68—Fe8—C2887.2 (11)H417—O47—H427103.0 (10)
O1—N11—Fe1169.8 (19)O38—O48—Ba7i133.9 (9)
O2—N12—Fe2170.2 (17)O38—O48—O33xii167.7 (10)
O3—N13—Fe3172.4 (18)Ba7i—O48—O33xii55.5 (7)
O4—N14—Fe4173.8 (18)O38—O48—Ba4ii61.1 (8)
O5—N15—Fe5173.6 (19)Ba7i—O48—Ba4ii159.0 (10)
O6—N16—Fe6172.9 (18)O33xii—O48—Ba4ii107.7 (8)
O7—N17—Fe7172.4 (18)O38—O48—H41835 (2)
O8—N18—Fe8176.0 (18)Ba7i—O48—H41899 (2)
N21—C21—Fe1169.8 (18)O33xii—O48—H418153 (2)
N22—C22—Fe2172 (2)Ba4ii—O48—H41896 (2)
N24—C24—Fe4169.7 (16)O38—O48—H428105 (2)
N25—C25—Fe5171.2 (15)Ba7i—O48—H42884 (3)
N26—C26—Fe6168.2 (17)O33xii—O48—H42883 (2)
N27—C27—Fe7172.2 (17)Ba4ii—O48—H428108 (3)
N28—C28—Fe8177.7 (18)H418—O48—H428103.4 (10)
N31—C31—Fe1176.4 (19)O31ii—O42—Ba162.2 (7)
N32—C32—Fe2174.4 (18)O31ii—O42—O32167.3 (11)
N34—C34—Fe4174.7 (15)Ba1—O42—O32106.2 (8)
N35—C35—Fe5170.9 (18)O31ii—O42—Ba2ii133.7 (10)
N36—C36—Fe6177 (2)Ba1—O42—Ba2ii160.5 (9)
N37—C37—Fe7178 (2)O32—O42—Ba2ii56.6 (7)
N38—C38—Fe8177 (2)O31ii—O42—H41299.9 (19)
N41—C41—Fe1171.4 (18)Ba1—O42—H412104 (3)
N42—C42—Fe2177 (2)O32—O42—H41287.7 (18)
N43—C43—Fe3172 (2)Ba2ii—O42—H41285 (3)
N44—C44—Fe4177 (2)O31ii—O42—H42226 (3)
N45—C45—Fe5176 (2)Ba1—O42—H42286 (3)
N46—C46—Fe6176 (2)O32—O42—H422161 (3)
N47—C47—Fe7172.0 (19)Ba2ii—O42—H422108 (3)
N48—C48—Fe8173 (2)H412—O42—H422104.1 (10)
N51—C51—Fe1178 (2)O33ii—O43—Ba758.3 (8)
N52—C52—Fe2172.3 (19)O33ii—O43—O38166.0 (9)
N53—C53—Fe3180 (3)Ba7—O43—O38110.1 (8)
N54—C54—Fe4177 (2)O33ii—O43—Ba4ii130.3 (9)
N55—C55—Fe5176 (2)Ba7—O43—Ba4ii163.3 (10)
N56—C56—Fe6173 (2)O38—O43—Ba4ii58.8 (7)
N58—C58—Fe8172.7 (19)O33ii—O43—H413106 (2)
N61—C61—Fe1174 (2)Ba7—O43—H413116 (2)
N63—C63—Fe3170 (2)O38—O43—H41386 (2)
N64—C64—Fe4174.8 (19)Ba4ii—O43—H41378 (2)
N66—C66—Fe6172.4 (17)O33ii—O43—H42332 (2)
N67—C67—Fe7172 (2)Ba7—O43—H42389 (3)
N68—C68—Fe8176 (2)O38—O43—H423153 (3)
Ba1—O21—H211114 (2)Ba4ii—O43—H42398 (3)
Ba1—O21—H221121 (3)H413—O43—H423102.8 (10)
H211—O21—H221102.5 (10)O37ii—O44—Ba3xi60.8 (8)
Ba2—O22—H212127 (2)O37ii—O44—O34vi166.2 (10)
Ba2—O22—H222129 (2)Ba3xi—O44—O34vi107.6 (9)
H212—O22—H222103.2 (11)O37ii—O44—Ba8x131.4 (9)
Ba3—O23—H213115 (2)Ba3xi—O44—Ba8x161.9 (11)
Ba3—O23—H223135 (2)O34vi—O44—Ba8x58.0 (7)
H213—O23—H223103.6 (10)O37ii—O44—H414108 (2)
Ba4—O24—H214122 (2)Ba3xi—O44—H414110 (3)
Ba4—O24—H224134 (2)O34vi—O44—H41482 (2)
H214—O24—H224103.4 (10)Ba8x—O44—H41481 (3)
Ba5—O25—H215126 (3)O37ii—O44—H42425 (2)
