Reticular merohedral twinning within the La₉Sb₅O₅ structure family: structure of Pr₉Sb₅O₅, Sm₉Sb₅O₅ and Dy₉Sb₅O₅

The novel antimonide oxides Pr₉Sb₅O₅, Sm₉Sb₅O₅ and Dy₉Sb₅O₅ were synthesized from the respective RESb, the rare-earth metals (RE = Pr, Sm, Dy), and RE₂O₃ (RE = Sm, Dy) or Pr₄O₇, respectively, in sealed tantalum ampoules at 1920 K. Those compounds, which are sensitive against air and moisture, form black cube-like crystals with metallic lustre. They crystallize in the La₉Sb₅O₅ type of structure, which represents a fivefold superstructure of the KCoO₂ structure: O₁₀K₅Co₅ La₉□Sb₅O₅. The investigated crystals of the Sm and Dy compounds were twinned using the reticular merohedral law, with the twin symmetry 4/mm′m′, and the (310) and (120) mirror planes as twinning symmetry elements. The twin index is [j] = 5.

Computing details

For all compounds, data collection: Bruker Suite (Bruker AXS); cell refinement: SAINT32 (Bruker AXS); data reduction: SAINT32 (Bruker AXS); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2005); software used to prepare material for publication: CIFTAB.

Figures

(pr9Sb5o5)

Crystal data

Pr9Sb5O5	Dx = 6.799 Mg m^−3
Mr = 1956.94	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/n	Cell parameters from 7236 reflections
Hall symbol: -P 4a	θ = 2.2–33.9°
a = 10.2203 (3) Å	µ = 29.37 mm^−1
c = 9.1508 (3) Å	T = 296 K
V = 955.84 (5) Å^3	Block, metallic-dark-black
Z = 2	0.06 × 0.06 × 0.04 mm
F(000) = 1652

Data collection

SMART APEX I, Bruker AXS diffractometer	1957 independent reflections
Radiation source: fine-focus sealed tube	1827 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.045
ω–scans	θmax = 34.0°, θmin = 2.2°
Absorption correction: multi-scan SADABS (G. Sheldrick 2007)	h = −16→16
Tmin = 0.272, Tmax = 0.386	k = −15→15
19532 measured reflections	l = −14→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	w = 1/[σ^2(Fo^2) + (0.0189P)^2 + 2.3275P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max = 0.001
S = 1.22	Δρmax = 1.67 e Å^−3
1957 reflections	Δρmin = −1.52 e Å^−3
47 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00071 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Pr1	0.329973 (18)	0.021764 (19)	0.997938 (19)	0.01014 (6)
Pr2	0.2500	0.2500	0.33260 (4)	0.01104 (8)
Pr3	0.146184 (18)	0.953956 (17)	0.65373 (2)	0.01092 (6)
Sb1	0.2500	0.2500	0.69037 (5)	0.01158 (9)
Sb2	0.15307 (2)	0.94674 (2)	0.29828 (3)	0.01058 (7)
O1	0.2500	0.2500	0.0698 (6)	0.0172 (10)
O2	0.1280 (2)	0.9755 (3)	0.9097 (3)	0.0124 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pr1	0.00822 (8)	0.01167 (9)	0.01053 (10)	0.00016 (6)	−0.00045 (6)	0.00049 (6)
Pr2	0.01198 (11)	0.01198 (11)	0.00918 (16)	0.000	0.000	0.000
Pr3	0.01210 (9)	0.01245 (9)	0.00820 (11)	−0.00051 (6)	−0.00003 (6)	−0.00051 (6)
Sb1	0.01100 (12)	0.01100 (12)	0.0127 (2)	0.000	0.000	0.000
Sb2	0.01025 (11)	0.01156 (11)	0.00991 (14)	−0.00039 (6)	0.00013 (7)	0.00019 (7)
O1	0.0197 (16)	0.0197 (16)	0.012 (2)	0.000	0.000	0.000
O2	0.0110 (10)	0.0157 (11)	0.0103 (11)	−0.0016 (9)	0.0004 (9)	0.0001 (9)

Geometric parameters (Å, º)

