Penta­europium dicadmium penta­anti­monide oxide, Eu5Cd2Sb5O

Saparov, B.; Bobev, S.

doi:10.1107/S1600536811000274

inorganic compounds

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ISSN: 2056-9890

Volume 67| Part 2| February 2011| Page i11

doi:10.1107/S1600536811000274

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Pentaeuropium dicadmium pentaantimonide oxide, Eu₅Cd₂Sb₅O

Bayrammurad Saparov ^a and Svilen Bobev ^a ^*

^aDepartment of Chemistry and Biochemistry, University of Delaware, Newark, DE 19716, USA
^*Correspondence e-mail: sbobev@mail.chem.udel.edu

(Received 16 December 2010; accepted 4 January 2011; online 15 January 2011)

The title compound, Eu₅Cd₂Sb₅O adopts the Ba₅Cd₂Sb₅F-type structure (Pearson symbol oC52), which contains nine crystallographically unique sites in the asymmetric unit, all on special positions. One Eu, two Sb, and the Cd atom have site symmetry m..; two other Eu, the third Sb and the O atom have site symmetry m2m; the remaining Eu atom has 2/m.. symmetry. Eu atoms fill pentagonal channels built from corner-sharing CdSb₄ tetrahedra. The isolated O atom, i.e., an oxide ion O²⁻, is located in a distorted tetrahedral cavity formed by four Eu cations.

Related literature

For related ternary pnictides, see: Xia & Bobev (2007a ,b , 2008a ,b ); Saparov et al. (2008a ,b , 2010 , 2011 ); Park & Kim (2004 ). For related antimonide fluorides and oxides [A₅Cd₂Sb₅F (A = Sr, Ba, Eu); Ba₅Cd₂Sb₅O_x], see: Saparov & Bobev (2010 ). For another related bismuthide oxide (Ba₂Cd_2.13Bi₃O), see: Xia & Bobev (2010 ). For ionic and covalent radii, see: Shannon (1976 ); Pauling (1960 ).

Experimental

Crystal data

Eu₅Cd₂Sb₅O
M_r = 1609.37
Orthorhombic, C m c m
a = 4.7088 (5) Å
b = 21.965 (2) Å
c = 14.5982 (15) Å
V = 1509.9 (3) Å³
Z = 4
Mo Kα radiation
μ = 31.92 mm⁻¹
T = 120 K
0.06 × 0.05 × 0.04 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2002 ) T_min = 0.161, T_max = 0.279
10204 measured reflections
1092 independent reflections
1031 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.044
S = 1.14
1092 reflections
46 parameters
Δρ_max = 1.18 e Å⁻³
Δρ_min = −1.16 e Å⁻³

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811000274/mg2112sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811000274/mg2112Isup2.hkl

checkCIF report

Comment top

The title compound, Eu₅Cd₂Sb₅O, is isostructural to Ba₅Cd₂Sb₅F, recently reported (Saparov & Bobev, 2010). The structure contains one-dimensional [Cd₂Sb₅]^9- polyanions and isolated O^2- ions surrounded tetrahedrally by Eu cations (Fig. 1). The polyanions are constructed from two chains of corner-sharing CdSb₄ tetrahedra connected through Sb3 atoms and Sb2–Sb2 bonds [2.8078 (10) Å]. Similar strong homoatomic Sb–Sb interactions are found in related polyanionic Zn–Sb and Cd–Sb substructures [Ba₃Cd₂Sb₄ (Saparov et al., 2008a), Sr₁₁Cd₆Sb₁₂ (Park & Kim, 2004; Xia & Bobev, 2008a), Eu₁₁Cd₆Sb₁₂ and Eu₁₁Cd₆Sb₁₂ (Saparov et al., 2008b), Ba₂Cd₂Sb₃ (Saparov et al., 2010)]. The Cd–Sb interactions [2.8413 (5) Å to 2.9624 (8) Å] are comparable to the sum of the covalent radii (Pauling, 1960) and to distances found in other structures based on CdSb₄ tetrahedra [Ba₃Cd₂Sb₄ (Saparov et al., 2008a), Ba₂₁Cd₄Sb₁₈ (Xia and Bobev, 2008b), Eu₁₁Cd₆Sb₁₂ (Saparov et al., 2008b), A₂CdSb₂ (Xia & Bobev, 2007a; Saparov et al., 2011), Sr₉Cd_4.49 (1)Sb₉ (Xia & Bobev, 2007b)].

Band structure calculations highlight the importance of ionic Ba–F interations near the Fermi level to optimize bonding in Ba₅Cd₂Sb₅F, but exact electron balance is achieved in the corresponding oxide Ba₅Cd₂Sb₅O_x only when x = 0.5 (Saparov & Bobev, 2010). Whereas the fluoride is free of disorder, the oxide exhibits underoccupancy of the oxygen site, causing positional disorder of the next-nearest Ba atoms, as revealed by elongated atomic displacement parameters on the Ba2 site (modeled as a split position) in Ba₅Cd₂Sb₅O_0.59 (3). The Ba2 atoms move away from their equilibrium positions towards the empty space that results when the oxygen site is vacant. Thus, it is surprising that the present structure of Eu₅Cd₂Sb₅O contains a fully occupied oxygen site, because the formula would show a one-electron deficiency, viz. (Eu²⁺)₅(Cd²⁺)₂(Sb^3-)₃(Sb^2-)₂(O^2-). A possible resolution is to propose the occurrence of Eu in both +2 and +3 oxidation states. Because phase-pure samples were unavailable, magnetic measurements could not be performed to verify this proposal. Nevertheless, we note that the Eu1–O distance [2.528 (4) Å] is only 0.4% longer than the Eu1–F distance in Eu₅Cd₂Sb₅F (Saparov & Bobev, 2010); this increase does not scale with the difference between the ionic radii of O^2- and F^-, the former being nearly 5% bigger than the latter (Shannon, 1976). A similar conclusion can be drawn by comparing the Eu2–O [2.634 (3) Å] and Eu2–F [2.635 (3) Å] distances.

