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The crystal structures of isostructural 2,6-naphthalenedicarboxylate tetrahydrate salts of nickel(II) and cobalt(II) have been determined using Monte Carlo simulated annealing techniques and laboratory X-ray powder diffraction data. These compounds crystallize in the triclinic space group
P, with
Z = 2;
a = 10.0851 (4),
b = 10.9429 (5),
c = 6.2639 (3) Å, α = 98.989 (2), β = 87.428 (3), γ = 108.015 (2)°,
V = 649.32 (5) Å
3 for [Ni(C
12H
6O
4)(H
2O)
4], and
a = 10.1855 (6),
b = 10.8921 (6),
c = 6.2908 (5) Å, α = 98.519 (4), β = 87.563 (4), γ = 108.304 (3)°,
V = 655.28 (8) Å
3 for [Co(C
12H
6O
4)(H
2O)
4]. The water-molecule H atoms were located by quantum chemical geometry optimization using
CASTEP. The structure consists of alternating hydrocarbon and metal/oxygen layers parallel to the
ac plane. Each naphthalenedicarboxylate anion bridges two metal cations; each carboxyl group is monodentate. The resulting structure contains infinite chains parallel to [111]. The octahedral coordination sphere of the metal cations contains
trans carboxylates and four equatorial water molecules. The carboxyl groups are rotated by 15–20° out of the naphthalene plane. The metal/oxygen layers are characterized by an extensive hydrogen-bonding network. The orientations of the carboxyl groups are determined by the formation of short (O
O = 2.53 Å) hydrogen bonds between the carbonyl O atoms and the
cis water molecules. Molecular mechanics energy minimizations suggest that coordination and hydrogen-bonding interactions are most important in determining the crystal packing.
Supporting information
CCDC references: 214227; 214228
For both compounds, program(s) used to refine structure: GSAS.
Crystal data top
Triclinic, P1 | α = 98.987 (2)° |
a = 10.0848 (4) Å | β = 87.427 (3)° |
b = 10.9428 (5) Å | γ = 108.0158 (18)° |
c = 6.2639 (3) Å | KG1, KG2 radiation |
Data collection top
2θmin = 13.043°, 2θmax = 89.983°, 2θstep = 0.02° | |
Refinement top
Rp = 0.049 | 3848 data points |
Rwp = 0.065 | 52 parameters |
Rexp = 0.022 | 30 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.3539 (10) | 1.1253 (7) | 0.7132 (10) | 0.031 (2)* | |
C2 | 0.4652 (9) | 1.1749 (7) | 0.5782 (11) | 0.031 (2)* | |
C3 | 0.4631 (9) | 1.1189 (8) | 0.3616 (11) | 0.031 (2)* | |
C4 | 0.3497 (10) | 1.0133 (8) | 0.2805 (9) | 0.031 (2)* | |
C5 | 0.1241 (10) | 0.8574 (7) | 0.3347 (10) | 0.031 (2)* | |
C6 | 0.0128 (10) | 0.8077 (7) | 0.4697 (13) | 0.031 (2)* | |
C7 | 0.0148 (10) | 0.8638 (7) | 0.6862 (12) | 0.031 (2)* | |
C8 | 0.1282 (10) | 0.9694 (7) | 0.7673 (10) | 0.031 (2)* | |
C9 | 0.2400 (9) | 1.0195 (7) | 0.6326 (9) | 0.031 (2)* | |
C10 | 0.2379 (9) | 0.9632 (7) | 0.4153 (9) | 0.031 (2)* | |
H1 | 0.3568 (11) | 1.1698 (8) | 0.8812 (11) | 0.05* | |
H3 | 0.5496 (10) | 1.1574 (9) | 0.2565 (13) | 0.05* | |
H4 | 0.3495 (11) | 0.9707 (9) | 0.1119 (9) | 0.05* | |
H5 | 0.1211 (11) | 0.8129 (9) | 0.1667 (11) | 0.05* | |
H7 | −0.0716 (10) | 0.8253 (8) | 0.7914 (14) | 0.05* | |
H8 | 0.1284 (11) | 1.0120 (9) | 0.9360 (11) | 0.05* | |
C11 | 0.5877 (10) | 1.2891 (8) | 0.6662 (14) | 0.022 (2)* | |
C12 | −0.1097 (10) | 0.6936 (8) | 0.3817 (16) | 0.022 (2)* | |
O1 | 0.5949 (12) | 1.3121 (12) | 0.868 (2) | 0.022 (2)* | |
