metal-organic compounds
Bis(μ-3-nitrobenzene-1,2-dicarboxylato)-κ4O1,O2:O1,O1′;κ4O1,O1′:O1,O2-bis[triaqua(6-carboxy-2-nitrobenzoato-κ2O1,O6)neodymium(III)] dihydrate
aCollege of Science, Northwest A&F University, Yangling 712100, Shanxi Province, People's Republic of China
*Correspondence e-mail: peizc@nwsuaf.edu.cn, shuaiqi@nwsuaf.edu.cn
The title complex, [Nd2(C8H3NO6)2(C8H4NO6)2(H2O)6]·2H2O, consists of dimeric units related by an inversion center. The NdIII atom is nine-coordinated by three O atoms from water molecules and six from carboxylate atoms. The 1,2-dicarboxylate acid molecules are in a single and double deprotonation stage and exhibit two coordination modes, viz. μ2-(κ4, O1: O2: O2: O3) and μ1-(κ2, O2: O3), which are responsible for the dimeric structure framework. The dimeric structure is then assembled into a three-dimensional supramolecular framework via O—H⋯O hydrogen bonds.
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536812042754/vn2055sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812042754/vn2055Isup2.hkl
A mixture of neodymium chloride hexahydrate (0.03585 g, 0.1 mmol), sodium hydroxide (0.0080 g, 0.2 mmol), 3-nitrobenzene-1,2-dicarboxylic acid (0.0211 g, 0.1 mmol), and CH3OH (20 mL) was placed in a Parr Teflon-lined stainless stell vessel (25 ml), which was sealed and heated at 443.15 K for 4 days. Then the vessel was cooled to 373.15 K at a rate of 5 K h-1 and subsequently slowly to room temperature. Purple, block single crystals suitable for X-ray diffraction were obtained.
H atoms bonded to C atoms were placed geometrically and treated as riding, with C—H distances 0.93 Å for aryl type H-atoms, respectively with Uiso(H) = 1.2Ueq(C). H atoms attached to O atoms were found in a difference Fourier synthesis and were refined using a riding model, with the O–H distances fixed as initially found and with Uiso(H) values set at 1.2 Ueq(O). Positive and negative residual densities close to oxygen positions are most probably due to different orientational conformations of water molecules or hydroxyl groups. The most likely orientations were retained.
Data collection: SMART (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. Coordination environment of NdIII atoms; atoms are shown as 30% probability ellipsoids. Symmetry codes: (A) 1 - x, 1 - y, 1 - z; | |
Fig. 2. Coordination modes of 3-Nitrobenzene-1,2-dicarboxylic acid ligands in the title complex. Hydrogen atoms are omitted for clarity. |
[Nd2(C8H3NO6)2(C8H4NO6)2(H2O)6]·2H2O | Z = 1 |
