Bis(4-aminobenzenesulfonato)tri­aqua­bis(1,10-phenanthroline)neodymium(III) nitrate tetrahydrate

Ma, P.; Huang, M.-L.; Chen, K.-H.

doi:10.1107/S1600536810023445

metal-organic compounds

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Volume 66| Part 7| July 2010| Page m833

doi:10.1107/S1600536810023445

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Bis(4-aminobenzenesulfonato)triaquabis(1,10-phenanthroline)neodymium(III) nitrate tetrahydrate

Peng Ma,^a Miao-Ling Huang ^a ^* and Kai-Han Chen ^a

^aDepartment of Chemistry and Science of Life, Quanzhou Normal University, Fujian 362000, People's Republic of China
^*Correspondence e-mail: hml301@163.com

(Received 23 April 2010; accepted 17 June 2010; online 23 June 2010)

The title complex, [Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃·4H₂O, comprises a mononuclear cation, an NO₃⁻ anion and two uncoordinated water molecules; the Nd^III cation, one coordinated water molecule, and the NO₃⁻ anion each lie on a twofold axis of symmetry. The Nd^III ion exhibits an NdN₄O₅ coordination environment comprising two O atoms of two monodentate 4-aminobenzenesulfonato ligands, four N atoms of the bidentate 1,10-phenanthroline ligands, and three water-O atoms. The coordination geometry is based on a tricapped triangular-prismatic arrangement. The components are consolidated into a three-dimensional network via O—H⋯O, O—H⋯N and N—H⋯O hydrogen-bonding interactions

Related literature

For background to the applications of rare earth complexes, see: Li et al. (2007 ); Tang et al. (2006 ); Xie et al. (2009 ).

Experimental

Crystal data

[Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃·4H₂O
M_r = 1037.13
Orthorhombic, P c c n
a = 17.4990 (18) Å
b = 14.2788 (15) Å
c = 16.7045 (17) Å
V = 4173.9 (7) Å³
Z = 4
Mo Kα radiation
μ = 1.42 mm⁻¹
T = 293 K
0.32 × 0.22 × 0.16 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.656, T_max = 0.789
34751 measured reflections
3883 independent reflections
3287 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.066
S = 1.21
3883 reflections
282 parameters
H-atom parameters constrained
Δρ_max = 0.31 e Å⁻³
Δρ_min = −0.76 e Å⁻³

Table 1
Selected bond lengths (Å)

Nd1—O1	2.4007 (18)
Nd1—O5	2.462 (2)
Nd1—O4	2.528 (3)
Nd1—N3	2.703 (2)
Nd1—N2	2.763 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H6W⋯O3	0.85	1.97	2.810 (3)	171
O8—H5W⋯N4	0.86	2.61	3.391 (3)	152
O8—H5W⋯O7	0.86	2.53	3.109 (4)	126
O8—H5W⋯O6	0.86	1.99	2.842 (3)	170
O8—H4W⋯O3	0.83	2.03	2.861 (3)	174
O9—H7W⋯N1ⁱ	0.86	2.24	2.982 (4)	145
O5—H3W⋯O8ⁱⁱ	0.85	1.96	2.793 (3)	168
O5—H2W⋯O9ⁱⁱⁱ	0.85	1.83	2.670 (3)	171
O4—H1W⋯O2ⁱⁱⁱ	0.83	1.95	2.773 (3)	171
N1—H1A⋯O8^iv	0.89	2.29	3.127 (4)	158
Symmetry codes: (i) $[x-{\script{1\over 2}}, -y+1, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z]$ ; (iii) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (iv) -x+1, -y+1, -z.

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2003 ); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810023445/tk2665sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810023445/tk2665Isup2.hkl

checkCIF report

Comment top

Rare earth complexes have been extensively studied owing to their unique structures and potential applications as biomedical, catalytic, and magnetic agents, as well as nonlinear optical materials (Tang et al., 2006; Li et al., 2007). Therefore, the rational design and synthesis of rare earth supramolecular complexes are highlighted in supramolecular and biochemical research.