Pr1—O2^i	2.266 (3)	Pr3—Sb2^xvii	3.2483 (3)
Pr1—O2^ii	2.296 (2)	Pr3—Sb2^xviii	3.2522 (3)
Pr1—O2^iii	2.406 (3)	Pr3—Sb2	3.2542 (4)
Pr1—O1^iv	2.5576 (15)	Pr3—Sb2^xix	3.2902 (3)
Pr1—Sb2^v	3.3780 (3)	Pr3—Pr1^xvi	3.7323 (3)
Pr1—Sb2^vi	3.4590 (3)	Pr3—Pr1^xx	3.8357 (3)
Pr1—Pr1^vii	3.4954 (3)	Pr3—Pr1^xxi	4.0515 (3)
Pr1—Pr1^viii	3.4955 (3)	Sb1—Pr3^x	3.2237 (2)
Pr1—Pr1^ix	3.5041 (4)	Sb1—Pr3^xi	3.2238 (2)
Pr1—Pr3^i	3.7323 (3)	Sb1—Pr3^i	3.2238 (2)
Pr1—Pr3^ii	3.8357 (3)	Sb1—Pr3^iii	3.2238 (2)
Pr1—Pr2^iv	3.9354 (4)	Sb2—Pr3^xix	3.2484 (3)
Pr2—O1	2.405 (6)	Sb2—Pr3^xviii	3.2522 (3)
Pr2—Sb2^x	3.2690 (2)	Sb2—Pr2^xvi	3.2690 (2)
Pr2—Sb2^xi	3.2690 (2)	Sb2—Pr3^xvii	3.2901 (3)
Pr2—Sb2^i	3.2690 (2)	Sb2—Pr1^xxii	3.3779 (3)
Pr2—Sb2^iii	3.2690 (2)	Sb2—Pr1^xxiii	3.4590 (3)
Pr2—Sb1	3.2739 (6)	O1—Pr1^xii	2.5576 (15)
Pr2—Pr1^xii	3.9354 (4)	O1—Pr1^xiii	2.5576 (15)
Pr2—Pr1^xiii	3.9354 (4)	O1—Pr1^xiv	2.5577 (15)
Pr2—Pr1^xiv	3.9354 (4)	O1—Pr1^xv	2.5577 (15)
Pr2—Pr1^xv	3.9354 (4)	O2—Pr1^xvi	2.266 (2)
Pr3—O2	2.360 (3)	O2—Pr1^xx	2.296 (2)
Pr3—Sb1^xvi	3.2238 (2)	O2—Pr1^xxi	2.406 (3)
O2^i—Pr1—O2^ii	125.58 (13)	Sb2^i—Pr2—Pr1^xiv	107.565 (10)
O2^i—Pr1—O2^iii	136.68 (13)	Sb2^iii—Pr2—Pr1^xiv	54.985 (7)
O2^ii—Pr1—O2^iii	83.65 (10)	Sb1—Pr2—Pr1^xiv	141.093 (5)
O2^i—Pr1—O1^iv	89.49 (9)	Pr1^xii—Pr2—Pr1^xiv	52.732 (6)
O2^ii—Pr1—O1^iv	136.10 (13)	Pr1^xiii—Pr2—Pr1^xiv	77.814 (10)
O2^iii—Pr1—O1^iv	86.49 (8)	O1—Pr2—Pr1^xv	38.907 (5)
O2^i—Pr1—Sb2^v	75.83 (7)	Sb2^x—Pr2—Pr1^xv	107.565 (10)
O2^ii—Pr1—Sb2^v	84.01 (7)	Sb2^xi—Pr2—Pr1^xv	115.106 (11)
O2^iii—Pr1—Sb2^v	144.90 (7)	Sb2^i—Pr2—Pr1^xv	54.985 (7)
O1^iv—Pr1—Sb2^v	80.03 (10)	Sb2^iii—Pr2—Pr1^xv	63.174 (7)
O2^i—Pr1—Sb2^vi	85.81 (7)	Sb1—Pr2—Pr1^xv	141.093 (5)
O2^ii—Pr1—Sb2^vi	73.78 (7)	Pr1^xii—Pr2—Pr1^xv	77.814 (10)
O2^iii—Pr1—Sb2^vi	71.63 (6)	Pr1^xiii—Pr2—Pr1^xv	52.732 (6)
O1^iv—Pr1—Sb2^vi	141.52 (12)	Pr1^xiv—Pr2—Pr1^xv	52.732 (6)
Sb2^v—Pr1—Sb2^vi	134.830 (9)	O2—Pr3—Sb1^xvi	80.52 (6)
O2^i—Pr1—Pr1^vii	43.10 (7)	O2—Pr3—Sb2^xvii	86.04 (6)
O2^ii—Pr1—Pr1^vii	150.79 (7)	Sb1^xvi—Pr3—Sb2^xvii	166.092 (14)
O2^iii—Pr1—Pr1^vii	123.31 (6)	O2—Pr3—Sb2^xviii	76.29 (6)
O1^iv—Pr1—Pr1^vii	46.90 (3)	Sb1^xvi—Pr3—Sb2^xviii	90.149 (6)
Sb2^v—Pr1—Pr1^vii	67.423 (6)	Sb2^xvii—Pr3—Sb2^xviii	90.129 (9)
Sb2^vi—Pr1—Pr1^vii	122.334 (6)	O2—Pr3—Sb2	174.79 (7)
O2^i—Pr1—Pr1^viii	125.66 (7)	Sb1^xvi—Pr3—Sb2	96.783 (11)
O2^ii—Pr1—Pr1^viii	108.68 (7)	Sb2^xvii—Pr3—Sb2	96.891 (8)
O2^iii—Pr1—Pr1^viii	40.07 (6)	Sb2^xviii—Pr3—Sb2	99.344 (8)
O1^iv—Pr1—Pr1^viii	46.90 (3)	O2—Pr3—Sb2^xix	88.39 (7)
Sb2^v—Pr1—Pr1^viii	115.886 (5)	Sb1^xvi—Pr3—Sb2^xix	89.476 (6)
Sb2^vi—Pr1—Pr1^viii	108.419 (7)	Sb2^xvii—Pr3—Sb2^xix	86.570 (7)
Pr1^vii—Pr1—Pr1^viii	90.0	Sb2^xviii—Pr3—Sb2^xix	164.521 (13)
O2^i—Pr1—Pr1^ix	151.71 (7)	Sb2—Pr3—Sb2^xix	96.067 (8)
O2^ii—Pr1—Pr1^ix	43.02 (7)	O2—Pr3—Pr1^xvi	35.37 (6)
O2^iii—Pr1—Pr1^ix	40.62 (6)	Sb1^xvi—Pr3—Pr1^xvi	64.679 (9)
O1^iv—Pr1—Pr1^ix	115.47 (2)	Sb2^xvii—Pr3—Pr1^xvi	102.054 (8)
Sb2^v—Pr1—Pr1^ix	119.557 (9)	Sb2^xviii—Pr3—Pr1^xvi	107.542 (8)
Sb2^vi—Pr1—Pr1^ix	66.462 (7)	Sb2—Pr3—Pr1^xvi	146.810 (7)
Pr1^vii—Pr1—Pr1^ix	161.595 (10)	Sb2^xix—Pr3—Pr1^xvi	58.616 (6)
Pr1^viii—Pr1—Pr1^ix	71.606 (10)	O2—Pr3—Pr1^xx	33.98 (6)
O2^i—Pr1—Pr3^i	37.07 (7)	Sb1^xvi—Pr3—Pr1^xx	111.773 (11)
O2^ii—Pr1—Pr3^i	120.86 (7)	Sb2^xvii—Pr3—Pr1^xx	56.225 (7)
O2^iii—Pr1—Pr3^i	102.50 (7)	Sb2^xviii—Pr3—Pr1^xx	64.536 (7)
O1^iv—Pr1—Pr3^i	103.03 (10)	Sb2—Pr3—Pr1^xx	146.387 (7)
Sb2^v—Pr1—Pr3^i	112.033 (8)	Sb2^xix—Pr3—Pr1^xx	101.365 (8)
Sb2^vi—Pr1—Pr3^i	54.292 (6)	Pr1^xvi—Pr3—Pr1^xx	65.495 (6)
Pr1^vii—Pr1—Pr3^i	68.098 (5)	O2—Pr3—Pr1^xxi	32.11 (7)
Pr1^viii—Pr1—Pr3^i	112.675 (4)	Sb1^xvi—Pr3—Pr1^xxi	60.717 (9)
Pr1^ix—Pr1—Pr3^i	118.991 (8)	Sb2^xvii—Pr3—Pr1^xxi	108.612 (8)
O2^i—Pr1—Pr3^ii	120.24 (7)	Sb2^xviii—Pr3—Pr1^xxi	55.235 (6)
O2^ii—Pr1—Pr3^ii	35.07 (7)	Sb2—Pr3—Pr1^xxi	142.768 (7)
O2^iii—Pr1—Pr3^ii	102.00 (6)	Sb2^xix—Pr3—Pr1^xxi	111.744 (8)
O1^iv—Pr1—Pr3^ii	107.46 (12)	Pr1^xvi—Pr3—Pr1^xxi	53.175 (6)
Sb2^v—Pr1—Pr3^ii	53.065 (6)	Pr1^xx—Pr3—Pr1^xxi	52.667 (6)
Sb2^vi—Pr1—Pr3^ii	107.823 (7)	Pr3^x—Sb1—Pr3^xi	89.381 (2)
Pr1^vii—Pr1—Pr3^ii	119.452 (5)	Pr3^x—Sb1—Pr3^i	89.380 (2)
Pr1^viii—Pr1—Pr3^ii	105.073 (6)	Pr3^xi—Sb1—Pr3^i	168.06 (2)
Pr1^ix—Pr1—Pr3^ii	66.831 (6)	Pr3^x—Sb1—Pr3^iii	168.06 (2)
Pr3^i—Pr1—Pr3^ii	141.674 (8)	Pr3^xi—Sb1—Pr3^iii	89.380 (2)
O2^i—Pr1—Pr2^iv	102.24 (7)	Pr3^i—Sb1—Pr3^iii	89.379 (2)
O2^ii—Pr1—Pr2^iv	104.08 (7)	Pr3^x—Sb1—Pr2	84.030 (10)
O2^iii—Pr1—Pr2^iv	99.52 (6)	Pr3^xi—Sb1—Pr2	84.030 (10)
O1^iv—Pr1—Pr2^iv	36.19 (12)	Pr3^i—Sb1—Pr2	84.030 (10)
Sb2^v—Pr1—Pr2^iv	52.428 (5)	Pr3^iii—Sb1—Pr2	84.030 (10)
Sb2^vi—Pr1—Pr2^iv	170.988 (7)	Pr3^xix—Sb2—Pr3^xviii	164.423 (13)
Pr1^vii—Pr1—Pr2^iv	63.634 (3)	Pr3^xix—Sb2—Pr3	83.797 (8)
Pr1^viii—Pr1—Pr2^iv	63.634 (3)	Pr3^xviii—Sb2—Pr3	80.655 (8)
Pr1^ix—Pr1—Pr2^iv	105.835 (8)	Pr3^xix—Sb2—Pr2^xvi	88.700 (6)
Pr3^i—Pr1—Pr2^iv	131.474 (7)	Pr3^xviii—Sb2—Pr2^xvi	88.634 (6)
Pr3^ii—Pr1—Pr2^iv	71.771 (6)	Pr3—Sb2—Pr2^xvi	83.629 (10)
O1—Pr2—Sb2^x	84.488 (9)	Pr3^xix—Sb2—Pr3^xvii	91.358 (7)
O1—Pr2—Sb2^xi	84.488 (9)	Pr3^xviii—Sb2—Pr3^xvii	87.747 (8)
Sb2^x—Pr2—Sb2^xi	89.472 (2)	Pr3—Sb2—Pr3^xvii	83.140 (8)
O1—Pr2—Sb2^i	84.488 (9)	Pr2^xvi—Sb2—Pr3^xvii	166.684 (13)
Sb2^x—Pr2—Sb2^i	89.472 (2)	Pr3^xix—Sb2—Pr1^xxii	70.710 (7)
Sb2^xi—Pr2—Sb2^i	168.976 (18)	Pr3^xviii—Sb2—Pr1^xxii	122.846 (9)
O1—Pr2—Sb2^iii	84.488 (9)	Pr3—Sb2—Pr1^xxii	145.049 (8)
Sb2^x—Pr2—Sb2^iii	168.976 (18)	Pr2^xvi—Sb2—Pr1^xxii	72.586 (9)
Sb2^xi—Pr2—Sb2^iii	89.471 (2)	Pr3^xvii—Sb2—Pr1^xxii	119.899 (9)
Sb2^i—Pr2—Sb2^iii	89.470 (2)	Pr3^xix—Sb2—Pr1^xxiii	119.611 (9)
O1—Pr2—Sb1	180.0	Pr3^xviii—Sb2—Pr1^xxiii	74.199 (7)
Sb2^x—Pr2—Sb1	95.512 (9)	Pr3—Sb2—Pr1^xxiii	141.254 (8)
Sb2^xi—Pr2—Sb1	95.512 (9)	Pr2^xvi—Sb2—Pr1^xxiii	123.984 (11)
Sb2^i—Pr2—Sb1	95.512 (9)	Pr3^xvii—Sb2—Pr1^xxiii	67.092 (7)
Sb2^iii—Pr2—Sb1	95.512 (9)	Pr1^xxii—Sb2—Pr1^xxiii	73.573 (7)
O1—Pr2—Pr1^xii	38.906 (5)	Pr2—O1—Pr1^xii	104.90 (12)
Sb2^x—Pr2—Pr1^xii	63.175 (7)	Pr2—O1—Pr1^xiii	104.90 (12)
Sb2^xi—Pr2—Pr1^xii	54.986 (7)	Pr1^xii—O1—Pr1^xiii	86.21 (6)
Sb2^i—Pr2—Pr1^xii	115.106 (11)	Pr2—O1—Pr1^xiv	104.90 (12)
Sb2^iii—Pr2—Pr1^xii	107.565 (10)	Pr1^xii—O1—Pr1^xiv	86.21 (6)
Sb1—Pr2—Pr1^xii	141.094 (5)	Pr1^xiii—O1—Pr1^xiv	150.2 (2)
O1—Pr2—Pr1^xiii	38.907 (5)	Pr2—O1—Pr1^xv	104.90 (12)
Sb2^x—Pr2—Pr1^xiii	54.986 (7)	Pr1^xii—O1—Pr1^xv	150.2 (2)
Sb2^xi—Pr2—Pr1^xiii	107.566 (10)	Pr1^xiii—O1—Pr1^xv	86.21 (6)
Sb2^i—Pr2—Pr1^xiii	63.174 (7)	Pr1^xiv—O1—Pr1^xv	86.21 (6)
Sb2^iii—Pr2—Pr1^xiii	115.105 (11)	Pr1^xvi—O2—Pr1^xx	127.69 (12)
Sb1—Pr2—Pr1^xiii	141.093 (5)	Pr1^xvi—O2—Pr3	107.56 (10)
Pr1^xii—Pr2—Pr1^xiii	52.732 (6)	Pr1^xx—O2—Pr3	110.96 (10)
O1—Pr2—Pr1^xiv	38.907 (5)	Pr1^xvi—O2—Pr1^xxi	96.83 (9)
Sb2^x—Pr2—Pr1^xiv	115.106 (11)	Pr1^xx—O2—Pr1^xxi	96.35 (10)
Sb2^xi—Pr2—Pr1^xiv	63.174 (7)	Pr3—O2—Pr1^xxi	116.47 (11)

