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The title complex (systematic name: diaqua­{6,6′-dimeth­oxy-2,2′-[1,2-ethanediylbis(nitrilo­methyl­idyne)]­diphenolato}­di­nitrato­samarium(III)copper(II) nitrate), [CuSm(C18H18N2O4)(NO3)2(H2O)2]NO3, is composed of a discrete dinuclear cation with a salen-type Schiff base ligand and one uncoordinated nitrate anion. The copper and samarium are doubly bridged by two phenolate O atoms provided by the Schiff base ligand. There are some classical inter­molecular hydrogen bonds (O—H...O), and some weak O...Cu and N...Cu inter­actions are also observed. These inter­actions generate a two-dimensional infinite layer.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806032120/at2085sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806032120/at2085Isup2.hkl
Contains datablock I

CCDC reference: 620634

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.028
  • wR factor = 0.104
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O9 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N5 PLAT245_ALERT_2_C U(iso) H12B Smaller than U(eq) O12 by ... 0.02 AngSq
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 0 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: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: APEX2; program(s) used to refine structure: APEX2; molecular graphics: APEX2; software used to prepare material for publication: APEX2.

Diaqua{6,6'-dimethoxy-2,2'-[1,2- ethanediylbis(nitrilomethylidyne)]diphenolato}dinitratosamarium(III)copper(II) nitrate top
Crystal data top
[CuSm(C18H18N2O4)(NO3)2(H2O)2]NO3F(000) = 1504
Mr = 762.30Dx = 2.005 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 16313 reflections
a = 9.1526 (3) Åθ = 1.9–26.0°
b = 21.6121 (7) ŵ = 3.23 mm1
c = 13.4409 (4) ÅT = 296 K
β = 108.196 (1)°Block, red
V = 2525.75 (14) Å30.28 × 0.17 × 0.15 mm
Z = 4
Data collection top
Bruker APEX-II area-detector
diffractometer
4906 independent reflections
Radiation source: fine-focus sealed tube4310 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 0 pixels mm-1θmax = 26.0°, θmin = 1.9°
φ and ω scansh = 1011
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
k = 2626
Tmin = 0.528, Tmax = 0.622l = 1616
16313 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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.084P)2 + 0.4122P]
where P = (Fo2 + 2Fc2)/3
4906 reflections(Δ/σ)max = 0.001
