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The crystalline structure of a new three-dimensional coordination polymer based on LaIII and 1,4-phenyl­enedi­acetate ligands is described.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989019002378/vn2143sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989019002378/vn2143Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2056989019002378/vn2143sup3.pdf
Table 2. Valence angles and torsion angles around the ligands

CCDC reference: 1875083

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.030
  • wR factor = 0.068
  • Data-to-parameter ratio = 16.2

checkCIF/PLATON results

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Alert level B PLAT260_ALERT_2_B Large Average Ueq of Residue Including Ow4 0.154 Check PLAT417_ALERT_2_B Short Inter D-H..H-D Hw1A ..Hw1A . 1.91 Ang. 1-x,-y,1-z = 2_656 Check PLAT417_ALERT_2_B Short Inter D-H..H-D Hw2B ..Hw4A . 1.90 Ang. x,y,1+z = 1_556 Check
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.72 Report PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 --C1 . 5.5 s.u. PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of O4 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of La1 Check PLAT260_ALERT_2_C Large Average Ueq of Residue Including Ow1 0.133 Check PLAT260_ALERT_2_C Large Average Ueq of Residue Including Ow3 0.133 Check PLAT417_ALERT_2_C Short Inter D-H..H-D Hw1B ..Hw3B . 2.11 Ang. 1-x,-y,1-z = 2_656 Check PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 2.165 Check PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min). 10 Note PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.600 2 Report PLAT971_ALERT_2_C Check Calcd Resid. Dens. 1.30A From O4 1.83 eA-3 PLAT971_ALERT_2_C Check Calcd Resid. Dens. 1.33A From O6 1.75 eA-3 PLAT976_ALERT_2_C Check Calcd Resid. Dens. 0.85A From Ow3 -0.49 eA-3 PLAT976_ALERT_2_C Check Calcd Resid. Dens. 0.76A From Ow3 -0.42 eA-3 PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density. 0 Info
Alert level G PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 3 Info PLAT005_ALERT_5_G No Embedded Refinement Details Found in the CIF Please Do ! PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 2.00 Check PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.001 Degree PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K) 293 Check PLAT200_ALERT_1_G Reported _diffrn_ambient_temperature ..... (K) 293 Check PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 --O1 . 7.1 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 --O5_b . 14.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) La1 --O3_c . 8.0 s.u. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 12 Note PLAT794_ALERT_5_G Tentative Bond Valency for La1 (III) . 3.11 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 18 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 6 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 3 ALERT level B = A potentially serious problem, consider carefully 15 ALERT level C = Check. Ensure it is not caused by an omission or oversight 14 ALERT level G = General information/check it is not something unexpected 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 18 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 3 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Bruker, 2004); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: WinGX (Farrugia, 2012).

Poly[[tetraaquatris(µ-1,4-phenylenediacetato)dilanthanum(III)] octahydrate] top
Crystal data top
[La2(C10H8O4)3(H2O)4]·8H2OZ = 1
Mr = 1070.05F(000) = 534
Triclinic, P1Dx = 1.768 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.1197 (2) ÅCell parameters from 15558 reflections
b = 11.1231 (2) Åθ = 2.9–27.5°
c = 11.9434 (2) ŵ = 2.18 mm1
α = 107.049 (1)°T = 293 K
β = 107.729 (1)°Prism, colorless
γ = 106.622 (1)°0.08 × 0.06 × 0.05 mm
V = 1005.21 (3) Å3
Data collection top
Nonius KappaCCD
diffractometer
3751 reflections with I > 2σ(I)
Radiation source: Enraf Nonius FR590Rint = 0.045
Horizonally mounted graphite crystal monochromatorθmax = 27.5°, θmin = 3.6°
Detector resolution: 9 pixels mm-1h = 1011
CCD rotation images, thick slices scansk = 1414
4588 measured reflectionsl = 1515
4588 independent reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: dual
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: mixed
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0308P)2]
where P = (Fo2 + 2Fc2)/3
4588 reflections(Δ/σ)max = 0.001
283 parametersΔρmax = 1.76 e Å3
18 restraintsΔρmin = 0.65 e Å3
0 constraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
La10.75090 (2)0.52031 (2)0.47969 (2)0.02048 (7)
O50.4472 (3)0.3677 (2)0.4069 (2)0.0332 (6)
O31.0575 (3)0.5881 (3)0.6253 (2)0.0323 (6)
O10.7627 (3)0.3041 (3)0.5311 (2)0.0336 (6)
O60.8146 (3)0.7579 (3)0.6435 (3)0.0362 (6)
O20.7422 (3)0.4674 (3)0.6736 (2)0.0351 (6)
O40.6840 (3)0.3616 (3)0.2490 (2)0.0415 (7)
O70.5690 (4)0.5882 (4)0.3233 (3)0.0486 (8)
H7A0.468 (3)0.558 (4)0.307 (5)0.058*
H7B0.591 (5)0.651 (4)0.302 (5)0.058*
O80.9316 (4)0.7051 (3)0.4326 (4)0.0503 (8)
H8A0.947 (6)0.785 (3)0.470 (4)0.060*
H8B1.026 (4)0.712 (4)0.435 (5)0.060*
C60.6834 (4)0.7426 (3)0.6621 (3)0.0260 (7)
C110.8165 (4)0.3436 (3)0.2659 (3)0.0261 (7)
C10.7640 (4)0.3589 (4)0.6405 (4)0.0315 (8)
C130.6579 (5)0.1147 (4)0.0739 (4)0.0340 (9)