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

(sm9sb5o5)

Crystal data

Sm9Sb5O5	Dx = 7.497 Mg m^−3
Mr = 2041.90	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/n	Cell parameters from 7294 reflections
Hall symbol: -P 4a	θ = 2.3–36.8°
a = 10.0341 (4) Å	µ = 36.01 mm^−1
c = 8.9839 (3) Å	T = 296 K
V = 904.53 (6) Å^3	Block, metallic-dark-black
Z = 2	0.05 × 0.05 × 0.03 mm
F(000) = 1706

Data collection

SMART APEX II, Bruker AXS diffractometer	4116 independent reflections
Radiation source: fine-focus sealed tube	3266 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.050
ω–scans	θmax = 37.0°, θmin = 2.3°
Absorption correction: multi-scan TWINABS (G. Sheldrick 2007)	h = −11→12
Tmin = 0.185, Tmax = 0.339	k = 0→16
31237 measured reflections	l = 0→15

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.029	w = 1/[σ^2(Fo^2) + (0.0114P)^2 + 3.5785P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.057	(Δ/σ)max = 0.004
S = 1.08	Δρmax = 2.05 e Å^−3
4116 reflections	Δρmin = −1.87 e Å^−3
48 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00034 (2)

Special details

Experimental. due to the multiple twinned crystal no numerical absorption is possible

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 as a twin with the twinning matrices T1=1 0 0 / 0 1 0/ 0 0 1, T2=3/5 4/5 0 / −4/5 3/5 0 / 0 0 1, Respective volume fractions are t1=0.5680 (6); t2=0.4320 (6).