The molecules comprising the asymmetric unit of the title compound, (I), are presented in Fig 1. The structure comprises a mononuclear [Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]⁺ cation, one NO₃^- anion and two lattice water molecules. The Nd(III) cation, one coordinated water molecule (O4) and the NO₃^- anion are each located on a crystallographic 2-fold axis. The Nd(III) ion is within a distorted tricapped triangular prismatic coordination polyhedron completed by two O atoms from two 4-aminobenzenesulfonato ligands, three O atoms from three coordinated water, and four N atom from two 1,10-phenanthroline ligands; see Table 1 for bond distances. The average bond lengths of Nd—O and Nd—N are shorter than the averages of the comparable bond lengths in [Ln(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃.(H₂O)₂ for Ln = La^III and Ce^III (Xie et al., 2009), consistent with the lanthanide contraction.

The components of the structure are consolidated into a 3-D network via hydrogen bonding interactions, Table 2.

Related literature top

For background to the applications of rare earth complexes, see: Li et al. (2007); Tang et al. (2006); Xie et al. (2009).

Experimental top

An aqueous solution (5 ml) of Nd(NO₃)₃.6H₂O (1.0 mmol) was added slowly to a solution of p-aminobenzenesulfonilic acid (1.0 mmol) in H₂O (5 ml). After refluxing for 2 h, a solution of 1,10-phenanthroline (1.0 mmol) in ethanol (95%, 5 ml) was added slowly to the solution. Refluxing was continued for 2 h followed by filteration of the hot mixture. The purple single crystals suitable for X-ray analysis were obtained after three weeks by slow evaporation of the above filtrate held at room temperature. Yield 52%. IR (KBr): 3425(vs), 1666(s), 1624(s), 1600(s), 1572(m), 1515(s), 1506(s), 1419(vs), 1384(vs), 1342(w), 1316(m), 1304(m), 1231(s), 1122(vs), 1039(vs), 1012(s), 848(s), 825(m), 776(m), 729(s), 700(s), 632(m), 574(s) cm^-1.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. Molecular structures of the components of (I) showing the atom-labelling scheme and displacement ellipsoids at the 50% probability level. Hydrogen atoms have been omitted for reasons of clarity. Symmetry operation a: 1-x, 1-y, -z.

Bis(4-aminobenzenesulfonato)triaquabis(1,10-phenanthroline)neodymium(III) nitrate tetrahydrate top

Crystal data top

[Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃·4H₂O	F(000) = 2108
M_r = 1037.13	D_x = 1.650 Mg m⁻³
Orthorhombic, Pccn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2ac	Cell parameters from 2148 reflections
a = 17.4990 (18) Å	θ = 2.5–23.3°
b = 14.2788 (15) Å	µ = 1.42 mm⁻¹
c = 16.7045 (17) Å	T = 293 K
V = 4173.9 (7) Å³	Block, pink
Z = 4	0.32 × 0.22 × 0.16 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3883 independent reflections
Radiation source: fine-focus sealed tube	3287 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
ϕ and ω scans	θ_max = 25.5°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −21→21
T_min = 0.656, T_max = 0.789	k = −17→17
34751 measured reflections	l = −20→20

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.066	H-atom parameters constrained
S = 1.21	w = 1/[σ²(F_o²) + (0.0264P)² + 3.2531P] where P = (F_o² + 2F_c²)/3
3883 reflections	(Δ/σ)_max = 0.001
282 parameters	Δρ_max = 0.31 e Å⁻³
0 restraints	Δρ_min = −0.76 e Å⁻³

Crystal data top

[Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃·4H₂O	V = 4173.9 (7) Å³
M_r = 1037.13	Z = 4
Orthorhombic, Pccn	Mo Kα radiation
a = 17.4990 (18) Å	µ = 1.42 mm⁻¹
b = 14.2788 (15) Å	T = 293 K
c = 16.7045 (17) Å	0.32 × 0.22 × 0.16 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3883 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	3287 reflections with I > 2σ(I)
T_min = 0.656, T_max = 0.789	R_int = 0.027
34751 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.066	H-atom parameters constrained
S = 1.21	Δρ_max = 0.31 e Å⁻³
3883 reflections	Δρ_min = −0.76 e Å⁻³
282 parameters

Special details top

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.

