{μ-6,6'-Dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato}-μ-nitrato-dinitratoholmium(III)zinc(II).

In the title heteronuclear Zn(II)-Ho(III) complex (systematic name: {μ-6,6'-dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato-1κ(4)O(1),O(1'),O(6),O(6'):2κ(4)O(1),N,N',O(1'))-μ-nitrato-1:2κ(2)O:O'-dinitrato-1κ(4)O,O'-holmium(III)zinc(II)), [HoZn(C(18)H(18)N(2)O(4))(NO(3))(3)], with the hexa-dentate Schiff base compartmental ligand N,N'-bis-(3-methoxy-salicyl-idene)ethyl-enediamine (H(2)L), the Ho and Zn atoms are triply bridged by two phenolate O atoms of the Schiff base ligand and one nitrate ion. The five-coordinate Zn atom is in a square-pyramidal geometry with the donor centers of two imine N atoms, two phenolate O atoms and one of the bridging nitrate O atoms. The Ho(III) center has a ninefold coordination environment of O atoms, involving the phenolate O atoms, two meth-oxy O atoms, two O atoms from two nitrate ions and one from the bridging nitrate ion. Weak inter-molecular C-H⋯O inter-actions generate a two-dimensional double-layer structure.

Related literature

For related literature, see: Baggio et al. (2000 ▶); Caravan et al. (1999 ▶); Edder et al. (2000 ▶); Knoer et al. (2005 ▶); Sui et al. (2006 ▶, 2007 ▶).

Experimental

Crystal data

[HoZn(C18H18N2O4)(NO3)3]

M = 742.67

Monoclinic,

a = 10.694 (4) Å

b = 16.481 (7) Å

c = 14.921 (6) Å

β = 99.667 (6)°

V = 2592.4 (18) Å3

Z = 4

Mo Kα radiation

μ = 4.03 mm−1

T = 293 (2) K

0.16 × 0.16 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.565, T max = 0.689

15217 measured reflections

4499 independent reflections

3377 reflections with I > 2σ(I)

R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.034

wR(F 2) = 0.093

S = 1.02

4499 reflections

345 parameters

2 restraints

H-atom parameters constrained

Δρmax = 0.60 e Å−3

Δρmin = −1.18 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: APEX2; software used to prepare material for publication: APEX2 and publCIF (Westrip, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808013743/at2567sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808013743/at2567Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[HoZn(C18H18N2O4)(NO3)3]	F000 = 1448
Mr = 742.67	Dx = 1.903 Mg m−3
Monoclinic, P21/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5632 reflections
a = 10.694 (4) Å	θ = 2.2–25.3º
b = 16.481 (7) Å	µ = 4.03 mm−1
c = 14.921 (6) Å	T = 293 (2) K
β = 99.667 (6)º	Block, yellow
V = 2592.4 (18) Å3	0.16 × 0.16 × 0.10 mm
Z = 4

Bruker APEXII area-detector diffractometer	4499 independent reflections
Radiation source: fine-focus sealed tube	3377 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.037
T = 293(2) K	θmax = 25.0º
φ and ω scans	θmin = 2.2º
Absorption correction: multi-scan(SADABS; Bruker, 2004)	h = −12→12
Tmin = 0.565, Tmax = 0.689	k = −19→19
15217 measured reflections	l = −17→17

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034	H-atom parameters constrained
wR(F2) = 0.093	w = 1/[σ2(Fo2) + (0.0558P)2 + 0.1192P] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max < 0.001
4499 reflections	Δρmax = 0.61 e Å−3
345 parameters	Δρmin = −1.18 e Å−3
2 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

