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The Tb atom in the title compound, {(C2H10N2)3[Tb(SO4)3(H2O)]2·4H2O}n, exists in a nine-coordinate geometry; the anion is linked through sulfate bridges into a three-dimensional network. The counter-ions and water mol­ecules occupy the spaces within the framework and they consolidate the network structure through extensive hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806027322/bt2147sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806027322/bt2147Isup2.hkl
Contains datablock I

CCDC reference: 604762

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.040
  • wR factor = 0.081
  • Data-to-parameter ratio = 16.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 15
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Poly[[tris(ethylene-1,2-diammonium) bis[aqua(µ-sulfato-κ3O,O':O'')(µ-sulfato-κ4O,O':O'',O''')(sulfato- κO)terbate(III)] tetrahydrate] top
Crystal data top
(C2H10N2)3[Tb(SO4)3(H2O)]2·4H2OF(000) = 1172
Mr = 1188.66Dx = 2.390 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3109 reflections
a = 6.5024 (4) Åθ = 2.3–27.6°
b = 26.392 (2) ŵ = 4.75 mm1
c = 9.9070 (7) ÅT = 291 K
β = 103.733 (1)°Rod, colourless
V = 1651.5 (2) Å30.14 × 0.06 × 0.03 mm
Z = 2
Data collection top
Bruker SMART APEX area-detector
diffractometer
3763 independent reflections
Radiation source: fine-focus sealed tube3244 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
φ and ω scansθmax = 27.5°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.556, Tmax = 0.871k = 3334
13711 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0304P)2 + 2.0826P]
where P = (Fo2 + 2Fc2)/3
3763 reflections(Δ/σ)max = 0.001
229 parametersΔρmax = 1.19 e Å3
0 restraintsΔρmin = 1.53 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Tb10.45388 (4)0.321085 (9)0.54092 (3)0.01081 (8)
S10.5892 (2)0.43377 (5)0.7526 (1)0.0164 (3)
S20.0287 (2)0.34150 (5)0.4645 (1)0.0143 (3)
S30.4712 (2)0.25038 (5)0.2928 (1)0.0130 (3)
O10.5738 (6)0.37868 (14)0.7173 (4)0.022 (1)
O20.4272 (6)0.44660 (15)0.8256 (5)0.028 (1)
O30.5622 (7)0.46343 (15)0.6231 (4)0.025 (1)
O40.8014 (6)0.44414 (16)0.8401 (4)0.026 (1)
O50.0884 (6)0.29866 (15)0.4206 (4)0.021 (1)
O60.1358 (6)0.37160 (15)0.5603 (4)0.022 (1)
O70.1825 (6)0.32203 (14)0.5397 (4)0.019 (1)
O80.1350 (6)0.37155 (16)0.3449 (5)0.030 (1)
O90.4417 (6)0.30557 (14)0.2872 (4)0.019 (1)
O100.5009 (6)0.23655 (14)0.4409 (4)0.017 (1)
O110.6507 (6)0.23435 (14)0.2365 (4)0.017 (1)
O120.2848 (6)0.22422 (14)0.2054 (4)0.018 (1)