Related literature top

For related ternary pnictides, see: Xia & Bobev (2007a,b, 2008a,b); Saparov et al. (2008a,b, 2010, 2011); Park & Kim (2004). For related antimonide fluorides and oxides [A₅Cd₂Sb₅F (A = Sr, Ba, Eu); Ba₅Cd₂Sb₅O_x], see: Saparov & Bobev (2010). For another related bismuthide oxide (Ba₂Cd_2.13Bi₃O), see: Xia & Bobev (2010). For ionic and covalent radii, see: Shannon (1976); Pauling (1960).

Experimental top

The reagents were handled in an argon-filled glove box or under vacuum. All metals were with a stated purity higher than 99.9% (metal basis). They were purchased from Alfa, kept in the glove box, and were used as received.

A mixture of elemental Eu, Cd, Sb, and Pb (flux) in a molar ratio Eu:Cd:Sb:Pb = 2:1:2:10 was loaded in an alumina crucible. To prevent oxidation, the elements were weighed inside the glove box, but the mixture was accidently left in contact with ambient air for ca. 20–30 minutes, prior to sealing it under vacuum inside a silica tube. After that, the reaction mixture was put in a box-furnace and heated to 1273 K at a rate of 200 K h^-1, homogenized at this temperature for 24 h, and then slowly cooled to 823 K at a rate of 5 K h^-1. After an equilibration step at 823 K for 96 h, the crystals were separated from the Pb flux.

This reaction was aimed at obtaining large single-crystals of Eu₁₁Cd₆Sb₁₂ (Saparov et al., 2008b), which was indeed the major product. However, alongside the needle crystals of Eu₁₁Cd₆Sb₁₂, a small block-shaped crystal was also found. After the X-ray data were collected and the structure was solved, it turned out to be that of Eu₅Cd₂Sb₅O. Other reactions using the same starting materials produced only the intermetallic phase, suggesting that the likely source of oxygen in this particular experiment was an unexpected partial oxidation. Attempts to increase the yield by using Eu₂O₃ as a deliberate source of oxygen were not successful and yielded multiple phases. Reactions aimed at obtaining the isostructural Eu₅Cd₂Sb₅F (Saparov & Bobev, 2010) were successful – they were performed using CdF₂ (Alfa), Eu, Cd, and Sb.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. Projection of Eu₅Cd₂Sb₅O approximately along [100]. Displacement ellipsoids are drawn at the 95% probability level. Color key: Eu orange, Cd green, Sb turquoise, O red. Symmetry transformation used to generate the equivalent Sb atom: (vi) x,y,-z+1/2.

Pentaeuropium dicadmium pentaantimonide oxide top

Crystal data top

Eu₅Cd₂Sb₅O	F(000) = 2702
M_r = 1609.37	D_x = 7.078 Mg m⁻³
Orthorhombic, Cmcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2c 2	Cell parameters from 1092 reflections
a = 4.7088 (5) Å	θ = 1.9–28.3°
b = 21.965 (2) Å	µ = 31.92 mm⁻¹
c = 14.5982 (15) Å	T = 120 K
V = 1509.9 (3) Å³	Block, black
Z = 4	0.06 × 0.05 × 0.04 mm

Data collection top

Bruker SMART APEX diffractometer	1092 independent reflections
Radiation source: fine-focus sealed tube	1031 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
ω scans	θ_max = 28.3°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −6→6
T_min = 0.161, T_max = 0.279	k = −28→28
10204 measured reflections	l = −19→19

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)] = 0.020	w = 1/[σ²(F_o²) + (0.0174P)² + 9.1021P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.044	(Δ/σ)_max = 0.001
S = 1.14	Δρ_max = 1.18 e Å⁻³
1092 reflections	Δρ_min = −1.16 e Å⁻³
46 parameters	Extinction correction: SHELXTL (Bruker, 2002), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.000112 (14)

Crystal data top

Eu₅Cd₂Sb₅O	V = 1509.9 (3) Å³
M_r = 1609.37	Z = 4
Orthorhombic, Cmcm	Mo Kα radiation
a = 4.7088 (5) Å	µ = 31.92 mm⁻¹
b = 21.965 (2) Å	T = 120 K
c = 14.5982 (15) Å	0.06 × 0.05 × 0.04 mm

Data collection top

Bruker SMART APEX diffractometer	1092 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2002)	1031 reflections with I > 2σ(I)
T_min = 0.161, T_max = 0.279	R_int = 0.043
10204 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	46 parameters
wR(F²) = 0.044	0 restraints
S = 1.14	Δρ_max = 1.18 e Å⁻³
1092 reflections	Δρ_min = −1.16 e Å⁻³

Special details top

Experimental. Selected in the glove box, crystals were put in a Paratone N oil and cut to the desired dimensions. Chosen crystal was mounted on a tip of a glass fiber and quickly onto the goniometer. The crystal was kept under a cold nitrogen stream to protect from ambient conditions.