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
Ho1	0.36187 (2)	0.109293 (15)	0.723858 (16)	0.04439 (11)
Zn1	0.21999 (6)	0.03550 (4)	0.88927 (4)	0.04303 (17)
O1	0.2906 (4)	0.1419 (2)	0.8559 (2)	0.0493 (9)
O12	0.5712 (4)	0.1290 (3)	0.8198 (3)	0.0640 (12)
O2	0.3521 (4)	−0.0016 (2)	0.8158 (2)	0.0497 (9)
O4	0.4894 (3)	−0.0201 (2)	0.6956 (2)	0.0495 (9)
C17	0.4119 (5)	−0.0722 (3)	0.8204 (3)	0.0413 (12)
O8	0.2843 (4)	0.1975 (2)	0.5945 (2)	0.0582 (10)
N4	0.2806 (5)	0.1437 (3)	0.5329 (4)	0.0624 (14)
O6	0.1491 (4)	0.0740 (3)	0.6881 (3)	0.0613 (11)
C3	0.2935 (6)	0.3590 (4)	0.8767 (4)	0.0567 (15)
H3	0.3175	0.4036	0.8452	0.068*
N5	0.6224 (5)	0.1590 (4)	0.7564 (4)	0.0659 (15)
O5	0.0581 (3)	0.0283 (2)	0.8031 (3)	0.0543 (10)
C16	0.4896 (5)	−0.0846 (3)	0.7542 (4)	0.0460 (13)
O9	0.3274 (4)	0.0751 (3)	0.5596 (3)	0.0624 (11)
C2	0.3092 (5)	0.2813 (3)	0.8465 (3)	0.0448 (13)
C12	0.4039 (5)	−0.1325 (3)	0.8854 (4)	0.0457 (13)
N3	0.0556 (5)	0.0490 (3)	0.7206 (4)	0.0695 (14)
O11	0.5537 (4)	0.1634 (3)	0.6792 (3)	0.0612 (11)
O10	0.2350 (6)	0.1567 (3)	0.4552 (3)	0.107 (2)
N1	0.1978 (4)	0.0839 (3)	1.0120 (3)	0.0506 (12)
N2	0.2494 (4)	−0.0675 (3)	0.9634 (3)	0.0488 (11)
C11	0.3278 (5)	−0.1246 (4)	0.9578 (4)	0.0513 (15)
H11	0.3374	−0.1641	1.0030	0.062*
C7	0.2716 (5)	0.2135 (3)	0.8916 (3)	0.0428 (12)
C8	0.1985 (5)	0.1588 (4)	1.0310 (4)	0.0573 (16)
H8	0.1823	0.1728	1.0884	0.069*
C10	0.1754 (6)	−0.0615 (4)	1.0385 (4)	0.0590 (16)
H10A	0.2017	−0.1037	1.0830	0.071*
H10B	0.0859	−0.0688	1.0151	0.071*
C6	0.2222 (5)	0.2248 (3)	0.9720 (4)	0.0500 (14)
C18	0.5665 (6)	−0.0292 (4)	0.6251 (4)	0.0638 (17)
H18A	0.6543	−0.0328	0.6524	0.096*
H18B	0.5544	0.0168	0.5852	0.096*
H18C	0.5421	−0.0777	0.5910	0.096*
C5	0.2056 (6)	0.3045 (4)	1.0014 (4)	0.0631 (17)
H5	0.1699	0.3130	1.0533	0.076*
O13	0.7311 (5)	0.1830 (4)	0.7710 (4)	0.112 (2)
C4	0.2412 (7)	0.3697 (4)	0.9550 (4)	0.0643 (18)
H4	0.2302	0.4219	0.9762	0.077*
C15	0.5530 (6)	−0.1572 (4)	0.7500 (4)	0.0569 (15)
H15	0.6023	−0.1659	0.7052	0.068*
C9	0.1972 (6)	0.0203 (4)	1.0823 (4)	0.0612 (17)
H9A	0.1307	0.0317	1.1174	0.073*
H9B	0.2777	0.0205	1.1234	0.073*
C14	0.5419 (6)	−0.2169 (4)	0.8140 (5)	0.0701 (19)
H14	0.5833	−0.2662	0.8113	0.084*
C13	0.4716 (6)	−0.2043 (4)	0.8802 (4)	0.0623 (17)
H13	0.4683	−0.2446	0.9235	0.075*
O7	−0.0708 (6)	0.0407 (5)	0.6557 (5)	0.142 (3)
O3	0.3629 (4)	0.2616 (2)	0.7706 (2)	0.0502 (9)
C1	0.4246 (7)	0.3260 (4)	0.7307 (4)	0.0661 (17)
H1A	0.3638	0.3673	0.7090	0.099*
H1B	0.4611	0.3051	0.6808	0.099*
H1C	0.4903	0.3486	0.7755	0.099*