O1w0.4656 (7)0.39827 (15)0.4179 (4)0.025 (1)
O2w0.2285 (8)0.53190 (18)0.8914 (5)0.038 (1)
O3w0.4718 (10)0.3888 (3)1.1036 (8)0.091 (3)
N10.1301 (8)0.37330 (19)0.8606 (5)0.026 (1)
N20.0785 (8)0.29352 (19)1.1104 (5)0.027 (1)
N30.0860 (8)0.52929 (19)0.6494 (5)0.027 (1)
C10.0537 (10)0.3277 (2)0.9195 (7)0.026 (1)
C20.0138 (11)0.3404 (2)1.0496 (7)0.031 (2)
C30.0513 (10)0.5018 (3)0.5757 (6)0.032 (2)
H1w10.47840.42240.47600.030*
H1w20.53390.40510.35700.030*
H2w10.28760.50320.88920.046*
H2w20.22590.53900.97460.046*
H3w10.55750.41331.12650.110*
H3w20.52750.36141.13940.110*
H1n10.03720.39650.85150.040*
H1n20.15260.36620.78160.040*
H1n30.24440.38340.91470.040*
H2n10.19760.28371.06170.041*
H2n20.08880.29941.19300.041*
H2n30.01360.27061.11160.041*
H3n10.11900.55790.61090.040*
H3n20.02060.53370.73370.040*
H3n30.19780.51220.64620.040*
H1a0.16560.30250.93980.032*
H1b0.06500.31330.85200.032*
H2a0.10240.35631.11570.037*
H2b0.13130.36401.02880.037*
H3a0.07890.46800.61430.038*
H3b0.18570.51930.58840.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.0095 (1)0.0113 (1)0.0120 (1)0.0000 (1)0.0036 (1)0.0004 (1)
S10.0176 (7)0.0146 (7)0.0163 (7)0.0019 (5)0.0028 (5)0.0023 (5)
S20.0102 (6)0.0158 (6)0.0173 (7)0.0003 (5)0.0041 (5)0.0031 (5)
S30.0129 (6)0.0142 (6)0.0125 (6)0.0007 (5)0.0041 (5)0.0021 (5)
O10.030 (2)0.013 (2)0.020 (2)0.002 (2)0.002 (2)0.000 (2)
O20.027 (2)0.026 (2)0.034 (3)0.004 (2)0.013 (2)0.005 (2)
O30.034 (2)0.019 (2)0.021 (2)0.003 (2)0.005 (2)0.002 (2)
O40.020 (2)0.029 (2)0.025 (2)0.005 (2)0.001 (2)0.009 (2)
O50.015 (2)0.024 (2)0.023 (2)0.001 (2)0.006 (2)0.007 (2)
O60.018 (2)0.020 (2)0.027 (2)0.001 (2)0.006 (2)0.003 (2)
O70.011 (2)0.026 (2)0.022 (2)0.000 (2)0.008 (2)0.004 (2)
O80.019 (2)0.035 (3)0.034 (3)0.002 (2)0.003 (2)0.018 (2)
O90.024 (2)0.0162 (19)0.018 (2)0.001 (2)0.010 (2)0.001 (2)
O100.018 (2)0.020 (2)0.012 (2)0.001 (2)0.003 (2)0.001 (2)
O110.016 (2)0.018 (2)0.018 (2)0.001 (2)0.007 (2)0.0032 (16)
O120.017 (2)0.024 (2)0.014 (2)0.002 (2)0.004 (2)0.0055 (16)
O1w0.044 (3)0.015 (2)0.020 (2)0.001 (2)0.015 (2)0.0005 (17)
O2w0.048 (3)0.035 (3)0.027 (3)0.006 (2)0.003 (2)0.012 (2)
O3w0.063 (4)0.099 (6)0.095 (5)0.034 (4)0.018 (4)0.060 (5)
N10.027 (3)0.031 (3)0.026 (3)0.001 (2)0.015 (2)0.003 (2)
N20.030 (3)0.031 (3)0.023 (3)0.011 (2)0.008 (2)0.004 (2)
N30.025 (3)0.024 (3)0.030 (3)0.002 (2)0.006 (2)0.001 (2)
C10.026 (3)0.024 (3)0.034 (4)0.003 (3)0.018 (3)0.001 (3)
C20.037 (4)0.024 (3)0.038 (4)0.001 (3)0.021 (3)0.004 (3)
C30.027 (3)0.034 (4)0.032 (4)0.004 (3)0.003 (3)0.003 (3)
Geometric parameters (Å, º) top
