Related literature
For related structures, see: Liao et al. (2004
); Wang et al. (2004
).
Experimental
Data collection
Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) Tmin = 0.459, Tmax = 0.605 5967 measured reflections 4073 independent reflections 3923 reflections with I > 2σ(I) Rint = 0.017
|
Nd1—O1 | 2.428 (3) | Nd1—O2i | 2.392 (3) | Nd1—O3 | 2.446 (3) | Nd1—O4 | 2.571 (3) | Nd1—O5 | 2.651 (3) | Nd1—O7ii | 2.390 (3) | Nd1—O1W | 2.542 (3) | Nd1—O2W | 2.567 (3) | Nd1—O3W | 2.505 (3) | Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y, -z+1. | |
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | O4W—H7W⋯O12 | 0.84 | 2.59 | 3.256 (11) | 136 | O4W—H8W⋯O5i | 0.84 | 2.52 | 3.023 (8) | 119 | O4W—H8W⋯O8i | 0.84 | 2.04 | 2.801 (9) | 150 | O3W—H5W⋯O12ii | 0.84 | 2.11 | 2.945 (7) | 170 | O3W—H6W⋯O8 | 0.84 | 2.04 | 2.846 (8) | 162 | O2W—H3W⋯O1Wii | 0.84 | 2.12 | 2.900 (5) | 154 | O2W—H4W⋯O4iii | 0.84 | 2.04 | 2.861 (4) | 167 | O1W—H2W⋯O4W | 0.84 | 1.83 | 2.593 (7) | 150 | O1W—H1W⋯O6iv | 0.84 | 2.04 | 2.880 (5) | 178 | N2—H2A⋯O9iii | 0.86 | 2.51 | 3.045 (5) | 121 | N2—H2A⋯O13v | 0.86 | 2.48 | 3.033 (5) | 123 | N2—H2A⋯O10vi | 0.86 | 2.15 | 2.868 (5) | 141 | N1—H1⋯O13vii | 0.86 | 2.46 | 2.994 (6) | 121 | N1—H1⋯O9viii | 0.86 | 2.46 | 2.988 (6) | 120 | N1—H1⋯O14ix | 0.86 | 2.24 | 2.953 (6) | 140 | Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y, -z+1; (iii) -x+2, -y, -z+1; (iv) x-1, y, z; (v) -x+1, -y, -z+2; (vi) x, y-1, z+1; (vii) -x, -y+1, -z+1; (viii) -x+1, -y+1, -z; (ix) x, y+1, z-1. | |
Data collection: APEX2 (Bruker, 2007
); cell refinement: 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
A mixture of Nd2O3 (0.168 g, 0.5 mmol), isonicotinic acid (0.123 g, 1 mmol), HNO3 (0.12 ml) and H2O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 433 K for 3 d and then cooled to room temperature at a rate of 10 K h-1. The crystals obtained were washed with water and dried in air.
H atoms on C and N atoms were positioned geometrically and treated as riding atoms, with C—H = 0.93 Å and N—H = 0.86 Å and with Uiso(H) = 1.2Ueq(C,N). H atoms of water molecules were located in difference Fourier maps and fixed in refinements, with O—H = 0.84 Å and Uiso(H) = 1.5Ueq(O).
Data collection: APEX2 (Bruker, 2007); cell refinement: 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).
