Literature DB >> 21588108

catena-poly[[[(2,2'-bipyridine-2κN,N')-μ-cyanido-1:2κN:C-cyanido-2κC-tris-(methanol-1κO)(nitrato-1κO,O')iron(II)yttrium(III)]-di-μ-cyanido-1:2'κN:C;2:1'κC:N] methanol solvate hemihydrate].

Yan Xu, He-Qing Shu, Xiao-Ping Shen.   

Abstract

The title complex, {[Fe(II)Y(III)(CN)(4)(NO(3))(C(10)H(8)N(2))(CH(3)OH)(3)]·CH(3)OH·0.5H(2)O}(n), is built up of ladder-like chains oriented along the c axis. Each ladder consists of two strands based on alternating Fe(II) and Y(III) ions connected by cyanide bridges. Two such parallel chains are connected by additional cyanide anions (the 'rungs' of the ladder), which likewise connect Fe(II) and Y(III) ions, such that each [Fe(bipy)(CN)(4)](2-) (bipy is 2,2'-bipyridine) unit coordinates with three Y(III) ions and each Y(III) ion connects with three different [Fe(bipy)(CN)(4)](2-) units. The Fe(II) atom is six-coordinated in a distorted octa-hedral geometry and the Y(III) atom cation is eight-coordinated in a distorted dodeca-hedral environment. The uncoordinated methanol solvent mol-ecules are involved in hydrogen-bonding inter-actions with the one terminal cyanide group and a coordinated methanol mol-ecule from another [Y(III)(NO(3))(CH(3)OH)(3)](2+) unit. Adjacent ladder-like chains are also held together by hydrogen bonds between the terminal cyanide ligands of the [Fe(CN)(4)(bipy)](2-) units in one chain and the OH donors of CH(3)OH ligands from [Y(III)(NO(3))(CH(3)OH)(3)] units in neighboring chains. The water molecule exhibits half-occupation.

Entities:  

Year:  2010        PMID： 21588108      PMCID： PMC3007586          DOI： 10.1107/S1600536810029843

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background to the design, synthesis and properties of mixed rare earth–transition metal complexes, see: Wilson et al. (2009 ▶); Zhou et al. (2002 ▶); Li et al. (2008 ▶); Karan et al. (2002 ▶); Sokol et al. (2002 ▶); Toma et al. (2003 ▶); Xu et al. (2009 ▶). For related structures, see: Baca et al. (2007 ▶); Liu et al. (2008 ▶); Yuan et al. (2004 ▶).

Experimental

Crystal data

[FeY(CN)4(NO3)(C10H8N2)(CH4O)3]·CH4O·0.5H2O M = 604.21 Monoclinic, a = 12.803 (3) Å b = 18.132 (4) Å c = 10.728 (2) Å β = 103.439 (3)° V = 2422.2 (9) Å3 Z = 4 Mo Kα radiation μ = 3.04 mm−1 T = 173 K 0.26 × 0.22 × 0.20 mm

Data collection

Bruker SMART APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T min = 0.46, T max = 0.55 18891 measured reflections 4760 independent reflections 3490 reflections with I > 2σ(I) R int = 0.067