Tb1—O12.307 (4)C1—C21.495 (8)
Tb1—O52.465 (4)C3—C3iii1.49 (1)
Tb1—O62.506 (4)O1w—H1w10.85
Tb1—O7i2.368 (4)O1w—H1w20.85
Tb1—O92.530 (4)O2w—H2w10.85
Tb1—O102.489 (4)O2w—H2w20.85
Tb1—O11ii2.521 (4)O3w—H3w10.85
Tb1—O12ii2.479 (4)O3w—H3w20.85
Tb1—O1w2.385 (4)N1—H1n10.85
S1—O21.452 (4)N1—H1n20.85
S1—O41.470 (4)N1—H1n30.85
S1—O31.478 (4)N2—H2n10.85
S1—O11.493 (4)N2—H2n20.85
S2—O81.457 (4)N2—H2n30.85
S2—O71.473 (4)N3—H3n10.85
S2—O61.481 (4)N3—H3n20.85
S2—O51.485 (4)N3—H3n30.85
S3—O91.468 (4)C1—H1a0.97
S3—O111.470 (4)C1—H1b0.97
S3—O101.480 (4)C2—H2a0.97
S3—O121.482 (4)C2—H2b0.97
N1—C11.474 (7)C3—H3a0.97
N2—C21.480 (8)C3—H3b0.97
N3—C31.472 (8)
O1—Tb1—O5129.7 (1)O11—S3—O12104.9 (2)
O1—Tb1—O674.2 (1)O10—S3—O12111.1 (2)
O1—Tb1—O7i80.7 (1)S1—O1—Tb1144.2 (2)
O1—Tb1—O9141.7 (1)S2—O5—Tb1100.3 (2)
O1—Tb1—O10147.2 (1)S2—O6—Tb198.6 (2)
O1—Tb1—O11ii77.4 (1)S2—O7—Tb1iv143.6 (2)
O1—Tb1—O12ii86.7 (1)S3—O9—Tb198.6 (2)
O1—Tb1—O1w77.2 (1)S3—O10—Tb1100.0 (2)
O5—Tb1—O656.4 (1)S3—O11—Tb1v98.9 (2)
O5—Tb1—O7i148.2 (1)S3—O12—Tb1v100.4 (2)
O5—Tb1—O971.4 (1)N1—C1—C2110.7 (5)
O5—Tb1—O1077.8 (1)N2—C2—C1109.5 (5)
O5—Tb1—O11ii119.2 (1)N3—C3—C3iii110.5 (6)
O5—Tb1—O12ii71.0 (1)Tb1—O1w—H1w1107.7
O5—Tb1—O1w95.9 (1)Tb1—O1w—H1w2129.1
O6—Tb1—O7i147.0 (1)H1w1—O1w—H1w2109.8
O6—Tb1—O9109.3 (1)H2w1—O2w—H2w2109.6
O6—Tb1—O10133.5 (1)H3w1—O3w—H3w2110.4
O6—Tb1—O11ii121.8 (1)C1—N1—H1n1109.5
O6—Tb1—O12ii72.7 (1)C1—N1—H1n2109.5
O6—Tb1—O1w73.3 (1)H1n1—N1—H1n2109.5
O7i—Tb1—O978.0 (1)C1—N1—H1n3109.5
O7i—Tb1—O1077.9 (1)H1n1—N1—H1n3109.5
O7i—Tb1—O11ii71.6 (1)H1n2—N1—H1n3109.5
O7i—Tb1—O12ii127.4 (1)C2—N2—H2n1109.5
O7i—Tb1—O1w80.5 (1)C2—N2—H2n2109.5
O9—Tb1—O1055.8 (1)H2n1—N2—H2n2109.5
O9—Tb1—O11ii124.1 (1)C2—N2—H2n3109.5
O9—Tb1—O12ii131.4 (1)H2n1—N2—H2n3109.5
O9—Tb1—O1w68.1 (1)H2n2—N2—H2n3109.5
O10—Tb1—O11ii72.4 (1)C3—N3—H3n1109.5
O10—Tb1—O12ii86.8 (1)C3—N3—H3n2109.5
O10—Tb1—O1w122.7 (1)H3n1—N3—H3n2109.5
O11ii—Tb1—O12ii55.8 (1)C3—N3—H3n3109.5
O11ii—Tb1—O1w144.8 (1)H3n1—N3—H3n3109.5
O12ii—Tb1—O1w145.2 (1)H3n2—N3—H3n3109.5
O2—S1—O4110.7 (2)N1—C1—H1a109.5
O2—S1—O3111.0 (3)C2—C1—H1a109.5
O4—S1—O3108.4 (2)N1—C1—H1b109.5
O2—S1—O1109.1 (2)C2—C1—H1b109.5
O4—S1—O1108.7 (2)H1a—C1—H1b108.1
O3—S1—O1108.9 (2)N2—C2—H2a109.8
O8—S2—O7110.7 (2)C1—C2—H2a109.8
O8—S2—O6111.1 (3)N2—C2—H2b109.8
O7—S2—O6109.7 (2)C1—C2—H2b109.8
O8—S2—O5110.7 (3)H2a—C2—H2b108.2
O7—S2—O5109.8 (2)N3—C3—H3a109.5
O6—S2—O5104.7 (2)C3iii—C3—H3a109.5
O9—S3—O11112.3 (2)N3—C3—H3b109.5
O9—S3—O10105.5 (2)C3iii—C3—H3b109.5
O11—S3—O10112.1 (2)H3a—C3—H3b108.1
O9—S3—O12111.0 (2)