Ba5—O25—H225119 (2)Ba3xi—O44—H42486 (2)
H215—O25—H225103.0 (10)O34vi—O44—H424163 (2)
Ba6—O26—H216131.8 (19)Ba8x—O44—H424107 (2)
Ba6—O26—H226124.6 (19)H414—O44—H424103.7 (10)
H216—O26—H226103.2 (10)Ba5—O45—O35ii60.1 (8)
Ba7—O27—H217125 (2)Ba5—O45—O36i112.0 (8)
Ba7—O27—H227120 (2)O35ii—O45—O36i168.1 (9)
H217—O27—H227103.4 (10)Ba5—O45—H415110 (3)
Ba8—O28—H218122 (3)O35ii—O45—H415108 (2)
Ba8—O28—H228123 (3)O36i—O45—H41583 (2)
H218—O28—H228103.8 (11)Ba5—O45—H42592 (3)
O42iii—O31—Ba1iii60.2 (7)O35ii—O45—H42532 (3)
O42iii—O31—O41vii95.3 (7)O36i—O45—H425152 (3)
Ba1iii—O31—O41vii58.2 (6)H415—O45—H425103.7 (10)
O42iii—O31—H311118.8 (19)
Symmetry codes: (i) x, y, z1; (ii) x, y+1, z; (iii) x, y1, z; (iv) x1, y, z; (v) x1, y+1, z; (vi) x, y, z+1; (vii) x, y1, z1; (viii) x, y1, z+1; (ix) x+1, y1, z; (x) x, y+1, z+1; (xi) x+1, y, z; (xii) x, y+1, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O21—H211···N44ii0.97 (1)2.27 (3)3.21 (3)163 (3)
O21—H211···N340.97 (1)3.03 (3)3.49 (3)111 (3)
O21—H221···N54ii0.97 (1)2.61 (3)3.55 (3)164 (3)
O21—H221···N640.97 (1)2.81 (3)3.36 (3)117 (3)
O22—H212···N43iii0.97 (1)2.51 (3)3.39 (3)152 (3)
O22—H212···N330.97 (1)2.85 (3)3.53 (3)128 (3)
O22—H222···N53iii0.96 (1)2.87 (3)3.51 (3)124 (3)
O22—H222···N630.96 (1)2.58 (3)3.49 (3)157 (3)
O23—H213···N42ii0.96 (1)2.34 (3)3.26 (3)158 (3)
O23—H213···N320.96 (1)2.90 (3)3.42 (3)115 (3)
O23—H223···N52ii0.96 (1)2.87 (3)3.60 (3)133 (3)
O23—H223···N620.96 (1)2.50 (3)3.38 (3)151 (3)
O24—H214···N41iii0.96 (1)2.51 (3)3.38 (3)151 (3)
O24—H214···N310.96 (1)2.78 (3)3.47 (3)128 (3)
O24—H224···N51iii0.96 (1)2.80 (3)3.43 (3)124 (3)
O24—H224···N610.96 (1)2.61 (3)3.51 (3)157 (3)
O25—H215···N48ii0.96 (1)2.65 (3)3.56 (3)158 (3)
O25—H215···N380.96 (1)2.70 (3)3.35 (3)125 (3)
O25—H225···N58ii0.97 (1)2.56 (3)3.36 (3)140 (3)
O25—H225···N680.97 (1)2.55 (3)3.30 (3)134 (3)
O26—H216···N47iii0.97 (1)2.76 (3)3.43 (3)128 (3)
O26—H216···N370.97 (1)2.62 (3)3.51 (3)154 (3)
O26—H226···N57iii0.96 (1)2.69 (3)3.47 (3)138 (3)
O26—H226···N670.96 (1)2.63 (3)3.39 (3)136 (3)
O27—H217···N46ii0.96 (1)2.63 (3)3.57 (3)167 (3)
O27—H217···N360.96 (1)2.85 (3)3.37 (3)115 (3)
O27—H227···N56ii0.96 (1)2.58 (3)3.30 (3)132 (3)
O27—H227···N660.96 (1)2.68 (3)3.49 (3)143 (3)
O28—H218···N45iii0.96 (1)2.51 (3)3.46 (3)168 (3)
O28—H218···N350.96 (1)2.95 (3)3.44 (3)113 (3)
O28—H228···N55iii0.96 (1)2.66 (3)3.43 (3)137 (3)