Mr = 1271.08 | F(000) = 626 |
Triclinic, P1 | Dx = 2.041 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1460 (7) Å | Cell parameters from 2861 reflections |
b = 8.8090 (9) Å | θ = 2.6–27.9° |
c = 15.1670 (13) Å | µ = 2.60 mm−1 |
α = 100.434 (1)° | T = 298 K |
β = 91.106 (1)° | Block, purple |
γ = 104.482 (2)° | 0.16 × 0.14 × 0.10 mm |
V = 1033.96 (16) Å3 |
Bruker SMART CCD area-detector diffractometer | 3618 independent reflections |
Radiation source: fine-focus sealed tube | 3196 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
phi and ω scans | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | h = −9→8 |
Tmin = 0.681, Tmax = 0.781 | k = −10→10 |
5316 measured reflections | l = −14→18 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0341P)2] where P = (Fo2 + 2Fc2)/3 |
3618 reflections | (Δ/σ)max = 0.001 |
317 parameters | Δρmax = 1.51 e Å−3 |
0 restraints | Δρmin = −0.88 e Å−3 |
[Nd2(C8H3NO6)2(C8H4NO6)2(H2O)6]·2H2O | γ = 104.482 (2)° |
Mr = 1271.08 | V = 1033.96 (16) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.1460 (7) Å | Mo Kα radiation |
b = 8.8090 (9) Å | µ = 2.60 mm−1 |
c = 15.1670 (13) Å | T = 298 K |
α = 100.434 (1)° | 0.16 × 0.14 × 0.10 mm |
β = 91.106 (1)° |
Bruker SMART CCD area-detector diffractometer | 3618 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | 3196 reflections with I > 2σ(I) |
Tmin = 0.681, Tmax = 0.781 | Rint = 0.030 |
5316 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.51 e Å−3 |
3618 reflections | Δρmin = −0.88 e Å−3 |
317 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Nd1 | 0.34954 (3) | 0.61211 (3) | 0.432565 (17) | 0.02109 (10) | |
N1 | 0.6299 (5) | 0.3586 (5) | 0.0945 (3) | 0.0357 (11) | |
N2 | 1.0429 (5) | 0.8971 (5) | 0.8325 (3) | 0.0338 (10) | |
O1 | 0.2534 (4) | 0.6797 (4) | 0.2912 (2) | 0.0323 (8) | |
O2 | 0.0666 (4) | 0.6809 (4) | 0.1849 (2) | 0.0387 (9) | |
H2 | 0.0399 | 0.7439 | 0.2253 | 0.058* | |
O3 | 0.5209 (4) | 0.5333 (4) | 0.3102 (2) | 0.0239 (7) | |
O4 | 0.6217 (4) | 0.7219 (4) | 0.2293 (2) | 0.0317 (8) | |
O5 | 0.7245 (5) | 0.4265 (5) | 0.1614 (3) | 0.0525 (11) | |
O6 | 0.6688 (5) | 0.2711 (5) | 0.0317 (3) | 0.0594 (12) | |
O7 | 0.4497 (4) | 0.8304 (4) | 0.5729 (2) | 0.0313 (8) | |
O8 | 0.5879 (4) | 0.6447 (3) | 0.5528 (2) | 0.0222 (7) | |
O9 | 1.0001 (4) | 0.8529 (4) | 0.6082 (2) | 0.0354 (9) | |
O10 | 0.8932 (4) | 0.6062 (4) | 0.6320 (2) | 0.0282 (8) | |
O11 | 1.1186 (5) | 0.8219 (6) | 0.7825 (3) | 0.0686 (15) | |
O12 | 1.1035 (5) | 0.9742 (6) | 0.9051 (3) | 0.0666 (14) | |