C120.8247 (5)0.2382 (4)0.1565 (4)0.0390 (9)
H12A0.8573420.2812620.1028980.058*
H12B0.9105630.2079900.1922790.058*
C140.6017 (5)0.0190 (4)0.1196 (4)0.0427 (10)
H140.6695600.0301950.2011490.051*
C80.8472 (5)0.9325 (4)0.8881 (4)0.0340 (9)
C100.9564 (5)1.0646 (4)0.9217 (4)0.0433 (10)
H100.9284131.1099550.8697970.052*
C150.5547 (5)0.0946 (4)0.0469 (4)0.0412 (10)
H150.5890460.1571910.0807970.049*
C70.6832 (5)0.8578 (4)0.7675 (4)0.0445 (11)
H7C0.6607240.9237220.7344800.067*
H7D0.5921520.8197980.7899730.067*
C90.8927 (6)0.8687 (4)0.9685 (4)0.0461 (11)
H90.8204750.7795080.9481620.055*
C30.8997 (5)0.3972 (4)0.8732 (4)0.0392 (9)
C41.0738 (6)0.4427 (5)0.9267 (4)0.0514 (11)
H41.1254050.4053780.8782630.062*
C50.8281 (6)0.4561 (5)0.9477 (4)0.0501 (11)
H50.7114190.4274720.9131330.060*
C20.7931 (6)0.2928 (4)0.7347 (4)0.0460 (10)
H2A0.6847260.2358790.7272510.069*
H2B0.8483590.2330010.7115710.069*
OW10.6313 (10)0.0072 (5)0.4440 (6)0.1327 (17)
HW1A0.589 (11)0.025 (9)0.491 (8)0.159*
HW1B0.639 (13)0.072 (6)0.411 (8)0.159*
OW20.5351 (5)0.6185 (4)0.9718 (4)0.0741 (11)
HW2A0.476 (7)0.639 (6)0.920 (5)0.111*
HW2B0.622 (6)0.678 (5)1.033 (5)0.111*
OW30.0357 (9)0.0056 (6)0.3870 (6)0.1327 (17)
HW3A0.059 (10)0.059 (7)0.354 (7)0.159*
HW3B0.122 (7)0.023 (10)0.447 (6)0.159*
OW40.7105 (10)0.7873 (7)0.2433 (6)0.154 (3)
HW4A0.649 (10)0.805 (11)0.192 (8)0.185*
HW4B0.810 (5)0.831 (11)0.255 (10)0.185*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.01729 (10)0.02001 (10)0.01850 (10)0.00633 (7)0.00482 (7)0.00498 (7)
O50.0242 (13)0.0258 (13)0.0312 (13)0.0032 (10)0.0034 (11)0.0040 (11)
O30.0227 (13)0.0340 (14)0.0229 (12)0.0074 (11)0.0027 (10)0.0011 (11)
O10.0352 (14)0.0353 (14)0.0339 (14)0.0161 (12)0.0168 (12)0.0155 (12)
O60.0247 (13)0.0283 (13)0.0415 (15)0.0089 (10)0.0129 (12)0.0005 (11)
O20.0403 (15)0.0427 (15)0.0332 (14)0.0254 (13)0.0173 (12)0.0200 (12)
O40.0267 (14)0.0515 (17)0.0253 (13)0.0175 (12)0.0040 (11)0.0052 (12)
O70.0425 (17)0.075 (2)0.067 (2)0.0390 (17)0.0345 (17)0.0532 (18)
O80.0456 (18)0.0523 (18)0.088 (2)0.0315 (16)0.0434 (18)0.0469 (19)
C60.0228 (17)0.0219 (17)0.0260 (17)0.0100 (14)0.0051 (14)0.0052 (14)
C110.0187 (16)0.0250 (17)0.0236 (16)0.0060 (13)0.0062 (14)0.0018 (14)
C10.0184 (17)0.041 (2)0.0332 (19)0.0099 (15)0.0083 (15)0.0177 (17)
C130.0261 (19)0.030 (2)0.0297 (19)0.0117 (16)0.0070 (16)0.0041 (16)
C120.0233 (18)0.040 (2)0.0318 (19)0.0098 (16)0.0074 (16)0.0057 (17)
C140.039 (2)0.044 (2)0.028 (2)0.0198 (19)0.0002 (18)0.0047 (18)
C80.031 (2)0.0293 (19)0.0290 (19)0.0102 (16)0.0138 (16)0.0032 (16)
C100.042 (2)0.033 (2)0.037 (2)0.0058 (18)0.0114 (19)0.0059 (18)
C150.043 (2)0.037 (2)0.031 (2)0.0133 (19)0.0076 (18)0.0078 (17)