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

	x	y	z	U_iso*/U_eq
Nd1	0.2500	0.2500	0.038262 (10)	0.02429 (7)
S1	0.36306 (4)	0.36807 (5)	0.20699 (4)	0.03383 (16)
O1	0.31177 (10)	0.33811 (14)	0.14217 (11)	0.0411 (5)
O2	0.35809 (13)	0.3088 (2)	0.27640 (12)	0.0611 (7)
O3	0.35040 (13)	0.46714 (16)	0.22412 (13)	0.0529 (6)
O4	0.2500	0.2500	−0.11307 (15)	0.0374 (6)
H1W	0.2862	0.2332	−0.1422	0.056*
O5	0.24704 (12)	0.08714 (15)	−0.01000 (13)	0.0483 (5)
H2W	0.2473	0.0658	−0.0576	0.073*
H3W	0.2417	0.0418	0.0226	0.073*
O6	0.2500	0.7500	0.1311 (3)	0.0821 (12)
H4W	0.3105	0.5399	0.1283	0.123*
H5W	0.2734	0.6180	0.1017	0.123*
O7	0.2625 (2)	0.6779 (2)	0.2436 (2)	0.0967 (10)
H6W	0.2805	0.4911	0.3142	0.145*
H7W	0.2402	0.5571	0.3568	0.145*
O8	0.29153 (17)	0.56444 (16)	0.08766 (14)	0.0662 (7)
O9	0.24465 (15)	0.49835 (19)	0.34785 (14)	0.0708 (8)
N1	0.67660 (15)	0.3332 (2)	0.0745 (2)	0.0696 (9)
H1A	0.6763	0.3506	0.0233	0.104*
H1B	0.6911	0.2736	0.0780	0.104*
N2	0.36395 (12)	0.14185 (16)	0.10577 (13)	0.0346 (5)
N3	0.39407 (13)	0.26033 (15)	−0.01948 (13)	0.0311 (5)
N4	0.2500	0.7500	0.2066 (3)	0.0571 (11)
C1	0.45674 (14)	0.35885 (18)	0.16953 (14)	0.0292 (6)
C2	0.50570 (16)	0.2901 (2)	0.19801 (16)	0.0371 (6)
H2	0.4895	0.2495	0.2381	0.045*
C3	0.57842 (17)	0.2820 (2)	0.1670 (2)	0.0450 (7)
H3	0.6113	0.2365	0.1871	0.054*
C4	0.60297 (16)	0.3411 (2)	0.10621 (18)	0.0426 (7)
C5	0.55417 (17)	0.4112 (2)	0.07957 (17)	0.0422 (7)
H5	0.5707	0.4528	0.0404	0.051*
C6	0.48166 (16)	0.4196 (2)	0.11059 (16)	0.0370 (6)
H6	0.4493	0.4663	0.0918	0.044*
C7	0.35188 (18)	0.0874 (2)	0.16914 (19)	0.0480 (8)
H7	0.3047	0.0908	0.1946	0.058*
C8	0.4070 (2)	0.0249 (3)	0.1995 (2)	0.0576 (9)
H8	0.3959	−0.0118	0.2441	0.069*
C9	0.4759 (2)	0.0187 (2)	0.1636 (2)	0.0548 (9)
H9	0.5125	−0.0230	0.1827	0.066*
C10	0.49175 (16)	0.0758 (2)	0.09720 (18)	0.0423 (7)
C11	0.56503 (18)	0.0738 (3)	0.0574 (2)	0.0541 (9)
H11	0.6023	0.0318	0.0743	0.065*
C12	0.57972 (17)	0.1318 (3)	−0.0037 (2)	0.0528 (9)
H12	0.6271	0.1293	−0.0288	0.063*
C13	0.52349 (16)	0.1980 (2)	−0.03103 (17)	0.0397 (7)
C14	0.53933 (17)	0.2646 (2)	−0.09115 (18)	0.0467 (8)
H14	0.5869	0.2657	−0.1159	0.056*
C15	0.48461 (17)	0.3270 (2)	−0.11248 (17)	0.0427 (7)
H15	0.4948	0.3727	−0.1506	0.051*
C16	0.41244 (16)	0.3217 (2)	−0.07639 (16)	0.0361 (6)
H16	0.3751	0.3636	−0.0932	0.043*
C17	0.44996 (14)	0.19932 (19)	0.00458 (16)	0.0305 (6)
C18	0.43377 (15)	0.13720 (18)	0.07021 (16)	0.0319 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nd1	0.02232 (11)	0.02820 (11)	0.02233 (11)	0.00157 (8)	0.000	0.000