Refinement

R[F 2 > 2σ(F 2)] = 0.052 wR(F 2) = 0.107 S = 1.07 4760 reflections 316 parameters H-atom parameters constrained Δρmax = 0.49 e Å−3 Δρmin = −0.57 e Å−3 Data collection: SMART (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810029843/nc2192sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810029843/nc2192Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[FeY(CN)4(NO3)(C10H8N2)(CH4O)3]·CH4O·0.5H2OF(000) = 1228
Mr = 604.21Dx = 1.657 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 838 reflections
a = 12.803 (3) Åθ = 3.0–23.5°
b = 18.132 (4) ŵ = 3.04 mm−1
c = 10.728 (2) ÅT = 173 K
β = 103.439 (3)°Prism, red brown
V = 2422.2 (9) Å30.26 × 0.22 × 0.20 mm
Z = 4
Bruker SMART APEX CCD diffractometer4760 independent reflections
Radiation source: sealed tube3490 reflections with I > 2σ(I)
graphiteRint = 0.067
phi and ω scansθmax = 26.0°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2002)h = −14→15
Tmin = 0.46, Tmax = 0.55k = −22→22
18891 measured reflectionsl = −13→12
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.0481P)2] where P = (Fo2 + 2Fc2)/3
4760 reflections(Δ/σ)max < 0.001
316 parametersΔρmax = 0.49 e Å−3
0 restraintsΔρmin = −0.57 e Å−3
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.
xyzUiso*/UeqOcc. (<1)
C10.7345 (4)−0.1231 (2)0.3081 (4)0.0385 (10)
H10.6595−0.12590.30290.046*
C20.7916 (4)−0.1886 (2)0.3052 (4)0.0347 (10)
H20.7570−0.23530.29750.042*
C30.9033 (4)−0.1825 (3)0.3155 (4)0.0394 (10)
H30.9455−0.22580.31740.047*
C40.9530 (4)−0.1133 (3)0.3213 (4)0.0419 (11)
H41.0277−0.10890.32570.050*
C50.8893 (3)−0.0504 (3)0.3225 (5)0.0391 (10)
C60.9318 (3)0.0236 (3)0.3317 (4)0.0384 (10)
C71.0374 (4)0.0395 (3)0.3333 (5)0.0452 (11)
H71.08580.00140.32380.054*
C81.0714 (3)0.1123 (2)0.3497 (4)0.0348 (10)
H81.14390.12410.35040.042*
C91.0006 (3)0.1689 (3)0.3651 (4)0.0354 (10)
H91.02400.21850.37900.042*
C100.8930 (3)0.1483 (2)0.3587 (4)0.0281 (8)
H100.84230.18530.36630.034*
C110.7170 (3)0.0426 (2)0.4978 (4)0.0363 (10)
C120.5697 (3)0.0028 (2)0.2858 (4)0.0363 (10)
C130.6951 (3)0.0482 (2)0.1340 (4)0.0298 (9)
C140.6443 (3)0.1349 (3)0.3103 (4)0.0385 (10)
C150.8118 (4)−0.0835 (3)0.9317 (4)0.0427 (11)
H15A0.8576−0.04700.98590.064*
H15B0.8564−0.11630.89330.064*
H15C0.7734−0.11240.98400.064*
C160.7459 (4)0.2236 (3)0.6177 (4)0.0390 (10)
H16A0.81810.21520.67120.059*
H16B0.73190.27670.60940.059*
H16C0.74080.20220.53260.059*
C170.4893 (4)0.1450 (3)0.9517 (5)0.0429 (11)
H17A0.49070.09160.96600.064*
H17B0.41550.16080.91390.064*
H17C0.51580.17041.03360.064*
C180.4471 (3)0.1056 (3)0.4540 (4)0.0385 (10)
H18A0.41350.13430.50890.058*
H18B0.43070.05440.46170.058*
H18C0.52350.11250.47850.058*
Fe10.70769 (5)0.04235 (3)0.31568 (6)0.03166 (16)
N10.7825 (3)−0.05414 (19)0.3170 (4)0.0338 (8)
N20.8605 (3)0.07728 (19)0.3405 (3)0.0307 (7)
N30.7168 (3)0.0475 (2)0.6043 (4)0.0364 (8)
N40.4832 (3)−0.0227 (2)0.2667 (4)0.0394 (9)
N50.6896 (3)0.05129 (18)0.0266 (4)0.0339 (8)
N60.6040 (3)0.1931 (2)0.3041 (4)0.0385 (9)
N70.8853 (3)0.1436 (2)0.9291 (3)0.0354 (8)
O10.8747 (2)0.08407 (17)0.8686 (3)0.0398 (7)
O20.7993 (2)0.17623 (15)0.9284 (3)0.0367 (7)
O30.9709 (2)0.16875 (16)0.9851 (3)0.0399 (7)
O40.7341 (2)−0.04552 (16)0.8312 (3)0.0361 (7)