379 parametersΔρmax = 0.68 e Å3
6 restraintsΔρmin = 0.81 e Å3
Special details top

Experimental. IR (KBr, cm-1): 1638 (C=N), 1385, 1490 (nitrate).

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*/Ueq
Sm10.33576 (2)0.152879 (8)0.644834 (15)0.02714 (10)
Cu10.40856 (5)0.296609 (19)0.55545 (4)0.02686 (13)
O20.2505 (3)0.26033 (11)0.6011 (2)0.0286 (6)
O10.4955 (3)0.21498 (11)0.5708 (2)0.0265 (5)
O60.6205 (4)0.15087 (11)0.7735 (2)0.0376 (7)
O30.5308 (3)0.09452 (12)0.5650 (2)0.0316 (6)
O40.0887 (3)0.19543 (12)0.6849 (2)0.0322 (6)
O110.2086 (4)0.15571 (14)0.4508 (2)0.0416 (8)
O50.4992 (3)0.23461 (13)0.7850 (2)0.0373 (7)
O70.7446 (3)0.22838 (14)0.8651 (2)0.0384 (7)
C20.6182 (4)0.13160 (19)0.5174 (3)0.0280 (8)
N10.5736 (4)0.33252 (16)0.5169 (3)0.0319 (7)
N30.6212 (4)0.20505 (15)0.8083 (2)0.0302 (7)
O120.1642 (4)0.06441 (16)0.5747 (3)0.0513 (9)
O100.3984 (5)0.04504 (16)0.9190 (3)0.0628 (11)
C30.5962 (4)0.19571 (17)0.5243 (3)0.0252 (8)
N40.3767 (4)0.07320 (16)0.8375 (3)0.0393 (8)
C80.6751 (5)0.30294 (19)0.4887 (3)0.0321 (9)
H80.74770.32610.46940.039*
O90.4050 (4)0.05033 (14)0.7593 (3)0.0507 (8)
O80.3243 (4)0.12759 (15)0.8269 (2)0.0445 (8)
C160.0597 (6)0.3512 (2)0.7150 (4)0.0413 (11)
H160.12860.37070.74310.050*
C130.1525 (4)0.29259 (16)0.6351 (3)0.0249 (7)
C150.0430 (5)0.2876 (2)0.7213 (3)0.0346 (9)
H150.10230.26430.75240.041*
C50.7877 (5)0.2104 (2)0.4369 (3)0.0415 (10)
H50.84690.23670.41040.050*
C120.1305 (5)0.35720 (17)0.6260 (3)0.0293 (8)
C110.2183 (5)0.39658 (17)0.5770 (3)0.0315 (8)
H110.19340.43840.57000.038*
C40.6857 (4)0.23581 (19)0.4843 (3)0.0298 (8)
C70.7166 (5)0.1087 (2)0.4682 (3)0.0415 (10)
H70.72530.06610.46140.050*
C140.0601 (4)0.25859 (17)0.6819 (3)0.0262 (8)
C60.8031 (6)0.1482 (2)0.4285 (4)0.0458 (12)
H60.87140.13240.39620.055*
C180.0159 (5)0.15646 (19)0.7177 (4)0.0361 (10)
H18A0.01010.16650.78840.054*
H18B0.01180.11390.71410.054*
H18C0.11890.16310.67250.054*
C170.0250 (5)0.3854 (2)0.6677 (4)0.0392 (10)
H170.01240.42810.66300.047*
C10.6092 (6)0.0393 (2)0.6155 (4)0.0467 (11)
H1A0.64290.01570.56630.070*
H1B0.54000.01480.64010.070*
H1C0.69650.05080.67370.070*
N20.3248 (4)0.37834 (14)0.5437 (3)0.0321 (7)
C90.5705 (5)0.40028 (19)0.5181 (4)0.0398 (10)
H9A0.61550.41680.46720.048*
H9B0.62890.41560.58690.048*
C100.4022 (6)0.42016 (19)0.4909 (4)0.0404 (10)
H10A0.39600.46240.51380.049*
H10B0.35310.41830.41570.049*
N50.0308 (5)0.03323 (17)0.2889 (3)0.0401 (9)