	U11	U22	U33	U12	U13	U23
Ho1	0.05102 (19)	0.04515 (17)	0.04112 (16)	0.00162 (12)	0.01960 (11)	0.00255 (11)
Zn1	0.0470 (4)	0.0447 (4)	0.0411 (3)	−0.0003 (3)	0.0182 (3)	0.0028 (3)
O1	0.067 (3)	0.036 (2)	0.052 (2)	−0.0004 (19)	0.034 (2)	−0.0054 (18)
O12	0.050 (2)	0.091 (3)	0.053 (2)	−0.010 (2)	0.0144 (19)	0.013 (2)
O2	0.064 (3)	0.042 (2)	0.051 (2)	0.0077 (19)	0.0327 (19)	0.0102 (17)
O4	0.060 (2)	0.048 (2)	0.047 (2)	0.0107 (19)	0.0264 (18)	0.0023 (18)
C17	0.035 (3)	0.037 (3)	0.051 (3)	0.003 (2)	0.006 (2)	0.000 (3)
O8	0.081 (3)	0.049 (2)	0.045 (2)	0.013 (2)	0.014 (2)	0.0020 (19)
N4	0.076 (4)	0.063 (3)	0.053 (3)	0.018 (3)	0.024 (3)	0.004 (3)
O6	0.058 (3)	0.074 (3)	0.052 (2)	−0.010 (2)	0.0101 (18)	0.007 (2)
C3	0.068 (4)	0.039 (3)	0.060 (4)	0.001 (3)	0.003 (3)	0.001 (3)
N5	0.056 (4)	0.079 (4)	0.068 (4)	−0.008 (3)	0.024 (3)	0.003 (3)
O5	0.047 (2)	0.055 (2)	0.064 (2)	−0.0028 (19)	0.0182 (19)	0.0082 (19)
C16	0.044 (3)	0.047 (3)	0.048 (3)	0.004 (3)	0.010 (2)	−0.002 (3)
O9	0.088 (3)	0.055 (3)	0.047 (2)	0.015 (2)	0.021 (2)	0.000 (2)
C2	0.053 (3)	0.035 (3)	0.045 (3)	0.003 (3)	0.004 (2)	−0.001 (2)
C12	0.041 (3)	0.044 (3)	0.053 (3)	−0.002 (3)	0.009 (3)	0.002 (3)
N3	0.065 (3)	0.072 (4)	0.072 (3)	−0.007 (3)	0.015 (3)	0.010 (3)
O11	0.060 (3)	0.079 (3)	0.048 (2)	−0.007 (2)	0.021 (2)	0.014 (2)
O10	0.154 (5)	0.118 (5)	0.043 (3)	0.058 (4)	0.003 (3)	0.004 (3)
N1	0.052 (3)	0.062 (3)	0.044 (3)	−0.005 (2)	0.024 (2)	−0.001 (2)
N2	0.047 (3)	0.052 (3)	0.049 (3)	0.001 (2)	0.015 (2)	0.010 (2)
C11	0.049 (4)	0.053 (4)	0.050 (3)	−0.007 (3)	0.003 (3)	0.011 (3)
C7	0.043 (3)	0.049 (3)	0.037 (3)	−0.001 (3)	0.008 (2)	−0.012 (3)
C8	0.055 (4)	0.078 (5)	0.044 (3)	0.000 (3)	0.025 (3)	−0.013 (3)
C10	0.056 (4)	0.070 (4)	0.055 (3)	−0.006 (3)	0.021 (3)	0.024 (3)
C6	0.058 (4)	0.048 (3)	0.045 (3)	0.001 (3)	0.012 (3)	−0.013 (3)
C18	0.071 (4)	0.068 (4)	0.063 (4)	0.011 (3)	0.040 (3)	0.003 (3)
C5	0.069 (4)	0.072 (5)	0.051 (3)	0.010 (4)	0.016 (3)	−0.022 (3)
O13	0.064 (3)	0.173 (6)	0.100 (4)	−0.036 (4)	0.021 (3)	0.026 (4)
C4	0.085 (5)	0.051 (4)	0.056 (4)	0.013 (4)	0.009 (3)	−0.016 (3)
C15	0.053 (4)	0.055 (4)	0.065 (4)	0.014 (3)	0.018 (3)	−0.007 (3)
C9	0.065 (4)	0.077 (5)	0.046 (3)	0.000 (3)	0.023 (3)	0.007 (3)
C14	0.067 (4)	0.046 (4)	0.102 (5)	0.021 (3)	0.025 (4)	0.006 (4)
C13	0.062 (4)	0.045 (4)	0.080 (4)	0.009 (3)	0.013 (3)	0.020 (3)
O7	0.099 (5)	0.175 (7)	0.138 (6)	−0.011 (5)	−0.026 (4)	−0.001 (5)
O3	0.067 (3)	0.038 (2)	0.049 (2)	−0.0051 (19)	0.0216 (18)	0.0003 (18)
C1	0.092 (5)	0.048 (4)	0.063 (4)	−0.013 (4)	0.026 (3)	0.005 (3)