H4A0.6659−0.07240.82530.054*
O50.6676 (2)0.18859 (16)0.6775 (3)0.0379 (7)
H5A0.64520.22800.72970.057*
O60.5579 (2)0.16346 (17)0.8642 (3)0.0354 (7)
H6A0.59930.20770.90020.053*
O70.4061 (2)0.12975 (17)0.3204 (3)0.0408 (7)
H7B0.45820.14510.29070.061*
O80.3088 (5)0.2478 (4)0.4772 (7)0.0489 (17)0.50
H8B0.24470.23220.46700.073*0.50
H8C0.33180.26220.55400.073*0.50
Y10.68339 (3)0.08045 (2)0.80828 (4)0.03110 (12)
U11U22U33U12U13U23
C10.040 (2)0.028 (2)0.045 (3)−0.0085 (19)0.005 (2)0.0008 (19)
C20.044 (2)0.033 (2)0.028 (2)−0.0147 (19)0.0103 (18)−0.0087 (17)
C30.039 (2)0.037 (2)0.042 (3)−0.0070 (19)0.0076 (19)−0.003 (2)
C40.051 (3)0.035 (2)0.043 (3)−0.009 (2)0.017 (2)−0.002 (2)
C50.030 (2)0.043 (3)0.046 (3)0.0014 (19)0.0119 (19)0.001 (2)
C60.029 (2)0.048 (3)0.039 (3)−0.0038 (19)0.0103 (18)−0.003 (2)
C70.041 (3)0.050 (3)0.044 (3)−0.003 (2)0.008 (2)0.002 (2)
C80.036 (2)0.038 (2)0.036 (2)−0.0024 (18)0.0191 (18)0.0030 (19)
C90.036 (2)0.043 (3)0.029 (2)0.0085 (19)0.0124 (17)−0.0080 (19)
C100.034 (2)0.027 (2)0.0260 (19)0.0081 (16)0.0131 (16)0.0043 (16)
C110.036 (2)0.033 (2)0.038 (3)−0.0010 (19)0.0049 (19)0.001 (2)
C120.028 (2)0.031 (2)0.045 (3)−0.0038 (18)−0.0014 (19)−0.0016 (19)
C130.027 (2)0.029 (2)0.032 (2)−0.0095 (16)0.0043 (17)0.0037 (17)
C140.033 (2)0.042 (3)0.046 (3)0.0122 (19)0.0193 (19)−0.002 (2)
C150.034 (2)0.044 (3)0.040 (3)−0.013 (2)−0.0127 (19)−0.001 (2)
C160.037 (2)0.041 (3)0.042 (3)0.003 (2)0.015 (2)−0.010 (2)
C170.041 (3)0.038 (3)0.054 (3)0.011 (2)0.018 (2)0.019 (2)
C180.034 (2)0.037 (2)0.044 (3)−0.0078 (18)0.009 (2)0.008 (2)
Fe10.0315 (3)0.0311 (3)0.0327 (3)−0.0019 (2)0.0080 (2)−0.0011 (2)
N10.0317 (19)0.0258 (18)0.045 (2)−0.0048 (14)0.0115 (16)−0.0053 (15)
N20.0281 (17)0.0279 (18)0.0366 (19)−0.0061 (14)0.0088 (14)0.0024 (15)
N30.0317 (19)0.041 (2)0.040 (2)−0.0017 (15)0.0149 (16)0.0024 (17)
N40.037 (2)0.035 (2)0.045 (2)0.0037 (16)0.0059 (17)−0.0022 (17)
N50.0308 (19)0.0293 (19)0.043 (2)−0.0113 (15)0.0113 (16)0.0014 (16)
N60.036 (2)0.034 (2)0.047 (2)0.0065 (16)0.0133 (17)−0.0072 (17)
N70.0316 (19)0.044 (2)0.0310 (19)0.0007 (16)0.0075 (15)−0.0157 (17)
O10.0346 (16)0.0331 (17)0.0493 (19)0.0044 (13)0.0050 (14)−0.0012 (14)
O20.0293 (16)0.0297 (16)0.0476 (19)−0.0013 (13)0.0014 (13)0.0034 (13)
O30.0343 (17)0.0299 (16)0.0509 (19)−0.0084 (13)0.0004 (14)0.0013 (14)
O40.0432 (17)0.0295 (15)0.0309 (16)−0.0158 (13)−0.0010 (13)−0.0060 (12)
O50.0487 (18)0.0341 (17)0.0327 (16)−0.0156 (14)0.0128 (13)−0.0033 (13)
O60.0306 (16)0.0370 (17)0.0412 (17)−0.0026 (12)0.0137 (13)0.0023 (13)
O70.0412 (18)0.0439 (19)0.0346 (17)−0.0068 (14)0.0034 (13)0.0051 (14)
O80.041 (4)0.045 (4)0.058 (4)0.012 (3)0.006 (3)−0.001 (3)
Y10.0295 (2)0.0324 (2)0.0303 (2)−0.00059 (17)0.00460 (15)0.00014 (17)
C1—N11.386 (5)C16—H16A0.9799
C1—C21.399 (6)C16—H16B0.9800
C1—H10.9500C16—H16C0.9800
C2—C31.413 (6)C17—O61.465 (5)
C2—H20.9500C17—H17A0.9799
C3—C41.402 (6)C17—H17B0.9800
C3—H30.9500C17—H17C0.9799
C4—C51.404 (6)C18—O71.474 (5)
C4—H40.9502C18—H18A0.9599
C5—N11.356 (6)C18—H18B0.9600
C5—C61.442 (6)C18—H18C0.9600
C6—N21.353 (6)Fe1—N11.993 (4)
C6—C71.379 (6)Fe1—N22.015 (3)
C7—C81.387 (7)N3—Y12.401 (4)
C7—H70.9500N4—Y1i2.344 (4)
C8—C91.405 (6)N5—Y1ii2.384 (4)
