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In the title samarium coordination polymer, [Sm(C14H8O4)(C14H9O4)(H2O)2]n, the Sm cation is located on a twofold axis and coordinated in an irregular SmO8 polyhedron, which is linked by the carboxyl­ate groups to form a three-dimensional framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806043340/ng2106sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806043340/ng2106Isup2.hkl
Contains datablock I

CCDC reference: 621668

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.083
  • Data-to-parameter ratio = 15.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.50 Ratio PLAT245_ALERT_2_C U(iso) H4O Smaller than U(eq) O4 by ... 0.01 AngSq PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.27 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 SM1 -O2 -C1 -O1 66.00 5.00 5.666 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 SM1 -O2 -C1 -C2 -117.00 5.00 5.666 1.555 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.848(10) ...... 4.00 su-Ra O1W -H2W 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(4), Rep 110.2(18) ...... 2.22 su-Ra H1W -O1W -H2W 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.848(10) ...... 4.00 su-Ra O1W -H2W 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Poly[[diaquasamarium(III)]-µ3-biphenyl-4,4'-dicarboxylato- µ3-4'-carboxylbiphenyl-4-carboxylato] top
Crystal data top
[Sm(C14H8O4)(C14H9O4)(H2O)2]F(000) = 1324
Mr = 667.80Dx = 1.866 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 6997 reflections
a = 27.665 (2) Åθ = 2.5–28.3°
b = 8.6510 (14) ŵ = 2.53 mm1
c = 9.9345 (15) ÅT = 298 K
V = 2377.6 (6) Å3Prism, yellow
Z = 40.28 × 0.26 × 0.25 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
2880 independent reflections
Radiation source: fine-focus sealed tube2392 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
Detector resolution: none pixels mm-1θmax = 28.3°, θmin = 1.5°
φ and ω scansh = 1936
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1111
Tmin = 0.497, Tmax = 0.531l = 1312
14000 measured reflections
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.083H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0312P)2 + 9.0839P]
where P = (Fo2 + 2Fc2)/3
2880 reflections(Δ/σ)max < 0.001
189 parametersΔρmax = 0.46 e Å3
4 restraintsΔρmin = 0.83 e Å3
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.

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*/UeqOcc. (<1)
Sm10.50000.44555 (3)0.25000.01461 (9)
O10.56528 (9)0.3577 (3)0.3855 (3)0.0218 (6)
O20.55228 (10)0.4545 (3)0.5885 (3)0.0233 (6)
O30.96490 (10)0.2827 (3)0.6297 (3)0.0210 (6)
O40.95630 (10)0.5115 (4)0.7284 (4)0.0339 (8)
H4O0.9836 (14)0.498 (11)0.766 (8)0.02 (2)*0.50
O1W0.45959 (12)0.6833 (3)0.1515 (3)0.0276 (7)
H1W0.463 (2)0.707 (6)0.0695 (18)0.06 (2)*
H2W0.452 (2)0.763 (4)0.196 (4)0.07 (2)*
C10.57921 (13)0.3940 (4)0.5015 (4)0.0146 (7)
