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The title compound, [La{Fe(CN)6}(C2H5NO2)3(H2O)]2·2H2O, consists of Fe(CN)6 octahedra connected to an eight-coordinate lanthanum via two cyanide bridging La—N—C—Fe links. The La3+ ions are bridged by four glycine molecules, forming a binuclear complex: La—(O—gly—O)4—La. The three-dimensional framework is completed through hydrogen-bonding interactions.
Supporting information
CCDC reference: 183768
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.011 Å
- R factor = 0.056
- wR factor = 0.154
- Data-to-parameter ratio = 12.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
PLAT_420 Alert B D-H Without Acceptor O(8) - H(8G) ?
Alert Level C:
PLAT_420 Alert C D-H Without Acceptor N(8) - H(8E) ?
General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced
by the scaled T values. Since the ratio of scaled T's is
identical to the ratio of reported T values, the scaling does
not imply a change to the absorption corrections used in the
study.
Ratio of Tmax expected/reported 0.649
Tmax scaled 0.577 Tmin scaled 0.552
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: PLATON (Spek, 1990), PARST (Nardelli, 1995) and PARSTCIF (Nardelli, 1991).
Aqua(hexacyano ferrato-
N)bis(µ-glycine)glycinelantanum(III) monohydrate
top
Crystal data top
[LaFe(CN)6(C2H5NO2)3(H2O)]·H2O | Z = 2 |
Mr = 612.12 | F(000) = 602 |
Triclinic, P1 | Dx = 1.928 Mg m−3 |
a = 10.029 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.198 (2) Å | Cell parameters from 25 reflections |
c = 12.233 (2) Å | θ = 10–30° |
α = 74.96 (2)° | µ = 2.75 mm−1 |
β = 88.12 (2)° | T = 293 K |
γ = 61.38 (2)° | Prismatic, red |
V = 1054.5 (3) Å3 | 0.3 × 0.2 × 0.2 mm |
Data collection top
Siemens P3/PC diffractometer | 3270 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.058 |
Graphite monochromator | θmax = 25.0°, θmin = 1.7° |
ω/2θ scans | h = −11→11 |
Absorption correction: ψ scan (North et al., 1968) | k = −11→11 |
Tmin = 0.851, Tmax = 0.890 | l = −14→14 |
7294 measured reflections | 3 standard reflections every 200 reflections |
3656 independent reflections | intensity decay: 4.0% |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.155 | w = 1/[σ2(Fo2) + (0.1095P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.003 |
3656 reflections | Δρmax = 2.58 e Å−3 |
287 parameters | Δρmin = −2.18 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
La | 0.20316 (4) | 0.34117 (4) | 0.45298 (3) | 0.01607 (19) | |