O28—H228···N650.96 (1)2.63 (3)3.45 (3)143 (3)
O31—H321···N210.96 (1)2.24 (3)3.08 (3)146 (3)
O31—H311···N610.96 (1)2.40 (3)3.24 (3)146 (3)
O31—H321···O40.96 (1)2.98 (3)3.55 (3)119 (3)
O32—H322···N220.97 (1)2.38 (3)3.19 (3)141 (3)
O32—H312···N620.97 (1)2.48 (3)3.33 (3)148 (3)
O32—H322···O30.97 (1)2.92 (3)3.56 (3)125 (3)
O33—H323···N230.96 (1)2.28 (3)3.18 (3)155 (3)
O33—H313···N330.97 (1)2.58 (3)3.45 (3)150 (3)
O33—H323···O60.96 (1)3.10 (3)3.58 (3)113 (3)
O34—H324···N24xi0.96 (1)2.20 (3)3.08 (3)151 (3)
O34—H314···N64xi0.96 (1)2.37 (3)3.31 (3)166 (3)
O34—H324···O50.96 (1)3.04 (3)3.57 (3)116 (3)
O35—H325···N250.96 (1)2.17 (3)3.10 (3)162 (3)
O35—H315···N350.96 (1)2.49 (3)3.43 (3)165 (3)
O35—H325···O80.96 (1)3.25 (3)3.61 (3)105 (3)
O36—H326···N260.96 (1)2.30 (3)3.18 (3)152 (3)
O36—H316···N360.96 (1)2.50 (3)3.46 (3)169 (3)
O36—H326···O70.96 (1)3.13 (3)3.53 (3)107 (3)
O37—H327···N270.96 (1)2.23 (3)3.15 (3)161 (3)
O37—H317···N670.97 (1)2.46 (3)3.29 (3)145 (3)
O37—H327···O2xi0.96 (1)3.19 (3)3.55 (3)104 (3)
O38—H328···N280.96 (1)2.26 (3)3.13 (3)150 (3)
O38—H318···N380.97 (1)2.47 (3)3.43 (3)174 (3)
O38—H328···O10.96 (1)3.01 (3)3.51 (3)114 (3)
O41—H411···N42ii0.96 (1)2.12 (3)2.94 (3)142 (3)
O41—H421···O320.96 (1)2.08 (3)2.85 (3)137 (3)
O41—H421···N320.96 (1)2.75 (3)3.17 (3)107 (3)
O42—H412···N410.96 (1)2.26 (3)3.05 (3)138 (3)
O42—H422···O31ii0.96 (1)2.07 (3)2.89 (3)143 (3)
O42—H422···N31ii0.96 (1)2.90 (3)3.25 (3)103 (3)
O43—H413···N530.96 (1)2.16 (3)3.01 (3)146 (3)
O43—H423···O33ii0.97 (1)2.10 (3)2.86 (3)134 (3)
O43—H423···N63ii0.97 (1)2.75 (3)3.23 (3)112 (3)
O44—H414···N470.96 (1)2.11 (3)2.96 (3)145 (3)
O44—H424···O37ii0.96 (1)2.05 (3)2.88 (3)144 (3)
O44—H424···N37ii0.96 (1)2.92 (3)3.32 (3)107 (3)
O45—H415···N550.96 (1)2.16 (3)2.98 (3)142 (3)
O45—H425···O35ii0.96 (1)2.11 (3)2.86 (3)134 (3)
O45—H425···N65ii0.96 (1)2.69 (3)3.23 (3)116 (3)
O46—H416···N56ii0.96 (1)2.10 (3)2.97 (3)149 (3)
O46—H426···O360.96 (1)2.07 (3)2.78 (3)130 (3)
O46—H426···N660.96 (1)2.55 (3)3.13 (3)119 (3)
O47—H427···N44xiii0.96 (1)2.21 (3)2.98 (3)135 (3)
O47—H417···O340.97 (1)2.01 (3)2.83 (3)141 (3)
O47—H417···N34xi0.97 (1)2.75 (3)3.18 (3)108 (3)
O48—H418···O380.96 (1)2.13 (3)2.84 (3)130 (3)
O48—H428···N58ii0.96 (1)2.14 (3)2.96 (3)143 (3)
O48—H418···N680.96 (1)2.53 (3)3.07 (3)116 (3)
Symmetry codes: (ii) x, y+1, z; (iii) x, y1, z; (xi) x+1, y, z; (xiii) x+1, y+1, z.