Data collection is performed with four batch runs at ϕ = 0.00 ° (600 frames), at ϕ = 90.00 ° (600 frames), at ϕ = 180.00 ° (600 frames), and at ϕ = 270.00 (600 frames). Frame width = 0.30 ° in ω. Data are merged and treated with multi-scan absorption corrections.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Eu1	0.0000	0.270509 (17)	0.61940 (3)	0.01436 (11)
Eu2	0.0000	0.10016 (3)	0.2500	0.02034 (14)
Eu3	0.0000	0.90247 (2)	0.2500	0.01461 (12)
Eu4	0.0000	0.0000	0.0000	0.01393 (12)
Sb1	0.0000	0.14937 (2)	0.02068 (3)	0.01333 (12)
Sb2	0.0000	0.49492 (2)	0.15383 (3)	0.01439 (12)
Sb3	0.0000	0.29312 (3)	0.2500	0.01319 (15)
Cd	0.0000	0.36803 (3)	0.08509 (4)	0.01540 (13)
O	0.0000	0.6539 (3)	0.2500	0.0058 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu1	0.01347 (18)	0.01609 (19)	0.01352 (19)	0.000	0.000	0.00131 (14)
Eu2	0.0283 (3)	0.0179 (3)	0.0148 (3)	0.000	0.000	0.000
Eu3	0.0119 (2)	0.0152 (3)	0.0167 (3)	0.000	0.000	0.000
Eu4	0.0145 (3)	0.0151 (3)	0.0122 (2)	0.000	0.000	−0.00009 (19)
Sb1	0.0121 (2)	0.0142 (2)	0.0136 (2)	0.000	0.000	−0.00025 (18)
Sb2	0.0137 (2)	0.0171 (2)	0.0123 (2)	0.000	0.000	0.00042 (18)
Sb3	0.0123 (3)	0.0146 (3)	0.0127 (3)	0.000	0.000	0.000
Cd	0.0137 (3)	0.0186 (3)	0.0140 (3)	0.000	0.000	−0.0012 (2)
O	0.006 (3)	0.008 (3)	0.003 (3)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Eu1—Oⁱ	2.528 (4)	Sb1—Eu1^xvi	3.2738 (5)
Eu1—Sb1ⁱⁱ	3.2738 (5)	Sb1—Eu1^xvii	3.2738 (5)
Eu1—Sb1ⁱⁱⁱ	3.2738 (5)	Sb1—Eu1^vi	3.3559 (7)
Eu1—Sb3^iv	3.3363 (4)	Sb2—Sb2^vi	2.8078 (10)
Eu1—Sb3^v	3.3363 (4)	Sb2—Cd	2.9624 (8)
Eu1—Sb1^vi	3.3559 (7)	Sb2—Eu4^ix	3.2556 (4)
Eu2—O^vii	2.634 (3)	Sb2—Eu4^x	3.2556 (4)
Eu2—O^viii	2.634 (3)	Sb2—Eu3^viii	3.4115 (5)
Eu3—Sb3^ix	3.3634 (7)	Sb2—Eu3^vii	3.4115 (5)
Eu3—Sb3^x	3.3634 (7)	Sb3—Cd	2.9160 (7)
Eu3—Sb2^xi	3.4115 (5)	Sb3—Cd^vi	2.9160 (7)
Eu3—Sb2^x	3.4115 (5)	Sb3—Eu1^xvii	3.3363 (4)
Eu3—Sb2^ix	3.4115 (5)	Sb3—Eu1^iv	3.3363 (4)
Eu3—Sb2^xii	3.4115 (5)	Sb3—Eu1^v	3.3363 (4)
Eu3—Cd^ix	3.4512 (5)	Sb3—Eu1^xvi	3.3363 (4)
Eu3—Cd^xi	3.4512 (5)	Sb3—Eu3^vii	3.3634 (7)
Eu3—Cd^xii	3.4512 (5)	Sb3—Eu3^viii	3.3634 (7)
Eu3—Cd^x	3.4512 (5)	Cd—Sb1^xiii	2.8413 (5)
Eu4—Sb2^xiii	3.2556 (4)	Cd—Sb1^xiv	2.8413 (5)
Eu4—Sb2^vii	3.2556 (4)	Cd—Eu3^vii	3.4512 (5)
Eu4—Sb2^xiv	3.2556 (4)	Cd—Eu3^viii	3.4512 (5)
Eu4—Sb2^viii	3.2556 (4)	O—Eu1ⁱ	2.528 (4)
Eu4—Sb1	3.2947 (6)	O—Eu1^xviii	2.528 (4)
Eu4—Sb1^xv	3.2948 (6)	O—Eu2^ix	2.634 (3)
Sb1—Cd^xiii	2.8413 (5)	O—Eu2^x	2.634 (3)
Sb1—Cd^xiv	2.8413 (5)