S1	0.0281 (3)	0.0459 (4)	0.0275 (3)	−0.0015 (3)	−0.0001 (3)	−0.0048 (3)
O1	0.0293 (10)	0.0500 (12)	0.0442 (11)	−0.0011 (9)	−0.0082 (8)	−0.0131 (10)
O2	0.0438 (13)	0.099 (2)	0.0406 (12)	0.0019 (13)	0.0119 (10)	0.0245 (12)
O3	0.0455 (13)	0.0524 (13)	0.0607 (14)	0.0027 (10)	0.0018 (10)	−0.0276 (11)
O4	0.0294 (13)	0.0596 (18)	0.0231 (13)	0.0086 (12)	0.000	0.000
O5	0.0782 (16)	0.0345 (11)	0.0323 (10)	0.0046 (10)	−0.0075 (10)	−0.0015 (9)
O6	0.112 (4)	0.070 (3)	0.064 (3)	0.030 (2)	0.000	0.000
O7	0.136 (3)	0.0635 (19)	0.091 (2)	0.0118 (18)	0.003 (2)	0.0209 (19)
O8	0.095 (2)	0.0502 (14)	0.0531 (14)	0.0019 (14)	0.0048 (14)	−0.0095 (12)
O9	0.099 (2)	0.0661 (17)	0.0477 (14)	0.0286 (14)	0.0217 (13)	0.0124 (13)
N1	0.0397 (16)	0.081 (2)	0.088 (2)	−0.0044 (15)	0.0208 (16)	−0.0120 (19)
N2	0.0288 (12)	0.0390 (13)	0.0359 (12)	0.0026 (10)	−0.0036 (10)	0.0035 (10)
N3	0.0296 (12)	0.0345 (13)	0.0291 (11)	−0.0014 (9)	−0.0006 (9)	−0.0023 (10)
N4	0.055 (3)	0.052 (3)	0.064 (3)	0.0073 (19)	0.000	0.000
C1	0.0276 (13)	0.0366 (15)	0.0233 (12)	−0.0038 (11)	−0.0015 (10)	−0.0030 (11)
C2	0.0365 (16)	0.0398 (15)	0.0352 (15)	−0.0041 (13)	−0.0041 (12)	0.0061 (13)
C3	0.0324 (16)	0.0465 (17)	0.0559 (19)	0.0029 (13)	−0.0060 (14)	0.0006 (15)
C4	0.0315 (15)	0.0512 (18)	0.0449 (17)	−0.0100 (13)	0.0041 (13)	−0.0140 (15)
C5	0.0458 (17)	0.0458 (17)	0.0349 (15)	−0.0116 (14)	0.0068 (13)	0.0031 (14)
C6	0.0400 (16)	0.0374 (15)	0.0337 (14)	−0.0013 (12)	−0.0018 (12)	0.0031 (12)
C7	0.0408 (17)	0.056 (2)	0.0474 (18)	0.0022 (15)	−0.0044 (14)	0.0198 (16)
C8	0.057 (2)	0.060 (2)	0.056 (2)	0.0021 (17)	−0.0161 (17)	0.0238 (17)
C9	0.052 (2)	0.0476 (19)	0.065 (2)	0.0147 (15)	−0.0201 (17)	0.0099 (17)
C10	0.0363 (16)	0.0383 (16)	0.0523 (18)	0.0098 (13)	−0.0122 (13)	−0.0072 (14)
C11	0.0380 (18)	0.056 (2)	0.068 (2)	0.0207 (15)	−0.0120 (16)	−0.0133 (18)
C12	0.0272 (15)	0.068 (2)	0.064 (2)	0.0101 (15)	0.0037 (15)	−0.0190 (19)
C13	0.0302 (15)	0.0477 (18)	0.0412 (16)	−0.0022 (13)	0.0007 (12)	−0.0165 (14)
C14	0.0310 (15)	0.069 (2)	0.0399 (16)	−0.0109 (15)	0.0081 (13)	−0.0170 (16)
C15	0.0450 (17)	0.0521 (18)	0.0312 (14)	−0.0155 (14)	0.0048 (13)	−0.0052 (14)
C16	0.0361 (15)	0.0407 (16)	0.0315 (14)	−0.0054 (12)	−0.0002 (12)	−0.0016 (13)
C17	0.0242 (13)	0.0335 (15)	0.0337 (14)	0.0001 (11)	−0.0038 (11)	−0.0110 (12)
C18	0.0283 (14)	0.0320 (14)	0.0354 (14)	0.0015 (11)	−0.0072 (11)	−0.0072 (12)

