A series of two-dimensional lanthanide coordination polymers: synthesis, structures, magnetism and selective luminescence detection for heavy metal ions and toxic solvents

A series of two-dimensional (2D) coordination polymers (CPs), namely poly[[bis(μ-acetato)di­aqua­(μ₆-biphenyl-3,3′,5,5′-tetra­carboxyl­ato)bis(N,N-di­methyl­ace­ta­mide)di­gadolinium(III)] N,N-di­methyl­ace­ta­mide monosolvate], {[Gd₂(C₁₆H₆O₈)(C₂H₃O₂)₂(C₄H₉NO)₂(H₂O)₂]·C₄H₉NO}_n (CP1), poly[[bis(μ-acetato)diaqua­(μ₆-biphenyl-3,3′,5,5′-tetra­carboxyl­ato)bis(N,N-di­methyl­ace­t­amide)­di­dysprosium(III)] N,N-di­methyl­ace­ta­mide monosolvate], {[Dy₂(C₁₆H₆O₈)(C₂H₃O₂)₂(C₄H₉NO)₂(H₂O)₂]·C₄H₉NO}_n (CP2), poly[bis­(μ-ace­tato)diaqua­(μ₆-bi­phenyl-3,3′,5,5′-tetra­carboxyl­ato)bis(N,N-di­methyl­ace­tamide)dineodymium(III)], [Nd₂(C₁₆H₆O₈)(C₂H₃O₂)₂(C₄H₉NO)₂(H₂O)₂]_n (CP3), poly[bis(μ-acetato)di­aqua­(μ₆-biphenyl-3,3′,5,5′-tetra­carboxyl­ato)bis(N,N-di­methyl­acetamide)di­sam­arium(III)], [Sm₂(C₁₆H₆O₈)(C₂H₃O₂)₂(C₄H₉NO)₂(H₂O)₂]_n (CP4), has been synthesized from rigid biphenyl-3,3′,5,5′-tetra­carb­oxy­lic acid under solvothermal conditions. Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, powder X-ray diffraction and thermogravimetric analyses, and CP1–CP4 crystallize in the monoclinic space group P2₁/n. CP1–CP4 are isomorphous and feature similar 2D double layers, which are further extended via inter­layer hydrogen-bonding inter­actions into a three-dimensional (3D) supra­molecular structure. Hydrogen-bonding inter­actions between N,N-di­methyl­acetamide mol­ecules and carboxyl­ate O atoms strengthen the packing of the layers. The organic ligands inter­connect with metal ions to generate 2D layered structures with a (4,4)-connected net having {4⁴.6²} topology. CP1 has been investigated for its magnetic properties and magnetic susceptibility measurements were carried out in the range 2.0–300 K. The results of the magnetic measurements show weak anti­ferromagnetic coupling between the Gd^III ions in CP1. Moreover, the strong luminescence of CP2 and CP4 can be selectively quenched by the Fe³⁺ ion and toxic solvents (e.g. acetone).

Computing details

For all structures, data collection: APEX2 (Bruker, 2010); cell refinement: SAINT (Bruker, 2010); data reduction: SAINT (Bruker, 2010); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2015 (Sheldrick, 2015b); software used to prepare material for publication: SHELXL2015 (Sheldrick, 2015b).

Poly[[bis(µ-acetato)diaqua(µ₆-biphenyl-3,3',5,5'-tetracarboxylato)bis(N,N-dimethylacetamide)gadolinium(III)] N,N-dimethylacetamide monosolvate] (150912a)

Crystal data

[Gd2(C16H6O8)(C2H3O2)2(C4H9NO)2(H2O)2]·C4H9NO	F(000) = 944
Mr = 1043.12	Dx = 1.720 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.3992 (8) Å	Cell parameters from 2563 reflections
b = 17.6714 (15) Å	θ = 2.5–26.8°
c = 11.2971 (9) Å	µ = 3.58 mm^−1
β = 94.318 (1)°	T = 298 K
V = 1871.1 (3) Å^3	Bloc, colorless
Z = 2	0.29 × 0.26 × 0.24 mm

Data collection

Bruker SMART APEXII CCD diffractometer	2109 reflections with I > 2σ(I)
phi and ω scans	Rint = 0.080
Absorption correction: multi-scan	θmax = 25.0°, θmin = 2.9°
Tmin = 0.368, Tmax = 0.423	h = −11→11
8560 measured reflections	k = −20→21
3193 independent reflections	l = −13→8