C8—H80.9500N7—O31.210 (4)
C9—C101.413 (6)N7—O21.248 (4)
C9—H90.9500N7—O11.251 (4)
C10—N21.353 (5)N7—Y12.849 (4)
C10—H100.9500O1—Y12.384 (3)
C11—N31.146 (6)O2—Y12.448 (3)
C11—Fe11.930 (5)O4—Y12.372 (3)
C12—N41.173 (5)O4—H4A0.9900
C12—Fe11.865 (4)O5—Y12.392 (3)
C13—N51.140 (5)O5—H5A0.9900
C13—Fe11.921 (4)O6—Y12.378 (3)
C14—N61.169 (5)O6—H6A0.9901
C14—Fe11.860 (4)O7—H7B0.8501
C15—O41.459 (5)O8—H8B0.8499
C15—H15A0.9801O8—H8C0.8500
C15—H15B0.9800Y1—N4i2.344 (4)
C15—H15C0.9800Y1—N5iii2.384 (4)
C16—O51.455 (5)
N1—C1—C2122.8 (4)C12—Fe1—N2175.02 (17)
N1—C1—H1118.7C13—Fe1—N288.11 (15)
C2—C1—H1118.5C11—Fe1—N292.05 (16)
C1—C2—C3117.2 (4)N1—Fe1—N279.90 (14)
C1—C2—H2121.6C5—N1—C1118.3 (4)
C3—C2—H2121.2C5—N1—Fe1115.7 (3)
C4—C3—C2120.9 (4)C1—N1—Fe1125.9 (3)
C4—C3—H3119.3C6—N2—C10120.4 (3)
C2—C3—H3119.9C6—N2—Fe1114.5 (3)
C3—C4—C5118.0 (4)C10—N2—Fe1125.1 (3)
C3—C4—H4121.3C11—N3—Y1165.9 (4)
C5—C4—H4120.7C12—N4—Y1i169.3 (4)
N1—C5—C4122.7 (4)C13—N5—Y1ii169.9 (3)
N1—C5—C6114.2 (4)O3—N7—O2121.4 (4)
C4—C5—C6123.1 (4)O3—N7—O1124.0 (4)
N2—C6—C7121.6 (4)O2—N7—O1114.6 (3)
N2—C6—C5115.1 (4)O3—N7—Y1177.2 (3)
C7—C6—C5123.3 (4)O2—N7—Y158.8 (2)
C6—C7—C8118.6 (5)O1—N7—Y155.87 (19)
C6—C7—H7120.5N7—O1—Y198.4 (2)
C8—C7—H7120.9N7—O2—Y195.3 (2)
C7—C8—C9121.1 (4)C15—O4—Y1130.8 (2)
C7—C8—H8119.5C15—O4—H4A104.8
C9—C8—H8119.3Y1—O4—H4A104.6
C8—C9—C10116.8 (4)C16—O5—Y1130.0 (3)
C8—C9—H9121.5C16—O5—H5A104.7
C10—C9—H9121.7Y1—O5—H5A104.8
N2—C10—C9121.4 (4)C17—O6—Y1123.9 (2)
N2—C10—H10119.5C17—O6—H6A106.4
C9—C10—H10119.1Y1—O6—H6A106.2
N3—C11—Fe1174.3 (4)C18—O7—H7B109.2
N4—C12—Fe1179.4 (4)H8B—O8—H8C109.5
N5—C13—Fe1178.7 (4)N4i—Y1—O479.10 (11)
N6—C14—Fe1178.6 (4)N4i—Y1—O675.80 (12)
O4—C15—H15A109.3O4—Y1—O6140.19 (10)
O4—C15—H15B109.9N4i—Y1—N5iii93.33 (12)
H15A—C15—H15B109.5O4—Y1—N5iii74.86 (11)
O4—C15—H15C109.2O6—Y1—N5iii76.29 (11)
H15A—C15—H15C109.5N4i—Y1—O1154.27 (12)
H15B—C15—H15C109.5O4—Y1—O176.06 (10)
O5—C16—H16A109.1O6—Y1—O1128.74 (11)
O5—C16—H16B109.8N5iii—Y1—O186.64 (12)
H16A—C16—H16B109.5N4i—Y1—O5102.62 (12)
O5—C16—H16C109.5O4—Y1—O5146.51 (11)
H16A—C16—H16C109.5O6—Y1—O570.07 (10)
H16B—C16—H16C109.5N5iii—Y1—O5137.47 (11)
O6—C17—H17A109.6O1—Y1—O594.49 (11)
O6—C17—H17B109.4N4i—Y1—N385.22 (13)
H17A—C17—H17B109.5O4—Y1—N375.66 (12)
O6—C17—H17C109.4O6—Y1—N3131.40 (11)
H17A—C17—H17C109.5N5iii—Y1—N3150.21 (13)
H17B—C17—H17C109.5O1—Y1—N382.26 (12)
O7—C18—H18A109.0O5—Y1—N371.22 (12)
O7—C18—H18B109.6N4i—Y1—O2152.81 (12)
H18A—C18—H18B109.5O4—Y1—O2120.72 (10)
O7—C18—H18C109.8O6—Y1—O277.33 (10)
H18A—C18—H18C109.5N5iii—Y1—O276.24 (11)
H18B—C18—H18C109.5O1—Y1—O251.58 (10)
C14—Fe1—C1287.3 (2)O5—Y1—O271.68 (10)
C14—Fe1—C1389.19 (19)N3—Y1—O2116.23 (11)
C12—Fe1—C1389.64 (18)N4i—Y1—N7173.07 (12)
C14—Fe1—C1187.33 (19)O4—Y1—N798.20 (10)
C12—Fe1—C1190.5 (2)O6—Y1—N7103.03 (10)
C13—Fe1—C11176.51 (19)N5iii—Y1—N779.78 (11)
C14—Fe1—N1176.55 (18)O1—Y1—N725.75 (10)
C12—Fe1—N195.62 (17)O5—Y1—N783.18 (11)
C13—Fe1—N188.99 (17)N3—Y1—N7100.36 (11)
C11—Fe1—N194.48 (17)O2—Y1—N725.85 (9)
C14—Fe1—N297.11 (18)
D—H···AD—HH···AD···AD—H···A
O5—H5A···N6iv0.991.782.762 (5)172
O7—H7B···N60.852.032.823 (5)154
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H5A⋯N6i0.991.782.762 (5)172
O7—H7B⋯N60.852.032.823 (5)154