Fe | 0.36441 (11) | 0.78099 (11) | 0.21712 (8) | 0.0213 (3) | |
C1 | 0.4646 (9) | 0.7818 (8) | 0.3498 (6) | 0.0256 (16) | |
C2 | 0.3585 (8) | 0.5963 (9) | 0.3052 (7) | 0.0274 (16) | |
C3 | 0.3653 (9) | 0.9707 (9) | 0.1339 (6) | 0.0299 (17) | |
C4 | 0.5676 (10) | 0.6518 (10) | 0.1774 (7) | 0.0319 (18) | |
C5 | 0.1624 (10) | 0.9054 (9) | 0.2588 (7) | 0.0332 (18) | |
C6 | 0.2737 (10) | 0.7767 (9) | 0.0804 (7) | 0.0328 (18) | |
N1 | 0.5323 (8) | 0.7767 (8) | 0.4261 (6) | 0.0337 (15) | |
N2 | 0.3504 (8) | 0.4910 (8) | 0.3590 (6) | 0.0344 (16) | |
N3 | 0.3667 (10) | 1.0802 (9) | 0.0841 (6) | 0.0444 (19) | |
N4 | 0.6841 (10) | 0.5707 (10) | 0.1561 (7) | 0.049 (2) | |
N5 | 0.0434 (9) | 0.9750 (10) | 0.2833 (9) | 0.058 (2) | |
N6 | 0.2272 (11) | 0.7734 (10) | −0.0019 (7) | 0.054 (2) | |
O1 | −0.0927 (6) | 0.4209 (6) | 0.4778 (4) | 0.0271 (11) | |
O2 | 0.0196 (6) | 0.2743 (7) | 0.3637 (5) | 0.0376 (14) | |
C7 | −0.0902 (8) | 0.3375 (8) | 0.4163 (6) | 0.0235 (15) | |
C8 | −0.2242 (9) | 0.3089 (10) | 0.4099 (8) | 0.0321 (18) | |
H8A | −0.2183 | 0.2317 | 0.4783 | 0.085 (10)* | |
H8B | −0.3192 | 0.4043 | 0.4042 | 0.085 (10)* | |
N7 | −0.2208 (8) | 0.2529 (9) | 0.3083 (7) | 0.0394 (17) | |
H7A | −0.2995 | 0.2359 | 0.3043 | 0.085 (10)* | |
H7B | −0.1339 | 0.1649 | 0.3143 | 0.085 (10)* | |
H7C | −0.2272 | 0.3245 | 0.2457 | 0.085 (10)* | |
O3 | 0.0421 (6) | 0.5634 (6) | 0.2791 (5) | 0.0313 (12) | |
O4 | −0.1620 (6) | 0.7379 (6) | 0.3402 (4) | 0.0317 (12) | |
C9 | −0.0787 (8) | 0.6909 (8) | 0.2666 (6) | 0.0233 (15) | |
C10 | −0.1214 (10) | 0.8004 (9) | 0.1468 (6) | 0.0319 (18) | |
H10A | −0.0415 | 0.8271 | 0.1262 | 0.085 (10)* | |
H10B | −0.1301 | 0.7486 | 0.0934 | 0.085 (10)* | |
N8 | −0.2661 (10) | 0.9422 (8) | 0.1394 (6) | 0.051 (2) | |
H8C | −0.2891 | 1.0047 | 0.0688 | 0.085 (10)* | |
H8D | −0.2577 | 0.9905 | 0.1876 | 0.085 (10)* | |
H8E | −0.3398 | 0.9179 | 0.1573 | 0.085 (10)* | |
O5 | 0.3275 (6) | 0.2399 (6) | 0.2950 (4) | 0.0277 (11) | |
O6 | 0.5752 (6) | 0.1547 (6) | 0.2696 (5) | 0.0306 (12) | |
C11 | 0.4334 (8) | 0.2418 (8) | 0.2386 (6) | 0.0220 (15) | |
C12 | 0.3917 (9) | 0.3619 (9) | 0.1228 (6) | 0.0278 (16) | |
H12A | 0.4260 | 0.4353 | 0.1257 | 0.085 (10)* | |
H12B | 0.4430 | 0.3102 | 0.0656 | 0.085 (10)* | |
N9 | 0.2252 (8) | 0.4459 (9) | 0.0913 (6) | 0.045 (2) | |
H9A | 0.2027 | 0.5154 | 0.0237 | 0.085 (10)* | |
H9B | 0.1783 | 0.4944 | 0.1433 | 0.085 (10)* | |
H9C | 0.1940 | 0.3786 | 0.0877 | 0.085 (10)* | |
O7 | 0.3086 (7) | 0.0481 (6) | 0.5172 (5) | 0.0389 (14) | |