Refinement

Refinement on F^2	450 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.076	H-atom parameters constrained
wR(F^2) = 0.196	w = 1/[σ^2(Fo^2) + (0.1P)^2 + 9.6297P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max < 0.001
3193 reflections	Δρmax = 1.51 e Å^−3
209 parameters	Δρmin = −1.79 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Gd1	0.48332 (7)	0.39865 (4)	0.06975 (6)	0.0314 (3)
N1	0.0722 (18)	0.3152 (13)	0.1729 (18)	0.103 (7)
O1	0.4420 (14)	0.2638 (6)	0.0138 (10)	0.0562 (19)
O2	0.5865 (13)	0.2880 (6)	0.1697 (10)	0.0545 (18)
O3	0.6745 (14)	0.3637 (7)	−0.0539 (11)	0.058 (2)
O4	0.6091 (13)	0.4807 (6)	−0.0810 (10)	0.051 (2)
O5	0.6739 (13)	0.4654 (6)	0.1732 (10)	0.054 (2)
O6	0.6648 (12)	0.5859 (5)	0.1079 (9)	0.049 (2)
O10	0.4602 (19)	0.4146 (9)	0.2762 (8)	0.097 (3)
H10B	0.370843	0.422564	0.273674	0.117*
H10C	0.496215	0.458585	0.283564	0.117*
O9	0.2771 (16)	0.3715 (8)	0.1585 (12)	0.080 (2)
C1	0.528 (2)	0.2395 (9)	0.0991 (15)	0.054 (2)
C2	0.5550 (12)	0.1567 (3)	0.1115 (8)	0.047 (2)
C3	0.4966 (11)	0.1037 (5)	0.0309 (7)	0.048 (2)
H3	0.433764	0.119077	−0.031986	0.058*
C4	0.5321 (11)	0.0277 (4)	0.0444 (7)	0.046 (2)
C5	0.6261 (11)	0.0046 (3)	0.1384 (8)	0.045 (2)
H5	0.649837	−0.046228	0.147452	0.054*
C6	0.6845 (11)	0.0577 (4)	0.2190 (7)	0.045 (2)
C7	0.6490 (12)	0.1337 (4)	0.2055 (7)	0.046 (2)
H7	0.688054	0.169159	0.259403	0.055*
C8	0.695 (2)	0.4233 (10)	−0.1016 (16)	0.055 (2)
C9	0.835 (2)	0.4436 (12)	−0.165 (2)	0.082 (5)
H9A	0.914172	0.416327	−0.127529	0.122*
H9B	0.852422	0.496959	−0.158298	0.122*
H9C	0.821992	0.429744	−0.247178	0.122*
C10	0.709 (2)	0.5348 (9)	0.1778 (15)	0.052 (3)
C20	0.031 (3)	0.3611 (17)	0.070 (2)	0.112 (5)
H20A	0.007906	0.411237	0.094865	0.169*
H20B	−0.050527	0.339026	0.026803	0.169*
H20C	0.108847	0.363561	0.019447	0.169*
C23	−0.040 (3)	0.2698 (15)	0.236 (2)	0.106 (5)
H23A	0.000323	0.222385	0.263544	0.158*
H23B	−0.121814	0.260496	0.182171	0.158*
H23C	−0.068569	0.298204	0.303089	0.158*
C24	0.267 (3)	0.3090 (14)	0.3426 (15)	0.105 (4)
H24A	0.368498	0.301648	0.345306	0.158*
H24B	0.222529	0.264009	0.369693	0.158*
H24C	0.246134	0.350725	0.392932	0.158*
C25	0.2145 (18)	0.3248 (11)	0.2250 (15)	0.077 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd1	0.0406 (4)	0.0152 (4)	0.0357 (4)	−0.0032 (3)	−0.0149 (3)	0.0035 (3)
N1	0.110 (16)	0.117 (18)	0.084 (14)	−0.019 (14)	0.020 (12)	0.023 (13)
O1	0.079 (4)	0.032 (4)	0.054 (4)	−0.001 (3)	−0.019 (4)	0.002 (3)
O2	0.079 (4)	0.029 (3)	0.052 (4)	−0.003 (3)	−0.018 (3)	0.000 (3)
O3	0.081 (4)	0.035 (4)	0.057 (4)	0.010 (4)	−0.003 (4)	0.002 (3)
O4	0.068 (5)	0.028 (4)	0.056 (4)	0.010 (4)	−0.003 (4)	0.002 (4)
O5	0.075 (4)	0.025 (3)	0.057 (4)	0.006 (4)	−0.021 (4)	0.000 (3)
O6	0.069 (5)	0.025 (4)	0.048 (4)	0.002 (4)	−0.020 (4)	0.003 (4)
O10	0.113 (7)	0.078 (7)	0.098 (7)	0.002 (6)	−0.008 (6)	0.001 (6)
O9	0.098 (5)	0.059 (5)	0.083 (5)	−0.002 (4)	0.000 (5)	0.007 (4)
C1	0.076 (4)	0.031 (4)	0.051 (4)	0.000 (4)	−0.016 (4)	−0.001 (3)
C2	0.071 (4)	0.024 (4)	0.043 (4)	0.000 (4)	−0.020 (4)	−0.004 (4)
C3	0.072 (4)	0.025 (4)	0.044 (4)	−0.002 (4)	−0.022 (4)	−0.003 (4)
C4	0.069 (5)	0.024 (4)	0.041 (4)	0.001 (4)	−0.025 (4)	−0.009 (4)
C5	0.067 (5)	0.023 (4)	0.040 (5)	−0.001 (4)	−0.029 (4)	−0.004 (4)
C6	0.068 (5)	0.021 (4)	0.042 (4)	0.000 (4)	−0.022 (4)	−0.006 (4)
C7	0.069 (4)	0.021 (4)	0.044 (4)	−0.001 (4)	−0.020 (4)	−0.001 (4)
C8	0.073 (5)	0.033 (4)	0.058 (5)	0.011 (4)	−0.001 (5)	−0.001 (4)
C9	0.097 (10)	0.069 (9)	0.082 (9)	0.011 (9)	0.026 (9)	0.006 (8)
C10	0.070 (5)	0.026 (5)	0.056 (5)	0.002 (5)	−0.015 (5)	0.000 (4)
C20	0.124 (10)	0.100 (10)	0.110 (10)	−0.001 (10)	−0.006 (10)	0.004 (9)
C23	0.116 (10)	0.090 (10)	0.108 (10)	−0.020 (9)	−0.003 (10)	0.011 (9)
C24	0.120 (9)	0.091 (8)	0.104 (8)	0.005 (8)	0.000 (8)	0.005 (8)
C25	0.096 (5)	0.057 (5)	0.076 (5)	−0.001 (5)	−0.010 (5)	0.005 (5)

Geometric parameters (Å, º)