Experimental details

Crystal data
Chemical formulaBa[Fe(CN)5(NO)]·3H2O
Mr407.32
Crystal system, space groupTriclinic, P1
Temperature (K)20
a, b, c (Å)37.91 (7), 7.694 (7), 8.705 (9)
α, β, γ (°)90.03 (1), 90.086 (7), 90.146 (2)
V3)2539 (6)
Z8
Radiation typeNeutron, λ = 1.54800 Å
µ (mm1)0.16
Crystal size (mm)5.5 × 2.5 × 1.5
Data collection
DiffractometerFour-circle
diffractometer, 6T2 Orphee reactor
Absorption correctionNumerical
(CRYSTAL SHAPE; local program)
Tmin, Tmax0.498, 0.794
No. of measured, independent and
observed [I > 2σ(I)] reflections
3218, 3021, 2676
Rint0.012
θmax (°)55.0
(sin θ/λ)max1)0.529
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.068, 0.072, 3.24
No. of reflections3021
No. of parameters565
No. of restraints72
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)1.06, 0.83

Computer programs: 4c-edi (Person et al., 1995), 4c-edi, COLL5 (Lehmann & Larsen, 1974), SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), CAMERON (Pearce et al., 2000), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O21—H211···N44i0.965 (6)2.27 (3)3.21 (3)163 (3)
O21—H211···N340.965 (6)3.03 (3)3.49 (3)111 (3)
O21—H221···N54i0.967 (6)2.61 (3)3.55 (3)164 (3)
O21—H221···N640.967 (6)2.81 (3)3.36 (3)117 (3)
O22—H212···N43ii0.965 (6)2.51 (3)3.39 (3)152 (3)
O22—H212···N330.965 (6)2.85 (3)3.53 (3)128 (3)
O22—H222···N53ii0.964 (6)2.87 (3)3.51 (3)124 (3)
O22—H222···N630.964 (6)2.58 (3)3.49 (3)157 (3)
O23—H213···N42i0.964 (6)2.34 (3)3.26 (3)158 (3)
O23—H213···N320.964 (6)2.90 (3)3.42 (3)115 (3)
O23—H223···N52i0.963 (6)2.87 (3)3.60 (3)133 (3)
O23—H223···N620.963 (6)2.50 (3)3.38 (3)151 (3)
O24—H214···N41ii0.963 (6)2.51 (3)3.38 (3)151 (3)
O24—H214···N310.963 (6)2.78 (3)3.47 (3)128 (3)
O24—H224···N51ii0.964 (6)2.80 (3)3.43 (3)124 (3)
O24—H224···N610.964 (6)2.61 (3)3.51 (3)157 (3)
O25—H215···N48i0.964 (6)2.65 (3)3.56 (3)158 (3)
O25—H215···N380.964 (6)2.70 (3)3.35 (3)125 (3)
O25—H225···N58i0.965 (6)2.56 (3)3.36 (3)140 (3)
O25—H225···N680.965 (6)2.55 (3)3.30 (3)134 (3)
O26—H216···N47ii0.965 (7)2.76 (3)3.43 (3)128 (3)
O26—H216···N370.965 (7)2.62 (3)3.51 (3)154 (3)
O26—H226···N57ii0.963 (6)2.69 (3)3.47 (3)138 (3)
O26—H226···N670.963 (6)2.63 (3)3.39 (3)136 (3)
O27—H217···N46i0.964 (7)2.63 (3)3.57 (3)167 (3)
O27—H217···N360.964 (7)2.85 (3)3.37 (3)115 (3)
O27—H227···N56i0.964 (7)2.58 (3)3.30 (3)132 (3)
O27—H227···N660.964 (6)2.68 (3)3.49 (3)143 (3)
O28—H218···N45ii0.963 (6)2.51 (3)3.46 (3)168 (3)
O28—H218···N350.963 (6)2.95 (3)3.44 (3)113 (3)
