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In the title compound, [Tb(C2H4N4)2(H2O)6]Cl3, the coord­ination of the terbium(III) ion is a square-antiprismatic arrangement by six O atoms and two monodentate cyano­guanidine (cnge) mol­ecules forming covalent Tb-N bonds of 2.446 (4) Å through their nitrile N atoms. The crystal structure consists of metal ion layers separated by the organic mol­ecules along the a axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803025509/bt6375sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803025509/bt6375Isup2.hkl
Contains datablock I

CCDC reference: 227748

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](N-C) = 0.007 Å
  • R factor = 0.022
  • wR factor = 0.055
  • Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Tb PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.10 PLAT420_ALERT_2_C D-H Without Acceptor N4 - H42 ... ? PLAT731_ALERT_1_C Bond Calc 0.82(5), Rep 0.82(2) ...... 2.50 su-Rat O1 -H12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.82(6), Rep 0.82(2) ...... 3.00 su-Rat O2 -H22 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat O3 -H31 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat O3 -H32 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(6), Rep 0.85(2) ...... 3.00 su-Rat N4 -H42 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.82(5), Rep 0.82(2) ...... 2.50 su-Rat O1 -H12 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.82(6), Rep 0.82(2) ...... 3.00 su-Rat O2 -H22 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat O3 -H31 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat O3 -H32 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(6), Rep 0.85(2) ...... 3.00 su-Rat N4 -H42 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.31(6), Rep 2.31(2) ...... 3.00 su-Rat H31 -CL1 1.555 8.544 PLAT736_ALERT_1_C H...A Calc 2.23(5), Rep 2.23(2) ...... 2.50 su-Rat H32 -CL1 1.555 1.555
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.29 From the CIF: _reflns_number_total 2185 Count of symmetry unique reflns 1203 Completeness (_total/calc) 181.63% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 982 Fraction of Friedel pairs measured 0.816 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 13 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL.

Hexaaquabis(dicyanoguanidine)terbium(III) trichloride top
Crystal data top
[Tb(C2H4N4)2(H2O)6]·Cl3F(000) = 2112
Mr = 541.55Dx = 1.928 Mg m3
Orthorhombic, Fdd2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: F 2 -2dCell parameters from 6486 reflections
a = 29.425 (5) Åθ = 2.7–28.3°
b = 9.2613 (14) ŵ = 4.26 mm1
c = 13.690 (2) ÅT = 293 K
V = 3730.6 (10) Å3Prism, colourless
Z = 80.31 × 0.08 × 0.05 mm
Data collection top
Bruker AXS APEX CCD
diffractometer
2185 independent reflections
Radiation source: fine-focus sealed tube2065 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 28.3°, θmin = 2.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 3939
Tmin = 0.290, Tmax = 0.808k = 128
6486 measured reflectionsl = 1817
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.022 w = 1/[σ2(Fo2) + (0.0315P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max < 0.001
S = 1.10Δρmax = 0.43 e Å3
2185 reflectionsΔρmin = 0.60 e Å3
142 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
11 restraintsExtinction coefficient: 0.00174 (7)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.030 (13)
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.

PLAT731 Type_1 Test for consistency of Bond su's and Coordinate su's in CIF A large ratio of the reported and calculated bond s.u.'s is found. The use of a DFIX instruction might cause such a warning since calculated s.u.'s are based on reported variances only. Note_1: su's on the unitcell dimensions are taken into account in the calculation of expected su's. This may result in large differences between expected and reported su's when this contribution is not included in the reported su's, in particular for inaccurate unitcells. Note_2: Another source for the discrepancy between calculated and reported su's can be that the validation software has access only to the variances of the refined parameters as opposed to the full co-variance matrix used by e.g. SHELXL for the calculation of derived parameters with associated su's. Constrained/restrained refinement may cause largei co-variances.