Gd1—O9	2.298 (15)	C2—C7	1.3900
Gd1—O4^i	2.309 (10)	C3—C4	1.3900
Gd1—O10	2.375 (9)	C3—H3	0.9300
Gd1—O6^i	2.370 (10)	C4—C5	1.3900
Gd1—O5	2.377 (11)	C4—C4^ii	1.495 (8)
Gd1—O2	2.423 (11)	C5—C6	1.3900
Gd1—O3	2.437 (13)	C5—H5	0.9300
Gd1—O1	2.488 (11)	C6—C7	1.3900
Gd1—O4	2.589 (11)	C6—C10^iii	1.534 (17)
Gd1—Gd1^i	3.9352 (13)	C7—H7	0.9300
Gd1—H10C	2.6318	C8—C9	1.58 (3)
N1—C25	1.431 (10)	C9—H9A	0.9600
N1—C20	1.45 (3)	C9—H9B	0.9600
N1—C23	1.55 (3)	C9—H9C	0.9600
O1—C1	1.28 (2)	C20—H20A	0.9600
O2—C1	1.269 (19)	C20—H20B	0.9600
O3—C8	1.21 (2)	C20—H20C	0.9600
O4—C8	1.33 (2)	C23—H23A	0.9600
O5—C10	1.269 (18)	C23—H23B	0.9600
O6—C10	1.249 (18)	C23—H23C	0.9600
O10—H10B	0.8500	C24—C25	1.410 (9)
O10—H10C	0.8500	C24—H24A	0.9600
O9—C25	1.288 (9)	C24—H24B	0.9600
C1—C2	1.491 (17)	C24—H24C	0.9600
C2—C3	1.3900
O9—Gd1—O4^i	80.5 (5)	C8—O4—Gd1	90.0 (10)
O9—Gd1—O10	56.9 (6)	Gd1^i—O4—Gd1	106.8 (4)
O4^i—Gd1—O10	76.9 (5)	C10—O5—Gd1	133.0 (10)
O9—Gd1—O6^i	86.1 (5)	C10—O6—Gd1^i	139.8 (10)
O4^i—Gd1—O6^i	75.0 (4)	Gd1—O10—H10B	98.7
O10—Gd1—O6^i	136.6 (5)	Gd1—O10—H10C	98.0
O9—Gd1—O5	121.2 (5)	H10B—O10—H10C	103.7
O4^i—Gd1—O5	77.7 (4)	C25—O9—Gd1	145.7 (13)
O10—Gd1—O5	65.2 (5)	O2—C1—O1	117.7 (14)
O6^i—Gd1—O5	137.0 (4)	O2—C1—C2	122.7 (14)
O9—Gd1—O2	87.1 (5)	O1—C1—C2	119.5 (13)
O4^i—Gd1—O2	149.1 (4)	C3—C2—C7	120.0
O10—Gd1—O2	72.6 (5)	C3—C2—C1	122.9 (8)
O6^i—Gd1—O2	132.6 (3)	C7—C2—C1	117.0 (8)
O5—Gd1—O2	84.9 (4)	C4—C3—C2	120.0
O9—Gd1—O3	151.5 (5)	C4—C3—H3	120.0
O4^i—Gd1—O3	124.2 (4)	C2—C3—H3	120.0
O10—Gd1—O3	135.9 (5)	C5—C4—C3	120.0
O6^i—Gd1—O3	87.4 (4)	C5—C4—C4^ii	121.5 (11)
O5—Gd1—O3	81.2 (4)	C3—C4—C4^ii	118.5 (11)
O2—Gd1—O3	77.0 (4)	C4—C5—C6	120.0
O9—Gd1—O1	77.9 (5)	C4—C5—H5	120.0
O4^i—Gd1—O1	147.8 (4)	C6—C5—H5	120.0
O10—Gd1—O1	109.8 (5)	C7—C6—C5	120.0
O6^i—Gd1—O1	79.9 (3)	C7—C6—C10^iii	118.4 (7)
O5—Gd1—O1	134.2 (4)	C5—C6—C10^iii	121.6 (7)
O2—Gd1—O1	52.8 (4)	C6—C7—C2	120.0
O3—Gd1—O1	73.7 (4)	C6—C7—H7	120.0
O9—Gd1—O4	147.7 (4)	C2—C7—H7	120.0
O4^i—Gd1—O4	73.2 (4)	O3—C8—O4	118.1 (17)
O10—Gd1—O4	131.3 (5)	O3—C8—C9	124.4 (17)
O6^i—Gd1—O4	69.3 (4)	O4—C8—C9	116.2 (15)
O5—Gd1—O4	71.4 (4)	C8—C9—H9A	109.5
O2—Gd1—O4	124.9 (4)	C8—C9—H9B	109.5
O3—Gd1—O4	51.1 (4)	H9A—C9—H9B	109.5
O1—Gd1—O4	116.1 (4)	C8—C9—H9C	109.5
O9—Gd1—Gd1^i	117.4 (3)	H9A—C9—H9C	109.5
O4^i—Gd1—Gd1^i	39.1 (3)	H9B—C9—H9C	109.5
O10—Gd1—Gd1^i	107.5 (4)	O6—C10—O5	126.9 (15)
O6^i—Gd1—Gd1^i	67.4 (2)	O6—C10—C6^iv	117.2 (14)
O5—Gd1—Gd1^i	70.4 (2)	O5—C10—C6^iv	115.9 (14)
O2—Gd1—Gd1^i	151.6 (3)	N1—C20—H20A	109.5
O3—Gd1—Gd1^i	85.2 (3)	N1—C20—H20B	109.5
O1—Gd1—Gd1^i	141.8 (3)	H20A—C20—H20B	109.5
O4—Gd1—Gd1^i	34.2 (2)	N1—C20—H20C	109.5
O9—Gd1—H10C	70.5	H20A—C20—H20C	109.5
O4^i—Gd1—H10C	64.5	H20B—C20—H20C	109.5
O10—Gd1—H10C	18.7	N1—C23—H23A	109.5
O6^i—Gd1—H10C	135.6	N1—C23—H23B	109.5
O5—Gd1—H10C	50.8	H23A—C23—H23B	109.5
O2—Gd1—H10C	84.7	N1—C23—H23C	109.5
O3—Gd1—H10C	130.0	H23A—C23—H23C	109.5
O1—Gd1—H10C	127.9	H23B—C23—H23C	109.5
O4—Gd1—H10C	112.7	C25—C24—H24A	109.5
Gd1^i—Gd1—H10C	90.1	C25—C24—H24B	109.5
C25—N1—C20	116.7 (19)	H24A—C24—H24B	109.5
C25—N1—C23	121.4 (17)	C25—C24—H24C	109.5
C20—N1—C23	121 (2)	H24A—C24—H24C	109.5
C1—O1—Gd1	93.0 (9)	H24B—C24—H24C	109.5
C1—O2—Gd1	96.4 (10)	O9—C25—C24	122.2 (12)
C8—O3—Gd1	100.6 (11)	O9—C25—N1	106.8 (14)
C8—O4—Gd1^i	162.1 (12)	C24—C25—N1	128.0 (17)

Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) −x+3/2, y+1/2, −z+1/2.

Poly[[bis(µ-acetato)diaqua(µ₆-biphenyl-3,3',5,5'-tetracarboxylato)bis(N,N-dimethylacetamide)didysprosium(III)] N,N-dimethylacetamide monosolvate] (150915a_sq)

Crystal data

[Dy2(C16H6O8)(C2H3O2)2(C4H9NO)2(H2O)2]·C4H9NO	F(000) = 1048
Mr = 1067.12	Dx = 1.895 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.3529 (9) Å	Cell parameters from 4295 reflections
b = 17.6217 (15) Å	θ = 3.0–28.1°
c = 11.3758 (11) Å	µ = 4.04 mm^−1
β = 94.494 (1)°	T = 298 K
V = 1869.1 (3) Å^3	Block, colorless
Z = 2	0.28 × 0.25 × 0.24 mm

Data collection

Bruker SMART APEXII CCD diffractometer	2687 reflections with I > 2σ(I)
phi and ω scans	Rint = 0.060
Absorption correction: multi-scan	θmax = 25.0°, θmin = 2.5°
Tmin = 0.643, Tmax = 0.688	h = −11→9
9326 measured reflections	k = −14→20
3293 independent reflections	l = −12→13