Oⁱ—Eu1—Sb1ⁱⁱ	88.79 (8)	Sb2^xiii—Eu4—Sb2^viii	87.362 (15)
Oⁱ—Eu1—Sb1ⁱⁱⁱ	88.79 (8)	Sb2^vii—Eu4—Sb2^viii	92.638 (15)
Sb1ⁱⁱ—Eu1—Sb1ⁱⁱⁱ	91.972 (17)	Sb2^xiv—Eu4—Sb2^viii	180.00 (2)
Oⁱ—Eu1—Sb3^iv	81.04 (8)	Sb2^xiii—Eu4—Sb1	91.665 (10)
Sb1ⁱⁱ—Eu1—Sb3^iv	88.237 (12)	Sb2^vii—Eu4—Sb1	88.335 (10)
Sb1ⁱⁱⁱ—Eu1—Sb3^iv	169.821 (18)	Sb2^xiv—Eu4—Sb1	91.665 (10)
Oⁱ—Eu1—Sb3^v	81.04 (8)	Sb2^viii—Eu4—Sb1	88.335 (10)
Sb1ⁱⁱ—Eu1—Sb3^v	169.821 (18)	Sb2^xiii—Eu4—Sb1^xv	88.335 (10)
Sb1ⁱⁱⁱ—Eu1—Sb3^v	88.237 (12)	Sb2^vii—Eu4—Sb1^xv	91.665 (10)
Sb3^iv—Eu1—Sb3^v	89.772 (15)	Sb2^xiv—Eu4—Sb1^xv	88.335 (10)
Oⁱ—Eu1—Sb1^vi	168.60 (11)	Sb2^viii—Eu4—Sb1^xv	91.665 (10)
Sb1ⁱⁱ—Eu1—Sb1^vi	99.089 (14)	Sb1—Eu4—Sb1^xv	180.0
Sb1ⁱⁱⁱ—Eu1—Sb1^vi	99.089 (14)	Sb2^xiii—Eu4—Cd^xiv	100.934 (11)
Sb3^iv—Eu1—Sb1^vi	90.921 (15)	Sb2^vii—Eu4—Cd^xiv	79.066 (11)
Sb3^v—Eu1—Sb1^vi	90.921 (15)	Sb2^xiv—Eu4—Cd^xiv	47.500 (11)
Oⁱ—Eu1—Cd^vi	103.28 (11)	Sb2^viii—Eu4—Cd^xiv	132.500 (11)
Sb1ⁱⁱ—Eu1—Cd^vi	47.849 (9)	Sb1—Eu4—Cd^xiv	45.208 (9)
Sb1ⁱⁱⁱ—Eu1—Cd^vi	47.849 (9)	Sb1^xv—Eu4—Cd^xiv	134.793 (9)
Sb3^iv—Eu1—Cd^vi	135.111 (8)	Sb2^xiii—Eu4—Cd^viii	79.066 (11)
Sb3^v—Eu1—Cd^vi	135.111 (7)	Sb2^vii—Eu4—Cd^viii	100.934 (11)
Sb1^vi—Eu1—Cd^vi	88.118 (17)	Sb2^xiv—Eu4—Cd^viii	132.500 (11)
Oⁱ—Eu1—Eu1^xix	41.06 (11)	Sb2^viii—Eu4—Cd^viii	47.500 (11)
Sb1ⁱⁱ—Eu1—Eu1^xix	116.120 (11)	Sb1—Eu4—Cd^viii	134.792 (9)
Sb1ⁱⁱⁱ—Eu1—Eu1^xix	116.120 (11)	Sb1^xv—Eu4—Cd^viii	45.207 (9)
Sb3^iv—Eu1—Eu1^xix	55.150 (8)	Cd^xiv—Eu4—Cd^viii	180.000 (19)
Sb3^v—Eu1—Eu1^xix	55.150 (8)	Sb2^xiii—Eu4—Cd^xiii	47.500 (11)
Sb1^vi—Eu1—Eu1^xix	127.542 (11)	Sb2^vii—Eu4—Cd^xiii	132.500 (11)
Cd^vi—Eu1—Eu1^xix	144.340 (11)	Sb2^xiv—Eu4—Cd^xiii	100.934 (11)
Oⁱ—Eu1—Cdⁱⁱⁱ	127.77 (7)	Sb2^viii—Eu4—Cd^xiii	79.066 (11)
Sb1ⁱⁱ—Eu1—Cdⁱⁱⁱ	143.242 (16)	Sb1—Eu4—Cd^xiii	45.208 (9)
Sb1ⁱⁱⁱ—Eu1—Cdⁱⁱⁱ	85.892 (12)	Sb1^xv—Eu4—Cd^xiii	134.793 (9)
Sb3^iv—Eu1—Cdⁱⁱⁱ	99.991 (16)	Cd^xiv—Eu4—Cd^xiii	73.486 (12)
Sb3^v—Eu1—Cdⁱⁱⁱ	46.924 (12)	Cd^viii—Eu4—Cd^xiii	106.514 (12)
Sb1^vi—Eu1—Cdⁱⁱⁱ	45.530 (10)	Sb2^xiii—Eu4—Cd^vii	132.500 (11)
Cd^vi—Eu1—Cdⁱⁱⁱ	110.630 (13)	Sb2^vii—Eu4—Cd^vii	47.500 (11)
Eu1^xix—Eu1—Cdⁱⁱⁱ	97.418 (10)	Sb2^xiv—Eu4—Cd^vii	79.066 (11)
Oⁱ—Eu1—Cdⁱⁱ	127.77 (7)	Sb2^viii—Eu4—Cd^vii	100.934 (11)
Sb1ⁱⁱ—Eu1—Cdⁱⁱ	85.892 (13)	Sb1—Eu4—Cd^vii	134.792 (9)
Sb1ⁱⁱⁱ—Eu1—Cdⁱⁱ	143.242 (17)	Sb1^xv—Eu4—Cd^vii	45.207 (9)
Sb3^iv—Eu1—Cdⁱⁱ	46.924 (12)	Cd^xiv—Eu4—Cd^vii	106.514 (12)
Sb3^v—Eu1—Cdⁱⁱ	99.991 (17)	Cd^viii—Eu4—Cd^vii	73.486 (12)
Sb1^vi—Eu1—Cdⁱⁱ	45.530 (10)	Cd^xiii—Eu4—Cd^vii	180.000 (19)
Cd^vi—Eu1—Cdⁱⁱ	110.630 (13)	Sb2^xiii—Eu4—Eu3^xxiv	127.751 (9)
Eu1^xix—Eu1—Cdⁱⁱ	97.418 (10)	Sb2^vii—Eu4—Eu3^xxiv	52.249 (9)
Cdⁱⁱⁱ—Eu1—Cdⁱⁱ	74.719 (14)	Sb2^xiv—Eu4—Eu3^xxiv	127.751 (9)
Oⁱ—Eu1—Eu2^iv	37.31 (4)	Sb2^viii—Eu4—Eu3^xxiv	52.249 (9)