O13 | 0.2084 (4) | 0.5262 (4) | 0.5708 (2) | 0.0362 (9) | |
H13C | 0.2752 | 0.5118 | 0.6104 | 0.043* | |
H13D | 0.1227 | 0.5482 | 0.5960 | 0.043* | |
O14 | 0.5560 (4) | 0.8539 (4) | 0.4017 (2) | 0.0363 (9) | |
H14B | 0.5211 | 0.9371 | 0.4185 | 0.044* | |
H14C | 0.5732 | 0.8444 | 0.3461 | 0.044* | |
O15 | 0.1355 (4) | 0.7563 (4) | 0.4572 (2) | 0.0374 (9) | |
H15C | 0.0946 | 0.7860 | 0.5066 | 0.045* | |
H15D | 0.0798 | 0.7770 | 0.4150 | 0.045* | |
O16 | 0.9404 (4) | 0.8298 (4) | 0.3189 (2) | 0.0382 (9) | |
H16C | 0.8423 | 0.7975 | 0.2915 | 0.046* | |
H16D | 0.9577 | 0.9285 | 0.3414 | 0.046* | |
C1 | 0.1920 (6) | 0.6321 (6) | 0.2148 (3) | 0.0278 (11) | |
C2 | 0.5315 (6) | 0.5899 (5) | 0.2390 (3) | 0.0249 (11) | |
C3 | 0.2498 (6) | 0.5176 (6) | 0.1470 (3) | 0.0264 (11) | |
C4 | 0.4139 (6) | 0.4937 (5) | 0.1582 (3) | 0.0244 (11) | |
C5 | 0.4606 (6) | 0.3880 (5) | 0.0893 (3) | 0.0292 (11) | |
C6 | 0.3539 (7) | 0.3078 (6) | 0.0136 (4) | 0.0395 (14) | |
H6 | 0.3899 | 0.2386 | −0.0312 | 0.047* | |
C7 | 0.1944 (7) | 0.3323 (6) | 0.0059 (4) | 0.0397 (14) | |
H7 | 0.1217 | 0.2795 | −0.0444 | 0.048* | |
C8 | 0.1426 (7) | 0.4342 (6) | 0.0721 (3) | 0.0334 (12) | |
H8 | 0.0335 | 0.4480 | 0.0669 | 0.040* | |
C9 | 0.5563 (6) | 0.7666 (5) | 0.6009 (3) | 0.0225 (10) | |
C10 | 0.9095 (6) | 0.7554 (6) | 0.6468 (3) | 0.0258 (11) | |
C11 | 0.6390 (6) | 0.8337 (5) | 0.6931 (3) | 0.0221 (10) | |
C12 | 0.8033 (6) | 0.8239 (5) | 0.7179 (3) | 0.0208 (10) | |
C13 | 0.8675 (6) | 0.8954 (5) | 0.8048 (3) | 0.0244 (11) | |
C14 | 0.7784 (6) | 0.9698 (6) | 0.8671 (3) | 0.0314 (12) | |
H14 | 0.8264 | 1.0151 | 0.9250 | 0.038* | |
C15 | 0.6166 (7) | 0.9762 (6) | 0.8425 (4) | 0.0354 (13) | |
H15 | 0.5539 | 1.0254 | 0.8838 | 0.042* | |
C16 | 0.5485 (6) | 0.9089 (5) | 0.7558 (3) | 0.0271 (11) | |
H16 | 0.4399 | 0.9141 | 0.7391 | 0.032* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.02379 (15) | 0.02005 (14) | 0.01938 (16) | 0.00804 (10) | −0.00171 (10) | 0.00071 (11) |
N1 | 0.037 (3) | 0.030 (2) | 0.040 (3) | 0.009 (2) | 0.014 (2) | 0.002 (2) |
N2 | 0.033 (3) | 0.031 (2) | 0.032 (3) | 0.005 (2) | −0.009 (2) | −0.002 (2) |
O1 | 0.038 (2) | 0.045 (2) | 0.0184 (19) | 0.0203 (17) | −0.0029 (15) | 0.0049 (17) |
O2 | 0.038 (2) | 0.046 (2) | 0.034 (2) | 0.0232 (18) | −0.0095 (17) | −0.0026 (18) |
O3 | 0.0257 (18) | 0.0293 (17) | 0.0194 (18) | 0.0123 (14) | 0.0027 (14) | 0.0043 (15) |
O4 | 0.0310 (19) | 0.0286 (18) | 0.032 (2) | 0.0014 (15) | 0.0011 (15) | 0.0071 (16) |
O5 | 0.040 (2) | 0.063 (3) | 0.053 (3) | 0.025 (2) | −0.002 (2) | −0.009 (2) |