Refinement

Refinement on F^2	437 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.053	H-atom parameters constrained
wR(F^2) = 0.154	w = 1/[σ^2(Fo^2) + (0.090P)^2 + 5.6013P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max < 0.001
3293 reflections	Δρmax = 1.56 e Å^−3
215 parameters	Δρmin = −2.70 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	1.0244 (12)	0.2576 (6)	0.6009 (9)	0.0488 (16)
C2	1.0568 (10)	0.3406 (5)	0.6140 (8)	0.0397 (15)
C3	1.1546 (10)	0.3644 (5)	0.7063 (8)	0.0406 (15)
H3	1.196097	0.328866	0.759033	0.049*
C4	1.1898 (10)	0.4403 (5)	0.7194 (8)	0.0425 (17)
C5	1.1294 (10)	0.4936 (5)	0.6380 (8)	0.0437 (17)
H5	1.153953	0.544513	0.647040	0.052*
C6	1.0332 (11)	0.4716 (5)	0.5438 (8)	0.0424 (17)
C7	1.0008 (11)	0.3937 (5)	0.5336 (9)	0.0448 (16)
H7	0.939430	0.377381	0.470367	0.054*
C8	1.1947 (13)	0.0731 (6)	0.4001 (10)	0.0588 (19)
C9	1.3166 (17)	0.0601 (10)	0.3257 (15)	0.105 (4)
H9A	1.395377	0.092354	0.352159	0.157*
H9B	1.286760	0.071668	0.244970	0.157*
H9C	1.346071	0.008020	0.331900	0.157*
C10	1.2074 (11)	−0.0346 (5)	0.6768 (8)	0.0484 (19)
C11	0.7133 (11)	0.1689 (7)	0.7235 (10)	0.081 (2)
C12	0.758 (2)	0.1963 (11)	0.8453 (12)	0.121 (4)
H12A	0.703527	0.170104	0.900952	0.182*
H12B	0.740021	0.249842	0.850017	0.182*
H12C	0.858073	0.186594	0.863030	0.182*
C13	0.5309 (18)	0.1427 (12)	0.5635 (13)	0.138 (5)
H13A	0.597038	0.150688	0.504344	0.207*
H13B	0.438506	0.162480	0.536236	0.207*
H13C	0.522944	0.089391	0.578859	0.207*
C14	0.4738 (15)	0.2282 (11)	0.7264 (15)	0.126 (4)
H14A	0.424529	0.258777	0.666238	0.189*
H14B	0.518095	0.260495	0.786732	0.189*
H14C	0.406499	0.195133	0.760224	0.189*
Dy1	0.98337 (4)	0.10087 (2)	0.56765 (3)	0.0342 (2)
N1	0.5840 (12)	0.1828 (8)	0.6746 (11)	0.123 (5)
O1	0.9389 (8)	0.2350 (4)	0.5146 (6)	0.0517 (14)
O2	1.0873 (6)	0.2098 (3)	0.6697 (5)	0.0342 (2)
O3	1.1785 (9)	0.1365 (4)	0.4492 (7)	0.0603 (15)
O4	1.1115 (7)	0.0191 (4)	0.4205 (6)	0.0495 (14)
O5	1.1686 (7)	0.0339 (3)	0.6732 (6)	0.0530 (14)
O6	1.1625 (8)	−0.0865 (4)	0.6065 (6)	0.0530 (16)
O8	0.7848 (11)	0.1272 (6)	0.6605 (9)	0.0861 (19)
O7	0.9685 (15)	0.0853 (7)	0.7841 (10)	0.115 (3)
H7B	1.010575	0.042595	0.789446	0.138*
H7C	0.880085	0.073775	0.782036	0.138*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.064 (3)	0.028 (3)	0.052 (3)	0.000 (3)	−0.014 (3)	−0.004 (3)
C2	0.054 (3)	0.019 (3)	0.043 (3)	0.001 (3)	−0.019 (3)	−0.002 (3)
C3	0.055 (3)	0.020 (3)	0.044 (3)	0.001 (3)	−0.022 (3)	0.001 (3)
C4	0.054 (3)	0.022 (3)	0.046 (3)	−0.002 (3)	−0.024 (3)	−0.002 (3)
C5	0.061 (4)	0.019 (3)	0.047 (4)	−0.002 (3)	−0.023 (3)	−0.002 (3)
C6	0.056 (4)	0.020 (3)	0.047 (3)	0.000 (3)	−0.025 (3)	0.000 (3)
C7	0.058 (3)	0.023 (3)	0.049 (3)	−0.002 (3)	−0.027 (3)	−0.003 (3)
C8	0.076 (4)	0.038 (4)	0.061 (4)	−0.012 (4)	0.001 (4)	−0.004 (3)
C9	0.115 (8)	0.088 (8)	0.117 (9)	−0.028 (8)	0.041 (8)	−0.012 (8)
C10	0.069 (4)	0.024 (3)	0.047 (4)	−0.003 (3)	−0.029 (3)	0.000 (3)
C11	0.094 (4)	0.061 (4)	0.088 (4)	0.002 (4)	0.002 (4)	−0.014 (4)
C12	0.136 (8)	0.106 (8)	0.121 (8)	0.008 (8)	0.009 (7)	−0.022 (7)
C13	0.152 (10)	0.127 (10)	0.136 (10)	0.009 (10)	0.012 (9)	−0.008 (9)
C14	0.138 (9)	0.114 (9)	0.128 (9)	0.019 (8)	0.024 (8)	−0.015 (8)
Dy1	0.0429 (3)	0.0148 (3)	0.0416 (3)	0.00278 (15)	−0.01716 (19)	−0.00354 (15)
N1	0.088 (9)	0.134 (14)	0.142 (12)	0.005 (9)	−0.024 (9)	0.035 (10)
O1	0.071 (3)	0.023 (2)	0.056 (3)	−0.002 (2)	−0.028 (3)	−0.005 (2)
O2	0.0429 (3)	0.0148 (3)	0.0416 (3)	0.00278 (15)	−0.01716 (19)	−0.00354 (15)
O3	0.080 (3)	0.035 (3)	0.065 (3)	−0.013 (3)	0.001 (3)	−0.007 (3)
O4	0.067 (3)	0.027 (3)	0.053 (3)	−0.007 (3)	−0.006 (3)	−0.003 (2)
O5	0.075 (3)	0.024 (3)	0.054 (3)	0.001 (3)	−0.034 (3)	−0.001 (2)
O6	0.075 (4)	0.026 (3)	0.051 (3)	0.005 (3)	−0.036 (3)	−0.008 (3)
O8	0.096 (4)	0.065 (4)	0.099 (4)	0.003 (4)	0.021 (4)	−0.019 (4)
O7	0.143 (6)	0.116 (6)	0.087 (4)	−0.004 (6)	0.007 (5)	−0.001 (5)

Geometric parameters (Å, º)

C1—O2	1.264 (11)	C11—O8	1.255 (8)
C1—O1	1.280 (12)	C11—N1	1.313 (8)
C1—C2	1.498 (12)	C11—C12	1.495 (9)
C2—C7	1.382 (12)	C13—N1	1.498 (8)
C2—C3	1.402 (11)	C14—N1	1.465 (8)
C3—C4	1.383 (13)	Dy1—O8	2.255 (9)
C4—C5	1.405 (12)	Dy1—O4^iii	2.300 (6)
C4—C10^i	1.529 (12)	Dy1—O6^iii	2.329 (6)
C5—C6	1.400 (11)	Dy1—O5	2.347 (6)
C6—C7	1.408 (12)	Dy1—O2	2.409 (5)
C6—C6^ii	1.511 (17)	Dy1—O3	2.435 (8)
C8—O3	1.262 (14)	Dy1—O1	2.467 (6)
C8—O4	1.263 (12)	Dy1—O7	2.492 (11)
C8—C9	1.490 (17)	Dy1—O4	2.575 (7)
C10—O6	1.266 (10)	Dy1—Dy1^iii	3.8959 (8)
C10—O5	1.260 (11)
O2—C1—O1	120.0 (8)	O6^iii—Dy1—O1	79.6 (2)
O2—C1—C2	120.6 (8)	O5—Dy1—O1	135.3 (2)
O1—C1—C2	119.3 (8)	O2—Dy1—O1	53.71 (18)
C7—C2—C3	119.0 (8)	O3—Dy1—O1	74.8 (3)
C7—C2—C1	122.1 (8)	O8—Dy1—O7	56.5 (4)
C3—C2—C1	118.7 (8)	O4^iii—Dy1—O7	77.9 (3)
C4—C3—C2	120.3 (8)	O6^iii—Dy1—O7	138.9 (4)
C5—C4—C3	119.7 (7)	O5—Dy1—O7	62.3 (4)
C5—C4—C10^i	120.7 (8)	O2—Dy1—O7	70.3 (3)
C3—C4—C10^i	119.6 (8)	O3—Dy1—O7	132.7 (4)
C4—C5—C6	121.4 (8)	O1—Dy1—O7	109.0 (3)
C5—C6—C7	117.0 (8)	O8—Dy1—O4	149.5 (3)
C5—C6—C6^ii	121.9 (10)	O4^iii—Dy1—O4	74.0 (3)
C7—C6—C6^ii	121.1 (9)	O6^iii—Dy1—O4	70.0 (2)
C2—C7—C6	122.5 (8)	O5—Dy1—O4	71.9 (2)
O3—C8—O4	119.2 (10)	O2—Dy1—O4	124.7 (2)
O3—C8—C9	120.7 (11)	O3—Dy1—O4	51.5 (2)
O4—C8—C9	119.9 (11)	O1—Dy1—O4	117.1 (2)
O6—C10—O5	126.3 (8)	O7—Dy1—O4	130.2 (3)
O6—C10—C4^iv	115.9 (8)	O8—Dy1—Dy1^iii	117.8 (3)
O5—C10—C4^iv	117.7 (8)	O4^iii—Dy1—Dy1^iii	39.46 (17)
O8—C11—N1	112.4 (10)	O6^iii—Dy1—Dy1^iii	67.95 (16)
O8—C11—C12	126.6 (11)	O5—Dy1—Dy1^iii	70.43 (15)
N1—C11—C12	120.8 (11)	O2—Dy1—Dy1^iii	151.18 (13)
O8—Dy1—O4^iii	80.0 (3)	O3—Dy1—Dy1^iii	85.98 (17)
O8—Dy1—O6^iii	88.4 (3)	O1—Dy1—Dy1^iii	142.64 (15)
O4^iii—Dy1—O6^iii	75.4 (2)	O7—Dy1—Dy1^iii	107.6 (3)
O8—Dy1—O5	117.7 (3)	O4—Dy1—Dy1^iii	34.59 (14)
O4^iii—Dy1—O5	77.3 (2)	C11—N1—C14	125.8 (8)
O6^iii—Dy1—O5	137.7 (2)	C11—N1—C13	120.2 (8)
O8—Dy1—O2	85.8 (3)	C14—N1—C13	113.5 (7)
O4^iii—Dy1—O2	147.9 (2)	C1—O1—Dy1	91.6 (5)
O6^iii—Dy1—O2	133.1 (2)	C1—O2—Dy1	94.7 (5)
O5—Dy1—O2	84.28 (19)	C8—O3—Dy1	97.9 (7)
O8—Dy1—O3	152.5 (3)	C8—O4—Dy1^iii	161.8 (7)
O4^iii—Dy1—O3	125.4 (2)	C8—O4—Dy1	91.3 (6)
O6^iii—Dy1—O3	88.4 (3)	Dy1^iii—O4—Dy1	106.0 (3)
O5—Dy1—O3	81.8 (3)	C10—O5—Dy1	134.2 (6)
O2—Dy1—O3	76.7 (2)	C10—O6—Dy1^iii	139.4 (6)
O8—Dy1—O1	77.8 (3)	C11—O8—Dy1	152.0 (9)
O4^iii—Dy1—O1	146.7 (2)