catena-Poly[[[triaqua(nitrato-
κ2O,
O')neodymium(III)]- bis(µ
2-pyridinium-4-carboxylato-
κ2O:
O')] bis(perchlorate) monohydrate]
top Crystal data top [Nd(NO3)(C6H5NO2)2(H2O)3](ClO4)2·H2O | Z = 2 |
Mr = 723.43 | F(000) = 714 |
Triclinic, P1 | Dx = 2.072 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.3962 (7) Å | Cell parameters from 8000 reflections |
b = 10.1119 (8) Å | θ = 1.7–26.0° |
c = 14.7229 (12) Å | µ = 2.57 mm−1 |
α = 81.663 (1)° | T = 273 K |
β = 79.601 (1)° | Block, colourless |
γ = 71.334 (1)° | 0.32 × 0.26 × 0.20 mm |
V = 1159.68 (16) Å3 | |
Data collection top Bruker APEXII CCD diffractometer | 4073 independent reflections |
Radiation source: fine-focus sealed tube | 3923 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
ϕ and ω scans | θmax = 25.2°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→10 |
Tmin = 0.459, Tmax = 0.605 | k = −11→12 |
5967 measured reflections | l = −16→17 |
Refinement top 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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0448P)2 + 3.0364P] where P = (Fo2 + 2Fc2)/3 |
4073 reflections | (Δ/σ)max = 0.001 |
334 parameters | Δρmax = 1.00 e Å−3 |
12 restraints | Δρmin = −1.11 e Å−3 |
Crystal data top [Nd(NO3)(C6H5NO2)2(H2O)3](ClO4)2·H2O | γ = 71.334 (1)° |
Mr = 723.43 | V = 1159.68 (16) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.3962 (7) Å | Mo Kα radiation |
b = 10.1119 (8) Å | µ = 2.57 mm−1 |
c = 14.7229 (12) Å | T = 273 K |
α = 81.663 (1)° | 0.32 × 0.26 × 0.20 mm |
β = 79.601 (1)° | |
Data collection top Bruker APEXII CCD diffractometer | 4073 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3923 reflections with I > 2σ(I) |
Tmin = 0.459, Tmax = 0.605 | Rint = 0.017 |
5967 measured reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.029 | 12 restraints |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 0.99 | Δρmax = 1.00 e Å−3 |
4073 reflections | Δρmin = −1.11 e Å−3 |
334 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.3296 (5) | 0.6208 (4) | 0.2806 (3) | 0.0285 (8) | |
Cl1 | 0.75800 (16) | 0.47280 (12) | 0.09482 (8) | 0.0430 (3) | |
N1 | 0.2205 (6) | 0.7323 (4) | 0.1159 (3) | 0.0493 (11) | |
H1 | 0.1879 | 0.7654 | 0.0628 | 0.059* | |
Nd1 | 0.61497 (2) | 0.219206 (19) | 0.462773 (12) | 0.02175 (9) | |
O1 | 0.4362 (4) | 0.4217 (3) | 0.3801 (2) | 0.0329 (6) | |
C2 | 0.2041 (6) | 0.5822 (5) | 0.2522 (3) | 0.0432 (11) | |
