Aqua­(hexa­cyano­ferrato-N)­bis(μ-glycine)­glycinelanthanum(III) monohydrate

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.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](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

---

Computing details

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

Crystal data

[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) Å^3	0.3 × 0.2 × 0.2 mm

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.056	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.155	w = 1/[σ^2(Fo^2) + (0.1095P)^2] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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—O1^i	2.502 (5)	N8—C10	1.461 (13)
La—O4^i	2.532 (5)	N9—C12	1.474 (13)
La—N1^ii	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)	La^ii—N1—C1	148.9 (7)
O1—La—O1^i	73.6 (2)	La—N2—C2	154.3 (7)
O1—La—O4^i	68.21 (18)	C8—N7—H7B	109.40
O1—La—N1^ii	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
O1^i—La—O2	119.1 (2)	C10—N8—H8C	109.50
O2—La—O4^i	98.4 (2)	H8C—N8—H8E	109.44
O2—La—N1^ii	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
O1^i—La—O3	75.47 (17)	C12—N9—H9A	109.48
O3—La—O4^i	134.73 (19)	C12—N9—H9C	109.47
O3—La—N1^ii	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
O1^i—La—O5	142.54 (18)	H9A—N9—H9C	109.42
O4^i—La—O5	143.60 (18)	Fe—C1—N1	175.8 (8)
O5—La—N1^ii	92.1 (2)	Fe—C2—N2	177.4 (8)
O7—La—N2	127.0 (2)	Fe—C3—N3	178.9 (8)
O1^i—La—O7	143.28 (18)	Fe—C4—N4	176.5 (9)
O4^i—La—O7	71.04 (19)	Fe—C5—N5	178.1 (9)
O7—La—N1^ii	73.7 (2)	Fe—C6—N6	176.5 (10)
O1^i—La—N2	75.1 (2)	O1—C7—C8	118.9 (7)
O4^i—La—N2	129.4 (2)	O2—C7—C8	118.5 (7)
N1^ii—La—N2	69.9 (2)	O1—C7—O2	122.6 (8)
O1^i—La—O4^i	72.52 (17)	N7—C8—C7	109.2 (8)
O1^i—La—N1^ii	91.7 (2)	O3—C9—O4	127.8 (7)
O4^i—La—N1^ii	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—La^i	106.4 (2)	N9—C12—H12A	109.54
La^i—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
La^i—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)

D—H···A	D—H	H···A	D···A	D—H···A
N7—H7A···O6^iii	0.89	1.91	2.771 (11)	162
N7—H7B···N5^iv	0.89	2.02	2.890 (13)	164
N7—H7C···N4^iii	0.89	2.19	2.984 (12)	148
O7—H7D···O6^v	0.85	1.92	2.744 (8)	164
O7—H7E···N1^iv	0.85	2.24	3.070 (10)	165
N8—H8C···N3^vi	0.89	2.54	3.045 (11)	117
N8—H8C···N6^vi	0.89	2.55	3.146 (13)	125
N8—H8D···O6^vii	0.89	2.16	2.844 (10)	132
O8—H8F···O2	0.90 (16)	2.14 (15)	3.027 (10)	170 (14)
N9—H9A···O8^viii	0.89	2.34	3.046 (12)	136
N9—H9A···N4^ix	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.