Symmetry codes: (i) −x+5/2, y+1/2, −z+3/2; (ii) −x+2, −y+1, −z+1; (iii) −x+2, −y, −z+1; (iv) −x+5/2, y−1/2, −z+3/2.

Poly[bis(µ-acetato)diaqua(µ₆-biphenyl-3,3',5,5'-tetracarboxylato)bis(N,N-dimethylacetamide)dineodymium(III)] (150910g_sq)

Crystal data

[Nd2(C16H6O8)(C2H3O2)2(C4H9NO)2(H2O)2]	F(000) = 928
Mr = 943.05	Dx = 1.612 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.5383 (8) Å	Cell parameters from 3098 reflections
b = 17.9660 (15) Å	θ = 2.7–25.4°
c = 11.3703 (9) Å	µ = 2.71 mm^−1
β = 94.402 (1)°	T = 298 K
V = 1942.7 (3) Å^3	Bloc
Z = 2	0.33 × 0.29 × 0.27 mm

Data collection

Bruker SMART APEXII CCD diffractometer	2229 reflections with I > 2σ(I)
phi and ω scans	Rint = 0.099
Absorption correction: multi-scan	θmax = 25.0°, θmin = 2.3°
Tmin = 0.774, Tmax = 0.833	h = −11→11
9559 measured reflections	k = −21→21
3384 independent reflections	l = −13→8