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 (Ų)

	x	y	z	Uiso*/Ueq
Sm1	0.331062 (15)	0.022362 (16)	0.99790 (2)	0.00766 (4)
Sm2	0.2500	0.2500	0.33213 (4)	0.00877 (6)
Sm3	0.146291 (17)	0.954159 (16)	0.65454 (2)	0.00861 (4)
Sb1	0.2500	0.2500	0.68789 (6)	0.01000 (8)
Sb2	0.15360 (2)	0.94649 (2)	0.29929 (3)	0.00843 (5)
O1	0.2500	0.2500	0.0664 (6)	0.0150 (10)
O2	0.1290 (2)	0.9749 (3)	0.9108 (3)	0.0098 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sm1	0.00639 (7)	0.00935 (7)	0.00723 (6)	0.00003 (5)	−0.00033 (6)	0.00052 (6)
Sm2	0.01017 (9)	0.01017 (9)	0.00598 (14)	0.000	0.000	0.000
Sm3	0.01015 (8)	0.01027 (7)	0.00542 (7)	−0.00046 (5)	0.00018 (5)	−0.00048 (5)
Sb1	0.00931 (11)	0.00931 (11)	0.01137 (19)	0.000	0.000	0.000
Sb2	0.00862 (9)	0.00972 (9)	0.00694 (10)	−0.00029 (6)	0.00019 (7)	−0.00004 (7)
O1	0.0160 (15)	0.0160 (15)	0.013 (2)	0.000	0.000	0.000
O2	0.0086 (10)	0.0137 (11)	0.0070 (10)	−0.0014 (8)	0.0008 (8)	−0.0012 (9)

Geometric parameters (Å, º)