O2—S1—O1—Tb1101.5 (4)S3ii—Tb1—O6—S293.0 (2)
O4—S1—O1—Tb1137.7 (4)S3—Tb1—O6—S222.0 (2)
O3—S1—O1—Tb119.9 (5)O8—S2—O7—Tb1iv0.3 (5)
O7i—Tb1—O1—S1101.1 (4)O6—S2—O7—Tb1iv122.6 (4)
O1W—Tb1—O1—S118.8 (4)O5—S2—O7—Tb1iv122.8 (4)
O5—Tb1—O1—S168.2 (5)O11—S3—O9—Tb1125.1 (2)
O12ii—Tb1—O1—S1130.2 (4)O10—S3—O9—Tb12.7 (2)
O10—Tb1—O1—S1150.8 (3)O12—S3—O9—Tb1117.8 (2)
O6—Tb1—O1—S157.2 (4)O1—Tb1—O9—S3142.9 (2)
O11ii—Tb1—O1—S1174.2 (4)O7i—Tb1—O9—S385.3 (2)
O9—Tb1—O1—S144.2 (5)O1W—Tb1—O9—S3169.7 (2)
S2—Tb1—O1—S161.2 (4)O5—Tb1—O9—S385.7 (2)
S3ii—Tb1—O1—S1157.8 (4)O12ii—Tb1—O9—S344.6 (3)
S3—Tb1—O1—S191.8 (5)O10—Tb1—O9—S31.9 (2)
O8—S2—O5—Tb1116.9 (2)O6—Tb1—O9—S3128.3 (2)
O7—S2—O5—Tb1120.6 (2)O11ii—Tb1—O9—S327.5 (2)
O6—S2—O5—Tb12.9 (2)S2—Tb1—O9—S3107.6 (2)
O1—Tb1—O5—S214.8 (3)S3ii—Tb1—O9—S36.5 (2)
O7i—Tb1—O5—S2144.9 (2)O9—S3—O10—Tb12.7 (2)
O1W—Tb1—O5—S263.4 (2)O11—S3—O10—Tb1125.3 (2)
O12ii—Tb1—O5—S283.5 (2)O12—S3—O10—Tb1117.7 (2)
O10—Tb1—O5—S2174.3 (2)O1—Tb1—O10—S3135.9 (2)
O6—Tb1—O5—S21.99 (17)O7i—Tb1—O10—S385.5 (2)
O11ii—Tb1—O5—S2112.7 (2)O1W—Tb1—O10—S315.2 (3)
O9—Tb1—O5—S2128.0 (2)O5—Tb1—O10—S373.9 (2)
S3ii—Tb1—O5—S297.86 (19)O12ii—Tb1—O10—S3145.2 (2)
S3—Tb1—O5—S2157.4 (2)O6—Tb1—O10—S382.7 (2)
O8—S2—O6—Tb1116.7 (2)O11ii—Tb1—O10—S3159.8 (2)
O7—S2—O6—Tb1120.6 (2)O9—Tb1—O10—S31.9 (2)
O5—S2—O6—Tb12.8 (2)S2—Tb1—O10—S376.7 (2)
O1—Tb1—O6—S2171.8 (2)S3ii—Tb1—O10—S3171.9 (2)
O7i—Tb1—O6—S2146.1 (2)O9—S3—O11—Tb1v119.5 (2)
O1W—Tb1—O6—S2107.2 (2)O10—S3—O11—Tb1v121.9 (2)
O5—Tb1—O6—S22.0 (2)O12—S3—O11—Tb1v1.2 (2)
O12ii—Tb1—O6—S280.3 (2)O9—S3—O12—Tb1v120.3 (2)
O10—Tb1—O6—S212.3 (3)O11—S3—O12—Tb1v1.2 (2)
O11ii—Tb1—O6—S2108.0 (2)O10—S3—O12—Tb1v122.6 (2)
O9—Tb1—O6—S248.3 (2)N1—C1—C2—N2176.9 (5)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1/2, z+1/2; (iii) x, y+1, z+1; (iv) x1, y, z; (v) x, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O30.851.792.623 (6)165
O1w—H1w2···O8i0.852.362.942 (6)127
O2w—H2w1···O20.851.932.750 (6)161
O2w—H2w2···O4vi0.851.942.785 (6)176
O3w—H3w1···O2wvi0.852.042.852 (8)159
O3w—H3w2···O9vii0.852.242.888 (7)133
N1—H1n1···O4iv0.851.972.811 (6)173
N1—H1n2···O60.852.172.984 (6)159
N1—H1n3···O3w0.852.102.891 (8)156
N2—H2n1···O10viii0.852.112.958 (6)177
N2—H2n2···O5vii0.852.283.009 (6)145
N2—H2n3···O12vii0.852.172.959 (7)155
N3—H3n1···O6iii0.852.503.308 (6)159
N3—H3n2···O2w0.851.972.758 (7)155
N3—H3n3···O3iv0.851.992.835 (6)171
Symmetry codes: (i) x+1, y, z; (iii) x, y+1, z+1; (iv) x1, y, z; (vi) x+1, y+1, z+2; (vii) x, y, z+1; (viii) x1, y+1/2, z+1/2.
 

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