Refinement

Refinement on F^2	440 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.054	H-atom parameters constrained
wR(F^2) = 0.139	w = 1/[σ^2(Fo^2) + (0.0606P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.041
3384 reflections	Δρmax = 1.35 e Å^−3
221 parameters	Δρmin = −0.82 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C15	0.7047 (15)	0.1734 (11)	0.7204 (14)	0.156 (5)
Nd1	0.98318 (5)	0.10226 (2)	0.57076 (4)	0.0421 (2)
C1	1.0274 (11)	0.2621 (5)	0.5988 (9)	0.057 (2)
C2	1.0585 (10)	0.3435 (4)	0.6115 (8)	0.047 (2)
C3	1.0010 (10)	0.3960 (5)	0.5331 (8)	0.053 (2)
H3	0.939258	0.380227	0.470733	0.064*
C4	1.0320 (9)	0.4722 (4)	0.5438 (7)	0.047 (2)
C5	1.1246 (10)	0.4927 (5)	0.6387 (8)	0.052 (2)
H5	1.147185	0.542806	0.648773	0.063*
C6	1.1855 (10)	0.4409 (4)	0.7201 (7)	0.048 (2)
C7	1.1510 (10)	0.3661 (5)	0.7065 (8)	0.049 (2)
H7	1.189176	0.331128	0.760132	0.059*
C8	1.2147 (10)	−0.0344 (5)	0.6759 (8)	0.055 (2)
C9	1.1936 (13)	0.0735 (6)	0.3951 (10)	0.073 (3)
C10	1.3086 (18)	0.0580 (9)	0.3143 (16)	0.137 (6)
H10A	1.377827	0.096829	0.322533	0.206*
H10B	1.269070	0.056303	0.234079	0.206*
H10C	1.352018	0.011099	0.334784	0.206*
O1	1.0878 (7)	0.2160 (3)	0.6695 (6)	0.0603 (17)
O2	0.9417 (8)	0.2395 (3)	0.5145 (6)	0.0653 (18)
O3	1.1818 (9)	0.1354 (4)	0.4451 (7)	0.0785 (19)
O4	1.1106 (7)	0.0209 (3)	0.4168 (6)	0.0621 (17)
O5	1.1789 (7)	0.0332 (3)	0.6698 (6)	0.0687 (19)
O6	1.1676 (8)	−0.0856 (3)	0.6079 (6)	0.068 (2)
O7	0.9721 (16)	0.0887 (7)	0.7954 (10)	0.160 (4)
H7B	1.008006	0.045466	0.802710	0.192*
H7C	0.884117	0.080506	0.793240	0.192*
O8	0.7712 (12)	0.1327 (6)	0.6565 (10)	0.130 (3)
N1	0.5716 (15)	0.1863 (10)	0.6610 (13)	0.163 (5)
C12	0.4556 (17)	0.2264 (14)	0.721 (2)	0.189 (7)
H12A	0.493355	0.246557	0.794950	0.284*
H12B	0.381742	0.191848	0.734643	0.284*
H12C	0.418520	0.266008	0.671190	0.284*
C13	0.517 (2)	0.1352 (14)	0.5571 (18)	0.195 (8)
H13A	0.479773	0.165271	0.492417	0.293*
H13B	0.445305	0.102961	0.582311	0.293*
H13C	0.593889	0.105773	0.532337	0.293*
C14	0.759 (2)	0.2003 (12)	0.8438 (15)	0.200 (7)
H14A	0.716918	0.171044	0.902441	0.300*
H14B	0.734372	0.251686	0.852964	0.300*
H14C	0.859267	0.194950	0.853236	0.300*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C15	0.172 (10)	0.137 (9)	0.163 (10)	−0.008 (9)	0.029 (9)	−0.018 (9)
Nd1	0.0535 (3)	0.0223 (3)	0.0468 (3)	0.0034 (2)	−0.0195 (2)	−0.0040 (2)
C1	0.075 (5)	0.027 (4)	0.065 (5)	−0.004 (4)	−0.027 (4)	−0.005 (4)
C2	0.061 (5)	0.023 (4)	0.054 (4)	−0.002 (3)	−0.021 (4)	−0.004 (3)
C3	0.065 (5)	0.033 (4)	0.054 (4)	0.000 (4)	−0.034 (4)	−0.002 (3)
C4	0.060 (5)	0.025 (4)	0.051 (4)	0.012 (4)	−0.026 (4)	−0.003 (3)
C5	0.068 (5)	0.026 (4)	0.058 (5)	−0.001 (4)	−0.029 (4)	−0.003 (4)
C6	0.060 (5)	0.027 (4)	0.050 (4)	0.001 (4)	−0.027 (4)	0.000 (3)
C7	0.066 (5)	0.029 (4)	0.047 (4)	0.002 (4)	−0.028 (4)	−0.001 (3)
C8	0.070 (5)	0.031 (4)	0.059 (5)	0.002 (4)	−0.031 (4)	−0.008 (4)
C9	0.081 (6)	0.051 (5)	0.087 (6)	−0.010 (5)	0.009 (5)	−0.004 (5)
C10	0.140 (12)	0.114 (11)	0.166 (13)	−0.031 (10)	0.067 (11)	−0.027 (10)
O1	0.082 (4)	0.029 (3)	0.063 (3)	0.007 (3)	−0.037 (3)	−0.002 (3)
O2	0.093 (4)	0.034 (3)	0.062 (4)	0.000 (3)	−0.039 (3)	0.000 (3)
O3	0.100 (5)	0.048 (4)	0.087 (5)	−0.022 (4)	0.008 (4)	−0.007 (4)
O4	0.076 (4)	0.041 (3)	0.067 (4)	−0.005 (3)	−0.006 (3)	−0.004 (3)
O5	0.092 (4)	0.032 (3)	0.074 (4)	0.009 (3)	−0.051 (3)	−0.005 (3)
O6	0.089 (4)	0.038 (3)	0.068 (4)	0.013 (3)	−0.056 (4)	−0.009 (3)
O7	0.208 (10)	0.148 (9)	0.127 (7)	−0.027 (8)	0.032 (8)	−0.018 (7)
O8	0.130 (6)	0.105 (6)	0.161 (7)	0.006 (5)	0.053 (5)	−0.030 (6)
N1	0.138 (9)	0.159 (10)	0.192 (11)	−0.002 (9)	0.018 (9)	−0.013 (9)
C12	0.175 (14)	0.207 (15)	0.191 (14)	0.031 (13)	0.049 (12)	−0.059 (13)
C13	0.182 (15)	0.204 (17)	0.201 (16)	0.013 (14)	0.023 (14)	−0.018 (14)
C14	0.219 (15)	0.156 (14)	0.229 (15)	−0.018 (13)	0.046 (14)	−0.094 (12)

Geometric parameters (Å, º)

C15—O8	1.239 (9)	C2—C3	1.382 (11)
C15—N1	1.410 (9)	C2—C7	1.401 (11)
C15—C14	1.536 (9)	C3—C4	1.404 (12)
Nd1—O8	2.376 (10)	C4—C5	1.390 (10)
Nd1—O4^i	2.396 (6)	C4—C4^ii	1.507 (15)
Nd1—O6^i	2.416 (5)	C5—C6	1.406 (11)
Nd1—O5	2.443 (6)	C6—C7	1.390 (11)
Nd1—O1	2.502 (5)	C6—C8^iii	1.526 (11)
Nd1—O3	2.530 (8)	C8—O5	1.262 (10)
Nd1—O7	2.576 (12)	C8—O6	1.263 (9)
Nd1—O2	2.571 (6)	C9—O3	1.259 (13)
Nd1—O4	2.647 (7)	C9—O4	1.267 (12)
Nd1—Nd1^i	4.0338 (9)	C9—C10	1.510 (19)
C1—O2	1.277 (10)	N1—C12	1.524 (9)
C1—O1	1.261 (10)	N1—C13	1.553 (10)
C1—C2	1.498 (11)
O8—C15—N1	107.4 (12)	O6^i—Nd1—Nd1^i	67.19 (14)
O8—C15—C14	124.7 (11)	O5—Nd1—Nd1^i	68.91 (14)
N1—C15—C14	127.8 (13)	O1—Nd1—Nd1^i	151.85 (15)
O8—Nd1—O4^i	81.7 (3)	O3—Nd1—Nd1^i	84.46 (17)
O8—Nd1—O6^i	84.4 (3)	O7—Nd1—Nd1^i	108.6 (3)
O4^i—Nd1—O6^i	74.6 (2)	O2—Nd1—Nd1^i	142.18 (14)
O8—Nd1—O5	124.9 (4)	O4—Nd1—Nd1^i	34.78 (15)
O4^i—Nd1—O5	77.3 (2)	O2—C1—O1	120.4 (8)
O6^i—Nd1—O5	135.2 (2)	O2—C1—C2	119.5 (8)
O8—Nd1—O1	87.2 (3)	O1—C1—C2	120.1 (7)
O4^i—Nd1—O1	150.0 (2)	C3—C2—C7	119.7 (7)
O6^i—Nd1—O1	132.02 (19)	C3—C2—C1	122.6 (7)
O5—Nd1—O1	86.76 (18)	C7—C2—C1	117.7 (7)
O8—Nd1—O3	151.1 (4)	C2—C3—C4	122.6 (7)
O4^i—Nd1—O3	123.4 (2)	C5—C4—C3	116.3 (7)
O6^i—Nd1—O3	88.7 (3)	C5—C4—C4^ii	122.6 (9)
O5—Nd1—O3	78.5 (3)	C3—C4—C4^ii	121.1 (8)
O1—Nd1—O3	76.7 (2)	C4—C5—C6	122.7 (7)
O8—Nd1—O7	60.9 (5)	C7—C6—C5	119.0 (7)
O4^i—Nd1—O7	79.0 (3)	C7—C6—C8^iii	119.7 (7)
O6^i—Nd1—O7	139.0 (4)	C5—C6—C8^iii	121.3 (7)
O5—Nd1—O7	65.4 (4)	C6—C7—C2	119.7 (7)
O1—Nd1—O7	71.2 (3)	O5—C8—O6	125.9 (8)
O3—Nd1—O7	132.2 (4)	O5—C8—C6^iv	118.2 (7)
O8—Nd1—O2	76.2 (3)	O6—C8—C6^iv	115.7 (7)
O4^i—Nd1—O2	148.2 (2)	O3—C9—O4	119.5 (11)
O6^i—Nd1—O2	80.73 (19)	O3—C9—C10	122.1 (11)
O5—Nd1—O2	134.4 (2)	O4—C9—C10	118.4 (11)
O1—Nd1—O2	51.44 (17)	C1—O1—Nd1	95.9 (5)
O3—Nd1—O2	75.0 (3)	C1—O2—Nd1	92.3 (5)
O7—Nd1—O2	108.7 (3)	C9—O3—Nd1	98.2 (7)
O8—Nd1—O4	147.9 (3)	C9—O4—Nd1^i	160.2 (8)
O4^i—Nd1—O4	73.9 (3)	C9—O4—Nd1	92.5 (7)
O6^i—Nd1—O4	69.5 (2)	Nd1^i—O4—Nd1	106.1 (3)
O5—Nd1—O4	69.6 (2)	C8—O5—Nd1	135.1 (5)
O1—Nd1—O4	124.1 (2)	C8—O6—Nd1^i	140.0 (5)
O3—Nd1—O4	49.8 (2)	C15—O8—Nd1	150.1 (12)
O7—Nd1—O4	131.3 (4)	C15—N1—C12	121.4 (10)
O2—Nd1—O4	115.8 (2)	C15—N1—C13	120.1 (15)
O8—Nd1—Nd1^i	118.0 (3)	C12—N1—C13	114.2 (14)
O4^i—Nd1—Nd1^i	39.07 (17)