Sm1—O2^i	2.225 (2)	Sm3—Sb2^xviii	3.1970 (3)
Sm1—O2^ii	2.250 (2)	Sm3—Sb2^xix	3.2272 (3)
Sm1—O2^iii	2.355 (3)	Sm3—Sm1^xvi	3.6635 (3)
Sm1—O1^iv	2.5016 (14)	Sm3—Sm1^xx	3.7602 (3)
Sm1—Sb2^v	3.3289 (3)	Sm3—Sm1^xxi	3.9631 (3)
Sm1—Sb2^vi	3.4040 (3)	Sb1—Sm3^x	3.1598 (2)
Sm1—Sm1^vii	3.4201 (3)	Sb1—Sm3^xi	3.1598 (2)
Sm1—Sm1^viii	3.4289 (3)	Sb1—Sm3^i	3.1598 (2)
Sm1—Sm1^ix	3.4290 (3)	Sb1—Sm3^iii	3.1598 (2)
Sm1—Sm3^i	3.6635 (3)	Sb1—Sm1^xxii	3.6927 (4)
Sm1—Sb1	3.6927 (4)	Sb1—Sm1^viii	3.6927 (4)
Sm1—Sm3^ii	3.7602 (3)	Sb1—Sm1^ix	3.6927 (4)
Sm2—O1	2.387 (6)	Sb2—Sm3^xix	3.1835 (3)
Sm2—Sb1	3.1962 (6)	Sb2—Sm3^xviii	3.1970 (3)
Sm2—Sb2^x	3.2090 (2)	Sb2—Sm2^xvi	3.2090 (2)
Sm2—Sb2^xi	3.2090 (2)	Sb2—Sm3^xvii	3.2272 (3)
Sm2—Sb2^i	3.2090 (2)	Sb2—Sm1^xxiii	3.3289 (3)
Sm2—Sb2^iii	3.2090 (2)	Sb2—Sm1^xxiv	3.4040 (3)
Sm2—Sm1^xii	3.8593 (4)	O1—Sm1^xii	2.5016 (14)
Sm2—Sm1^xiii	3.8593 (4)	O1—Sm1^xiii	2.5016 (14)
Sm2—Sm1^xiv	3.8594 (4)	O1—Sm1^xv	2.5016 (14)
Sm2—Sm1^xv	3.8594 (4)	O1—Sm1^xiv	2.5016 (14)
Sm3—O2	2.318 (3)	O2—Sm1^xvi	2.225 (2)
Sm3—Sb1^xvi	3.1598 (2)	O2—Sm1^xx	2.250 (2)
Sm3—Sb2^xvii	3.1834 (3)	O2—Sm1^xxi	2.355 (3)
Sm3—Sb2	3.1933 (3)
O2^i—Sm1—O2^ii	124.64 (13)	Sm1^xiv—Sm2—Sm1^xv	52.750 (6)
O2^i—Sm1—O2^iii	137.20 (13)	O2—Sm3—Sb1^xvi	81.15 (6)
O2^ii—Sm1—O2^iii	84.11 (9)	O2—Sm3—Sb2^xvii	86.20 (6)
O2^i—Sm1—O1^iv	89.18 (8)	Sb1^xvi—Sm3—Sb2^xvii	166.891 (13)
O2^ii—Sm1—O1^iv	137.32 (13)	O2—Sm3—Sb2	175.19 (7)
O2^iii—Sm1—O1^iv	86.32 (8)	Sb1^xvi—Sm3—Sb2	96.307 (11)
O2^i—Sm1—Sb2^v	75.50 (7)	Sb2^xvii—Sm3—Sb2	96.553 (8)
O2^ii—Sm1—Sb2^v	83.81 (7)	O2—Sm3—Sb2^xviii	76.86 (6)
O2^iii—Sm1—Sb2^v	144.71 (7)	Sb1^xvi—Sm3—Sb2^xviii	90.271 (6)
O1^iv—Sm1—Sb2^v	80.49 (10)	Sb2^xvii—Sm3—Sb2^xviii	90.186 (8)
O2^i—Sm1—Sb2^vi	85.60 (7)	Sb2—Sm3—Sb2^xviii	99.139 (7)
O2^ii—Sm1—Sb2^vi	73.60 (7)	O2—Sm3—Sb2^xix	88.42 (6)
O2^iii—Sm1—Sb2^vi	72.17 (6)	Sb1^xvi—Sm3—Sb2^xix	89.724 (6)
O1^iv—Sm1—Sb2^vi	141.01 (12)	Sb2^xvii—Sm3—Sb2^xix	86.490 (7)
Sb2^v—Sm1—Sb2^vi	134.534 (8)	Sb2—Sm3—Sb2^xix	95.680 (8)
O2^i—Sm1—Sm1^vii	151.54 (7)	Sb2^xviii—Sm3—Sb2^xix	165.091 (11)
O2^ii—Sm1—Sm1^vii	43.24 (7)	O2—Sm3—Sm1^xvi	35.40 (6)
O2^iii—Sm1—Sm1^vii	40.87 (6)	Sb1^xvi—Sm3—Sm1^xvi	65.039 (9)
O1^iv—Sm1—Sm1^vii	116.07 (2)	Sb2^xvii—Sm3—Sm1^xvi	102.429 (7)
Sb2^v—Sm1—Sm1^vii	119.424 (9)	Sb2—Sm3—Sm1^xvi	146.556 (7)
Sb2^vi—Sm1—Sm1^vii	66.628 (7)	Sb2^xviii—Sm3—Sm1^xvi	107.989 (7)
O2^i—Sm1—Sm1^viii	42.99 (7)	Sb2^xix—Sm3—Sm1^xvi	58.800 (6)
O2^ii—Sm1—Sm1^viii	150.34 (7)	O2—Sm3—Sm1^xx	34.01 (6)
O2^iii—Sm1—Sm1^viii	123.50 (6)	Sb1^xvi—Sm3—Sm1^xx	112.214 (11)
O1^iv—Sm1—Sm1^viii	46.74 (3)	Sb2^xvii—Sm3—Sm1^xx	56.563 (6)
Sb2^v—Sm1—Sm1^viii	67.350 (5)	Sb2—Sm3—Sm1^xx	146.341 (7)
Sb2^vi—Sm1—Sm1^viii	121.995 (5)	Sb2^xviii—Sm3—Sm1^xx	64.601 (6)
Sm1^vii—Sm1—Sm1^viii	162.131 (8)	Sb2^xix—Sm3—Sm1^xx	101.727 (7)
O2^i—Sm1—Sm1^ix	125.75 (7)	Sm1^xvi—Sm3—Sm1^xx	65.790 (5)
O2^ii—Sm1—Sm1^ix	109.55 (7)	O2—Sm3—Sm1^xxi	32.29 (7)
O2^iii—Sm1—Sm1^ix	40.11 (6)	Sb1^xvi—Sm3—Sm1^xxi	61.228 (9)
O1^iv—Sm1—Sm1^ix	46.74 (3)	Sb2^xvii—Sm3—Sm1^xxi	108.782 (7)
Sb2^v—Sm1—Sm1^ix	115.851 (5)	Sb2—Sm3—Sm1^xxi	142.963 (7)
Sb2^vi—Sm1—Sm1^ix	108.822 (6)	Sb2^xviii—Sm3—Sm1^xxi	55.535 (6)
Sm1^vii—Sm1—Sm1^ix	72.142 (8)	Sb2^xix—Sm3—Sm1^xxi	112.024 (7)
Sm1^viii—Sm1—Sm1^ix	90.0	Sm1^xvi—Sm3—Sm1^xxi	53.260 (5)
O2^i—Sm1—Sm3^i	37.13 (7)	Sm1^xx—Sm3—Sm1^xxi	52.488 (5)
O2^ii—Sm1—Sm3^i	120.37 (7)	Sm3^x—Sb1—Sm3^xi	89.485 (2)
O2^iii—Sm1—Sm3^i	102.91 (7)	Sm3^x—Sb1—Sm3^i	89.485 (2)
O1^iv—Sm1—Sm3^i	102.31 (11)	Sm3^xi—Sb1—Sm3^i	169.12 (2)
Sb2^v—Sm1—Sm3^i	111.805 (7)	Sm3^x—Sb1—Sm3^iii	169.12 (2)
Sb2^vi—Sm1—Sm3^i	54.188 (6)	Sm3^xi—Sb1—Sm3^iii	89.485 (2)
Sm1^vii—Sm1—Sm3^i	119.107 (9)	Sm3^i—Sb1—Sm3^iii	89.484 (2)
Sm1^viii—Sm1—Sm3^i	67.850 (4)	Sm3^x—Sb1—Sm2	84.559 (10)
Sm1^ix—Sm1—Sm3^i	112.694 (4)	Sm3^xi—Sb1—Sm2	84.559 (10)
O2^i—Sm1—Sb1	70.51 (7)	Sm3^i—Sb1—Sm2	84.559 (10)