C20.63187 (12)0.3711 (4)0.5352 (4)0.0158 (7)
C30.66351 (13)0.3173 (5)0.4364 (4)0.0209 (8)
H30.65140.28390.35400.025*
C40.71273 (13)0.3135 (5)0.4605 (4)0.0207 (8)
H40.73340.27540.39450.025*
C50.73209 (13)0.3660 (4)0.5825 (4)0.0181 (7)
C60.69946 (14)0.4131 (5)0.6829 (4)0.0212 (8)
H60.71120.44310.76670.025*
C70.65012 (14)0.4156 (5)0.6592 (4)0.0202 (8)
H70.62910.44740.72680.024*
C80.93949 (14)0.3936 (4)0.6669 (4)0.0188 (8)
C90.88602 (13)0.3935 (5)0.6409 (4)0.0196 (8)
C100.85532 (14)0.4984 (5)0.7043 (4)0.0232 (8)
H100.86810.57500.75940.028*
C110.80581 (14)0.4888 (5)0.6854 (5)0.0246 (9)
H110.78570.55940.72840.030*
C120.78563 (13)0.3757 (4)0.6036 (4)0.0181 (7)
C130.81660 (14)0.2724 (5)0.5387 (4)0.0235 (8)
H130.80390.19740.48180.028*
C140.86624 (14)0.2806 (5)0.5582 (4)0.0225 (8)
H140.88640.20980.51560.027*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.00953 (13)0.01897 (13)0.01533 (13)0.0000.00177 (11)0.000
O10.0124 (12)0.0300 (15)0.0228 (14)0.0036 (11)0.0062 (11)0.0022 (12)
O20.0088 (12)0.0352 (16)0.0259 (15)0.0037 (11)0.0023 (11)0.0025 (12)
O30.0138 (12)0.0255 (14)0.0238 (14)0.0043 (11)0.0007 (11)0.0007 (11)
O40.0147 (13)0.0272 (15)0.060 (2)0.0029 (12)0.0123 (14)0.0133 (15)
O1W0.0329 (17)0.0266 (15)0.0234 (15)0.0081 (14)0.0036 (13)0.0021 (13)
C10.0080 (16)0.0174 (16)0.0185 (18)0.0008 (13)0.0015 (13)0.0022 (14)
C20.0079 (16)0.0211 (18)0.0185 (17)0.0008 (14)0.0017 (14)0.0002 (14)
C30.0143 (18)0.031 (2)0.0176 (18)0.0009 (16)0.0051 (14)0.0040 (16)
C40.0138 (17)0.032 (2)0.0165 (17)0.0040 (16)0.0013 (15)0.0027 (16)
C50.0091 (16)0.0234 (19)0.0219 (18)0.0016 (14)0.0022 (14)0.0037 (15)
C60.0139 (18)0.033 (2)0.0163 (19)0.0011 (16)0.0047 (15)0.0032 (16)
C70.0100 (17)0.032 (2)0.0191 (18)0.0005 (15)0.0011 (14)0.0009 (16)
C80.0136 (17)0.0198 (18)0.0229 (19)0.0001 (15)0.0019 (15)0.0019 (15)
C90.0101 (17)0.0210 (18)0.028 (2)0.0017 (14)0.0017 (15)0.0045 (16)
C100.0152 (18)0.0199 (18)0.035 (2)0.0007 (16)0.0043 (16)0.0060 (17)
C110.0121 (17)0.026 (2)0.036 (2)0.0060 (16)0.0033 (17)0.0073 (18)
C120.0120 (17)0.0203 (18)0.0219 (18)0.0011 (14)0.0023 (14)0.0020 (15)
C130.0152 (18)0.029 (2)0.027 (2)0.0008 (16)0.0026 (16)0.0072 (17)
C140.0128 (18)0.027 (2)0.028 (2)0.0044 (15)0.0008 (15)0.0033 (16)
Geometric parameters (Å, º) top
Sm1—O2i2.327 (3)C3—C41.383 (5)
Sm1—O2ii2.327 (3)C3—H30.9300
Sm1—O12.377 (3)C4—C51.400 (5)
Sm1—O1iii2.377 (3)C4—H40.9300
Sm1—O3iv2.504 (3)C5—C61.406 (5)
Sm1—O3v2.504 (3)C5—C121.499 (5)
Sm1—O1Wiii2.537 (3)C6—C71.385 (5)
Sm1—O1W2.537 (3)C6—H60.9300
O1—C11.255 (4)C7—H70.9300
O2—C11.255 (4)C8—C91.501 (5)
O2—Sm1ii2.327 (3)C9—C141.389 (6)
O3—C81.246 (5)C9—C101.393 (6)
O3—Sm1vi2.504 (3)C10—C111.385 (5)
O4—C81.277 (5)C10—H100.9300
O4—H4O0.850 (10)C11—C121.389 (6)
O1W—H1W0.846 (10)C11—H110.9300
O1W—H2W0.848 (10)C12—C131.395 (5)
C1—C21.508 (5)C13—C141.389 (5)
C2—C71.385 (5)C13—H130.9300
C2—C31.395 (5)C14—H140.9300
O2i—Sm1—O2ii136.36 (14)C7—C2—C1120.8 (3)
O2i—Sm1—O192.13 (10)C3—C2—C1119.6 (3)