O28—H228···N55ii0.964 (6)2.66 (3)3.43 (3)137 (3)
O28—H228···N650.964 (6)2.63 (3)3.45 (3)143 (3)
O31—H321···N210.963 (6)2.24 (3)3.08 (3)146 (3)
O31—H311···N610.964 (6)2.40 (3)3.24 (3)146 (3)
O31—H321···O40.963 (6)2.98 (3)3.55 (3)119 (3)
O32—H322···N220.965 (6)2.38 (3)3.19 (3)141 (3)
O32—H312···N620.965 (6)2.48 (3)3.33 (3)148 (3)
O32—H322···O30.965 (6)2.92 (3)3.56 (3)125 (3)
O33—H323···N230.963 (6)2.28 (3)3.18 (3)155 (3)
O33—H313···N330.965 (6)2.58 (3)3.45 (3)150 (3)
O33—H323···O60.963 (6)3.10 (3)3.58 (3)113 (3)
O34—H324···N24iii0.964 (6)2.20 (3)3.08 (3)151 (3)
O34—H314···N64iii0.964 (7)2.37 (3)3.31 (3)166 (3)
O34—H324···O50.964 (6)3.04 (3)3.57 (3)116 (3)
O35—H325···N250.963 (6)2.17 (3)3.10 (3)162 (3)
O35—H315···N350.963 (7)2.49 (3)3.43 (3)165 (3)
O35—H325···O80.963 (6)3.25 (3)3.61 (3)105 (3)
O36—H326···N260.964 (6)2.30 (3)3.18 (3)152 (3)
O36—H316···N360.963 (6)2.50 (3)3.46 (3)169 (3)
O36—H326···O70.964 (6)3.13 (3)3.53 (3)107 (3)
O37—H327···N270.964 (6)2.23 (3)3.15 (3)161 (3)
O37—H317···N670.965 (6)2.46 (3)3.29 (3)145 (3)
O37—H327···O2iii0.964 (6)3.19 (3)3.55 (3)104 (3)
O38—H328···N280.963 (6)2.26 (3)3.13 (3)150 (3)
O38—H318···N380.965 (7)2.47 (3)3.43 (3)174 (3)
O38—H328···O10.963 (6)3.01 (3)3.51 (3)114 (3)
O41—H411···N42i0.964 (7)2.12 (3)2.94 (3)142 (3)
O41—H421···O320.962 (6)2.08 (3)2.85 (3)137 (3)
O41—H421···N320.962 (6)2.75 (3)3.17 (3)107 (3)
O42—H412···N410.963 (7)2.26 (3)3.05 (3)138 (3)
O42—H422···O31i0.961 (6)2.07 (3)2.89 (3)143 (3)
O42—H422···N31i0.961 (6)2.90 (3)3.25 (3)103 (3)
O43—H413···N530.964 (7)2.16 (3)3.01 (3)146 (3)
O43—H423···O33i0.966 (6)2.10 (3)2.86 (3)134 (3)
O43—H423···N63i0.966 (6)2.75 (3)3.23 (3)112 (3)
O44—H414···N470.963 (7)2.11 (3)2.96 (3)145 (3)
O44—H424···O37i0.961 (6)2.05 (3)2.88 (3)144 (3)
O44—H424···N37i0.961 (6)2.92 (3)3.32 (3)107 (3)
O45—H415···N550.963 (7)2.16 (3)2.98 (3)142 (3)
O45—H425···O35i0.962 (6)2.11 (3)2.86 (3)134 (3)
O45—H425···N65i0.962 (6)2.69 (3)3.23 (3)116 (3)
O46—H416···N56i0.964 (7)2.10 (3)2.97 (3)149 (3)
O46—H426···O360.961 (6)2.07 (3)2.78 (3)130 (3)
O46—H426···N660.961 (6)2.55 (3)3.13 (3)119 (3)
O47—H427···N44iv0.964 (7)2.21 (3)2.98 (3)135 (3)
O47—H417···O340.965 (6)2.01 (3)2.83 (3)141 (3)
O47—H417···N34iii0.965 (6)2.75 (3)3.18 (3)108 (3)
O48—H418···O380.962 (6)2.13 (3)2.84 (3)130 (3)
O48—H428···N58i0.963 (6)2.14 (3)2.96 (3)143 (3)
O48—H418···N680.963 (6)2.53 (3)3.07 (3)116 (3)
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x+1, y, z; (iv) x+1, y+1, z.
 

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