Geometric parameters (Å, º) top

Nd1—O1	2.4007 (18)	C1—C2	1.387 (4)
Nd1—O1ⁱ	2.4007 (18)	C1—C6	1.383 (4)
Nd1—O5ⁱ	2.462 (2)	C2—C3	1.379 (4)
Nd1—O5	2.462 (2)	C2—H2	0.9300
Nd1—O4	2.528 (3)	C3—C4	1.389 (4)
Nd1—N3ⁱ	2.703 (2)	C3—H3	0.9300
Nd1—N3	2.703 (2)	C4—C5	1.389 (4)
Nd1—N2	2.763 (2)	C5—C6	1.376 (4)
Nd1—N2ⁱ	2.763 (2)	C5—H5	0.9300
S1—O2	1.438 (2)	C6—H6	0.9300
S1—O3	1.460 (2)	C7—C8	1.408 (4)
S1—O1	1.4701 (18)	C7—H7	0.9300
S1—C1	1.760 (3)	C8—C9	1.350 (5)
O4—H1W	0.8343	C8—H8	0.9300
O5—H2W	0.8517	C9—C10	1.404 (4)
O5—H3W	0.8502	C9—H9	0.9300
O6—N4	1.262 (6)	C10—C18	1.415 (4)
O7—N4	1.220 (4)	C10—C11	1.445 (4)
O8—H4W	0.8327	C11—C12	1.339 (5)
O8—H5W	0.8602	C11—H11	0.9300
O9—H6W	0.8478	C12—C13	1.439 (4)
O9—H7W	0.8562	C12—H12	0.9300
N1—C4	1.398 (4)	C13—C14	1.411 (4)
N1—H1A	0.8900	C13—C17	1.418 (4)
N1—H1B	0.8900	C14—C15	1.355 (4)
N2—C7	1.330 (4)	C14—H14	0.9300
N2—C18	1.360 (3)	C15—C16	1.401 (4)
N3—C16	1.332 (3)	C15—H15	0.9300
N3—C17	1.370 (3)	C16—H16	0.9300
N4—O7ⁱⁱ	1.220 (4)	C17—C18	1.438 (4)