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y+1, −z+1; (iii) −x+5/2, y+1/2, −z+3/2; (iv) −x+5/2, y−1/2, −z+3/2.

Poly[bis(µ-acetato)diaqua(µ₆-biphenyl-3,3',5,5'-tetracarboxylato)bis(N,N-dimethylacetamide)disamarium(III)] (150917a_sq)

Crystal data

[Sm2(C16H6O8)(C2H3O2)2(C4H9NO)2(H2O)2]	F(000) = 936
Mr = 960.03	Dx = 1.665 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.4469 (9) Å	Cell parameters from 2807 reflections
b = 17.8037 (18) Å	θ = 2.7–28.2°
c = 11.3621 (12) Å	µ = 3.12 mm^−1
β = 94.319 (1)°	T = 298 K
V = 1905.6 (3) Å^3	Bloc
Z = 2	0.38 × 0.36 × 0.35 mm

Data collection

Bruker SMART APEXII CCD diffractometer	2288 reflections with I > 2σ(I)
phi and ω scans	Rint = 0.082
Absorption correction: multi-scan	θmax = 25.0°, θmin = 2.7°
Tmin = 0.745, Tmax = 0.811	h = −11→11
9042 measured reflections	k = −16→21
3327 independent reflections	l = −12→13

Refinement

Refinement on F^2	329 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.067	H-atom parameters constrained
wR(F^2) = 0.170	w = 1/[σ^2(Fo^2) + (0.080P)^2 + 7.4231P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max < 0.001
3327 reflections	Δρmax = 1.78 e Å^−3
204 parameters	Δρmin = −1.67 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
N1	0.5760 (17)	0.1834 (10)	0.6727 (16)	0.131 (7)
O1	0.9415 (10)	0.2380 (4)	0.5147 (7)	0.050 (2)
O2	1.0858 (9)	0.2142 (4)	0.6707 (7)	0.043 (2)
O3	1.1761 (10)	0.0342 (4)	0.6721 (7)	0.054 (2)
O4	1.1656 (10)	−0.0861 (4)	0.6083 (7)	0.045 (2)
O5	1.1811 (12)	0.1359 (5)	0.4483 (9)	0.067 (3)
O6	1.1109 (9)	0.0198 (5)	0.4182 (7)	0.047 (2)
O7	0.960 (3)	0.0864 (12)	0.806 (2)	0.200 (9)
H7B	0.996711	0.042940	0.812685	0.239*
H7C	0.871131	0.077730	0.802595	0.239*
O8	0.7725 (15)	0.1289 (8)	0.6557 (12)	0.107 (3)
Sm1	0.98307 (7)	0.10172 (3)	0.57024 (5)	0.0331 (3)
C1	1.0262 (15)	0.2593 (7)	0.5985 (11)	0.046 (2)
C2	1.0571 (9)	0.3439 (2)	0.6114 (6)	0.0369 (19)
C3	0.9973 (8)	0.3964 (3)	0.5317 (5)	0.0405 (19)
H3	0.934790	0.380859	0.469350	0.049*
C4	1.0311 (8)	0.4720 (3)	0.5453 (6)	0.039 (2)
C5	1.1246 (8)	0.4952 (2)	0.6386 (6)	0.039 (2)
H5	1.147183	0.545845	0.647681	0.047*
C6	1.1843 (8)	0.4428 (3)	0.7182 (5)	0.039 (2)
C7	1.1506 (9)	0.3671 (3)	0.7046 (6)	0.040 (2)
H7	1.190545	0.332046	0.757884	0.048*
C8	1.2112 (15)	−0.0351 (7)	0.6779 (11)	0.048 (3)
C9	1.1989 (17)	0.0744 (9)	0.3971 (13)	0.059 (3)
C10	1.320 (3)	0.0556 (14)	0.326 (2)	0.129 (8)
H10A	1.297538	0.070500	0.245797	0.193*
H10B	1.336558	0.002489	0.329685	0.193*
H10C	1.403055	0.081768	0.357628	0.193*
C12	0.7124 (17)	0.1684 (12)	0.7260 (15)	0.107 (3)
C13	0.751 (3)	0.2043 (18)	0.843 (2)	0.177 (8)
H13A	0.713251	0.174928	0.904201	0.265*
H13B	0.711806	0.254060	0.843608	0.265*
H13C	0.852337	0.206956	0.856156	0.265*
C14	0.531 (3)	0.1401 (18)	0.5665 (19)	0.184 (9)
H14A	0.608508	0.109295	0.544837	0.275*
H14B	0.503644	0.173870	0.503059	0.275*
H14C	0.452132	0.108719	0.582240	0.275*
C15	0.464 (2)	0.2266 (17)	0.724 (2)	0.166 (8)
H15A	0.429071	0.198884	0.788757	0.249*
H15B	0.387217	0.235212	0.665338	0.249*
H15C	0.501182	0.273896	0.752692	0.249*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
N1	0.124 (10)	0.132 (10)	0.137 (10)	0.007 (8)	0.008 (8)	0.004 (8)
O1	0.062 (5)	0.031 (4)	0.052 (5)	0.003 (4)	−0.032 (4)	−0.007 (4)
O2	0.060 (5)	0.023 (4)	0.041 (4)	0.005 (4)	−0.023 (4)	−0.002 (3)
O3	0.075 (6)	0.030 (4)	0.050 (5)	0.000 (4)	−0.036 (4)	−0.004 (4)
O4	0.065 (5)	0.025 (4)	0.040 (4)	0.002 (4)	−0.027 (4)	−0.003 (3)
O5	0.089 (6)	0.039 (5)	0.076 (6)	−0.017 (5)	0.027 (5)	−0.008 (4)
O6	0.054 (5)	0.033 (4)	0.055 (5)	−0.013 (4)	0.013 (4)	−0.006 (4)
O7	0.205 (16)	0.151 (14)	0.243 (17)	−0.041 (13)	0.021 (14)	−0.005 (13)
O8	0.107 (5)	0.102 (5)	0.116 (5)	0.007 (5)	0.031 (4)	−0.022 (4)
Sm1	0.0438 (4)	0.0164 (3)	0.0361 (4)	0.0034 (3)	−0.0156 (2)	−0.0042 (3)
C1	0.053 (4)	0.037 (4)	0.045 (4)	0.004 (4)	−0.007 (4)	−0.006 (4)
C2	0.046 (4)	0.028 (3)	0.034 (4)	0.002 (3)	−0.013 (3)	0.002 (3)
C3	0.049 (4)	0.032 (4)	0.037 (3)	−0.002 (3)	−0.019 (3)	0.000 (3)
C4	0.047 (4)	0.032 (4)	0.035 (4)	−0.001 (3)	−0.019 (3)	0.008 (3)
C5	0.047 (4)	0.029 (4)	0.039 (4)	−0.002 (3)	−0.020 (3)	−0.001 (3)
C6	0.047 (4)	0.031 (4)	0.037 (4)	0.001 (3)	−0.017 (3)	0.001 (3)
C7	0.048 (4)	0.034 (4)	0.036 (4)	0.001 (3)	−0.015 (3)	0.002 (3)
C8	0.056 (6)	0.036 (5)	0.049 (6)	−0.004 (5)	−0.009 (5)	0.002 (5)
C9	0.070 (6)	0.049 (6)	0.060 (6)	−0.011 (5)	0.017 (5)	−0.001 (5)
C10	0.130 (14)	0.128 (14)	0.134 (13)	−0.015 (12)	0.041 (12)	−0.022 (12)
C12	0.107 (5)	0.102 (5)	0.116 (5)	0.007 (5)	0.031 (4)	−0.022 (4)
C13	0.171 (13)	0.174 (13)	0.188 (13)	0.009 (12)	0.037 (12)	−0.048 (12)
C14	0.180 (14)	0.194 (14)	0.180 (14)	0.010 (12)	0.032 (12)	−0.017 (12)
C15	0.156 (13)	0.175 (13)	0.170 (13)	0.039 (12)	0.036 (12)	−0.025 (12)