Sb1ⁱⁱ—Eu1—Eu2^iv	55.018 (11)	Sb1—Eu4—Eu3^xxiv	115.157 (11)
Sb1ⁱⁱⁱ—Eu1—Eu2^iv	104.009 (15)	Sb1^xv—Eu4—Eu3^xxiv	64.843 (11)
Sb3^iv—Eu1—Eu2^iv	67.923 (14)	Cd^xiv—Eu4—Eu3^xxiv	130.170 (8)
Sb3^v—Eu1—Eu2^iv	115.104 (14)	Cd^viii—Eu4—Eu3^xxiv	49.830 (8)
Sb1^vi—Eu1—Eu2^iv	145.294 (6)	Cd^xiii—Eu4—Eu3^xxiv	130.170 (8)
Cd^vi—Eu1—Eu2^iv	88.522 (13)	Cd^vii—Eu4—Eu3^xxiv	49.830 (8)
Eu1^xix—Eu1—Eu2^iv	62.674 (7)	Sb2^xiii—Eu4—Eu3^xxv	52.249 (9)
Cdⁱⁱⁱ—Eu1—Eu2^iv	160.009 (14)	Sb2^vii—Eu4—Eu3^xxv	127.751 (9)
Cdⁱⁱ—Eu1—Eu2^iv	104.580 (11)	Sb2^xiv—Eu4—Eu3^xxv	52.249 (9)
Oⁱ—Eu1—Eu2^v	37.31 (4)	Sb2^viii—Eu4—Eu3^xxv	127.751 (9)
Sb1ⁱⁱ—Eu1—Eu2^v	104.009 (15)	Sb1—Eu4—Eu3^xxv	64.843 (11)
Sb1ⁱⁱⁱ—Eu1—Eu2^v	55.018 (11)	Sb1^xv—Eu4—Eu3^xxv	115.157 (11)
Sb3^iv—Eu1—Eu2^v	115.104 (13)	Cd^xiv—Eu4—Eu3^xxv	49.830 (8)
Sb3^v—Eu1—Eu2^v	67.923 (14)	Cd^viii—Eu4—Eu3^xxv	130.170 (8)
Sb1^vi—Eu1—Eu2^v	145.294 (6)	Cd^xiii—Eu4—Eu3^xxv	49.830 (8)
Cd^vi—Eu1—Eu2^v	88.522 (12)	Cd^vii—Eu4—Eu3^xxv	130.170 (8)
Eu1^xix—Eu1—Eu2^v	62.674 (6)	Eu3^xxiv—Eu4—Eu3^xxv	180.000 (12)
Cdⁱⁱⁱ—Eu1—Eu2^v	104.580 (11)	Cd^xiii—Sb1—Cd^xiv	111.92 (3)
Cdⁱⁱ—Eu1—Eu2^v	160.009 (14)	Cd^xiii—Sb1—Eu1^xvi	155.15 (2)
Eu2^iv—Eu1—Eu2^v	69.070 (12)	Cd^xiv—Sb1—Eu1^xvi	73.476 (13)
O^vii—Eu2—O^viii	126.7 (2)	Cd^xiii—Sb1—Eu1^xvii	73.476 (13)
O^vii—Eu2—Sb1	82.09 (3)	Cd^xiv—Sb1—Eu1^xvii	155.15 (2)
O^viii—Eu2—Sb1	82.09 (3)	Eu1^xvi—Sb1—Eu1^xvii	91.971 (17)
O^vii—Eu2—Sb1^vi	82.09 (3)	Cd^xiii—Sb1—Eu4	79.416 (15)
O^viii—Eu2—Sb1^vi	82.09 (3)	Cd^xiv—Sb1—Eu4	79.416 (15)
Sb1—Eu2—Sb1^vi	144.21 (2)	Eu1^xvi—Sb1—Eu4	125.146 (12)
O^vii—Eu2—Sb2^viii	151.15 (7)	Eu1^xvii—Sb1—Eu4	125.146 (11)
O^viii—Eu2—Sb2^viii	72.66 (11)	Cd^xiii—Sb1—Eu1^vi	77.026 (16)
Sb1—Eu2—Sb2^viii	79.950 (11)	Cd^xiv—Sb1—Eu1^vi	77.026 (16)
Sb1^vi—Eu2—Sb2^viii	124.796 (11)	Eu1^xvi—Sb1—Eu1^vi	80.908 (14)
O^vii—Eu2—Sb2^xx	151.15 (7)	Eu1^xvii—Sb1—Eu1^vi	80.908 (14)
O^viii—Eu2—Sb2^xx	72.66 (11)	Eu4—Sb1—Eu1^vi	137.202 (18)
Sb1—Eu2—Sb2^xx	124.795 (11)	Cd^xiii—Sb1—Eu2	118.413 (15)
Sb1^vi—Eu2—Sb2^xx	79.951 (11)	Cd^xiv—Sb1—Eu2	118.413 (15)
Sb2^viii—Eu2—Sb2^xx	46.098 (17)	Eu1^xvi—Sb1—Eu2	75.300 (13)
O^vii—Eu2—Sb2^xxi	72.66 (11)	Eu1^xvii—Sb1—Eu2	75.300 (13)
O^viii—Eu2—Sb2^xxi	151.15 (7)	Eu4—Sb1—Eu2	77.364 (14)
Sb1—Eu2—Sb2^xxi	124.795 (11)	Eu1^vi—Sb1—Eu2	145.435 (19)
Sb1^vi—Eu2—Sb2^xxi	79.951 (11)	Sb2^vi—Sb2—Cd	109.800 (15)
Sb2^viii—Eu2—Sb2^xxi	99.72 (2)	Sb2^vi—Sb2—Eu4^ix	133.614 (8)
Sb2^xx—Eu2—Sb2^xxi	82.082 (16)	Cd—Sb2—Eu4^ix	78.379 (13)
O^vii—Eu2—Sb2^vii	72.66 (11)	Sb2^vi—Sb2—Eu4^x	133.614 (8)
O^viii—Eu2—Sb2^vii	151.15 (7)	Cd—Sb2—Eu4^x	78.379 (13)
Sb1—Eu2—Sb2^vii	79.950 (11)	Eu4^ix—Sb2—Eu4^x	92.637 (15)
Sb1^vi—Eu2—Sb2^vii	124.796 (11)	Sb2^vi—Sb2—Eu3^viii	65.699 (9)