O6 | 0.060 (3) | 0.069 (3) | 0.048 (3) | 0.031 (2) | 0.017 (2) | −0.013 (2) |
O7 | 0.037 (2) | 0.0268 (17) | 0.031 (2) | 0.0167 (15) | −0.0086 (16) | −0.0019 (16) |
O8 | 0.0302 (18) | 0.0204 (16) | 0.0161 (17) | 0.0115 (14) | −0.0017 (13) | −0.0032 (14) |
O9 | 0.039 (2) | 0.0296 (18) | 0.037 (2) | 0.0069 (16) | 0.0173 (17) | 0.0048 (17) |
O10 | 0.0263 (18) | 0.0225 (17) | 0.033 (2) | 0.0081 (14) | −0.0031 (15) | −0.0031 (15) |
O11 | 0.045 (3) | 0.101 (4) | 0.056 (3) | 0.039 (3) | −0.016 (2) | −0.020 (3) |
O12 | 0.056 (3) | 0.078 (3) | 0.052 (3) | 0.025 (2) | −0.032 (2) | −0.029 (3) |
O13 | 0.031 (2) | 0.050 (2) | 0.034 (2) | 0.0165 (17) | 0.0089 (16) | 0.0136 (18) |
O14 | 0.047 (2) | 0.0233 (17) | 0.039 (2) | 0.0116 (16) | 0.0102 (17) | 0.0047 (16) |
O15 | 0.047 (2) | 0.051 (2) | 0.024 (2) | 0.0328 (19) | 0.0043 (16) | 0.0055 (18) |
O16 | 0.042 (2) | 0.0252 (18) | 0.046 (2) | 0.0133 (16) | −0.0067 (18) | −0.0017 (17) |
C1 | 0.027 (3) | 0.029 (3) | 0.028 (3) | 0.008 (2) | 0.002 (2) | 0.009 (2) |
C2 | 0.024 (3) | 0.028 (3) | 0.023 (3) | 0.013 (2) | 0.003 (2) | −0.003 (2) |
C3 | 0.028 (3) | 0.030 (3) | 0.023 (3) | 0.007 (2) | 0.000 (2) | 0.009 (2) |
C4 | 0.027 (3) | 0.024 (2) | 0.022 (3) | 0.005 (2) | 0.003 (2) | 0.006 (2) |
C5 | 0.039 (3) | 0.024 (2) | 0.026 (3) | 0.008 (2) | 0.005 (2) | 0.009 (2) |
C6 | 0.061 (4) | 0.030 (3) | 0.024 (3) | 0.008 (3) | 0.003 (3) | −0.001 (2) |
C7 | 0.049 (4) | 0.037 (3) | 0.027 (3) | 0.006 (3) | −0.015 (3) | 0.000 (3) |
C8 | 0.041 (3) | 0.030 (3) | 0.029 (3) | 0.011 (2) | −0.011 (2) | 0.003 (2) |
C9 | 0.022 (2) | 0.022 (2) | 0.021 (3) | 0.002 (2) | 0.001 (2) | 0.002 (2) |
C10 | 0.022 (3) | 0.031 (3) | 0.021 (3) | 0.010 (2) | −0.005 (2) | −0.005 (2) |
C11 | 0.026 (3) | 0.020 (2) | 0.020 (3) | 0.0053 (19) | 0.002 (2) | 0.002 (2) |
C12 | 0.024 (2) | 0.017 (2) | 0.019 (3) | 0.0029 (19) | −0.0009 (19) | 0.001 (2) |
C13 | 0.030 (3) | 0.019 (2) | 0.023 (3) | 0.006 (2) | −0.001 (2) | 0.001 (2) |
C14 | 0.041 (3) | 0.030 (3) | 0.017 (3) | 0.004 (2) | 0.001 (2) | −0.002 (2) |
C15 | 0.047 (3) | 0.029 (3) | 0.028 (3) | 0.013 (2) | 0.010 (2) | −0.004 (2) |
C16 | 0.026 (3) | 0.026 (2) | 0.029 (3) | 0.011 (2) | 0.004 (2) | 0.000 (2) |
Nd1—O1 | 2.489 (3) | O14—H14B | 0.8500 |
Nd1—O3 | 2.447 (3) | O14—H14C | 0.8500 |
Nd1—O7 | 2.561 (3) | O15—H15C | 0.8500 |
Nd1—O8 | 2.564 (3) | O15—H15D | 0.8500 |
Nd1—O8i | 2.486 (3) | O16—H16C | 0.8500 |
Nd1—O10i | 2.431 (3) | O16—H16D | 0.8499 |
Nd1—O13 | 2.554 (3) | C1—C3 | 1.475 (7) |