Geometric parameters (Å, º)

N1—C12	1.407 (7)	O7—Sm1	2.71 (2)
N1—C15	1.468 (6)	O8—C12	1.235 (9)
N1—C14	1.468 (6)	O8—Sm1	2.329 (13)
O1—C1	1.255 (14)	Sm1—Sm1^i	3.9806 (11)
O1—Sm1	2.531 (8)	C1—C2	1.539 (13)
O2—C1	1.252 (14)	C2—C3	1.3900
O2—Sm1	2.467 (7)	C2—C7	1.3900
O3—C8	1.278 (14)	C3—C4	1.3900
O3—Sm1	2.407 (8)	C4—C5	1.3900
O4—C8	1.258 (14)	C4—C4^ii	1.519 (7)
O4—Sm1^i	2.395 (7)	C5—C6	1.3900
O5—C9	1.258 (17)	C6—C7	1.3900
O5—Sm1	2.486 (10)	C6—C8^iii	1.532 (13)
O6—C9	1.313 (16)	C9—C10	1.48 (3)
O6—Sm1^i	2.346 (8)	C12—C13	1.494 (10)
O6—Sm1	2.624 (8)
C12—N1—C15	126.4 (13)	O6^i—Sm1—O7	78.1 (5)
C12—N1—C14	116.9 (8)	O4^i—Sm1—O7	137.5 (6)
C15—N1—C14	115.5 (8)	O3—Sm1—O7	65.8 (6)
C1—O1—Sm1	91.3 (7)	O2—Sm1—O7	71.6 (5)
C1—O2—Sm1	94.3 (7)	O5—Sm1—O7	133.9 (6)
C8—O3—Sm1	133.8 (8)	O1—Sm1—O7	108.6 (5)
C8—O4—Sm1^i	140.2 (8)	O6—Sm1—O7	132.0 (5)
C9—O5—Sm1	100.2 (9)	O8—Sm1—Sm1^i	116.9 (4)
C9—O6—Sm1^i	160.2 (9)	O6^i—Sm1—Sm1^i	39.2 (2)
C9—O6—Sm1	92.2 (8)	O4^i—Sm1—Sm1^i	67.30 (18)
Sm1^i—O6—Sm1	106.3 (3)	O3—Sm1—Sm1^i	69.96 (18)
C12—O8—Sm1	146.8 (14)	O2—Sm1—Sm1^i	152.0 (2)
O8—Sm1—O6^i	80.2 (4)	O5—Sm1—Sm1^i	85.0 (2)
O8—Sm1—O4^i	85.0 (4)	O1—Sm1—Sm1^i	142.02 (19)
O6^i—Sm1—O4^i	74.9 (3)	O6—Sm1—Sm1^i	34.45 (17)
O8—Sm1—O3	122.9 (4)	O7—Sm1—Sm1^i	108.6 (5)
O6^i—Sm1—O3	77.8 (3)	O2—C1—O1	122.2 (11)
O4^i—Sm1—O3	136.4 (3)	O2—C1—C2	119.6 (10)
O8—Sm1—O2	87.6 (4)	O1—C1—C2	118.2 (10)
O6^i—Sm1—O2	149.3 (3)	C3—C2—C7	120.0
O4^i—Sm1—O2	132.2 (2)	C3—C2—C1	122.1 (6)
O3—Sm1—O2	85.7 (2)	C7—C2—C1	117.9 (6)
O8—Sm1—O5	152.1 (5)	C4—C3—C2	120.0
O6^i—Sm1—O5	124.1 (3)	C3—C4—C5	120.0
O4^i—Sm1—O5	88.5 (3)	C3—C4—C4^ii	119.1 (8)
O3—Sm1—O5	79.4 (4)	C5—C4—C4^ii	120.9 (8)
O2—Sm1—O5	76.9 (3)	C4—C5—C6	120.0
O8—Sm1—O1	77.5 (4)	C7—C6—C5	120.0
O6^i—Sm1—O1	147.8 (3)	C7—C6—C8^iii	117.6 (6)
O4^i—Sm1—O1	80.2 (2)	C5—C6—C8^iii	122.4 (6)
O3—Sm1—O1	134.2 (3)	C6—C7—C2	120.0
O2—Sm1—O1	52.1 (2)	O4—C8—O3	126.0 (11)
O5—Sm1—O1	74.6 (3)	O4—C8—C6^iv	118.0 (11)
O8—Sm1—O6	147.1 (4)	O3—C8—C6^iv	115.9 (10)
O6^i—Sm1—O6	73.7 (3)	O5—C9—O6	116.8 (13)
O4^i—Sm1—O6	69.3 (3)	O5—C9—C10	125.7 (16)
O3—Sm1—O6	70.7 (3)	O6—C9—C10	117.1 (15)
O2—Sm1—O6	124.8 (3)	O8—C12—N1	106.3 (13)
O5—Sm1—O6	50.7 (3)	O8—C12—C13	136.6 (19)
O1—Sm1—O6	116.0 (3)	N1—C12—C13	117.1 (17)
O8—Sm1—O7	58.3 (7)

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y+1, −z+1; (iii) −x+5/2, y+1/2, −z+3/2; (iv) −x+5/2, y−1/2, −z+3/2.