O1—Nd1—O1ⁱ	87.40 (10)	O7ⁱⁱ—N4—O7	119.2 (5)
O1—Nd1—O5ⁱ	74.47 (7)	O7ⁱⁱ—N4—O6	120.4 (3)
O1ⁱ—Nd1—O5ⁱ	137.84 (7)	O7—N4—O6	120.4 (3)
O1—Nd1—O5	137.84 (7)	C2—C1—C6	119.6 (2)
O1ⁱ—Nd1—O5	74.47 (7)	C2—C1—S1	120.4 (2)
O5ⁱ—Nd1—O5	141.77 (10)	C6—C1—S1	120.0 (2)
O1—Nd1—O4	136.30 (5)	C1—C2—C3	120.1 (3)
O1ⁱ—Nd1—O4	136.30 (5)	C1—C2—H2	120.0
O5ⁱ—Nd1—O4	70.89 (5)	C3—C2—H2	120.0
O5—Nd1—O4	70.89 (5)	C2—C3—C4	120.6 (3)
O1—Nd1—N3ⁱ	134.94 (6)	C2—C3—H3	119.7
O1ⁱ—Nd1—N3ⁱ	79.02 (6)	C4—C3—H3	119.7
O5ⁱ—Nd1—N3ⁱ	87.38 (7)	C5—C4—C3	118.8 (3)
O5—Nd1—N3ⁱ	79.16 (7)	C5—C4—N1	120.2 (3)
O4—Nd1—N3ⁱ	69.10 (5)	C3—C4—N1	120.9 (3)
O1—Nd1—N3	79.02 (6)	C6—C5—C4	120.6 (3)
O1ⁱ—Nd1—N3	134.94 (6)	C6—C5—H5	119.7
O5ⁱ—Nd1—N3	79.16 (7)	C4—C5—H5	119.7
O5—Nd1—N3	87.38 (7)	C5—C6—C1	120.3 (3)
O4—Nd1—N3	69.10 (5)	C5—C6—H6	119.9
N3ⁱ—Nd1—N3	138.20 (9)	C1—C6—H6	119.9
O1—Nd1—N2	70.91 (7)	N2—C7—C8	123.3 (3)
O1ⁱ—Nd1—N2	74.75 (6)	N2—C7—H7	118.4
O5ⁱ—Nd1—N2	130.28 (7)	C8—C7—H7	118.4
O5—Nd1—N2	67.72 (7)	C9—C8—C7	119.5 (3)
O4—Nd1—N2	114.09 (5)	C9—C8—H8	120.2
N3ⁱ—Nd1—N2	142.02 (6)	C7—C8—H8	120.2
N3—Nd1—N2	60.20 (7)	C8—C9—C10	119.3 (3)
O1—Nd1—N2ⁱ	74.75 (6)	C8—C9—H9	120.3
O1ⁱ—Nd1—N2ⁱ	70.91 (7)	C10—C9—H9	120.3
O5ⁱ—Nd1—N2ⁱ	67.72 (7)	C9—C10—C18	118.0 (3)
O5—Nd1—N2ⁱ	130.28 (7)	C9—C10—C11	121.9 (3)
O4—Nd1—N2ⁱ	114.09 (5)	C18—C10—C11	120.1 (3)
N3ⁱ—Nd1—N2ⁱ	60.20 (7)	C12—C11—C10	120.6 (3)
N3—Nd1—N2ⁱ	142.02 (6)	C12—C11—H11	119.7
N2—Nd1—N2ⁱ	131.82 (9)	C10—C11—H11	119.7
O2—S1—O3	113.77 (15)	C11—C12—C13	121.1 (3)
O2—S1—O1	112.68 (14)	C11—C12—H12	119.4
O3—S1—O1	109.49 (12)	C13—C12—H12	119.4
O2—S1—C1	107.40 (13)	C14—C13—C17	117.9 (3)
O3—S1—C1	106.48 (13)	C14—C13—C12	122.3 (3)
O1—S1—C1	106.57 (11)	C17—C13—C12	119.8 (3)
S1—O1—Nd1	163.72 (13)	C15—C14—C13	119.4 (3)
Nd1—O4—H1W	125.7	C15—C14—H14	120.3
Nd1—O5—H2W	130.1	C13—C14—H14	120.3
Nd1—O5—H3W	120.8	C14—C15—C16	119.2 (3)
H2W—O5—H3W	109.0	C14—C15—H15	120.4
H4W—O8—H5W	107.4	C16—C15—H15	120.4
H6W—O9—H7W	107.6	N3—C16—C15	124.0 (3)
C4—N1—H1A	109.6	N3—C16—H16	118.0
C4—N1—H1B	108.3	C15—C16—H16	118.0
H1A—N1—H1B	109.5	N3—C17—C13	122.2 (3)
C7—N2—C18	117.5 (2)	N3—C17—C18	118.4 (2)
C7—N2—Nd1	122.47 (18)	C13—C17—C18	119.4 (2)
C18—N2—Nd1	119.83 (17)	N2—C18—C10	122.4 (3)
C16—N3—C17	117.1 (2)	N2—C18—C17	118.7 (2)
C16—N3—Nd1	121.03 (18)	C10—C18—C17	118.9 (2)
C17—N3—Nd1	121.76 (17)