H7D | 0.3356 | 0.0007 | 0.5876 | 0.085 (10)* | |
H7E | 0.3622 | −0.0155 | 0.4798 | 0.085 (10)* | |
O8 | 0.0136 (10) | 0.3221 (10) | 0.1088 (7) | 0.064 (2) | |
H8F | 0.027 (16) | 0.299 (16) | 0.185 (13) | 0.085 (10)* | |
H8G | 0.016 (17) | 0.235 (16) | 0.094 (12) | 0.085 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
La | 0.0123 (3) | 0.0180 (3) | 0.0172 (3) | −0.00685 (19) | 0.00355 (15) | −0.00506 (16) |
Fe | 0.0211 (5) | 0.0210 (5) | 0.0227 (5) | −0.0118 (4) | 0.0019 (4) | −0.0043 (4) |
C1 | 0.023 (4) | 0.021 (4) | 0.026 (4) | −0.007 (3) | 0.005 (3) | −0.005 (3) |
C2 | 0.018 (4) | 0.032 (4) | 0.029 (4) | −0.007 (3) | 0.002 (3) | −0.013 (3) |
C3 | 0.038 (5) | 0.024 (4) | 0.023 (4) | −0.013 (3) | −0.002 (3) | −0.004 (3) |
C4 | 0.036 (5) | 0.036 (5) | 0.027 (4) | −0.021 (4) | 0.007 (3) | −0.009 (3) |
C5 | 0.030 (5) | 0.027 (4) | 0.039 (5) | −0.013 (4) | 0.000 (3) | −0.005 (3) |
C6 | 0.038 (5) | 0.028 (4) | 0.034 (4) | −0.019 (4) | −0.002 (4) | −0.004 (3) |
N1 | 0.027 (3) | 0.042 (4) | 0.030 (4) | −0.015 (3) | 0.000 (3) | −0.010 (3) |
N2 | 0.038 (4) | 0.026 (3) | 0.041 (4) | −0.020 (3) | 0.010 (3) | −0.005 (3) |
N3 | 0.070 (6) | 0.034 (4) | 0.036 (4) | −0.032 (4) | 0.002 (4) | −0.005 (3) |
N4 | 0.038 (5) | 0.055 (5) | 0.043 (4) | −0.015 (4) | 0.014 (4) | −0.013 (4) |
N5 | 0.031 (5) | 0.048 (5) | 0.083 (7) | −0.006 (4) | 0.017 (4) | −0.027 (5) |
N6 | 0.073 (6) | 0.054 (5) | 0.040 (5) | −0.034 (5) | −0.012 (4) | −0.011 (4) |
O1 | 0.029 (3) | 0.031 (3) | 0.029 (3) | −0.019 (2) | 0.009 (2) | −0.013 (2) |
O2 | 0.020 (3) | 0.047 (4) | 0.062 (4) | −0.018 (3) | 0.012 (3) | −0.037 (3) |
C7 | 0.015 (3) | 0.025 (4) | 0.035 (4) | −0.011 (3) | 0.002 (3) | −0.013 (3) |
C8 | 0.025 (4) | 0.036 (4) | 0.048 (5) | −0.020 (4) | 0.012 (3) | −0.022 (4) |
N7 | 0.028 (4) | 0.042 (4) | 0.061 (5) | −0.023 (3) | 0.002 (3) | −0.022 (4) |
O3 | 0.023 (3) | 0.031 (3) | 0.026 (3) | −0.004 (2) | 0.002 (2) | −0.006 (2) |
O4 | 0.030 (3) | 0.032 (3) | 0.024 (3) | −0.011 (2) | 0.008 (2) | −0.004 (2) |
C9 | 0.021 (4) | 0.024 (4) | 0.023 (4) | −0.011 (3) | 0.005 (3) | −0.003 (3) |
C10 | 0.036 (4) | 0.025 (4) | 0.023 (4) | −0.008 (3) | 0.006 (3) | −0.003 (3) |
N8 | 0.053 (5) | 0.035 (4) | 0.029 (4) | 0.006 (4) | 0.003 (3) | −0.007 (3) |
O5 | 0.027 (3) | 0.027 (3) | 0.029 (3) | −0.012 (2) | 0.010 (2) | −0.010 (2) |
O6 | 0.024 (3) | 0.030 (3) | 0.036 (3) | −0.013 (2) | 0.004 (2) | −0.006 (2) |
C11 | 0.014 (3) | 0.026 (4) | 0.028 (4) | −0.008 (3) | 0.003 (3) | −0.015 (3) |