H2 | 0.1574 | 0.5168 | 0.2886 | 0.052* | |
Cl2 | 0.24041 (16) | 0.02494 (12) | 0.89509 (8) | 0.0416 (3) | |
N2 | 0.7879 (5) | −0.2315 (4) | 0.8926 (2) | 0.0364 (8) | |
H2A | 0.8157 | −0.2643 | 0.9467 | 0.044* | |
O2 | 0.4255 (4) | 0.6291 (3) | 0.4190 (2) | 0.0406 (7) | |
C3 | 0.1495 (7) | 0.6428 (6) | 0.1687 (4) | 0.0557 (14) | |
H3 | 0.0624 | 0.6207 | 0.1494 | 0.067* | |
O3 | 0.6604 (4) | 0.0616 (3) | 0.6047 (2) | 0.0374 (7) | |
C4 | 0.3394 (7) | 0.7728 (5) | 0.1414 (3) | 0.0440 (11) | |
H4 | 0.3859 | 0.8362 | 0.1025 | 0.053* | |
N4 | 0.9277 (5) | 0.3174 (4) | 0.4383 (3) | 0.0388 (9) | |
O4 | 0.9213 (4) | 0.1992 (3) | 0.4802 (3) | 0.0451 (8) | |
C5 | 0.3937 (6) | 0.7207 (5) | 0.2256 (3) | 0.0380 (10) | |
H5 | 0.4729 | 0.7523 | 0.2456 | 0.046* | |
O5 | 0.7969 (4) | 0.3949 (3) | 0.4069 (2) | 0.0455 (8) | |
C6 | 0.4021 (5) | 0.5516 (4) | 0.3681 (3) | 0.0247 (8) | |
O6 | 1.0567 (5) | 0.3518 (5) | 0.4292 (3) | 0.0688 (12) | |
C7 | 0.6913 (5) | −0.1202 (4) | 0.7252 (3) | 0.0246 (8) | |
O7 | 0.5371 (4) | −0.1017 (3) | 0.6025 (2) | 0.0350 (7) | |
C8 | 0.8138 (6) | −0.0818 (5) | 0.7579 (3) | 0.0336 (9) | |
H8 | 0.8628 | −0.0169 | 0.7227 | 0.040* | |
O8 | 0.8174 (13) | 0.4411 (6) | 0.1813 (4) | 0.152 (4) | |
C9 | 0.8617 (6) | −0.1400 (5) | 0.8421 (3) | 0.0380 (10) | |
H9 | 0.9450 | −0.1164 | 0.8643 | 0.046* | |
O9 | 0.8797 (5) | 0.3853 (5) | 0.0322 (3) | 0.0626 (11) | |
C10 | 0.6734 (6) | −0.2736 (5) | 0.8629 (3) | 0.0376 (10) | |
H10 | 0.6267 | −0.3387 | 0.8995 | 0.045* | |
O10 | 0.7386 (6) | 0.6160 (4) | 0.0700 (3) | 0.0720 (13) | |
C11 | 0.6248 (6) | −0.2203 (4) | 0.7777 (3) | 0.0329 (9) | |
H11 | 0.5475 | −0.2513 | 0.7553 | 0.039* | |
O11 | 0.6059 (8) | 0.4456 (7) | 0.1061 (8) | 0.177 (5) | |
C12 | 0.6247 (5) | −0.0482 (4) | 0.6362 (3) | 0.0256 (8) | |
O12 | 0.1848 (15) | 0.0322 (7) | 0.8114 (4) | 0.197 (5) | |
O13 | 0.1153 (5) | 0.1236 (5) | 0.9500 (3) | 0.0634 (11) | |
O14 | 0.2627 (8) | −0.1133 (5) | 0.9314 (4) | 0.108 (2) | |
O15 | 0.3841 (9) | 0.0555 (9) | 0.8782 (10) | 0.256 (8) | |
O1W | 0.3147 (4) | 0.2628 (4) | 0.5492 (2) | 0.0426 (7) | |
H1W | 0.2375 | 0.2900 | 0.5154 | 0.064* | |
H2W | 0.2927 | 0.3121 | 0.5938 | 0.064* | |
O2W | 0.8124 (4) | −0.0227 (3) | 0.4206 (2) | 0.0397 (7) | |
H4W | 0.8961 | −0.0633 | 0.4488 | 0.060* | |
H3W | 0.7594 | −0.0782 | 0.4151 | 0.060* | |
O3W | 0.7472 (4) | 0.2088 (3) | 0.2962 (2) | 0.0430 (8) | |