O140.0013 (4)0.02785 (16)0.3724 (3)0.0563 (9)
O150.0256 (5)0.00207 (18)0.2159 (3)0.0698 (12)
O130.1222 (5)0.07411 (19)0.2840 (3)0.0712 (12)
H11A0.198 (8)0.1299 (17)0.404 (3)0.08 (2)*
H11B0.208 (7)0.1910 (10)0.430 (4)0.055 (16)*
H12B0.120 (5)0.0575 (19)0.5116 (15)0.031 (12)*
H12A0.138 (7)0.037 (2)0.608 (3)0.09 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.02798 (16)0.02291 (14)0.03121 (15)0.00062 (7)0.01022 (10)0.00116 (7)
Cu10.0285 (3)0.0201 (2)0.0360 (3)0.00052 (17)0.0159 (2)0.00332 (18)
O20.0293 (15)0.0211 (13)0.0418 (15)0.0035 (10)0.0203 (12)0.0051 (11)
O10.0268 (14)0.0233 (12)0.0344 (13)0.0025 (10)0.0170 (11)0.0009 (10)
O60.0391 (19)0.0278 (15)0.0405 (17)0.0030 (11)0.0047 (14)0.0086 (11)
O30.0276 (15)0.0259 (13)0.0436 (16)0.0060 (11)0.0143 (12)0.0010 (12)
O40.0282 (15)0.0279 (14)0.0452 (16)0.0014 (11)0.0180 (13)0.0097 (12)
O110.057 (2)0.0312 (17)0.0301 (16)0.0075 (13)0.0040 (15)0.0035 (12)
O50.0337 (17)0.0357 (16)0.0414 (16)0.0028 (12)0.0102 (13)0.0090 (13)
O70.0335 (17)0.0431 (17)0.0348 (15)0.0114 (13)0.0052 (12)0.0068 (13)
C20.023 (2)0.0304 (19)0.0288 (18)0.0043 (15)0.0061 (15)0.0024 (16)
N10.032 (2)0.0304 (16)0.0327 (17)0.0076 (14)0.0089 (15)0.0059 (14)
N30.0317 (19)0.0354 (18)0.0251 (15)0.0026 (14)0.0109 (14)0.0002 (13)
O120.064 (2)0.0436 (19)0.0381 (17)0.0301 (17)0.0048 (16)0.0032 (15)
O100.095 (3)0.0445 (19)0.0379 (18)0.0092 (18)0.0052 (18)0.0182 (15)
C30.0197 (19)0.033 (2)0.0228 (17)0.0007 (14)0.0072 (14)0.0003 (14)
N40.042 (2)0.0322 (19)0.0381 (19)0.0063 (15)0.0043 (16)0.0060 (15)
C80.027 (2)0.043 (2)0.0263 (19)0.0088 (16)0.0087 (16)0.0050 (16)
O90.070 (2)0.0328 (16)0.0517 (19)0.0053 (15)0.0222 (17)0.0033 (15)
O80.057 (2)0.0403 (17)0.0418 (17)0.0159 (15)0.0238 (16)0.0126 (14)
C160.036 (3)0.046 (3)0.046 (3)0.0113 (18)0.019 (2)0.0069 (19)
C130.024 (2)0.0243 (18)0.0258 (17)0.0027 (14)0.0074 (14)0.0003 (14)
C150.023 (2)0.048 (2)0.034 (2)0.0035 (17)0.0111 (16)0.0030 (18)
C50.029 (2)0.066 (3)0.035 (2)0.002 (2)0.0183 (18)0.006 (2)
C120.031 (2)0.0255 (18)0.031 (2)0.0062 (15)0.0081 (16)0.0007 (15)
C110.034 (2)0.0184 (17)0.040 (2)0.0021 (15)0.0093 (18)0.0016 (15)
C40.024 (2)0.041 (2)0.0252 (18)0.0008 (15)0.0090 (15)0.0019 (16)
C70.038 (3)0.045 (2)0.042 (2)0.0082 (19)0.013 (2)0.009 (2)
C140.0209 (19)0.0296 (19)0.0283 (18)0.0054 (14)0.0078 (15)0.0032 (15)
C60.038 (3)0.065 (3)0.043 (3)0.013 (2)0.025 (2)0.004 (2)
C180.028 (2)0.042 (2)0.042 (2)0.0099 (16)0.0157 (19)0.0065 (17)