O2ii—Sm1—O1101.56 (10)C4—C3—C2120.3 (3)
O2i—Sm1—O1iii101.56 (10)C4—C3—H3119.9
O2ii—Sm1—O1iii92.13 (10)C2—C3—H3119.9
O1—Sm1—O1iii142.72 (14)C3—C4—C5121.2 (3)
O2i—Sm1—O3iv73.91 (10)C3—C4—H4119.4
O2ii—Sm1—O3iv149.69 (10)C5—C4—H4119.4
O1—Sm1—O3iv73.97 (9)C4—C5—C6117.6 (3)
O1iii—Sm1—O3iv76.83 (9)C4—C5—C12121.2 (3)
O2i—Sm1—O3v149.69 (9)C6—C5—C12121.3 (3)
O2ii—Sm1—O3v73.91 (10)C7—C6—C5121.1 (4)
O1—Sm1—O3v76.83 (9)C7—C6—H6119.5
O1iii—Sm1—O3v73.97 (9)C5—C6—H6119.5
O3iv—Sm1—O3v75.91 (13)C6—C7—C2120.4 (4)
O2i—Sm1—O1Wiii71.98 (10)C6—C7—H7119.8
O2ii—Sm1—O1Wiii72.95 (10)C2—C7—H7119.8
O1—Sm1—O1Wiii72.90 (10)O3—C8—O4123.5 (3)
O1iii—Sm1—O1Wiii144.31 (10)O3—C8—C9120.3 (3)
O3iv—Sm1—O1Wiii130.72 (10)O4—C8—C9116.2 (3)
O3v—Sm1—O1Wiii128.75 (9)C14—C9—C10119.0 (4)
O2i—Sm1—O1W72.95 (10)C14—C9—C8119.4 (4)
O2ii—Sm1—O1W71.98 (10)C10—C9—C8121.5 (4)
O1—Sm1—O1W144.31 (10)C11—C10—C9120.2 (4)
O1iii—Sm1—O1W72.90 (10)C11—C10—H10119.9
O3iv—Sm1—O1W128.75 (9)C9—C10—H10119.9
O3v—Sm1—O1W130.72 (10)C10—C11—C12121.2 (4)
O1Wiii—Sm1—O1W71.69 (15)C10—C11—H11119.4
C1—O1—Sm1132.3 (2)C12—C11—H11119.4
C1—O2—Sm1ii177.0 (3)C11—C12—C13118.3 (3)
C8—O3—Sm1vi133.2 (2)C11—C12—C5121.2 (3)
C8—O4—H4O115 (6)C13—C12—C5120.4 (3)
Sm1—O1W—H1W121 (4)C14—C13—C12120.7 (4)
Sm1—O1W—H2W125 (4)C14—C13—H13119.7
H1W—O1W—H2W110.2 (18)C12—C13—H13119.7
O2—C1—O1123.7 (3)C13—C14—C9120.5 (4)
O2—C1—C2118.4 (3)C13—C14—H14119.7
O1—C1—C2117.9 (3)C9—C14—H14119.7
C7—C2—C3119.3 (3)
O2i—Sm1—O1—C1116.0 (3)C3—C2—C7—C62.8 (6)
O2ii—Sm1—O1—C122.3 (3)C1—C2—C7—C6171.5 (4)
O1iii—Sm1—O1—C1131.6 (3)Sm1vi—O3—C8—O478.8 (5)
O3iv—Sm1—O1—C1171.4 (3)Sm1vi—O3—C8—C9100.8 (4)
O3v—Sm1—O1—C192.5 (3)O3—C8—C9—C149.4 (6)
O1Wiii—Sm1—O1—C145.6 (3)O4—C8—C9—C14170.9 (4)
O1W—Sm1—O1—C152.9 (4)O3—C8—C9—C10166.6 (4)
Sm1ii—O2—C1—O166 (5)O4—C8—C9—C1013.0 (6)
Sm1ii—O2—C1—C2117 (5)C14—C9—C10—C110.5 (6)
Sm1—O1—C1—O222.8 (6)C8—C9—C10—C11175.6 (4)
Sm1—O1—C1—C2153.9 (3)C9—C10—C11—C120.1 (7)
O2—C1—C2—C70.0 (5)C10—C11—C12—C130.9 (6)
O1—C1—C2—C7176.9 (4)C10—C11—C12—C5179.6 (4)
O2—C1—C2—C3174.2 (4)C4—C5—C12—C11147.9 (4)
O1—C1—C2—C32.7 (5)C6—C5—C12—C1130.4 (6)
C7—C2—C3—C42.2 (6)C4—C5—C12—C1330.7 (6)
C1—C2—C3—C4172.1 (4)C6—C5—C12—C13151.0 (4)
C2—C3—C4—C51.3 (6)C11—C12—C13—C141.5 (6)
C3—C4—C5—C64.1 (6)C5—C12—C13—C14179.8 (4)
C3—C4—C5—C12174.2 (4)C12—C13—C14—C91.2 (6)
C4—C5—C6—C73.5 (6)C10—C9—C14—C130.1 (6)
C12—C5—C6—C7174.8 (4)C8—C9—C14—C13176.3 (4)
C5—C6—C7—C20.2 (6)
Symmetry codes: (i) x, y+1, z1/2; (ii) x+1, y+1, z+1; (iii) x+1, y, z+1/2; (iv) x+3/2, y+1/2, z1/2; (v) x1/2, y+1/2, z+1; (vi) x+3/2, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4O···O4vii0.85 (1)1.67 (4)2.455 (6)153 (8)
O4—H4O···O3vii0.85 (1)2.56 (6)3.265 (4)140 (8)
O1W—H1W···O3viii0.85 (1)2.09 (1)2.927 (4)173 (5)
O1W—H2W···O4ix0.85 (1)2.10 (3)2.898 (4)158 (6)
Symmetry codes: (vii) x+2, y, z+3/2; (viii) x1/2, y+1/2, z+1/2; (ix) x1/2, y+3/2, z+1.
 

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