O2^ii—Sm1—Sb1	146.49 (7)	Sm3^iii—Sb1—Sm2	84.559 (10)
O2^iii—Sm1—Sb1	69.55 (6)	Sm3^x—Sb1—Sm1^xxii	70.177 (6)
O1^iv—Sm1—Sb1	63.20 (13)	Sm3^xi—Sb1—Sm1^xxii	64.084 (7)
Sb2^v—Sm1—Sb1	129.577 (7)	Sm3^i—Sb1—Sm1^xxii	125.456 (12)
Sb2^vi—Sm1—Sb1	78.710 (8)	Sm3^iii—Sb1—Sm1^xxii	118.826 (11)
Sm1^vii—Sm1—Sb1	107.929 (8)	Sm2—Sb1—Sm1^xxii	138.958 (6)
Sm1^viii—Sm1—Sb1	62.336 (4)	Sm3^x—Sb1—Sm1^viii	64.085 (6)
Sm1^ix—Sm1—Sb1	62.336 (4)	Sm3^xi—Sb1—Sm1^viii	118.827 (11)
Sm3^i—Sm1—Sb1	50.876 (6)	Sm3^i—Sb1—Sm1^viii	70.176 (6)
O2^i—Sm1—Sm3^ii	119.67 (7)	Sm3^iii—Sb1—Sm1^viii	125.455 (12)
O2^ii—Sm1—Sm3^ii	35.19 (7)	Sm2—Sb1—Sm1^viii	138.958 (6)
O2^iii—Sm1—Sm3^ii	102.05 (6)	Sm1^xxii—Sb1—Sm1^viii	55.329 (7)
O1^iv—Sm1—Sm3^ii	108.26 (13)	Sm3^x—Sb1—Sm1	118.826 (11)
Sb2^v—Sm1—Sm3^ii	52.942 (6)	Sm3^xi—Sb1—Sm1	125.456 (12)
Sb2^vi—Sm1—Sm3^ii	107.824 (7)	Sm3^i—Sb1—Sm1	64.084 (7)
Sm1^vii—Sm1—Sm3^ii	66.806 (6)	Sm3^iii—Sb1—Sm1	70.176 (6)
Sm1^viii—Sm1—Sm3^ii	119.326 (4)	Sm2—Sb1—Sm1	138.958 (6)
Sm1^ix—Sm1—Sm3^ii	105.406 (5)	Sm1^xxii—Sb1—Sm1	82.084 (12)
Sm3^i—Sm1—Sm3^ii	141.387 (7)	Sm1^viii—Sb1—Sm1	55.329 (7)
Sb1—Sm1—Sm3^ii	167.700 (7)	Sm3^x—Sb1—Sm1^ix	125.456 (12)
O1—Sm2—Sb1	180.0	Sm3^xi—Sb1—Sm1^ix	70.176 (6)
O1—Sm2—Sb2^x	84.725 (8)	Sm3^i—Sb1—Sm1^ix	118.826 (11)
Sb1—Sm2—Sb2^x	95.275 (8)	Sm3^iii—Sb1—Sm1^ix	64.084 (6)
O1—Sm2—Sb2^xi	84.725 (8)	Sm2—Sb1—Sm1^ix	138.958 (6)
Sb1—Sm2—Sb2^xi	95.275 (8)	Sm1^xxii—Sb1—Sm1^ix	55.329 (7)
Sb2^x—Sm2—Sb2^xi	89.516 (1)	Sm1^viii—Sb1—Sm1^ix	82.084 (12)
O1—Sm2—Sb2^i	84.725 (8)	Sm1—Sb1—Sm1^ix	55.329 (7)
Sb1—Sm2—Sb2^i	95.275 (8)	Sm3^xix—Sb2—Sm3	84.179 (7)
Sb2^x—Sm2—Sb2^i	89.516 (1)	Sm3^xix—Sb2—Sm3^xviii	165.011 (11)
Sb2^xi—Sm2—Sb2^i	169.451 (16)	Sm3—Sb2—Sm3^xviii	80.862 (7)
O1—Sm2—Sb2^iii	84.725 (8)	Sm3^xix—Sb2—Sm2^xvi	88.854 (6)
Sb1—Sm2—Sb2^iii	95.275 (8)	Sm3—Sb2—Sm2^xvi	83.809 (9)
Sb2^x—Sm2—Sb2^iii	169.451 (16)	Sm3^xviii—Sb2—Sm2^xvi	88.617 (6)
Sb2^xi—Sm2—Sb2^iii	89.515 (1)	Sm3^xix—Sb2—Sm3^xvii	91.588 (7)
Sb2^i—Sm2—Sb2^iii	89.515 (1)	Sm3—Sb2—Sm3^xvii	83.473 (7)
O1—Sm2—Sm1^xii	38.921 (5)	Sm3^xviii—Sb2—Sm3^xvii	87.650 (8)
Sb1—Sm2—Sm1^xii	141.079 (5)	Sm2^xvi—Sb2—Sm3^xvii	167.163 (12)
Sb2^x—Sm2—Sm1^xii	55.272 (6)	Sm3^xix—Sb2—Sm1^xxiii	70.495 (6)
Sb2^xi—Sm2—Sm1^xii	107.872 (9)	Sm3—Sb2—Sm1^xxiii	145.053 (9)
Sb2^i—Sm2—Sm1^xii	63.260 (6)	Sm3^xviii—Sb2—Sm1^xxiii	122.528 (8)
Sb2^iii—Sm2—Sm1^xii	115.254 (10)	Sm2^xvi—Sb2—Sm1^xxiii	72.331 (8)
O1—Sm2—Sm1^xiii	38.921 (5)	Sm3^xvii—Sb2—Sm1^xxiii	119.818 (8)
Sb1—Sm2—Sm1^xiii	141.079 (5)	Sm3^xix—Sb2—Sm1^xxiv	119.610 (8)
Sb2^x—Sm2—Sm1^xiii	63.260 (6)	Sm3—Sb2—Sm1^xxiv	141.279 (9)
Sb2^xi—Sm2—Sm1^xiii	55.272 (6)	Sm3^xviii—Sb2—Sm1^xxiv	73.719 (7)
Sb2^i—Sm2—Sm1^xiii	115.255 (10)	Sm2^xvi—Sb2—Sm1^xxiv	123.461 (10)
Sb2^iii—Sm2—Sm1^xiii	107.872 (9)	Sm3^xvii—Sb2—Sm1^xxiv	67.011 (6)
Sm1^xii—Sm2—Sm1^xiii	52.750 (6)	Sm1^xxiii—Sb2—Sm1^xxiv	73.580 (7)
O1—Sm2—Sm1^xiv	38.921 (5)	Sm2—O1—Sm1^xii	104.25 (13)
Sb1—Sm2—Sm1^xiv	141.079 (5)	Sm2—O1—Sm1^xiii	104.25 (13)
Sb2^x—Sm2—Sm1^xiv	107.872 (9)	Sm1^xii—O1—Sm1^xiii	86.53 (6)
Sb2^xi—Sm2—Sm1^xiv	115.254 (10)	Sm2—O1—Sm1^xv	104.25 (13)
Sb2^i—Sm2—Sm1^xiv	55.272 (6)	Sm1^xii—O1—Sm1^xv	151.5 (3)
Sb2^iii—Sm2—Sm1^xiv	63.260 (6)	Sm1^xiii—O1—Sm1^xv	86.53 (6)
Sm1^xii—Sm2—Sm1^xiv	52.750 (6)	Sm2—O1—Sm1^xiv	104.25 (13)
Sm1^xiii—Sm2—Sm1^xiv	77.843 (9)	Sm1^xii—O1—Sm1^xiv	86.53 (6)
O1—Sm2—Sm1^xv	38.921 (5)	Sm1^xiii—O1—Sm1^xiv	151.5 (3)
Sb1—Sm2—Sm1^xv	141.079 (5)	Sm1^xv—O1—Sm1^xiv	86.53 (6)
Sb2^x—Sm2—Sm1^xv	115.255 (10)	Sm1^xvi—O2—Sm1^xx	128.62 (13)
Sb2^xi—Sm2—Sm1^xv	63.260 (6)	Sm1^xvi—O2—Sm3	107.47 (10)
Sb2^i—Sm2—Sm1^xv	107.872 (9)	Sm1^xx—O2—Sm3	110.80 (10)
Sb2^iii—Sm2—Sm1^xv	55.272 (6)	Sm1^xvi—O2—Sm1^xxi	96.90 (9)
Sm1^xii—Sm2—Sm1^xv	77.843 (9)	Sm1^xx—O2—Sm1^xxi	95.89 (9)
Sm1^xiii—Sm2—Sm1^xv	52.750 (6)	Sm3—O2—Sm1^xxi	115.99 (11)