Sb2^viii—Eu2—Sb2^vii	82.082 (17)	Cd—Sb2—Eu3^viii	65.122 (14)
Sb2^xx—Eu2—Sb2^vii	99.72 (2)	Eu4^ix—Sb2—Eu3^viii	78.764 (8)
Sb2^xxi—Eu2—Sb2^vii	46.098 (17)	Eu4^x—Sb2—Eu3^viii	143.452 (18)
O^vii—Eu2—Eu1^iv	35.58 (8)	Sb2^vi—Sb2—Eu3^vii	65.699 (9)
O^viii—Eu2—Eu1^iv	101.55 (11)	Cd—Sb2—Eu3^vii	65.122 (14)
Sb1—Eu2—Eu1^iv	103.103 (14)	Eu4^ix—Sb2—Eu3^vii	143.452 (18)
Sb1^vi—Eu2—Eu1^iv	49.682 (9)	Eu4^x—Sb2—Eu3^vii	78.764 (8)
Sb2^viii—Eu2—Eu1^iv	173.179 (9)	Eu3^viii—Sb2—Eu3^vii	87.282 (17)
Sb2^xx—Eu2—Eu1^iv	129.306 (11)	Sb2^vi—Sb2—Eu2^x	66.952 (9)
Sb2^xxi—Eu2—Eu1^iv	83.628 (11)	Cd—Sb2—Eu2^x	137.661 (10)
Sb2^vii—Eu2—Eu1^iv	104.387 (9)	Eu4^ix—Sb2—Eu2^x	136.289 (17)
O^vii—Eu2—Eu1^xvi	35.58 (8)	Eu4^x—Sb2—Eu2^x	76.887 (8)
O^viii—Eu2—Eu1^xvi	101.55 (11)	Eu3^viii—Sb2—Eu2^x	132.515 (16)
Sb1—Eu2—Eu1^xvi	49.683 (9)	Eu3^vii—Sb2—Eu2^x	76.673 (13)
Sb1^vi—Eu2—Eu1^xvi	103.102 (15)	Sb2^vi—Sb2—Eu2^ix	66.952 (8)
Sb2^viii—Eu2—Eu1^xvi	129.306 (11)	Cd—Sb2—Eu2^ix	137.661 (10)
Sb2^xx—Eu2—Eu1^xvi	173.179 (9)	Eu4^ix—Sb2—Eu2^ix	76.887 (7)
Sb2^xxi—Eu2—Eu1^xvi	104.387 (10)	Eu4^x—Sb2—Eu2^ix	136.289 (17)
Sb2^vii—Eu2—Eu1^xvi	83.628 (11)	Eu3^viii—Sb2—Eu2^ix	76.673 (14)
Eu1^iv—Eu2—Eu1^xvi	54.653 (13)	Eu3^vii—Sb2—Eu2^ix	132.515 (16)
O^vii—Eu2—Eu1^v	101.55 (11)	Eu2^x—Sb2—Eu2^ix	82.083 (17)
O^viii—Eu2—Eu1^v	35.58 (8)	Cd—Sb3—Cd^vi	111.30 (3)
Sb1—Eu2—Eu1^v	103.103 (15)	Cd—Sb3—Eu1^xvii	76.384 (11)
Sb1^vi—Eu2—Eu1^v	49.682 (9)	Cd^vi—Sb3—Eu1^xvii	135.084 (7)
Sb2^viii—Eu2—Eu1^v	104.387 (9)	Cd—Sb3—Eu1^iv	135.084 (7)
Sb2^xx—Eu2—Eu1^v	83.628 (11)	Cd^vi—Sb3—Eu1^iv	76.384 (11)
Sb2^xxi—Eu2—Eu1^v	129.306 (11)	Eu1^xvii—Sb3—Eu1^iv	130.47 (3)
Sb2^vii—Eu2—Eu1^v	173.179 (9)	Cd—Sb3—Eu1^v	135.084 (7)
Eu1^iv—Eu2—Eu1^v	69.069 (12)	Cd^vi—Sb3—Eu1^v	76.384 (12)
Eu1^xvi—Eu2—Eu1^v	93.682 (16)	Eu1^xvii—Sb3—Eu1^v	69.701 (15)
O^vii—Eu2—Eu1^xvii	101.55 (11)	Eu1^iv—Sb3—Eu1^v	89.770 (15)
O^viii—Eu2—Eu1^xvii	35.58 (8)	Cd—Sb3—Eu1^xvi	76.384 (11)
Sb1—Eu2—Eu1^xvii	49.683 (9)	Cd^vi—Sb3—Eu1^xvi	135.084 (7)
Sb1^vi—Eu2—Eu1^xvii	103.102 (14)	Eu1^xvii—Sb3—Eu1^xvi	89.770 (15)
Sb2^viii—Eu2—Eu1^xvii	83.628 (11)	Eu1^iv—Sb3—Eu1^xvi	69.701 (15)
Sb2^xx—Eu2—Eu1^xvii	104.387 (9)	Eu1^v—Sb3—Eu1^xvi	130.47 (3)
Sb2^xxi—Eu2—Eu1^xvii	173.179 (9)	Cd—Sb3—Eu3^vii	66.237 (13)
Sb2^vii—Eu2—Eu1^xvii	129.306 (11)	Cd^vi—Sb3—Eu3^vii	66.236 (13)
Eu1^iv—Eu2—Eu1^xvii	93.682 (16)	Eu1^xvii—Sb3—Eu3^vii	142.479 (13)
Eu1^xvi—Eu2—Eu1^xvii	69.069 (12)	Eu1^iv—Sb3—Eu3^vii	78.764 (10)
Eu1^v—Eu2—Eu1^xvii	54.653 (13)	Eu1^v—Sb3—Eu3^vii	142.479 (13)
Sb3^ix—Eu3—Sb3^x	88.85 (2)	Eu1^xvi—Sb3—Eu3^vii	78.764 (10)
Sb3^ix—Eu3—Sb2^xi	155.259 (10)	Cd—Sb3—Eu3^viii	66.237 (13)
Sb3^x—Eu3—Sb2^xi	86.675 (12)	Cd^vi—Sb3—Eu3^viii	66.236 (14)
Sb3^ix—Eu3—Sb2^x	155.259 (10)	Eu1^xvii—Sb3—Eu3^viii	78.764 (10)