C70.026 (2)0.040 (2)0.043 (2)0.0127 (17)0.0102 (18)0.0078 (19)
C90.042 (2)0.0225 (19)0.048 (2)0.0033 (17)0.016 (2)0.0006 (18)
C30.043 (2)0.044 (2)0.035 (2)0.0206 (19)0.0123 (18)0.0260 (18)
C40.051 (3)0.073 (3)0.041 (2)0.037 (2)0.022 (2)0.023 (2)
C50.032 (2)0.077 (3)0.042 (2)0.024 (2)0.0112 (19)0.027 (2)
C20.055 (3)0.040 (2)0.039 (2)0.017 (2)0.012 (2)0.0233 (19)
OW10.192 (4)0.069 (2)0.109 (3)0.009 (3)0.079 (3)0.028 (2)
OW20.063 (3)0.086 (3)0.074 (3)0.032 (2)0.020 (2)0.043 (2)
OW30.192 (4)0.069 (2)0.109 (3)0.009 (3)0.079 (3)0.028 (2)
OW40.158 (6)0.115 (4)0.103 (4)0.017 (4)0.019 (4)0.084 (4)
Geometric parameters (Å, º) top
La1—O52.507 (2)C12—H12B0.9700
La1—O5i2.905 (3)C14—H140.9300
La1—O3ii2.781 (2)C14—C15iii1.399 (6)
La1—O32.545 (2)C8—C101.373 (6)
La1—O12.673 (2)C8—C71.509 (5)
La1—O62.559 (2)C8—C91.388 (6)
La1—O22.569 (2)C10—H100.9300
La1—O42.566 (2)C10—C9iv1.382 (6)
La1—O72.543 (3)C15—H150.9300
La1—O82.562 (3)C7—H7C0.9700
La1—C113.066 (3)C7—H7D0.9700
La1—C12.988 (4)C9—H90.9300
O5—C6i1.255 (4)C3—C41.385 (6)
O3—C11ii1.264 (4)C3—C51.381 (6)
O1—C11.264 (4)C3—C21.509 (6)
O6—C61.256 (4)C4—H40.9300
O2—C11.248 (4)C4—C5v1.391 (6)
O4—C111.246 (4)C5—H50.9300
O7—H7A0.824 (19)C2—H2A0.9700
O7—H7B0.806 (18)C2—H2B0.9700
O8—H8A0.815 (19)OW1—HW1A0.87 (2)
O8—H8B0.833 (19)OW1—HW1B0.88 (2)
C6—C71.512 (5)OW2—HW2A0.821 (19)
C11—C121.516 (5)OW2—HW2B0.81 (2)
C1—C21.514 (5)OW3—HW3A0.82 (2)
C13—C121.507 (5)OW3—HW3B0.81 (2)
C13—C141.376 (6)OW4—HW4A0.81 (2)
C13—C151.371 (5)OW4—HW4B0.84 (2)
C12—H12A0.9700
O5—La1—O5i61.48 (9)C11—O4—La1101.3 (2)
O5—La1—O3146.45 (9)La1—O7—H7A116 (3)
O5—La1—O3ii118.58 (7)La1—O7—H7B133 (3)
O5—La1—O175.87 (8)H7A—O7—H7B109 (3)
O5—La1—O6107.86 (8)La1—O8—H8A118 (3)
O5—La1—O275.29 (8)La1—O8—H8B122 (3)
O5—La1—O480.33 (8)H8A—O8—H8B104 (3)
O5—La1—O771.93 (9)O5i—C6—La168.28 (18)
O5—La1—O8140.13 (9)O5i—C6—O6120.2 (3)
O5i—La1—C11156.28 (8)O5i—C6—C7120.1 (3)
O5—La1—C1198.48 (8)O6—C6—La152.33 (16)
O5—La1—C175.84 (9)O6—C6—C7119.7 (3)
O5i—La1—C188.69 (9)C7—C6—La1169.6 (2)
O3—La1—O5i118.22 (7)O3ii—C11—La165.08 (17)
O3ii—La1—O5i179.00 (7)O3ii—C11—C12120.3 (3)
O3—La1—O3ii61.11 (8)O4—C11—La155.16 (17)
O3—La1—O173.20 (8)O4—C11—O3ii119.9 (3)
O3—La1—O680.93 (8)O4—C11—C12119.8 (3)
O3—La1—O274.87 (8)C12—C11—La1171.2 (2)
O3—La1—O4108.82 (8)O1—C1—La163.39 (19)
O3—La1—O873.39 (9)O1—C1—C2119.8 (3)
O3ii—La1—C1124.36 (8)O2—C1—La158.58 (18)
O3—La1—C1185.47 (8)O2—C1—O1121.5 (3)
O3—La1—C170.64 (9)O2—C1—C2118.7 (3)
O3ii—La1—C190.37 (9)C2—C1—La1172.4 (3)
O1—La1—O5i109.68 (7)C14—C13—C12120.5 (4)
O1—La1—O3ii69.49 (8)C15—C13—C12122.1 (4)
O1—La1—C1174.29 (9)C15—C13—C14117.4 (4)
O1—La1—C125.01 (9)C11—C12—H12A109.2
O6—La1—O5i46.41 (7)C11—C12—H12B109.2