H6W | 0.7505 | 0.2762 | 0.2560 | 0.065* | |
H5W | 0.7699 | 0.1337 | 0.2717 | 0.065* | |
O4W | 0.2124 (9) | 0.3371 (7) | 0.7164 (4) | 0.123 (2) | |
H8W | 0.2054 | 0.4183 | 0.7270 | 0.184* | |
H7W | 0.2016 | 0.2855 | 0.7659 | 0.184* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.033 (2) | 0.0229 (19) | 0.029 (2) | −0.0026 (16) | −0.0122 (17) | −0.0030 (15) |
Cl1 | 0.0593 (7) | 0.0339 (6) | 0.0312 (5) | −0.0140 (5) | 0.0023 (5) | 0.0009 (4) |
N1 | 0.065 (3) | 0.048 (2) | 0.035 (2) | −0.011 (2) | −0.029 (2) | 0.0090 (18) |
Nd1 | 0.02726 (13) | 0.01985 (12) | 0.02122 (12) | −0.00926 (8) | −0.01255 (8) | 0.00457 (8) |
O1 | 0.0427 (17) | 0.0241 (14) | 0.0348 (15) | −0.0086 (12) | −0.0216 (13) | 0.0045 (12) |
C2 | 0.050 (3) | 0.042 (3) | 0.044 (3) | −0.018 (2) | −0.024 (2) | 0.008 (2) |
Cl2 | 0.0524 (7) | 0.0347 (6) | 0.0369 (6) | −0.0145 (5) | −0.0004 (5) | −0.0050 (4) |
N2 | 0.041 (2) | 0.045 (2) | 0.0238 (17) | −0.0116 (17) | −0.0175 (15) | 0.0086 (15) |
O2 | 0.065 (2) | 0.0323 (16) | 0.0311 (16) | −0.0156 (15) | −0.0235 (15) | −0.0024 (13) |
C3 | 0.062 (3) | 0.066 (4) | 0.052 (3) | −0.028 (3) | −0.038 (3) | 0.011 (3) |
O3 | 0.058 (2) | 0.0298 (15) | 0.0322 (15) | −0.0202 (14) | −0.0244 (14) | 0.0116 (12) |
C4 | 0.062 (3) | 0.036 (2) | 0.030 (2) | −0.011 (2) | −0.012 (2) | 0.0079 (19) |
N4 | 0.034 (2) | 0.047 (2) | 0.040 (2) | −0.0181 (17) | −0.0146 (16) | 0.0039 (17) |
O4 | 0.0366 (17) | 0.0373 (17) | 0.064 (2) | −0.0136 (14) | −0.0242 (16) | 0.0137 (16) |
C5 | 0.049 (3) | 0.034 (2) | 0.032 (2) | −0.012 (2) | −0.0127 (19) | 0.0032 (18) |
O5 | 0.0405 (18) | 0.0414 (18) | 0.059 (2) | −0.0164 (15) | −0.0250 (16) | 0.0149 (15) |
C6 | 0.0240 (19) | 0.027 (2) | 0.0237 (19) | −0.0069 (15) | −0.0082 (15) | 0.0011 (15) |
O6 | 0.047 (2) | 0.089 (3) | 0.086 (3) | −0.046 (2) | −0.029 (2) | 0.029 (2) |
C7 | 0.0282 (19) | 0.0228 (18) | 0.0221 (18) | −0.0047 (15) | −0.0090 (15) | 0.0001 (14) |
O7 | 0.0481 (18) | 0.0371 (16) | 0.0299 (15) | −0.0207 (14) | −0.0227 (13) | 0.0041 (12) |
C8 | 0.038 (2) | 0.037 (2) | 0.032 (2) | −0.0184 (19) | −0.0124 (18) | 0.0051 (17) |
O8 | 0.310 (11) | 0.075 (4) | 0.046 (3) | −0.008 (5) | −0.060 (4) | −0.001 (3) |
C9 | 0.041 (2) | 0.046 (3) | 0.034 (2) | −0.018 (2) | −0.0219 (19) | 0.0064 (19) |
O9 | 0.056 (2) | 0.070 (3) | 0.056 (2) | −0.003 (2) | −0.0086 (19) | −0.027 (2) |