Symmetry code: (i) .

  7 in total

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2.  Water-free rare earth-Prussian blue type analogues: synthesis, structure, computational analysis, and magnetic data of {Ln(III)(DMF)(6)Fe(III)(CN)(6)}(infinity) (Ln = rare earths excluding Pm).

Authors:  Duane C Wilson; Shengming Liu; Xuenian Chen; Edward A Meyers; Xiaoguang Bao; Andrey V Prosvirin; Kim R Dunbar; Christopher M Hadad; Sheldon G Shore
Journal:  Inorg Chem       Date:  2009-07-06       Impact factor: 5.165

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Tetraaqua-1kappa4O-bis(epsilon -caprolactam-1kappa O)-mu-cyano-1:2kappa 2N:C-pentacyano-2kappa 5C-iron(III)yttrium(III), a novel cyano-bridged dinuclear complex.

Authors:  Bei Chuan Zhou; Hui Zhong Kou; Yi He; Ming Xiong; Ru Ji Wang; Yadong Li
Journal:  Acta Crystallogr C       Date:  2002-08-21       Impact factor: 1.172

5.  Cyanide-bridged Fe(III)-Co(II) bis double zigzag chains with a slow relaxation of the magnetisation.

Authors:  Luminita Marilena Toma; Rodrigue Lescouëzec; Francesc Lloret; Miguel Julve; Jacqueline Vaissermann; Michel Verdaguer
Journal:  Chem Commun (Camb)       Date:  2003-08-07       Impact factor: 6.222

6.  A cyanide-bridged Fe(II)-Nd(III) bimetallic assembly with a one-dimensional ladder-like chain structure.

Authors:  Yan Xu; Hu Zhou; Ai-Hua Yuan; Xiao-Ping Shen; Qian Zhang
Journal:  Acta Crystallogr C       Date:  2009-04-10       Impact factor: 1.172

7.  Three-component coordination networks based on [Ru(phen)(CN)4(2-) anions, near-infrared luminescent lanthanide(III) cations, and ancillary oligopyridine ligands: structures and photophysical properties.

Authors:  Svetlana G Baca; Harry Adams; Daniel Sykes; Stephen Faulkner; Michael D Ward
Journal:  Dalton Trans       Date:  2007-06-21       Impact factor: 4.390
  7 in total

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