O6—La1—O3ii133.56 (8)C13—C12—C11112.0 (3)
O6—La1—O1126.21 (9)C13—C12—H12A109.2
O6—La1—O278.86 (9)C13—C12—H12B109.2
O6—La1—O4149.49 (10)H12A—C12—H12B107.9
O6—La1—O871.55 (10)C13—C14—H14119.1
O6—La1—C11149.62 (9)C13—C14—C15iii121.8 (4)
O6—La1—C1101.90 (10)C15iii—C14—H14119.1
O2—La1—O5i66.57 (8)C10—C8—C7121.6 (4)
O2—La1—O3ii112.44 (8)C10—C8—C9117.8 (4)
O2—La1—O149.39 (8)C9—C8—C7120.6 (4)
O2—La1—C11123.42 (9)C8—C10—H10119.5
O2—La1—C124.50 (9)C8—C10—C9iv121.1 (4)
O4—La1—O5i132.95 (7)C9iv—C10—H10119.5
O4—La1—O3ii47.75 (7)C13—C15—C14iii120.7 (4)
O4—La1—O184.13 (9)C13—C15—H15119.6
O4—La1—O2131.27 (9)C14iii—C15—H15119.6
O4—La1—C1123.49 (8)C6—C7—H7C108.9
O4—La1—C1108.61 (10)C6—C7—H7D108.9
O7—La1—O5i70.81 (9)C8—C7—C6113.4 (3)
O7—La1—O3141.53 (10)C8—C7—H7C108.9
O7—La1—O3ii110.19 (9)C8—C7—H7D108.9
O7—La1—O1142.43 (10)H7C—C7—H7D107.7
O7—La1—O682.59 (10)C8—C9—H9119.4
O7—La1—O2134.87 (9)C10iv—C9—C8121.1 (4)
O7—La1—O471.95 (10)C10iv—C9—H9119.4
O7—La1—O868.46 (10)C4—C3—C2120.7 (4)
O7—La1—C1191.69 (10)C5—C3—C4118.0 (4)
O7—La1—C1147.21 (10)C5—C3—C2121.2 (4)
O8—La1—O5i108.04 (8)C3—C4—H4119.8
O8—La1—O3ii72.59 (9)C3—C4—C5v120.4 (4)
O8—La1—O1138.11 (8)C5v—C4—H4119.8
O8—La1—O2139.28 (10)C3—C5—C4v121.6 (4)
O8—La1—O483.41 (11)C3—C5—H5119.2
O8—La1—C1178.57 (10)C4v—C5—H5119.2
O8—La1—C1144.03 (10)C1—C2—H2A109.0
C1—La1—C1198.95 (10)C1—C2—H2B109.0
La1—O5—La1i118.52 (9)C3—C2—C1112.8 (3)
C6i—O5—La1i88.1 (2)C3—C2—H2A109.0
C6i—O5—La1153.4 (2)C3—C2—H2B109.0
La1—O3—La1ii118.89 (8)H2A—C2—H2B107.8
C11ii—O3—La1150.5 (2)HW1A—OW1—HW1B88 (7)
C11ii—O3—La1ii90.56 (19)HW2A—OW2—HW2B121 (5)
C1—O1—La191.6 (2)HW3A—OW3—HW3B108 (4)
C6—O6—La1104.8 (2)HW4A—OW4—HW4B107 (4)
C1—O2—La196.9 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+1; (iii) x+1, y, z; (iv) x+2, y+2, z+2; (v) x+2, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—HW1A···OW1vi0.87 (9)2.40 (11)3.067 (13)133 (9)
OW1—HW1B···OW4vii0.89 (9)2.54 (10)3.298 (11)145 (7)
OW2—HW2A···O4i0.82 (6)2.10 (6)2.895 (5)164 (6)
OW2—HW2B···OW4viii0.82 (6)2.20 (5)2.855 (8)137 (5)
OW3—HW3A···O6i0.82 (8)2.02 (8)2.780 (8)154 (7)
OW3—HW3B···OW1vi0.81 (7)2.40 (8)3.162 (11)156 (8)
OW4—HW4A···OW2ix0.81 (10)2.49 (9)2.855 (8)109 (9)
O7—H7A···O2i0.82 (4)1.95 (4)2.741 (5)161 (5)
O7—H7B···OW40.81 (5)2.03 (5)2.800 (9)160 (5)
OW4—HW4B···OW3x0.84 (9)2.11 (10)2.824 (11)143 (8)
O8—H8A···OW3i0.82 (4)2.38 (4)3.175 (8)165 (4)
O8—H8B···O1ii0.83 (4)1.92 (4)2.725 (5)163 (5)
C7—H7D···O4i0.972.543.442 (6)154
C12—H12B···O6ii0.972.513.406 (6)154
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+1; (vi) x+1, y, z+1; (vii) x, y1, z; (viii) x, y, z+1; (ix) x, y, z1; (x) x+1, y+1, z.
 

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