Nd1—O14 | 2.487 (3) | C2—C4 | 1.520 (6) |
Nd1—O15 | 2.398 (3) | C3—C8 | 1.390 (6) |
N1—O6 | 1.212 (5) | C3—C4 | 1.416 (6) |
N1—O5 | 1.225 (6) | C4—C5 | 1.394 (7) |
N1—C5 | 1.469 (6) | C5—C6 | 1.391 (7) |
N2—O11 | 1.197 (6) | C6—C7 | 1.376 (8) |
N2—O12 | 1.208 (5) | C6—H6 | 0.9300 |
N2—C13 | 1.477 (6) | C7—C8 | 1.368 (7) |
O1—C1 | 1.211 (6) | C7—H7 | 0.9300 |
O2—C1 | 1.306 (6) | C8—H8 | 0.9300 |
O2—H2 | 0.8200 | C9—C11 | 1.491 (6) |
O3—C2 | 1.265 (6) | C10—C12 | 1.528 (6) |
O4—C2 | 1.246 (5) | C11—C16 | 1.389 (6) |
O7—C9 | 1.252 (5) | C11—C12 | 1.411 (6) |
O8—C9 | 1.270 (5) | C12—C13 | 1.384 (6) |
O8—Nd1i | 2.486 (3) | C13—C14 | 1.375 (7) |
O9—C10 | 1.228 (6) | C14—C15 | 1.381 (7) |
O10—C10 | 1.265 (5) | C14—H14 | 0.9300 |
O10—Nd1i | 2.431 (3) | C15—C16 | 1.383 (7) |
O13—H13C | 0.8500 | C15—H15 | 0.9300 |
O13—H13D | 0.8500 | C16—H16 | 0.9300 |
O15—Nd1—O10i | 82.46 (11) | Nd1—O14—H14C | 111.0 |
O15—Nd1—O3 | 137.86 (11) | H14B—O14—H14C | 109.2 |
O10i—Nd1—O3 | 90.90 (11) | Nd1—O15—H15C | 127.9 |
O15—Nd1—O8i | 142.35 (11) | Nd1—O15—H15D | 123.5 |
O10i—Nd1—O8i | 71.22 (10) | H15C—O15—H15D | 108.3 |
O3—Nd1—O8i | 70.52 (10) | H16C—O16—H16D | 108.4 |
O15—Nd1—O14 | 90.69 (12) | O1—C1—O2 | 121.7 (5) |
O10i—Nd1—O14 | 143.71 (12) | O1—C1—C3 | 124.5 (4) |
O3—Nd1—O14 | 70.66 (11) | O2—C1—C3 | 113.8 (4) |
O8i—Nd1—O14 | 126.35 (11) | O4—C2—O3 | 126.7 (4) |
O15—Nd1—O1 | 68.22 (11) | O4—C2—C4 | 115.8 (4) |
O10i—Nd1—O1 | 73.83 (11) | O3—C2—C4 | 117.3 (4) |
O3—Nd1—O1 | 69.96 (10) | C8—C3—C4 | 120.4 (5) |
O8i—Nd1—O1 | 125.78 (10) | C8—C3—C1 | 119.6 (4) |
O14—Nd1—O1 | 70.56 (12) | C4—C3—C1 | 120.1 (4) |
O15—Nd1—O13 | 75.73 (11) | C5—C4—C3 | 116.2 (4) |
O10i—Nd1—O13 | 76.95 (11) | C5—C4—C2 | 124.1 (4) |
O3—Nd1—O13 | 143.02 (11) | C3—C4—C2 | 119.6 (4) |
O8i—Nd1—O13 | 72.49 (10) | C6—C5—C4 | 123.0 (5) |
O14—Nd1—O13 | 135.72 (11) | C6—C5—N1 | 117.1 (5) |
O1—Nd1—O13 | 135.80 (11) | C4—C5—N1 | 119.9 (4) |
O15—Nd1—O7 | 72.57 (11) | C7—C6—C5 | 119.0 (5) |
O10i—Nd1—O7 | 141.54 (11) | C7—C6—H6 | 120.5 |
O3—Nd1—O7 | 127.18 (11) | C5—C6—H6 | 120.5 |
O8i—Nd1—O7 | 112.88 (10) | C8—C7—C6 | 120.1 (5) |
O14—Nd1—O7 | 66.79 (11) | C8—C7—H7 | 120.0 |
O1—Nd1—O7 | 120.33 (11) | C6—C7—H7 | 120.0 |
O13—Nd1—O7 | 68.93 (11) | C7—C8—C3 | 121.3 (5) |
O15—Nd1—O8 | 121.59 (10) | C7—C8—H8 | 119.4 |
O10i—Nd1—O8 | 133.76 (10) | C3—C8—H8 | 119.4 |
O3—Nd1—O8 | 92.65 (10) | O7—C9—O8 | 120.4 (4) |
O8i—Nd1—O8 | 66.76 (11) | O7—C9—C11 | 118.2 (4) |
O14—Nd1—O8 | 79.62 (11) | O8—C9—C11 | 121.4 (4) |
O1—Nd1—O8 | 149.00 (11) | O9—C10—O10 | 126.6 (4) |