O2—S1—O1—Nd1	−61.6 (5)	O1—S1—C1—C6	69.4 (2)
O3—S1—O1—Nd1	170.7 (4)	C6—C1—C2—C3	−0.7 (4)
C1—S1—O1—Nd1	55.9 (5)	S1—C1—C2—C3	178.5 (2)
O1ⁱ—Nd1—O1—S1	77.3 (4)	C1—C2—C3—C4	−1.2 (4)
O5ⁱ—Nd1—O1—S1	−141.2 (5)	C2—C3—C4—C5	2.8 (4)
O5—Nd1—O1—S1	14.0 (5)	C2—C3—C4—N1	−179.9 (3)
O4—Nd1—O1—S1	−102.7 (4)	C3—C4—C5—C6	−2.6 (4)
N3ⁱ—Nd1—O1—S1	148.9 (4)	N1—C4—C5—C6	−179.9 (3)
N3—Nd1—O1—S1	−59.5 (4)	C4—C5—C6—C1	0.8 (4)
N2—Nd1—O1—S1	2.5 (4)	C2—C1—C6—C5	0.9 (4)
N2ⁱ—Nd1—O1—S1	148.2 (5)	S1—C1—C6—C5	−178.3 (2)
O1—Nd1—N2—C7	88.4 (2)	C18—N2—C7—C8	−1.2 (5)
O1ⁱ—Nd1—N2—C7	−4.2 (2)	Nd1—N2—C7—C8	173.5 (3)
O5ⁱ—Nd1—N2—C7	136.7 (2)	N2—C7—C8—C9	0.0 (5)
O5—Nd1—N2—C7	−83.3 (2)	C7—C8—C9—C10	0.9 (5)
O4—Nd1—N2—C7	−138.5 (2)	C8—C9—C10—C18	−0.6 (5)
N3ⁱ—Nd1—N2—C7	−52.1 (3)	C8—C9—C10—C11	178.6 (3)
N3—Nd1—N2—C7	176.5 (2)	C9—C10—C11—C12	−177.1 (3)
N2ⁱ—Nd1—N2—C7	41.5 (2)	C18—C10—C11—C12	2.1 (5)
O1—Nd1—N2—C18	−96.98 (19)	C10—C11—C12—C13	0.4 (5)
O1ⁱ—Nd1—N2—C18	170.5 (2)	C11—C12—C13—C14	175.2 (3)
O5ⁱ—Nd1—N2—C18	−48.6 (2)	C11—C12—C13—C17	−2.9 (5)
O5—Nd1—N2—C18	91.31 (19)	C17—C13—C14—C15	0.2 (4)
O4—Nd1—N2—C18	36.1 (2)	C12—C13—C14—C15	−177.9 (3)
N3ⁱ—Nd1—N2—C18	122.54 (18)	C13—C14—C15—C16	−2.3 (4)
N3—Nd1—N2—C18	−8.93 (17)	C17—N3—C16—C15	0.1 (4)
N2ⁱ—Nd1—N2—C18	−143.9 (2)	Nd1—N3—C16—C15	−175.9 (2)
O1—Nd1—N3—C16	−101.0 (2)	C14—C15—C16—N3	2.3 (4)
O1ⁱ—Nd1—N3—C16	−176.01 (18)	C16—N3—C17—C13	−2.5 (4)
O5ⁱ—Nd1—N3—C16	−24.94 (19)	Nd1—N3—C17—C13	173.55 (18)
O5—Nd1—N3—C16	119.1 (2)	C16—N3—C17—C18	175.2 (2)
O4—Nd1—N3—C16	48.57 (18)	Nd1—N3—C17—C18	−8.8 (3)
N3ⁱ—Nd1—N3—C16	48.57 (18)	C14—C13—C17—N3	2.3 (4)
N2—Nd1—N3—C16	−175.2 (2)	C12—C13—C17—N3	−179.5 (3)
N2ⁱ—Nd1—N3—C16	−54.2 (2)	C14—C13—C17—C18	−175.3 (2)
O1—Nd1—N3—C17	83.12 (19)	C12—C13—C17—C18	2.8 (4)
O1ⁱ—Nd1—N3—C17	8.1 (2)	C7—N2—C18—C10	1.5 (4)
O5ⁱ—Nd1—N3—C17	159.2 (2)	Nd1—N2—C18—C10	−173.37 (19)
O5—Nd1—N3—C17	−56.76 (19)	C7—N2—C18—C17	−176.3 (3)
O4—Nd1—N3—C17	−127.28 (19)	Nd1—N2—C18—C17	8.8 (3)
N3ⁱ—Nd1—N3—C17	−127.28 (19)	C9—C10—C18—N2	−0.6 (4)
N2—Nd1—N3—C17	8.96 (17)	C11—C10—C18—N2	−179.8 (3)
N2ⁱ—Nd1—N3—C17	129.96 (18)	C9—C10—C18—C17	177.2 (3)
O2—S1—C1—C2	11.2 (3)	C11—C10—C18—C17	−2.0 (4)
O3—S1—C1—C2	133.4 (2)	N3—C17—C18—N2	−0.3 (4)
O1—S1—C1—C2	−109.8 (2)	C13—C17—C18—N2	177.5 (2)
O2—S1—C1—C6	−169.6 (2)	N3—C17—C18—C10	−178.1 (2)
O3—S1—C1—C6	−47.4 (2)	C13—C17—C18—C10	−0.4 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H6W···S1	0.85	2.90	3.646 (2)	149
O9—H6W···O3	0.85	1.97	2.810 (3)	171
O8—H5W···N4	0.86	2.61	3.391 (3)	152
O8—H5W···O7	0.86	2.53	3.109 (4)	126
O8—H5W···O6	0.86	1.99	2.842 (3)	170
O8—H4W···S1	0.83	2.93	3.661 (3)	148
O8—H4W···O3	0.83	2.03	2.861 (3)	174
O9—H7W···N1ⁱⁱⁱ	0.86	2.24	2.982 (4)	145
O5—H3W···O8ⁱ	0.85	1.96	2.793 (3)	168
O5—H2W···O9^iv	0.85	1.83	2.670 (3)	171
O4—H1W···O2^iv	0.83	1.95	2.773 (3)	171
N1—H1A···O8^v	0.89	2.29	3.127 (4)	158