C10 | 0.046 (3) | 0.037 (2) | 0.031 (2) | −0.018 (2) | −0.0105 (19) | 0.0115 (18) |
O10 | 0.101 (3) | 0.041 (2) | 0.057 (2) | −0.016 (2) | 0.005 (2) | 0.0161 (18) |
C11 | 0.038 (2) | 0.034 (2) | 0.031 (2) | −0.0159 (18) | −0.0149 (18) | 0.0057 (17) |
O11 | 0.071 (4) | 0.115 (5) | 0.352 (13) | −0.052 (4) | 0.074 (6) | −0.117 (7) |
C12 | 0.030 (2) | 0.0241 (19) | 0.0229 (18) | −0.0074 (16) | −0.0102 (15) | 0.0022 (15) |
O12 | 0.367 (14) | 0.100 (5) | 0.062 (3) | 0.058 (6) | −0.084 (6) | −0.037 (3) |
O13 | 0.056 (2) | 0.072 (3) | 0.058 (2) | 0.002 (2) | −0.0162 (19) | −0.030 (2) |
O14 | 0.131 (5) | 0.053 (3) | 0.093 (4) | 0.002 (3) | 0.023 (3) | 0.027 (3) |
O15 | 0.085 (5) | 0.160 (7) | 0.55 (2) | −0.082 (5) | 0.127 (8) | −0.224 (11) |
O1W | 0.0390 (17) | 0.058 (2) | 0.0377 (17) | −0.0217 (15) | −0.0107 (14) | −0.0038 (15) |
O2W | 0.0407 (17) | 0.0286 (15) | 0.0522 (19) | −0.0082 (13) | −0.0218 (15) | 0.0024 (13) |
O3W | 0.056 (2) | 0.0402 (18) | 0.0296 (16) | −0.0151 (15) | −0.0006 (14) | 0.0030 (13) |
O4W | 0.143 (6) | 0.133 (6) | 0.088 (4) | −0.048 (5) | 0.007 (4) | −0.009 (4) |
Geometric parameters (Å, º) top C1—C2 | 1.382 (6) | O2—C6 | 1.240 (5) |
C1—C5 | 1.385 (6) | O2—Nd1i | 2.392 (3) |
C1—C6 | 1.506 (5) | C3—H3 | 0.9300 |
Cl1—O11 | 1.367 (6) | O3—C12 | 1.245 (5) |
Cl1—O10 | 1.405 (4) | C4—C5 | 1.372 (6) |
Cl1—O8 | 1.408 (6) | C4—H4 | 0.9300 |
Cl1—O9 | 1.413 (4) | N4—O6 | 1.220 (5) |
N1—C4 | 1.321 (7) | N4—O5 | 1.250 (5) |
N1—C3 | 1.324 (7) | N4—O4 | 1.275 (5) |
N1—H1 | 0.8600 | C5—H5 | 0.9300 |
Nd1—O1 | 2.428 (3) | C7—C11 | 1.383 (6) |
Nd1—O2i | 2.392 (3) | C7—C8 | 1.389 (6) |
Nd1—O3 | 2.446 (3) | C7—C12 | 1.512 (5) |
Nd1—O4 | 2.571 (3) | C8—C9 | 1.365 (6) |
Nd1—O5 | 2.651 (3) | C8—H8 | 0.9300 |
Nd1—O7ii | 2.390 (3) | C9—H9 | 0.9300 |
Nd1—O1W | 2.542 (3) | C10—C11 | 1.371 (6) |
Nd1—O2W | 2.567 (3) | C10—H10 | 0.9300 |
Nd1—O3W | 2.505 (3) | C11—H11 | 0.9300 |
O1—C6 | 1.245 (5) | C12—O7 | 1.242 (5) |
C2—C3 | 1.379 (7) | O1W—H1W | 0.8400 |
C2—H2 | 0.9300 | O1W—H2W | 0.8400 |
Cl2—O15 | 1.311 (6) | O2W—H4W | 0.8400 |
Cl2—O12 | 1.379 (6) | O2W—H3W | 0.8400 |
Cl2—O14 | 1.388 (5) | O3W—H6W | 0.8400 |
Cl2—O13 | 1.417 (4) | O3W—H5W | 0.8400 |
N2—C10 | 1.329 (6) | O4W—H8W | 0.8400 |
N2—C9 | 1.339 (6) | O4W—H7W | 0.8400 |
N2—H2A | 0.8600 | | |
| | | |
C2—C1—C5 | 119.2 (4) | O12—Cl2—O14 | 104.1 (5) |
C2—C1—C6 | 120.9 (4) | O15—Cl2—O13 | 110.6 (4) |