Sb3^x—Eu3—Sb2^x	86.675 (12)	Eu1^iv—Sb3—Eu3^viii	142.479 (13)
Sb2^xi—Eu3—Sb2^x	48.601 (18)	Eu1^v—Sb3—Eu3^viii	78.764 (10)
Sb3^ix—Eu3—Sb2^ix	86.675 (12)	Eu1^xvi—Sb3—Eu3^viii	142.479 (13)
Sb3^x—Eu3—Sb2^ix	155.259 (10)	Eu3^vii—Sb3—Eu3^viii	88.86 (2)
Sb2^xi—Eu3—Sb2^ix	106.94 (2)	Sb1^xiii—Cd—Sb1^xiv	111.92 (3)
Sb2^x—Eu3—Sb2^ix	87.283 (17)	Sb1^xiii—Cd—Sb3	111.885 (17)
Sb3^ix—Eu3—Sb2^xii	86.675 (12)	Sb1^xiv—Cd—Sb3	111.885 (17)
Sb3^x—Eu3—Sb2^xii	155.259 (10)	Sb1^xiii—Cd—Sb2	108.095 (17)
Sb2^xi—Eu3—Sb2^xii	87.283 (17)	Sb1^xiv—Cd—Sb2	108.095 (17)
Sb2^x—Eu3—Sb2^xii	106.94 (2)	Sb3—Cd—Sb2	104.55 (2)
Sb2^ix—Eu3—Sb2^xii	48.601 (18)	Sb1^xiii—Cd—Eu3^vii	166.858 (18)
Sb3^ix—Eu3—Cd^ix	50.649 (11)	Sb1^xiv—Cd—Eu3^vii	80.981 (12)
Sb3^x—Eu3—Cd^ix	108.724 (16)	Sb3—Cd—Eu3^vii	63.115 (14)
Sb2^xi—Eu3—Cd^ix	152.666 (19)	Sb2—Cd—Eu3^vii	63.735 (14)
Sb2^x—Eu3—Cd^ix	108.315 (13)	Sb1^xiii—Cd—Eu3^viii	80.981 (12)
Sb2^ix—Eu3—Cd^ix	51.142 (13)	Sb1^xiv—Cd—Eu3^viii	166.858 (18)
Sb2^xii—Eu3—Cd^ix	86.946 (12)	Sb3—Cd—Eu3^viii	63.115 (14)
Sb3^ix—Eu3—Cd^xi	108.724 (17)	Sb2—Cd—Eu3^viii	63.735 (14)
Sb3^x—Eu3—Cd^xi	50.649 (11)	Eu3^vii—Cd—Eu3^viii	86.030 (15)
Sb2^xi—Eu3—Cd^xi	51.142 (13)	Sb1^xiii—Cd—Eu1^vi	58.674 (13)
Sb2^x—Eu3—Cd^xi	86.946 (12)	Sb1^xiv—Cd—Eu1^vi	58.674 (13)
Sb2^ix—Eu3—Cd^xi	152.666 (19)	Sb3—Cd—Eu1^vi	109.99 (2)
Sb2^xii—Eu3—Cd^xi	108.315 (14)	Sb2—Cd—Eu1^vi	145.46 (2)
Cd^ix—Eu3—Cd^xi	154.68 (3)	Eu3^vii—Cd—Eu1^vi	133.990 (11)
Sb3^ix—Eu3—Cd^xii	50.649 (11)	Eu3^viii—Cd—Eu1^vi	133.990 (11)
Sb3^x—Eu3—Cd^xii	108.724 (17)	Sb1^xiii—Cd—Eu1^xvii	57.443 (13)
Sb2^xi—Eu3—Cd^xii	108.315 (13)	Sb1^xiv—Cd—Eu1^xvii	117.87 (2)
Sb2^x—Eu3—Cd^xii	152.666 (19)	Sb3—Cd—Eu1^xvii	56.693 (13)
Sb2^ix—Eu3—Cd^xii	86.946 (12)	Sb2—Cd—Eu1^xvii	133.962 (13)
Sb2^xii—Eu3—Cd^xii	51.142 (13)	Eu3^vii—Cd—Eu1^xvii	119.724 (18)
Cd^ix—Eu3—Cd^xii	88.461 (16)	Eu3^viii—Cd—Eu1^xvii	70.603 (12)
Cd^xi—Eu3—Cd^xii	86.030 (15)	Eu1^vi—Cd—Eu1^xvii	69.370 (13)
Sb3^ix—Eu3—Cd^x	108.724 (16)	Sb1^xiii—Cd—Eu1^xvi	117.87 (2)
Sb3^x—Eu3—Cd^x	50.649 (11)	Sb1^xiv—Cd—Eu1^xvi	57.443 (13)
Sb2^xi—Eu3—Cd^x	86.946 (12)	Sb3—Cd—Eu1^xvi	56.693 (13)
Sb2^x—Eu3—Cd^x	51.142 (13)	Sb2—Cd—Eu1^xvi	133.962 (13)
Sb2^ix—Eu3—Cd^x	108.315 (13)	Eu3^vii—Cd—Eu1^xvi	70.603 (12)
Sb2^xii—Eu3—Cd^x	152.666 (19)	Eu3^viii—Cd—Eu1^xvi	119.724 (18)
Cd^ix—Eu3—Cd^x	86.030 (15)	Eu1^vi—Cd—Eu1^xvi	69.370 (13)
Cd^xi—Eu3—Cd^x	88.461 (16)	Eu1^xvii—Cd—Eu1^xvi	74.720 (15)
Cd^xii—Eu3—Cd^x	154.68 (3)	Sb1^xiii—Cd—Eu4^x	115.04 (2)
Sb3^ix—Eu3—Eu4^xxii	111.194 (5)	Sb1^xiv—Cd—Eu4^x	55.378 (13)
Sb3^x—Eu3—Eu4^xxii	111.194 (5)	Sb3—Cd—Eu4^x	132.546 (13)
Sb2^xi—Eu3—Eu4^xxii	48.986 (9)	Sb2—Cd—Eu4^x	54.120 (12)
Sb2^x—Eu3—Eu4^xxii	93.069 (14)	Eu3^vii—Cd—Eu4^x	69.550 (10)
Sb2^ix—Eu3—Eu4^xxii	93.069 (14)	Eu3^viii—Cd—Eu4^x	117.827 (18)