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

(dy9sb5o5)

Crystal data

Dy9Sb5O5	Dx = 8.388 Mg m^−3
Mr = 2151.25	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/n	Cell parameters from 9912 reflections
Hall symbol: -P 4a	θ = 2.3–35.4°
a = 9.8389 (3) Å	µ = 46.70 mm^−1
c = 8.7986 (3) Å	T = 296 K
V = 851.74 (5) Å^3	Block, metallic-dark-black
Z = 2	0.06 × 0.04 × 0.02 mm
F(000) = 1778

Data collection

SMART APEX II, Bruker AXS diffractometer	3725 independent reflections
Radiation source: fine-focus sealed tube	3165 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.051
ω–scans	θmax = 36.4°, θmin = 2.3°
Absorption correction: multi-scan TWINABS (G. Sheldrick 2007)	h = −11→11
Tmin = 0.143, Tmax = 0.391	k = 0→16
39009 measured reflections	l = 0→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.027	w = 1/[σ^2(Fo^2) + (0.0188P)^2 + 4.6683P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.058	(Δ/σ)max = 0.001
S = 1.08	Δρmax = 2.74 e Å^−3
3725 reflections	Δρmin = −2.42 e Å^−3
48 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00063 (3)
0 constraints

Special details

Experimental. due to the multiple twinned crystal no numerical absorption is possible

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 as a twin with the twinning matrices T1=1 0 0 / 0 1 0/ 0 0 1, T2=3/5 4/5 0 / −4/5 3/5 0 / 0 0 1, Respective volume fractions are t1=0.5542 (6); t2=0.4468 (6).

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 (Ų)

	x	y	z	Uiso*/Ueq
Dy1	0.331278 (16)	0.022614 (17)	0.99754 (2)	0.00693 (4)
Dy2	0.2500	0.2500	0.32965 (4)	0.00803 (6)
Dy3	0.145819 (17)	0.954888 (16)	0.65531 (2)	0.00763 (4)
Sb1	0.2500	0.2500	0.68476 (6)	0.00896 (8)
Sb2	0.15430 (2)	0.94561 (2)	0.30091 (3)	0.00731 (5)
O1	0.2500	0.2500	0.0641 (8)	0.0181 (12)
O2	0.1294 (3)	0.9751 (3)	0.9116 (3)	0.0086 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy1	0.00535 (6)	0.00841 (7)	0.00702 (7)	0.00002 (5)	−0.00046 (5)	0.00073 (6)
Dy2	0.00922 (8)	0.00922 (8)	0.00566 (14)	0.000	0.000	0.000
Dy3	0.00906 (7)	0.00925 (7)	0.00458 (8)	−0.00057 (5)	0.00012 (5)	−0.00041 (5)
Sb1	0.00795 (11)	0.00795 (11)	0.0110 (2)	0.000	0.000	0.000
Sb2	0.00743 (9)	0.00871 (9)	0.00579 (11)	−0.00023 (6)	0.00027 (7)	−0.00031 (7)
O1	0.0171 (17)	0.0171 (17)	0.020 (3)	0.000	0.000	0.000
O2	0.0090 (10)	0.0096 (11)	0.0074 (11)	−0.0007 (9)	0.0022 (9)	−0.0032 (9)

Geometric parameters (Å, º)