C5—C1—C6 | 119.9 (4) | O12—Cl2—O13 | 108.2 (4) |
O11—Cl1—O10 | 111.3 (4) | O14—Cl2—O13 | 113.7 (3) |
O11—Cl1—O8 | 107.8 (6) | C10—N2—C9 | 122.9 (4) |
O10—Cl1—O8 | 106.1 (3) | C10—N2—H2A | 118.6 |
O11—Cl1—O9 | 110.7 (4) | C9—N2—H2A | 118.6 |
O10—Cl1—O9 | 113.1 (3) | C6—O2—Nd1i | 162.7 (3) |
O8—Cl1—O9 | 107.4 (4) | N1—C3—C2 | 120.4 (5) |
C4—N1—C3 | 122.6 (4) | N1—C3—H3 | 119.8 |
C4—N1—H1 | 118.7 | C2—C3—H3 | 119.8 |
C3—N1—H1 | 118.7 | C12—O3—Nd1 | 134.0 (3) |
O7ii—Nd1—O2i | 140.53 (12) | N1—C4—C5 | 119.6 (5) |
O7ii—Nd1—O1 | 81.57 (10) | N1—C4—H4 | 120.2 |
O2i—Nd1—O1 | 85.82 (10) | C5—C4—H4 | 120.2 |
O7ii—Nd1—O3 | 97.66 (10) | O6—N4—O5 | 122.0 (4) |
O2i—Nd1—O3 | 75.38 (10) | O6—N4—O4 | 121.0 (4) |
O1—Nd1—O3 | 149.37 (11) | O5—N4—O4 | 117.0 (4) |
O7ii—Nd1—O3W | 75.54 (11) | N4—O4—Nd1 | 98.8 (2) |
O2i—Nd1—O3W | 136.17 (11) | C4—C5—C1 | 119.5 (4) |
O1—Nd1—O3W | 74.83 (10) | C4—C5—H5 | 120.2 |
O3—Nd1—O3W | 134.93 (11) | C1—C5—H5 | 120.2 |
O7ii—Nd1—O1W | 69.63 (11) | N4—O5—Nd1 | 95.6 (2) |
O2i—Nd1—O1W | 70.93 (11) | O2—C6—O1 | 127.0 (4) |
O1—Nd1—O1W | 73.20 (11) | O2—C6—C1 | 116.9 (3) |
O3—Nd1—O1W | 77.83 (11) | O1—C6—C1 | 116.1 (3) |
O3W—Nd1—O1W | 135.33 (11) | C11—C7—C8 | 119.0 (4) |
O7ii—Nd1—O2W | 70.39 (10) | C11—C7—C12 | 120.4 (4) |
O2i—Nd1—O2W | 137.28 (10) | C8—C7—C12 | 120.5 (3) |
O1—Nd1—O2W | 135.29 (10) | C9—C8—C7 | 119.4 (4) |
O3—Nd1—O2W | 70.71 (10) | C9—C8—H8 | 120.3 |
O3W—Nd1—O2W | 65.02 (10) | C7—C8—H8 | 120.3 |
O1W—Nd1—O2W | 124.20 (11) | N2—C9—C8 | 119.5 (4) |
O7ii—Nd1—O4 | 139.99 (11) | N2—C9—H9 | 120.2 |
O2i—Nd1—O4 | 77.38 (12) | C8—C9—H9 | 120.2 |
O1—Nd1—O4 | 122.18 (10) | N2—C10—C11 | 119.5 (4) |
O3—Nd1—O4 | 77.44 (10) | N2—C10—H10 | 120.3 |
O3W—Nd1—O4 | 80.43 (12) | C11—C10—H10 | 120.3 |
O1W—Nd1—O4 | 143.71 (11) | C10—C11—C7 | 119.6 (4) |
O2W—Nd1—O4 | 70.58 (10) | C10—C11—H11 | 120.2 |
O7ii—Nd1—O5 | 138.71 (10) | C7—C11—H11 | 120.2 |
O2i—Nd1—O5 | 70.41 (12) | O7—C12—O3 | 126.1 (3) |
O1—Nd1—O5 | 73.54 (10) | O7—C12—C7 | 117.5 (3) |
O3—Nd1—O5 | 120.41 (10) | O3—C12—C7 | 116.4 (3) |
O3W—Nd1—O5 | 66.52 (11) | Nd1—O1W—H1W | 115.1 |
O1W—Nd1—O5 | 130.00 (11) | Nd1—O1W—H2W | 114.5 |
O2W—Nd1—O5 | 105.70 (11) | H1W—O1W—H2W | 111.6 |
O4—Nd1—O5 | 48.66 (10) | Nd1—O2W—H4W | 120.0 |
C6—O1—Nd1 | 140.8 (3) | Nd1—O2W—H3W | 112.9 |
C3—C2—C1 | 118.4 (5) | H4W—O2W—H3W | 111.4 |
C3—C2—H2 | 120.8 | Nd1—O3W—H6W | 127.8 |
C1—C2—H2 | 120.8 | Nd1—O3W—H5W | 119.0 |