O2 | 0.6826 (15) | 1.3411 (12) | 0.5260 (19) | 0.022 (2)* | |
O3 | −0.2203 (17) | 0.6798 (13) | 0.4952 (18) | 0.022 (2)* | |
O4 | −0.0989 (15) | 0.6339 (12) | 0.214 (3) | 0.022 (2)* | |
Ni | 0.7479 (6) | 1.4790 (5) | 1.0272 (9) | 0.0357 (17)* | |
O5 | 0.8846 (15) | 1.4778 (14) | 0.760 (2) | 0.028 (3)* | |
O6 | 0.6051 (15) | 1.4822 (12) | 1.278 (2) | 0.028 (3)* | |
O7 | 0.8289 (13) | 1.3466 (11) | 1.145 (2) | 0.028 (3)* | |
O8 | 0.6873 (16) | 1.6231 (11) | 0.898 (2) | 0.028 (3)* | |
H5a | 0.86528 | 1.38675 | 0.74713 | 0.03* | |
H5b | 0.97172 | 1.50115 | 0.85866 | 0.03* | |
H6a | 0.53731 | 1.39076 | 1.26716 | 0.03* | |
H6b | 0.55396 | 1.54789 | 1.2619 | 0.03* | |
H7a | 0.84631 | 1.38881 | 1.30045 | 0.03* | |
H7b | 0.74702 | 1.27221 | 1.15524 | 0.03* | |
H8a | 0.67419 | 1.57228 | 0.75349 | 0.03* | |
H8b | 0.58858 | 1.59919 | 0.9664 | 0.03* | |
Crystal data top
Triclinic, P1 | α = 98.522 (4)° |
a = 10.1856 (6) Å | β = 87.573 (4)° |
b = 10.8931 (6) Å | γ = 108.300 (3)° |
c = 6.2902 (5) Å | KG1, KG2 radiation |
Data collection top
2θmin = 13.043°, 2θmax = 89.983°, 2θstep = 0.02° | |
Refinement top
Rp = 0.030 | 3848 data points |
Rwp = 0.040 | 52 parameters |
Rexp = 0.026 | 30 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.3455 (19) | 1.1260 (15) | 0.708 (2) | 0.041 (4)* | |
C2 | 0.4611 (18) | 1.1748 (15) | 0.581 (2) | 0.041 (4)* | |
C3 | 0.4669 (19) | 1.1159 (15) | 0.370 (2) | 0.041 (4)* | |
C4 | 0.357 (2) | 1.0084 (15) | 0.2846 (18) | 0.041 (4)* | |
C5 | 0.131 (2) | 0.8515 (14) | 0.326 (2) | 0.041 (4)* | |
C6 | 0.015 (2) | 0.8027 (13) | 0.452 (2) | 0.041 (4)* | |
C7 | 0.0092 (19) | 0.8615 (14) | 0.664 (3) | 0.041 (4)* | |
C8 | 0.1191 (19) | 0.9690 (15) | 0.749 (2) | 0.041 (4)* | |
C9 | 0.2352 (19) | 1.0183 (14) | 0.6229 (19) | 0.041 (4)* | |
C10 | 0.241 (2) | 0.9592 (13) | 0.4105 (18) | 0.041 (4)* | |
H1 | 0.342 (2) | 1.1727 (18) | 0.872 (2) | 0.05* | |
H3 | 0.557 (2) | 1.1538 (16) | 0.272 (2) | 0.05* | |
H4 | 0.363 (2) | 0.9637 (17) | 0.1198 (19) | 0.05* | |
H5 | 0.134 (2) | 0.8048 (16) | 0.162 (2) | 0.05* | |
H7 | −0.081 (2) | 0.8237 (15) | 0.762 (3) | 0.05* | |
H8 | 0.113 (2) | 1.0138 (18) | 0.914 (2) | 0.05* | |
C11 | 0.5798 (19) | 1.2910 (17) | 0.674 (3) | 0.003 (4)* | |
C12 | −0.104 (2) | 0.6865 (14) | 0.360 (3) | 0.003 (4)* | |
O1 | 0.587 (2) | 1.315 (3) | 0.864 (4) | 0.003 (4)* | |
O2 | 0.679 (2) | 1.333 (2) | 0.535 (4) | 0.003 (4)* | |
O3 | −0.227 (3) | 0.687 (2) | 0.491 (4) | 0.003 (4)* | |
O4 | −0.101 (3) | 0.635 (3) | 0.207 (4) | 0.003 (4)* | |
Co | 0.7467 (12) | 1.4819 (11) | 1.0291 (19) | 0.052 (4)* | |
O5 | 0.883 (3) | 1.466 (3) | 0.746 (4) | 0.023 (5)* | |
O6 | 0.602 (3) | 1.490 (2) | 1.272 (4) | 0.023 (5)* | |
O7 | 0.827 (2) | 1.348 (2) | 1.137 (4) | 0.023 (5)* | |
O8 | 0.694 (3) | 1.623 (2) | 0.902 (4) | 0.023 (5)* | |
H5a | 0.86416 | 1.38101 | 0.75995 | 0.03* | |
H5b | 0.96329 | 1.50775 | 0.86141 | 0.03* | |
H6a | 0.54693 | 1.39876 | 1.25994 | 0.03* | |
H6b | 0.66144 | 1.49091 | 1.39108 | 0.03* | |
H7a | 0.84693 | 1.37086 | 1.28164 | 0.03* | |
H7b | 0.75374 | 1.26519 | 1.11385 | 0.03* | |
H8a | 0.66284 | 1.56483 | 0.7441 | 0.03* | |
H8b | 0.59358 | 1.59916 | 0.96558 | 0.03* | |
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