Ho1—O1	2.293 (3)	C2—C7	1.398 (7)
Ho1—O2	2.298 (3)	C12—C13	1.396 (8)
Ho1—O3	2.604 (4)	C12—C11	1.463 (8)
Ho1—O4	2.604 (4)	N3—O7	1.531 (8)
Ho1—O6	2.323 (4)	N1—C8	1.267 (8)
Ho1—O8	2.448 (4)	N1—C9	1.484 (7)
Ho1—O9	2.481 (4)	N2—C11	1.273 (7)
Ho1—O11	2.430 (4)	N2—C10	1.480 (6)
Ho1—O12	2.468 (4)	C11—H11	0.9300
Zn1—O1	2.005 (4)	C7—C6	1.401 (7)
Zn1—O2	2.022 (3)	C8—C6	1.449 (8)
Zn1—O5	1.979 (4)	C8—H8	0.9300
Zn1—N1	2.047 (4)	C10—C9	1.498 (9)
Zn1—N2	2.021 (5)	C10—H10A	0.9700
O1—C7	1.324 (6)	C10—H10B	0.9700
O12—N5	1.269 (6)	C6—C5	1.406 (8)
O2—C17	1.325 (6)	C18—H18A	0.9600
O4—C16	1.376 (6)	C18—H18B	0.9600
O4—C18	1.449 (6)	C18—H18C	0.9600
C17—C12	1.402 (7)	C5—C4	1.367 (9)
C17—C16	1.408 (7)	C5—H5	0.9300
O8—N4	1.273 (6)	C4—H4	0.9300
N4—O10	1.199 (6)	C15—C14	1.390 (9)
N4—O9	1.272 (6)	C15—H15	0.9300
O6—N3	1.251 (6)	C9—H9A	0.9700
C3—C2	1.379 (8)	C9—H9B	0.9700
C3—C4	1.389 (9)	C14—C13	1.355 (9)
C3—H3	0.9300	C14—H14	0.9300
N5—O13	1.213 (7)	C13—H13	0.9300
N5—O11	1.260 (6)	O3—C1	1.431 (6)
O5—N3	1.274 (6)	C1—H1A	0.9600
C16—C15	1.382 (8)	C1—H1B	0.9600
C2—O3	1.390 (6)	C1—H1C	0.9600
O1—Ho1—O2	67.54 (12)	C15—C16—C17	120.6 (5)
O1—Ho1—O6	78.56 (14)	N4—O9—Ho1	95.4 (3)
O2—Ho1—O6	78.26 (14)	C3—C2—O3	124.9 (5)
O1—Ho1—O11	124.55 (14)	C3—C2—C7	121.6 (5)
O2—Ho1—O11	125.51 (14)	O3—C2—C7	113.4 (4)
O6—Ho1—O11	150.31 (13)	C13—C12—C17	118.0 (5)
O1—Ho1—O8	114.92 (13)	C13—C12—C11	118.3 (5)
O2—Ho1—O8	154.15 (14)	C17—C12—C11	123.7 (5)
O6—Ho1—O8	77.22 (14)	O6—N3—O5	125.0 (5)
O11—Ho1—O8	75.84 (14)	O6—N3—O7	117.5 (5)
O1—Ho1—O12	82.58 (14)	O5—N3—O7	117.4 (5)
O2—Ho1—O12	83.46 (14)	N5—O11—Ho1	96.7 (3)
O6—Ho1—O12	157.61 (13)	C8—N1—C9	122.1 (5)
O11—Ho1—O12	52.07 (13)	C8—N1—Zn1	125.6 (4)
O8—Ho1—O12	122.24 (14)	C9—N1—Zn1	111.8 (4)
O1—Ho1—O9	152.44 (15)	C11—N2—C10	122.7 (5)
O2—Ho1—O9	113.29 (14)	C11—N2—Zn1	129.0 (4)
O6—Ho1—O9	74.88 (14)	C10—N2—Zn1	107.7 (4)
O11—Ho1—O9	78.74 (14)	N2—C11—C12	124.6 (5)
O8—Ho1—O9	51.77 (13)	N2—C11—H11	117.7
O12—Ho1—O9	124.92 (14)	C12—C11—H11	117.7
O1—Ho1—O4	126.16 (12)	O1—C7—C2	116.2 (4)
O2—Ho1—O4	61.54 (11)	O1—C7—C6	124.6 (5)
O6—Ho1—O4	106.10 (14)	C2—C7—C6	119.1 (5)
O11—Ho1—O4	76.52 (13)	N1—C8—C6	126.2 (5)
O8—Ho1—O4	118.41 (12)	N1—C8—H8	116.9
O12—Ho1—O4	75.69 (14)	C6—C8—H8	116.9
O9—Ho1—O4	69.45 (12)	N2—C10—C9	109.0 (5)
O1—Ho1—O3	62.03 (12)	N2—C10—H10A	109.9
O2—Ho1—O3	127.20 (12)	C9—C10—H10A	109.9