C170.039 (3)0.030 (2)0.047 (2)0.0086 (17)0.0121 (19)0.0068 (18)
C10.056 (3)0.031 (2)0.057 (3)0.016 (2)0.023 (2)0.007 (2)
N20.039 (2)0.0204 (16)0.0384 (17)0.0012 (13)0.0136 (15)0.0042 (13)
C90.044 (3)0.029 (2)0.046 (2)0.0136 (18)0.014 (2)0.0024 (18)
C100.054 (3)0.0218 (19)0.049 (3)0.0044 (18)0.023 (2)0.0082 (18)
N50.052 (2)0.0308 (19)0.0369 (19)0.0018 (16)0.0129 (17)0.0010 (15)
O140.076 (3)0.051 (2)0.0473 (19)0.0253 (18)0.0274 (18)0.0049 (16)
O150.104 (4)0.049 (2)0.045 (2)0.017 (2)0.008 (2)0.0116 (17)
O130.099 (3)0.068 (3)0.059 (2)0.042 (2)0.043 (2)0.0140 (19)
Geometric parameters (Å, º) top
Sm1—O12.417 (2)C8—C41.456 (6)
Sm1—O22.462 (2)C8—H80.9300
Sm1—O32.670 (3)C16—C171.364 (7)
Sm1—O42.647 (3)C16—C151.385 (6)
Sm1—O52.674 (3)C16—H160.9300
Sm1—O62.640 (3)C13—C141.408 (5)
Sm1—O82.541 (3)C13—C121.411 (5)
Sm1—O92.659 (3)C15—C141.369 (5)
Sm1—O112.503 (3)C15—H150.9300
Sm1—O122.466 (3)C5—C61.360 (7)
Cu1—N11.908 (3)C5—C41.397 (6)
Cu1—N21.912 (3)C5—H50.9300
Cu1—O11.920 (3)C12—C171.399 (6)
Cu1—O21.908 (3)C12—C111.460 (6)
O2—C131.325 (4)C11—N21.257 (5)
O1—C31.331 (4)C11—H110.9300
O6—N31.260 (4)C7—C61.380 (7)
O3—C21.417 (5)C7—H70.9300
O3—C11.448 (5)C6—H60.9300
O4—C141.388 (4)C18—H18A0.9600
O4—C181.444 (4)C18—H18B0.9600
O11—H11A0.82 (4)C18—H18C0.9600
O11—H11B0.81 (2)C17—H170.9300
O5—N31.239 (4)C1—H1A0.9600
O7—N31.254 (4)C1—H1B0.9600
C2—C71.366 (6)C1—H1C0.9600
C2—C31.407 (5)N2—C101.461 (5)
N1—C81.280 (5)C9—C101.529 (7)
N1—C91.465 (5)C9—H9A0.9700
O12—H12B0.83 (2)C9—H9B0.9700
O12—H12A0.82 (5)C10—H10A0.9700
O10—N41.213 (5)C10—H10B0.9700
C3—C41.409 (5)N5—O151.223 (5)
N4—O91.259 (5)N5—O131.233 (5)
N4—O81.261 (5)N5—O141.250 (5)
O1—Sm1—O264.23 (8)Sm1—O12—H12B125 (3)
O1—Sm1—O361.97 (9)Sm1—O12—H12A128 (3)
O1—Sm1—O4123.77 (8)H12B—O12—H12A107 (3)
O1—Sm1—O569.28 (9)O1—C3—C2118.2 (3)
O1—Sm1—O671.26 (9)O1—C3—C4123.8 (3)
O1—Sm1—O8136.76 (10)C2—C3—C4117.9 (3)
O1—Sm1—O9129.48 (10)O10—N4—O9122.5 (4)
O1—Sm1—O1172.61 (10)O10—N4—O8121.3 (4)
O1—Sm1—O12131.91 (10)O9—N4—O8116.2 (3)
O2—Sm1—O3123.48 (8)N1—C8—C4125.0 (4)
O2—Sm1—O459.58 (8)N1—C8—H8117.5
O2—Sm1—O567.10 (9)C4—C8—H8117.5
O2—Sm1—O6110.26 (8)N4—O9—Sm194.7 (2)
O2—Sm1—O8109.11 (9)N4—O8—Sm1100.4 (2)
O2—Sm1—O9157.62 (10)C17—C16—C15119.9 (4)
O2—Sm1—O1173.67 (10)C17—C16—H16120.1
O2—Sm1—O12121.57 (11)C15—C16—H16120.1
O3—Sm1—O5107.35 (9)O2—C13—C14116.4 (3)
O4—Sm1—O3165.20 (9)O2—C13—C12125.8 (3)
O4—Sm1—O587.27 (9)C14—C13—C12117.8 (3)
O4—Sm1—O9103.66 (10)C14—C15—C16120.5 (4)