O15—Cl2—O12 | 107.9 (8) | H6W—O3W—H5W | 111.3 |
O15—Cl2—O14 | 111.9 (6) | H8W—O4W—H7W | 111.5 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O4W—H7W···O12 | 0.84 | 2.59 | 3.256 (11) | 136 |
O4W—H8W···O5i | 0.84 | 2.52 | 3.023 (8) | 119 |
O4W—H8W···O8i | 0.84 | 2.04 | 2.801 (9) | 150 |
O3W—H5W···O12ii | 0.84 | 2.11 | 2.945 (7) | 170 |
O3W—H6W···O8 | 0.84 | 2.04 | 2.846 (8) | 162 |
O2W—H3W···O1Wii | 0.84 | 2.12 | 2.900 (5) | 154 |
O2W—H4W···O4iii | 0.84 | 2.04 | 2.861 (4) | 167 |
O1W—H2W···O4W | 0.84 | 1.83 | 2.593 (7) | 150 |
O1W—H1W···O6iv | 0.84 | 2.04 | 2.880 (5) | 178 |
N2—H2A···O9iii | 0.86 | 2.51 | 3.045 (5) | 121 |
N2—H2A···O13v | 0.86 | 2.48 | 3.033 (5) | 123 |
N2—H2A···O10vi | 0.86 | 2.15 | 2.868 (5) | 141 |
N1—H1···O13vii | 0.86 | 2.46 | 2.994 (6) | 121 |
N1—H1···O9viii | 0.86 | 2.46 | 2.988 (6) | 120 |
N1—H1···O14ix | 0.86 | 2.24 | 2.953 (6) | 140 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+2, −y, −z+1; (iv) x−1, y, z; (v) −x+1, −y, −z+2; (vi) x, y−1, z+1; (vii) −x, −y+1, −z+1; (viii) −x+1, −y+1, −z; (ix) x, y+1, z−1. |
Experimental details
Crystal data |
Chemical formula | [Nd(NO3)(C6H5NO2)2(H2O)3](ClO4)2·H2O |
Mr | 723.43 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 273 |
a, b, c (Å) | 8.3962 (7), 10.1119 (8), 14.7229 (12) |
α, β, γ (°) | 81.663 (1), 79.601 (1), 71.334 (1) |
V (Å3) | 1159.68 (16) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.57 |
Crystal size (mm) | 0.32 × 0.26 × 0.20 |
|
Data collection |
Diffractometer | Bruker APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.459, 0.605 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5967, 4073, 3923 |
Rint | 0.017 |
(sin θ/λ)max (Å−1) | 0.599 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.077, 0.99 |
No. of reflections | 4073 |
No. of parameters | 334 |
No. of restraints | 12 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.00, −1.11 |
Selected bond lengths (Å) topNd1—O1 | 2.428 (3) | Nd1—O7ii | 2.390 (3) |
Nd1—O2i | 2.392 (3) | Nd1—O1W | 2.542 (3) |
Nd1—O3 | 2.446 (3) | Nd1—O2W | 2.567 (3) |
Nd1—O4 | 2.571 (3) | Nd1—O3W | 2.505 (3) |
Nd1—O5 | 2.651 (3) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O4W—H7W···O12 | 0.84 | 2.59 | 3.256 (11) | 136 |
O4W—H8W···O5i | 0.84 | 2.52 | 3.023 (8) | 119 |
O4W—H8W···O8i | 0.84 | 2.04 | 2.801 (9) | 150 |
O3W—H5W···O12ii | 0.84 | 2.11 | 2.945 (7) | 170 |