O13—Nd1—O8 | 72.89 (11) | O9—C10—C12 | 115.4 (4) |
O7—Nd1—O8 | 50.55 (9) | O10—C10—C12 | 117.9 (4) |
O6—N1—O5 | 124.0 (5) | C16—C11—C12 | 119.8 (4) |
O6—N1—C5 | 118.1 (5) | C16—C11—C9 | 117.6 (4) |
O5—N1—C5 | 117.9 (4) | C12—C11—C9 | 122.6 (4) |
O11—N2—O12 | 122.9 (5) | C13—C12—C11 | 116.8 (4) |
O11—N2—C13 | 118.9 (4) | C13—C12—C10 | 122.9 (4) |
O12—N2—C13 | 118.2 (4) | C11—C12—C10 | 119.8 (4) |
C1—O1—Nd1 | 147.6 (3) | C14—C13—C12 | 123.6 (4) |
C1—O2—H2 | 109.5 | C14—C13—N2 | 117.4 (4) |
C2—O3—Nd1 | 122.9 (3) | C12—C13—N2 | 119.0 (4) |
C9—O7—Nd1 | 94.6 (3) | C13—C14—C15 | 119.0 (5) |
C9—O8—Nd1i | 140.4 (3) | C13—C14—H14 | 120.5 |
C9—O8—Nd1 | 94.0 (3) | C15—C14—H14 | 120.5 |
Nd1i—O8—Nd1 | 113.24 (11) | C14—C15—C16 | 119.4 (5) |
C10—O10—Nd1i | 129.9 (3) | C14—C15—H15 | 120.3 |
Nd1—O13—H13C | 115.0 | C16—C15—H15 | 120.3 |
Nd1—O13—H13D | 130.1 | C15—C16—C11 | 121.4 (5) |
H13C—O13—H13D | 108.7 | C15—C16—H16 | 119.3 |
Nd1—O14—H14B | 111.1 | C11—C16—H16 | 119.3 |
O15—Nd1—O1—C1 | −122.1 (6) | O4—C2—C4—C5 | 88.0 (6) |
O10i—Nd1—O1—C1 | −33.8 (6) | O3—C2—C4—C5 | −96.1 (6) |
O3—Nd1—O1—C1 | 63.2 (6) | O4—C2—C4—C3 | −87.7 (5) |
O8i—Nd1—O1—C1 | 17.7 (6) | O3—C2—C4—C3 | 88.2 (5) |
O14—Nd1—O1—C1 | 139.0 (6) | C3—C4—C5—C6 | −0.6 (7) |
O13—Nd1—O1—C1 | −84.4 (6) | C2—C4—C5—C6 | −176.4 (5) |
O7—Nd1—O1—C1 | −174.6 (6) | C3—C4—C5—N1 | 178.8 (4) |
O8—Nd1—O1—C1 | 122.5 (6) | C2—C4—C5—N1 | 3.0 (7) |
O15—Nd1—O3—C2 | 12.2 (4) | O6—N1—C5—C6 | 2.4 (7) |
O10i—Nd1—O3—C2 | 91.9 (3) | O5—N1—C5—C6 | −179.0 (5) |
O8i—Nd1—O3—C2 | 161.6 (3) | O6—N1—C5—C4 | −177.0 (5) |
O14—Nd1—O3—C2 | −56.2 (3) | O5—N1—C5—C4 | 1.6 (7) |
O1—Nd1—O3—C2 | 19.5 (3) | C4—C5—C6—C7 | −0.4 (8) |
O13—Nd1—O3—C2 | 161.1 (3) | N1—C5—C6—C7 | −179.8 (5) |
O7—Nd1—O3—C2 | −94.0 (3) | C5—C6—C7—C8 | 0.0 (8) |
O8—Nd1—O3—C2 | −134.2 (3) | C6—C7—C8—C3 | 1.5 (8) |
O15—Nd1—O7—C9 | 161.9 (3) | C4—C3—C8—C7 | −2.5 (8) |
O10i—Nd1—O7—C9 | 109.9 (3) | C1—C3—C8—C7 | 177.1 (5) |
O3—Nd1—O7—C9 | −60.6 (3) | Nd1—O7—C9—O8 | 7.1 (4) |
O8i—Nd1—O7—C9 | 21.7 (3) | Nd1—O7—C9—C11 | −170.4 (3) |
O14—Nd1—O7—C9 | −99.6 (3) | Nd1i—O8—C9—O7 | −141.9 (4) |
O1—Nd1—O7—C9 | −147.5 (3) | Nd1—O8—C9—O7 | −7.1 (4) |
O13—Nd1—O7—C9 | 80.8 (3) | Nd1i—O8—C9—C11 | 35.6 (7) |
O8—Nd1—O7—C9 | −3.9 (2) | Nd1—O8—C9—C11 | 170.4 (4) |
O15—Nd1—O8—C9 | −12.1 (3) | Nd1i—O10—C10—O9 | −111.5 (5) |
O10i—Nd1—O8—C9 | −124.2 (3) | Nd1i—O10—C10—C12 | 66.6 (5) |
O3—Nd1—O8—C9 | 142.1 (3) | O7—C9—C11—C16 | 27.8 (6) |
O8i—Nd1—O8—C9 | −150.5 (3) | O8—C9—C11—C16 | −149.7 (4) |
O14—Nd1—O8—C9 | 72.3 (3) | O7—C9—C11—C12 | −151.8 (4) |