O6—Sm1—O366.95 (9)C14—C15—H15119.7
O6—Sm1—O4127.11 (9)C16—C15—H15119.7
O6—Sm1—O547.82 (8)C6—C5—C4121.9 (4)
O6—Sm1—O966.36 (10)C6—C5—H5119.1
O8—Sm1—O3121.29 (9)C4—C5—H5119.1
O8—Sm1—O465.42 (9)C17—C12—C13119.6 (4)
O8—Sm1—O569.25 (10)C17—C12—C11118.2 (4)
O8—Sm1—O672.22 (11)C13—C12—C11122.2 (4)
O8—Sm1—O948.52 (10)N2—C11—C12125.1 (3)
O9—Sm1—O376.73 (10)N2—C11—H11117.5
O9—Sm1—O599.38 (10)C12—C11—H11117.5
O11—Sm1—O375.18 (11)C5—C4—C3118.9 (4)
O11—Sm1—O493.15 (11)C5—C4—C8118.2 (4)
O11—Sm1—O5133.95 (9)C3—C4—C8122.9 (3)
O11—Sm1—O6136.53 (12)C2—C7—C6120.5 (4)
O11—Sm1—O8149.67 (12)C2—C7—H7119.8
O11—Sm1—O9124.93 (10)C6—C7—H7119.8
O12—Sm1—O384.61 (11)C15—C14—O4125.8 (3)
O12—Sm1—O482.24 (11)C15—C14—C13121.1 (4)
O12—Sm1—O5158.53 (11)O4—C14—C13113.1 (3)
O12—Sm1—O6128.16 (11)C5—C6—C7119.5 (4)
O12—Sm1—O889.33 (11)C5—C6—H6120.2
O12—Sm1—O965.37 (11)C7—C6—H6120.2
O12—Sm1—O1165.65 (10)O4—C18—H18A109.5
N1—Cu1—N286.14 (15)O4—C18—H18B109.5
N1—Cu1—O193.79 (14)H18A—C18—H18B109.5
N2—Cu1—O1178.59 (14)O4—C18—H18C109.5
O2—Cu1—N1177.06 (13)H18A—C18—H18C109.5
O2—Cu1—N294.68 (13)H18B—C18—H18C109.5
O2—Cu1—O185.32 (11)C16—C17—C12121.0 (4)
Cu1—O1—Sm1105.71 (10)C16—C17—H17119.5
C13—O2—Cu1123.9 (2)C12—C17—H17119.5
C13—O2—Sm1127.8 (2)O3—C1—H1A109.5
Cu1—O2—Sm1104.40 (11)O3—C1—H1B109.5
C3—O1—Cu1124.2 (2)H1A—C1—H1B109.5
C3—O1—Sm1128.0 (2)O3—C1—H1C109.5
N3—O6—Sm196.8 (2)H1A—C1—H1C109.5
C2—O3—C1114.3 (3)H1B—C1—H1C109.5
C2—O3—Sm1117.2 (2)C11—N2—C10121.8 (3)
C1—O3—Sm1119.7 (2)C11—N2—Cu1126.6 (3)
C14—O4—C18116.4 (3)C10—N2—Cu1111.6 (3)
C14—O4—Sm1120.1 (2)N1—C9—C10107.4 (3)
C18—O4—Sm1123.3 (2)N1—C9—H9A110.2
Sm1—O11—H11A133 (4)C10—C9—H9A110.2
Sm1—O11—H11B110 (3)N1—C9—H9B110.2
H11A—O11—H11B112 (3)C10—C9—H9B110.2
N3—O5—Sm195.7 (2)H9A—C9—H9B108.5
C7—C2—C3121.2 (4)N2—C10—C9108.3 (3)
C7—C2—O3124.3 (4)N2—C10—H10A110.0
C3—C2—O3114.5 (3)C9—C10—H10A110.0
C8—N1—C9121.4 (3)N2—C10—H10B110.0
C8—N1—Cu1126.0 (3)C9—C10—H10B110.0
C9—N1—Cu1112.6 (3)H10A—C10—H10B108.4
O5—N3—O7121.0 (3)O15—N5—O13121.8 (4)
O5—N3—O6119.0 (3)O15—N5—O14120.2 (4)
O7—N3—O6119.9 (3)O13—N5—O14117.9 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O12—H12A···O14i0.82 (5)1.95 (3)2.714 (4)154 (5)
O12—H12B···O140.83 (2)1.96 (2)2.783 (5)169 (4)
O11—H11A···O130.82 (4)1.96 (3)2.767 (5)166 (7)
O11—H11B···O7ii0.81 (2)2.02 (2)2.819 (4)167 (5)
Symmetry codes: (i) x, y, z+1; (ii) x1/2, y+1/2, z1/2.
 

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