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

Experimental details

Crystal data
Chemical formula	[Nd(C₆H₆NO₃S)₂(C₁₂H₈N₂)₂(H₂O)₃]NO₃·4H₂O
M_r	1037.13
Crystal system, space group	Orthorhombic, Pccn
Temperature (K)	293
a, b, c (Å)	17.4990 (18), 14.2788 (15), 16.7045 (17)
V (Å³)	4173.9 (7)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.42
Crystal size (mm)	0.32 × 0.22 × 0.16

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.656, 0.789
No. of measured, independent and observed [I > 2σ(I)] reflections	34751, 3883, 3287
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.066, 1.21
No. of reflections	3883
No. of parameters	282
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.31, −0.76

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2003), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Nd1—O1	2.4007 (18)	Nd1—N3	2.703 (2)
Nd1—O5	2.462 (2)	Nd1—N2	2.763 (2)
Nd1—O4	2.528 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H6W···S1	0.85	2.90	3.646 (2)	149
O9—H6W···O3	0.85	1.97	2.810 (3)	171
O8—H5W···N4	0.86	2.61	3.391 (3)	152
O8—H5W···O7	0.86	2.53	3.109 (4)	126
O8—H5W···O6	0.86	1.99	2.842 (3)	170
O8—H4W···S1	0.83	2.93	3.661 (3)	148
O8—H4W···O3	0.83	2.03	2.861 (3)	174
O9—H7W···N1ⁱ	0.86	2.24	2.982 (4)	145
O5—H3W···O8ⁱⁱ	0.85	1.96	2.793 (3)	168
O5—H2W···O9ⁱⁱⁱ	0.85	1.83	2.670 (3)	171
O4—H1W···O2ⁱⁱⁱ	0.83	1.95	2.773 (3)	171
N1—H1A···O8^iv	0.89	2.29	3.127 (4)	158

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

Acknowledgements

This work was supported by the Technology Gallery Foundation of Fujian Province of China (grant No. 2008 F5053).

References

Bruker (2001). SMART. Bruker AXS Inc., Madison,Wisconsin, USA. Google Scholar
Bruker (2003). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Li, Y. Q., Ju, Y. L., Zhang, Y. B., Wang, C. Y., Zhang, T. T. & Li, X. (2007). Chin. J. Inorg. Chem. 23, 969–974. CAS Google Scholar
Sheldrick, G. M. (2003). 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
Tang, Y., Tang, K. Z., Zhang, J., Qin, M. Y., Liu, M. Y. & Sun, Y. X. (2006). Acta Chim. Sin. 64, 444–449. CAS Google Scholar
Xie, Q. F., Huang, M. L. & Chen, Y. M. (2009). Chin. J. Inorg. Chem. 25, 249–255. CAS Google Scholar

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Volume 66| Part 7| July 2010| Page m833

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Bis(4-amino­benzene­sulfonato)tri­aqua­bis­(1,10-phenanthroline)neodymium(III) nitrate tetrahydrate

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Bis(4-aminobenzenesulfonato)triaquabis(1,10-phenanthroline)neodymium(III) nitrate tetrahydrate