O1—Nd1—O8—C9 | 88.1 (3) | O8—C9—C11—C12 | 30.7 (7) |
O13—Nd1—O8—C9 | −72.6 (3) | C16—C11—C12—C13 | −1.6 (6) |
O7—Nd1—O8—C9 | 3.9 (2) | C9—C11—C12—C13 | 178.0 (4) |
O15—Nd1—O8—Nd1i | 138.38 (13) | C16—C11—C12—C10 | −174.2 (4) |
O10i—Nd1—O8—Nd1i | 26.3 (2) | C9—C11—C12—C10 | 5.4 (7) |
O3—Nd1—O8—Nd1i | −67.47 (13) | O9—C10—C12—C13 | −82.4 (6) |
O8i—Nd1—O8—Nd1i | 0.0 | O10—C10—C12—C13 | 99.3 (5) |
O14—Nd1—O8—Nd1i | −137.26 (14) | O9—C10—C12—C11 | 89.8 (5) |
O1—Nd1—O8—Nd1i | −121.39 (18) | O10—C10—C12—C11 | −88.6 (5) |
O13—Nd1—O8—Nd1i | 77.86 (13) | C11—C12—C13—C14 | 1.8 (7) |
O7—Nd1—O8—Nd1i | 154.34 (19) | C10—C12—C13—C14 | 174.1 (5) |
Nd1—O1—C1—O2 | 131.8 (5) | C11—C12—C13—N2 | −176.4 (4) |
Nd1—O1—C1—C3 | −48.8 (9) | C10—C12—C13—N2 | −4.0 (7) |
Nd1—O3—C2—O4 | 79.5 (5) | O11—N2—C13—C14 | 173.7 (5) |
Nd1—O3—C2—C4 | −95.9 (4) | O12—N2—C13—C14 | −6.0 (7) |
O1—C1—C3—C8 | 160.5 (5) | O11—N2—C13—C12 | −8.0 (7) |
O2—C1—C3—C8 | −20.1 (7) | O12—N2—C13—C12 | 172.3 (5) |
O1—C1—C3—C4 | −19.9 (7) | C12—C13—C14—C15 | −0.8 (8) |
O2—C1—C3—C4 | 159.5 (4) | N2—C13—C14—C15 | 177.4 (4) |
C8—C3—C4—C5 | 2.0 (7) | C13—C14—C15—C16 | −0.4 (8) |
C1—C3—C4—C5 | −177.6 (4) | C14—C15—C16—C11 | 0.5 (8) |
C8—C3—C4—C2 | 178.0 (4) | C12—C11—C16—C15 | 0.5 (7) |
C1—C3—C4—C2 | −1.6 (7) | C9—C11—C16—C15 | −179.1 (4) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O16ii | 0.82 | 1.79 | 2.588 (4) | 163 |
O13—H13C···O3i | 0.85 | 2.19 | 3.026 (5) | 169 |
O13—H13D···O10ii | 0.85 | 2.12 | 2.952 (5) | 168 |
O14—H14B···O7iii | 0.85 | 1.98 | 2.750 (5) | 150 |
O14—H14C···O4 | 0.85 | 2.00 | 2.782 (4) | 152 |
O15—H15C···O9ii | 0.85 | 1.81 | 2.654 (4) | 177 |
O15—H15D···O16ii | 0.85 | 2.02 | 2.867 (5) | 177 |
O16—H16C···O4 | 0.85 | 1.92 | 2.767 (5) | 179 |
O16—H16D···O9iv | 0.85 | 1.88 | 2.730 (5) | 179 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+2, −z+1; (iv) −x+2, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Nd2(C8H3NO6)2(C8H4NO6)2(H2O)6]·2H2O |
Mr | 1271.08 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 8.1460 (7), 8.8090 (9), 15.1670 (13) |
α, β, γ (°) | 100.434 (1), 91.106 (1), 104.482 (2) |
V (Å3) | 1033.96 (16) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 2.60 |
Crystal size (mm) | 0.16 × 0.14 × 0.10 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2007) |
Tmin, Tmax | 0.681, 0.781 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5316, 3618, 3196 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.076, 1.03 |
No. of reflections | 3618 |