O6—Ho1—O3	105.25 (14)	N2—C10—H10B	109.9
O11—Ho1—O3	75.75 (13)	C9—C10—H10B	109.9
O8—Ho1—O3	67.95 (12)	H10A—C10—H10B	108.3
O12—Ho1—O3	75.82 (14)	C7—C6—C5	118.5 (6)
O9—Ho1—O3	118.46 (12)	C7—C6—C8	123.4 (5)
O4—Ho1—O3	148.63 (12)	C5—C6—C8	117.8 (5)
O5—Zn1—O1	102.49 (16)	O4—C18—H18A	109.5
O5—Zn1—N2	110.09 (18)	O4—C18—H18B	109.5
O1—Zn1—N2	147.12 (18)	H18A—C18—H18B	109.5
O5—Zn1—O2	104.16 (16)	O4—C18—H18C	109.5
O1—Zn1—O2	78.64 (14)	H18A—C18—H18C	109.5
N2—Zn1—O2	89.09 (16)	H18B—C18—H18C	109.5
O5—Zn1—N1	112.60 (18)	C4—C5—C6	121.1 (6)
O1—Zn1—N1	89.23 (17)	C4—C5—H5	119.5
N2—Zn1—N1	82.44 (19)	C6—C5—H5	119.5
O2—Zn1—N1	143.00 (18)	C5—C4—C3	120.8 (6)
C7—O1—Zn1	126.1 (3)	C5—C4—H4	119.6
C7—O1—Ho1	130.6 (3)	C3—C4—H4	119.6
Zn1—O1—Ho1	101.65 (15)	C16—C15—C14	118.9 (6)
N5—O12—Ho1	94.7 (3)	C16—C15—H15	120.5
C17—O2—Zn1	127.8 (3)	C14—C15—H15	120.5
C17—O2—Ho1	131.3 (3)	N1—C9—C10	110.3 (5)
Zn1—O2—Ho1	100.93 (15)	N1—C9—H9A	109.6
C16—O4—C18	116.2 (4)	C10—C9—H9A	109.6
C16—O4—Ho1	118.3 (3)	N1—C9—H9B	109.6
C18—O4—Ho1	125.5 (3)	C10—C9—H9B	109.6
O2—C17—C12	125.0 (5)	H9A—C9—H9B	108.1
O2—C17—C16	115.3 (5)	C13—C14—C15	121.0 (6)
C12—C17—C16	119.7 (5)	C13—C14—H14	119.5
N4—O8—Ho1	96.9 (3)	C15—C14—H14	119.5
O10—N4—O9	122.4 (5)	C14—C13—C12	121.8 (6)
O10—N4—O8	122.1 (5)	C14—C13—H13	119.1
O9—N4—O8	115.4 (5)	C12—C13—H13	119.1
N3—O6—Ho1	144.0 (4)	C2—O3—C1	116.6 (4)
C2—C3—C4	118.8 (6)	C2—O3—Ho1	117.3 (3)
C2—C3—H3	120.6	C1—O3—Ho1	125.8 (3)
C4—C3—H3	120.6	O3—C1—H1A	109.5
O13—N5—O11	122.6 (5)	O3—C1—H1B	109.5
O13—N5—O12	120.9 (6)	H1A—C1—H1B	109.5
O11—N5—O12	116.5 (5)	O3—C1—H1C	109.5
N3—O5—Zn1	119.1 (3)	H1A—C1—H1C	109.5
O4—C16—C15	126.0 (5)	H1B—C1—H1C	109.5
O4—C16—C17	113.3 (5)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1B···O11	0.96	2.54	3.167 (8)	123
C5—H5···O11i	0.93	2.45	3.377 (7)	174
C10—H10A···O13ii	0.97	2.54	3.483 (8)	165
C18—H18B···O9	0.96	2.58	3.100 (8)	114

Table 1

Selected bond lengths (Å)

Ho1—O1	2.293 (3)
Ho1—O2	2.298 (3)
Ho1—O3	2.604 (4)
Ho1—O4	2.604 (4)
Ho1—O6	2.323 (4)
Ho1—O8	2.448 (4)
Ho1—O9	2.481 (4)
Ho1—O11	2.430 (4)
Ho1—O12	2.468 (4)
Zn1—O1	2.005 (4)
Zn1—O2	2.022 (3)
Zn1—O5	1.979 (4)
Zn1—N1	2.047 (4)
Zn1—N2	2.021 (5)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C5—H5⋯O11i	0.93	2.45	3.377 (7)	174
C10—H10A⋯O13ii	0.97	2.54	3.483 (8)	165

Symmetry codes: (i) ; (ii) .