C12 | 0.026 (4) | 0.031 (4) | 0.028 (4) | −0.014 (3) | 0.008 (3) | −0.012 (3) |
N9 | 0.035 (4) | 0.050 (5) | 0.027 (4) | −0.008 (4) | 0.001 (3) | 0.002 (3) |
O7 | 0.054 (4) | 0.029 (3) | 0.029 (3) | −0.017 (3) | 0.007 (3) | −0.008 (2) |
O8 | 0.060 (5) | 0.065 (5) | 0.045 (4) | −0.015 (4) | 0.012 (4) | −0.013 (4) |
Geometric parameters (Å, º) top
La—O1 | 2.705 (7) | N2—C2 | 1.143 (12) |
La—O2 | 2.602 (7) | N3—C3 | 1.131 (12) |
La—O3 | 2.547 (5) | N4—C4 | 1.133 (14) |
La—O5 | 2.450 (5) | N5—C5 | 1.137 (14) |
La—O7 | 2.545 (6) | N6—C6 | 1.138 (13) |
La—N2 | 2.641 (8) | N7—C8 | 1.489 (13) |
La—O1i | 2.502 (5) | N8—C10 | 1.461 (13) |
La—O4i | 2.532 (5) | N9—C12 | 1.474 (13) |
La—N1ii | 2.637 (8) | N7—H7B | 0.8900 |
Fe—C1 | 1.941 (8) | N7—H7C | 0.8902 |
Fe—C2 | 1.939 (9) | N7—H7A | 0.8891 |
Fe—C3 | 1.942 (9) | N8—H8D | 0.8902 |
Fe—C4 | 1.954 (10) | N8—H8C | 0.8901 |
Fe—C5 | 1.944 (10) | N8—H8E | 0.8902 |
Fe—C6 | 1.950 (9) | N9—H9A | 0.8903 |
O1—C7 | 1.265 (9) | N9—H9B | 0.8896 |
O2—C7 | 1.237 (10) | N9—H9C | 0.8902 |
O3—C9 | 1.258 (10) | C7—C8 | 1.514 (14) |
O4—C9 | 1.237 (9) | C9—C10 | 1.520 (11) |
O5—C11 | 1.253 (10) | C11—C12 | 1.525 (10) |
O6—C11 | 1.267 (11) | C8—H8B | 0.9702 |
O7—H7E | 0.8498 | C8—H8A | 0.9693 |
O7—H7D | 0.8498 | C10—H10A | 0.9700 |
O8—H8F | 0.90 (16) | C10—H10B | 0.9697 |
O8—H8G | 0.94 (14) | C12—H12B | 0.9706 |
N1—C1 | 1.148 (11) | C12—H12A | 0.9701 |
| | | |
O1—La—O2 | 48.83 (18) | H7D—O7—H7E | 107.72 |
O1—La—O3 | 72.60 (18) | La—O7—H7D | 118.89 |
O1—La—O5 | 121.50 (19) | La—O7—H7E | 125.92 |
O1—La—O7 | 96.7 (2) | H8F—O8—H8G | 105 (13) |
O1—La—N2 | 135.3 (2) | Laii—N1—C1 | 148.9 (7) |
O1—La—O1i | 73.6 (2) | La—N2—C2 | 154.3 (7) |
O1—La—O4i | 68.21 (18) | C8—N7—H7B | 109.40 |
O1—La—N1ii | 141.22 (19) | H7A—N7—H7B | 109.55 |
O2—La—O3 | 70.6 (2) | C8—N7—H7A | 109.45 |
O2—La—O5 | 74.3 (2) | H7A—N7—H7C | 109.54 |
O2—La—O7 | 71.1 (2) | H7B—N7—H7C | 109.46 |
O2—La—N2 | 131.4 (2) | C8—N7—H7C | 109.43 |
O1i—La—O2 | 119.1 (2) | C10—N8—H8C | 109.50 |
O2—La—O4i | 98.4 (2) | H8C—N8—H8E | 109.44 |
O2—La—N1ii | 144.6 (2) | H8C—N8—H8D | 109.45 |
O3—La—O5 | 77.43 (18) | C10—N8—H8D | 109.51 |
O3—La—O7 | 136.43 (19) | H8D—N8—H8E | 109.43 |
O3—La—N2 | 69.3 (2) | C10—N8—H8E | 109.49 |
O1i—La—O3 | 75.47 (17) | C12—N9—H9A | 109.48 |
O3—La—O4i | 134.73 (19) | C12—N9—H9C | 109.47 |
O3—La—N1ii | 139.1 (2) | C12—N9—H9B | 109.49 |
O5—La—O7 | 72.91 (19) | H9B—N9—H9C | 109.49 |
O5—La—N2 | 71.4 (2) | H9A—N9—H9B | 109.48 |
O1i—La—O5 | 142.54 (18) | H9A—N9—H9C | 109.42 |