Sb2^xii—Eu3—Eu4^xxii	48.986 (8)	Eu1^vi—Cd—Eu4^x	99.961 (13)
Cd^ix—Eu3—Eu4^xxii	135.440 (10)	Eu1^xvii—Cd—Eu4^x	168.941 (17)
Cd^xi—Eu3—Eu4^xxii	60.620 (10)	Eu1^xvi—Cd—Eu4^x	104.797 (9)
Cd^xii—Eu3—Eu4^xxii	60.620 (10)	Sb1^xiii—Cd—Eu4^ix	55.378 (13)
Cd^x—Eu3—Eu4^xxii	135.440 (10)	Sb1^xiv—Cd—Eu4^ix	115.04 (2)
Sb3^ix—Eu3—Eu4^xxiii	111.194 (5)	Sb3—Cd—Eu4^ix	132.546 (13)
Sb3^x—Eu3—Eu4^xxiii	111.194 (5)	Sb2—Cd—Eu4^ix	54.120 (12)
Sb2^xi—Eu3—Eu4^xxiii	93.069 (14)	Eu3^vii—Cd—Eu4^ix	117.827 (18)
Sb2^x—Eu3—Eu4^xxiii	48.986 (8)	Eu3^viii—Cd—Eu4^ix	69.550 (10)
Sb2^ix—Eu3—Eu4^xxiii	48.986 (8)	Eu1^vi—Cd—Eu4^ix	99.961 (13)
Sb2^xii—Eu3—Eu4^xxiii	93.069 (14)	Eu1^xvii—Cd—Eu4^ix	104.797 (9)
Cd^ix—Eu3—Eu4^xxiii	60.620 (10)	Eu1^xvi—Cd—Eu4^ix	168.941 (17)
Cd^xi—Eu3—Eu4^xxiii	135.440 (10)	Eu4^x—Cd—Eu4^ix	73.485 (12)
Cd^xii—Eu3—Eu4^xxiii	135.440 (10)	Eu1ⁱ—O—Eu1^xviii	97.9 (2)
Cd^x—Eu3—Eu4^xxiii	60.620 (10)	Eu1ⁱ—O—Eu2^ix	107.12 (4)
Eu4^xxii—Eu3—Eu4^xxiii	119.173 (14)	Eu1^xviii—O—Eu2^ix	107.12 (4)
Sb2^xiii—Eu4—Sb2^vii	180.00 (2)	Eu1ⁱ—O—Eu2^x	107.12 (4)
Sb2^xiii—Eu4—Sb2^xiv	92.638 (15)	Eu1^xviii—O—Eu2^x	107.12 (4)
Sb2^vii—Eu4—Sb2^xiv	87.362 (15)	Eu2^ix—O—Eu2^x	126.7 (2)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1/2, −y+1/2, z+1/2; (iii) −x−1/2, −y+1/2, z+1/2; (iv) −x+1/2, −y+1/2, −z+1; (v) −x−1/2, −y+1/2, −z+1; (vi) x, y, −z+1/2; (vii) x+1/2, y−1/2, z; (viii) x−1/2, y−1/2, z; (ix) x−1/2, y+1/2, z; (x) x+1/2, y+1/2, z; (xi) x+1/2, y+1/2, −z+1/2; (xii) x−1/2, y+1/2, −z+1/2; (xiii) −x−1/2, −y+1/2, −z; (xiv) −x+1/2, −y+1/2, −z; (xv) −x, −y, −z; (xvi) −x+1/2, −y+1/2, z−1/2; (xvii) −x−1/2, −y+1/2, z−1/2; (xviii) −x, −y+1, z−1/2; (xix) x, y, −z+3/2; (xx) x−1/2, y−1/2, −z+1/2; (xxi) x+1/2, y−1/2, −z+1/2; (xxii) −x, −y+1, z+1/2; (xxiii) x, y+1, z; (xxiv) x, y−1, z; (xxv) −x, −y+1, −z.

Experimental details

Crystal data
Chemical formula	Eu₅Cd₂Sb₅O
M_r	1609.37
Crystal system, space group	Orthorhombic, Cmcm
Temperature (K)	120
a, b, c (Å)	4.7088 (5), 21.965 (2), 14.5982 (15)
V (Å³)	1509.9 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	31.92
Crystal size (mm)	0.06 × 0.05 × 0.04

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2002)
T_min, T_max	0.161, 0.279
No. of measured, independent and observed [I > 2σ(I)] reflections	10204, 1092, 1031
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.044, 1.14
No. of reflections	1092
No. of parameters	46
Δρ_max, Δρ_min (e Å⁻³)	1.18, −1.16

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), XP in SHELXTL (Sheldrick, 2008).

Acknowledgements

The authors acknowledge financial support from the University of Delaware and the Petroleum Research Fund (ACS–PRF).

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