O3W—H6W···O8 | 0.84 | 2.04 | 2.846 (8) | 162 |
O2W—H3W···O1Wii | 0.84 | 2.12 | 2.900 (5) | 154 |
O2W—H4W···O4iii | 0.84 | 2.04 | 2.861 (4) | 167 |
O1W—H2W···O4W | 0.84 | 1.83 | 2.593 (7) | 150 |
O1W—H1W···O6iv | 0.84 | 2.04 | 2.880 (5) | 178 |
N2—H2A···O9iii | 0.86 | 2.51 | 3.045 (5) | 121 |
N2—H2A···O13v | 0.86 | 2.48 | 3.033 (5) | 123 |
N2—H2A···O10vi | 0.86 | 2.15 | 2.868 (5) | 141 |
N1—H1···O13vii | 0.86 | 2.46 | 2.994 (6) | 121 |
N1—H1···O9viii | 0.86 | 2.46 | 2.988 (6) | 120 |
N1—H1···O14ix | 0.86 | 2.24 | 2.953 (6) | 140 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+2, −y, −z+1; (iv) x−1, y, z; (v) −x+1, −y, −z+2; (vi) x, y−1, z+1; (vii) −x, −y+1, −z+1; (viii) −x+1, −y+1, −z; (ix) x, y+1, z−1. |
Acknowledgements
The author acknowledges Zunyi Medical College for supporting this work.
References
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Liao, J.-H., Lai, C.-Y., Ho, C.-D. & Su, C.-T. (2004). Inorg. Chem. Commun. 7, 402–404. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, C.-M., Chuang, Y.-L., Chuang, S.-T. & Lii, K.-H. (2004). J. Solid State Chem. 177, 2305–2310. Web of Science CSD CrossRef CAS Google Scholar
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In the structural investigation of isonicotinate complexes, it has been found that the isonicotinate functions as a multidentate ligand with versatile binding and coordination modes (Liao et al., 2004; Wang et al., 2004). In this paper, we report the crystal structure of the title compound, a new NdIII complex resulted from the hydrothermal treatment of isonicotinic acid, Nd2O3 and a little nitric acid.
As depicted in Fig. 1, the asymmetric unit consists of one NdIII atom, two pyridinium-4-carboxylate (Hint) ligands, one coordinated nitrate anion, three coordinated water molecules, two perchlorate anions and one uncoordinated water molecule. The NdIII atom is nine-coordinated in a distorted tricapped trigonal prismatic coordination geometry, defined by four O atoms from four different Hint ligands, two O atoms from a nitrate anion and three water molecules (Table 1). The Hint ligands link the metal centres to form a polymeric chain (Fig. 2), in which the NdIII atoms are separated by 5.586 (2) and 5.281 (3) Å. The chains are further self-assembled into a three-dimensional supramolecular network through O—H···O and N—H···O hydrogen bonds (Table 2 and Fig. 3).