O4i—La—O5 | 143.60 (18) | Fe—C1—N1 | 175.8 (8) |
O5—La—N1ii | 92.1 (2) | Fe—C2—N2 | 177.4 (8) |
O7—La—N2 | 127.0 (2) | Fe—C3—N3 | 178.9 (8) |
O1i—La—O7 | 143.28 (18) | Fe—C4—N4 | 176.5 (9) |
O4i—La—O7 | 71.04 (19) | Fe—C5—N5 | 178.1 (9) |
O7—La—N1ii | 73.7 (2) | Fe—C6—N6 | 176.5 (10) |
O1i—La—N2 | 75.1 (2) | O1—C7—C8 | 118.9 (7) |
O4i—La—N2 | 129.4 (2) | O2—C7—C8 | 118.5 (7) |
N1ii—La—N2 | 69.9 (2) | O1—C7—O2 | 122.6 (8) |
O1i—La—O4i | 72.52 (17) | N7—C8—C7 | 109.2 (8) |
O1i—La—N1ii | 91.7 (2) | O3—C9—O4 | 127.8 (7) |
O4i—La—N1ii | 73.2 (2) | O3—C9—C10 | 114.8 (7) |
C1—Fe—C2 | 89.9 (3) | O4—C9—C10 | 117.4 (7) |
C1—Fe—C3 | 88.7 (3) | N8—C10—C9 | 110.9 (7) |
C1—Fe—C4 | 87.6 (4) | O5—C11—O6 | 126.1 (7) |
C1—Fe—C5 | 92.3 (4) | O5—C11—C12 | 118.4 (7) |
C1—Fe—C6 | 177.1 (4) | O6—C11—C12 | 115.5 (7) |
C2—Fe—C3 | 177.4 (3) | N9—C12—C11 | 110.5 (7) |
C2—Fe—C4 | 90.3 (4) | N7—C8—H8B | 109.79 |
C2—Fe—C5 | 88.4 (4) | C7—C8—H8A | 109.85 |
C2—Fe—C6 | 91.0 (4) | C7—C8—H8B | 109.81 |
C3—Fe—C4 | 91.8 (4) | H8A—C8—H8B | 108.31 |
C3—Fe—C5 | 89.5 (4) | N7—C8—H8A | 109.84 |
C3—Fe—C6 | 90.5 (4) | N8—C10—H10B | 109.47 |
C4—Fe—C5 | 178.7 (4) | C9—C10—H10A | 109.48 |
C4—Fe—C6 | 89.6 (4) | N8—C10—H10A | 109.44 |
C5—Fe—C6 | 90.5 (4) | H10A—C10—H10B | 108.08 |
La—O1—C7 | 91.2 (5) | C9—C10—H10B | 109.47 |
La—O1—Lai | 106.4 (2) | N9—C12—H12A | 109.54 |
Lai—O1—C7 | 155.5 (5) | N9—C12—H12B | 109.54 |
La—O2—C7 | 96.8 (5) | C11—C12—H12B | 109.55 |
La—O3—C9 | 133.2 (4) | H12A—C12—H12B | 108.04 |
Lai—O4—C9 | 143.2 (5) | C11—C12—H12A | 109.58 |
La—O5—C11 | 135.9 (5) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N7—H7A···O6iii | 0.89 | 1.91 | 2.771 (11) | 162 |
N7—H7B···N5iv | 0.89 | 2.02 | 2.890 (13) | 164 |
N7—H7C···N4iii | 0.89 | 2.19 | 2.984 (12) | 148 |
O7—H7D···O6v | 0.85 | 1.92 | 2.744 (8) | 164 |
O7—H7E···N1iv | 0.85 | 2.24 | 3.070 (10) | 165 |
N8—H8C···N3vi | 0.89 | 2.54 | 3.045 (11) | 117 |
N8—H8C···N6vi | 0.89 | 2.55 | 3.146 (13) | 125 |
N8—H8D···O6vii | 0.89 | 2.16 | 2.844 (10) | 132 |
O8—H8F···O2 | 0.90 (16) | 2.14 (15) | 3.027 (10) | 170 (14) |
N9—H9A···O8viii | 0.89 | 2.34 | 3.046 (12) | 136 |
N9—H9A···N4ix | 0.89 | 2.60 | 3.155 (11) | 121 |
N9—H9B···O3 | 0.89 | 2.16 | 3.022 (9) | 163 |
N9—H9C···O8 | 0.89 | 2.14 | 2.921 (14) | 147 |
Symmetry codes: (iii) x−1, y, z; (iv) x, y−1, z; (v) −x+1, −y, −z+1; (vi) −x, −y+2, −z; (vii) x−1, y+1, z; (viii) −x, −y+1, −z; (ix) −x+1, −y+1, −z. |
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