No. of parameters | 317 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.51, −0.88 |
Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Nd1—O1 | 2.489 (3) | Nd1—O10i | 2.431 (3) |
Nd1—O3 | 2.447 (3) | Nd1—O13 | 2.554 (3) |
Nd1—O7 | 2.561 (3) | Nd1—O14 | 2.487 (3) |
Nd1—O8 | 2.564 (3) | Nd1—O15 | 2.398 (3) |
Nd1—O8i | 2.486 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O16ii | 0.820 | 1.792 | 2.588 (4) | 163.03 |
O13—H13C···O3i | 0.850 | 2.189 | 3.026 (5) | 168.45 |
O13—H13D···O10ii | 0.850 | 2.115 | 2.952 (5) | 168.24 |
O14—H14B···O7iii | 0.850 | 1.981 | 2.750 (5) | 149.89 |
O14—H14C···O4 | 0.850 | 2.001 | 2.782 (4) | 152.21 |
O15—H15C···O9ii | 0.850 | 1.805 | 2.654 (4) | 177.03 |
O15—H15D···O16ii | 0.850 | 2.018 | 2.867 (5) | 177.39 |
O16—H16C···O4 | 0.850 | 1.917 | 2.767 (5) | 179.19 |
O16—H16D···O9iv | 0.850 | 1.880 | 2.730 (5) | 179.00 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+2, −z+1; (iv) −x+2, −y+2, −z+1. |
Acknowledgements
This work was supported by the National Natural Science Foundation of China (grant No. 21103140) and the PhD Programs Foundation of the Ministry of Education of China (No. 20110204120037)
References
Bruker (2007). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Xiong, L.-Q. & Qi, C.-M. (2007). Acta Cryst. C63, m10–m12. Web of Science CSD CrossRef IUCr Journals Google Scholar
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We report here a neodymium complex based on 3-nitrobenzene-1,2- dicarboxylic acid ligands. X-ray diffraction crystal structure analysis reveals that the complex forms a structure [Nd2(C8H4NO6)2(C8H3NO6)2 (H2O)6].2H2O, consisting of dimeric units related by an inversion center. The compound is isostructural to the corresponding La compound reported by Xiong & Qi (2007).
In the title complex, the central neodymium center is coordinated by nine oxygen atoms (Fig. 1), the coordination geometry of which can be described as distorted tricapped trigonal-prismatic. Six of the nine coordinating oxygens are from the two coordinating H2NPA (3-nitrobenzene-1,2-dicarboxylic acid) ligands and the remaining three from water molecules. 3-Nitrobenzene-1,2-dicarboxylic acid ligands exhibit two coordination modes (Fig. 2), which can be classified as µ2-(κ4, O1: O2: O2: O3) and µ1-(κ2, O2: O3). In one unit of the complex, there are four H2NPA anions. Two (NPA2-) ions are dianionic, so the other (HNPA-) anion is monoprotonated to maintain electroneutrality. Correspondingly, two types of coordination modes of H2NPA ligands exist in the structure.