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
xyzUiso*/Ueq
Tb0.00000.00000.10089 (3)0.01999 (9)
Cl10.16603 (4)0.02478 (13)0.12593 (7)0.0356 (2)
Cl20.00000.50000.1976 (2)0.0492 (5)
O10.04611 (10)0.1990 (3)0.1609 (2)0.0318 (6)
H110.0568 (18)0.199 (7)0.216 (2)0.048 (16)*
H120.032 (2)0.275 (5)0.155 (6)0.07 (2)*
O20.00361 (10)0.1841 (5)0.0176 (3)0.0485 (11)
H210.0287 (11)0.214 (6)0.033 (4)0.042 (16)*
H220.016 (2)0.200 (9)0.059 (5)0.07 (2)*
O30.07309 (11)0.0297 (4)0.0302 (3)0.0350 (7)
H310.079 (2)0.092 (6)0.010 (4)0.059 (18)*
H320.0965 (15)0.026 (7)0.062 (5)0.06 (2)*
C10.06201 (13)0.1393 (5)0.3052 (3)0.0287 (8)
C20.12159 (13)0.1881 (4)0.4076 (3)0.0285 (8)
N10.04525 (11)0.1007 (4)0.2344 (3)0.0354 (8)
N20.07682 (12)0.1836 (5)0.3896 (3)0.0358 (8)
N30.15310 (12)0.1520 (5)0.3449 (3)0.0439 (10)
H330.1797 (9)0.156 (5)0.369 (4)0.039 (14)*
H340.1485 (19)0.120 (6)0.287 (2)0.050 (16)*
N40.13413 (16)0.2305 (5)0.4966 (4)0.0440 (11)
H410.1621 (10)0.254 (6)0.507 (7)0.06 (2)*
H420.116 (2)0.232 (6)0.545 (4)0.05 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb0.01711 (11)0.02478 (12)0.01808 (12)0.00021 (10)0.0000.000
Cl10.0266 (5)0.0518 (6)0.0284 (6)0.0048 (4)0.0025 (3)0.0053 (5)
Cl20.0298 (8)0.0351 (9)0.0825 (16)0.0034 (6)0.0000.000
O10.0363 (16)0.0269 (15)0.0322 (16)0.0005 (12)0.0099 (13)0.0014 (13)
O20.0232 (16)0.073 (3)0.050 (2)0.0123 (16)0.0092 (14)0.037 (2)
O30.0196 (14)0.0504 (19)0.0352 (18)0.0024 (13)0.0000 (12)0.0114 (15)
C10.0239 (18)0.031 (2)0.031 (2)0.0048 (15)0.0011 (15)0.0074 (16)
C20.0295 (19)0.0258 (18)0.0301 (19)0.0023 (15)0.0072 (15)0.0067 (16)
N10.0309 (17)0.040 (2)0.0353 (19)0.0024 (15)0.0085 (15)0.0104 (16)
N20.0291 (18)0.046 (2)0.033 (2)0.0032 (15)0.0023 (14)0.0156 (18)
N30.0256 (17)0.064 (3)0.042 (2)0.0072 (17)0.0039 (17)0.018 (2)
N40.035 (2)0.055 (3)0.042 (3)0.0040 (18)0.0104 (19)0.0144 (19)
Geometric parameters (Å, º) top
Tb—O12.432 (3)O3—H310.81 (2)
Tb—O1i2.432 (3)O3—H320.81 (2)
Tb—O22.356 (4)C1—N11.145 (5)
Tb—O2i2.356 (4)C1—N21.301 (5)
Tb—O32.374 (3)C2—N21.341 (5)
Tb—O3i2.374 (3)C2—N31.307 (5)
Tb—N12.446 (4)C2—N41.332 (6)
Tb—N1i2.446 (4)N3—H330.853 (19)
O1—H110.82 (2)N3—H340.86 (2)
O1—H120.82 (2)N4—H410.86 (2)
O2—H210.82 (2)N4—H420.85 (2)
O2—H220.82 (2)
O2i—Tb—O293.0 (3)O1—Tb—N1i76.24 (11)
O2i—Tb—O3i76.25 (13)O1i—Tb—N1i74.50 (11)
O2—Tb—O3i71.12 (11)N1—Tb—N1i83.32 (19)
O2i—Tb—O371.12 (11)Tb—O1—H11122 (4)
O2—Tb—O376.25 (13)Tb—O1—H12110 (6)
O3i—Tb—O3131.88 (17)H11—O1—H12107 (7)
O2i—Tb—O1143.75 (11)Tb—O2—H21118 (4)
O2—Tb—O170.06 (13)Tb—O2—H22125 (6)
O3i—Tb—O1123.74 (12)H21—O2—H22113 (8)
O3—Tb—O173.75 (12)Tb—O3—H31123 (4)
O2i—Tb—O1i70.06 (13)Tb—O3—H32123 (5)
O2—Tb—O1i143.75 (12)H31—O3—H32102 (6)
O3i—Tb—O1i73.75 (12)N1—C1—N2174.0 (4)
O3—Tb—O1i123.74 (12)N3—C2—N4118.7 (4)
O1—Tb—O1i140.49 (16)N3—C2—N2124.6 (4)
O2i—Tb—N1105.24 (16)N4—C2—N2116.7 (4)
O2—Tb—N1139.99 (12)C1—N1—Tb170.5 (4)
O3i—Tb—N1147.33 (12)C1—N2—C2120.2 (4)
O3—Tb—N176.55 (13)C2—N3—H33113 (4)
O1—Tb—N174.50 (11)C2—N3—H34126 (4)
O1i—Tb—N176.24 (11)H33—N3—H34121 (5)
O2i—Tb—N1i139.99 (12)C2—N4—H41119 (6)
O2—Tb—N1i105.24 (16)C2—N4—H42123 (5)
O3i—Tb—N1i76.55 (13)H41—N4—H42117 (8)
O3—Tb—N1i147.33 (12)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···Cl1ii0.82 (2)2.34 (2)3.156 (3)174 (6)
O1—H12···Cl20.82 (2)2.36 (3)3.141 (3)159 (8)
O2—H21···N2iii0.82 (2)2.00 (3)2.785 (5)160 (6)
O2—H22···Cl1iv0.82 (2)2.29 (4)3.077 (3)159 (8)
O3—H31···Cl1v0.81 (2)2.31 (2)3.117 (4)172 (6)
O3—H32···Cl10.81 (2)2.23 (2)3.033 (3)171 (7)
N3—H33···Cl2vi0.85 (2)2.49 (2)3.306 (4)161 (4)
N3—H34···Cl10.86 (2)2.43 (3)3.243 (5)159 (5)
N4—H41···Cl2vi0.86 (2)2.71 (5)3.480 (5)149 (7)
N4—H42···O1vii0.85 (2)2.67 (3)3.492 (6)161 (6)
Symmetry codes: (ii) x+1/4, y+1/4, z+1/4; (iii) x, y+1/2, z1/2; (iv) x1/4, y+1/4, z1/4; (v) x+1/4, y1/4, z1/4; (vi) x+1/4, y+1/4, z+1/4; (vii) x, y1/2, z+1/2.
 

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