Dy1—O2^i	2.176 (3)	Dy3—Sb2^xviii	3.1347 (3)
Dy1—O2^ii	2.209 (3)	Dy3—Sb2^xix	3.1627 (3)
Dy1—O2^iii	2.303 (3)	Dy3—Dy1^xvi	3.5834 (3)
Dy1—O1^iv	2.4471 (17)	Dy3—Dy1^xx	3.6816 (3)
Dy1—Sb2^v	3.2757 (3)	Dy3—Dy1^xxi	3.8682 (3)
Dy1—Sb2^vi	3.3453 (3)	Sb1—Dy3^x	3.0901 (2)
Dy1—Dy1^vii	3.3501 (3)	Sb1—Dy3^i	3.0901 (2)
Dy1—Dy1^viii	3.3600 (2)	Sb1—Dy3^xi	3.0901 (2)
Dy1—Dy1^ix	3.3600 (2)	Sb1—Dy3^iii	3.0901 (2)
Dy1—Dy3^i	3.5834 (3)	Sb1—Dy1^viii	3.6357 (5)
Dy1—Sb1	3.6357 (5)	Sb1—Dy1^xxii	3.6357 (5)
Dy1—Dy3^ii	3.6817 (3)	Sb1—Dy1^ix	3.6357 (5)
Dy2—O1	2.336 (7)	Sb2—Dy3^xix	3.1152 (3)
Dy2—Sb1	3.1245 (6)	Sb2—Dy3^xviii	3.1346 (3)
Dy2—Sb2^x	3.1495 (2)	Sb2—Dy2^xvi	3.1495 (2)
Dy2—Sb2^i	3.1495 (2)	Sb2—Dy3^xvii	3.1627 (3)
Dy2—Sb2^xi	3.1496 (2)	Sb2—Dy1^xxiii	3.2758 (3)
Dy2—Sb2^iii	3.1496 (2)	Sb2—Dy1^xxiv	3.3453 (3)
Dy2—Dy1^xii	3.7661 (3)	O1—Dy1^xii	2.4470 (17)
Dy2—Dy1^xiii	3.7661 (3)	O1—Dy1^xiii	2.4471 (17)
Dy2—Dy1^xiv	3.7661 (3)	O1—Dy1^xiv	2.4471 (17)
Dy2—Dy1^xv	3.7661 (3)	O1—Dy1^xv	2.4471 (17)
Dy3—O2	2.270 (3)	O2—Dy1^xvi	2.176 (3)
Dy3—Sb1^xvi	3.0901 (2)	O2—Dy1^xx	2.209 (3)
Dy3—Sb2^xvii	3.1151 (3)	O2—Dy1^xxi	2.303 (3)
Dy3—Sb2	3.1207 (3)
O2^i—Dy1—O2^ii	124.42 (14)	Dy1^xiv—Dy2—Dy1^xv	52.985 (6)
O2^i—Dy1—O2^iii	137.64 (15)	O2—Dy3—Sb1^xvi	81.83 (7)
O2^ii—Dy1—O2^iii	84.12 (10)	O2—Dy3—Sb2^xvii	86.55 (7)
O2^i—Dy1—O1^iv	88.92 (10)	Sb1^xvi—Dy3—Sb2^xvii	167.824 (14)
O2^ii—Dy1—O1^iv	137.89 (16)	O2—Dy3—Sb2	175.78 (7)
O2^iii—Dy1—O1^iv	86.09 (9)	Sb1^xvi—Dy3—Sb2	95.877 (12)
O2^i—Dy1—Sb2^v	75.41 (7)	Sb2^xvii—Dy3—Sb2	95.941 (8)
O2^ii—Dy1—Sb2^v	83.64 (7)	O2—Dy3—Sb2^xviii	77.49 (7)
O2^iii—Dy1—Sb2^v	144.35 (7)	Sb1^xvi—Dy3—Sb2^xviii	90.500 (6)
O1^iv—Dy1—Sb2^v	80.95 (13)	Sb2^xvii—Dy3—Sb2^xviii	90.533 (9)
O2^i—Dy1—Sb2^vi	85.56 (7)	Sb2—Dy3—Sb2^xviii	99.039 (8)
O2^ii—Dy1—Sb2^vi	73.51 (7)	O2—Dy3—Sb2^xix	88.58 (7)
O2^iii—Dy1—Sb2^vi	72.64 (7)	Sb1^xvi—Dy3—Sb2^xix	89.977 (6)
O1^iv—Dy1—Sb2^vi	140.68 (16)	Sb2^xvii—Dy3—Sb2^xix	86.087 (7)
Sb2^v—Dy1—Sb2^vi	134.269 (9)	Sb2—Dy3—Sb2^xix	94.980 (8)
O2^i—Dy1—Dy1^vii	151.72 (7)	Sb2^xviii—Dy3—Sb2^xix	165.849 (12)
O2^ii—Dy1—Dy1^vii	43.14 (7)	O2—Dy3—Dy1^xvi	35.41 (7)
O2^iii—Dy1—Dy1^vii	40.98 (7)	Sb1^xvi—Dy3—Dy1^xvi	65.537 (10)
O1^iv—Dy1—Dy1^vii	116.24 (2)	Sb2^xvii—Dy3—Dy1^xvi	102.691 (8)
Sb2^v—Dy1—Dy1^vii	119.049 (9)	Sb2—Dy3—Dy1^xvi	146.250 (8)
Sb2^vi—Dy1—Dy1^vii	66.905 (7)	Sb2^xviii—Dy3—Dy1^xvi	108.564 (8)
O2^i—Dy1—Dy1^viii	42.84 (7)	Sb2^xix—Dy3—Dy1^xvi	59.064 (6)
O2^ii—Dy1—Dy1^viii	150.33 (7)	O2—Dy3—Dy1^xx	34.17 (7)
O2^iii—Dy1—Dy1^viii	123.53 (6)	Sb1^xvi—Dy3—Dy1^xx	112.964 (11)
O1^iv—Dy1—Dy1^viii	46.64 (4)	Sb2^xvii—Dy3—Dy1^xx	56.895 (6)
Sb2^v—Dy1—Dy1^viii	67.575 (6)	Sb2—Dy3—Dy1^xx	146.237 (8)
Sb2^vi—Dy1—Dy1^viii	121.773 (6)	Sb2^xviii—Dy3—Dy1^xx	64.990 (6)
Dy1^vii—Dy1—Dy1^viii	162.287 (9)	Sb2^xix—Dy3—Dy1^xx	101.920 (7)
O2^i—Dy1—Dy1^ix	125.77 (7)	Dy1^xvi—Dy3—Dy1^xx	66.015 (5)
O2^ii—Dy1—Dy1^ix	109.74 (7)	O2—Dy3—Dy1^xxi	32.49 (7)
O2^iii—Dy1—Dy1^ix	39.98 (7)	Sb1^xvi—Dy3—Dy1^xxi	61.810 (9)
O1^iv—Dy1—Dy1^ix	46.64 (4)	Sb2^xvii—Dy3—Dy1^xxi	109.247 (7)
Sb2^v—Dy1—Dy1^ix	115.879 (5)	Sb2—Dy3—Dy1^xxi	143.333 (7)
Sb2^vi—Dy1—Dy1^ix	109.051 (6)	Sb2^xviii—Dy3—Dy1^xxi	55.895 (6)
Dy1^vii—Dy1—Dy1^ix	72.303 (9)	Sb2^xix—Dy3—Dy1^xxi	112.471 (7)
Dy1^viii—Dy1—Dy1^ix	90.0	Dy1^xvi—Dy3—Dy1^xxi	53.438 (6)
O2^i—Dy1—Dy3^i	37.19 (7)	Dy1^xx—Dy3—Dy1^xxi	52.614 (5)
O2^ii—Dy1—Dy3^i	120.29 (8)	Dy3^x—Sb1—Dy3^i	89.598 (2)
O2^iii—Dy1—Dy3^i	103.31 (7)	Dy3^x—Sb1—Dy3^xi	89.597 (2)
O1^iv—Dy1—Dy3^i	101.82 (13)	Dy3^i—Sb1—Dy3^xi	170.38 (2)
Sb2^v—Dy1—Dy3^i	111.781 (7)	Dy3^x—Sb1—Dy3^iii	170.38 (2)
Sb2^vi—Dy1—Dy3^i	54.186 (6)	Dy3^i—Sb1—Dy3^iii	89.597 (2)
Dy1^vii—Dy1—Dy3^i	119.392 (8)	Dy3^xi—Sb1—Dy3^iii	89.596 (2)
Dy1^viii—Dy1—Dy3^i	67.624 (5)	Dy3^x—Sb1—Dy2	85.189 (11)
Dy1^ix—Dy1—Dy3^i	112.702 (4)	Dy3^i—Sb1—Dy2	85.189 (11)
O2^i—Dy1—Sb1	70.63 (7)	Dy3^xi—Sb1—Dy2	85.189 (11)
O2^ii—Dy1—Sb1	146.25 (7)	Dy3^iii—Sb1—Dy2	85.189 (11)
O2^iii—Dy1—Sb1	69.68 (7)	Dy3^x—Sb1—Dy1^viii	63.783 (7)
O1^iv—Dy1—Sb1	63.05 (16)	Dy3^i—Sb1—Dy1^viii	69.677 (7)
Sb2^v—Dy1—Sb1	129.956 (7)	Dy3^xi—Sb1—Dy1^viii	118.312 (12)
Sb2^vi—Dy1—Sb1	78.461 (9)	Dy3^iii—Sb1—Dy1^viii	124.662 (13)
Dy1^vii—Dy1—Sb1	108.028 (8)	Dy2—Sb1—Dy1^viii	139.196 (7)
Dy1^viii—Dy1—Sb1	62.478 (4)	Dy3^x—Sb1—Dy1^xxii	69.677 (7)
Dy1^ix—Dy1—Sb1	62.479 (4)	Dy3^i—Sb1—Dy1^xxii	124.663 (13)
Dy3^i—Dy1—Sb1	50.680 (6)	Dy3^xi—Sb1—Dy1^xxii	63.783 (7)
O2^i—Dy1—Dy3^ii	119.54 (7)	Dy3^iii—Sb1—Dy1^xxii	118.311 (12)
O2^ii—Dy1—Dy3^ii	35.26 (7)	Dy2—Sb1—Dy1^xxii	139.196 (6)
O2^iii—Dy1—Dy3^ii	101.80 (7)	Dy1^viii—Sb1—Dy1^xxii	55.043 (8)
O1^iv—Dy1—Dy3^ii	108.71 (16)	Dy3^x—Sb1—Dy1	118.312 (12)
Sb2^v—Dy1—Dy3^ii	52.806 (6)	Dy3^i—Sb1—Dy1	63.783 (7)
Sb2^vi—Dy1—Dy3^ii	107.814 (7)	Dy3^xi—Sb1—Dy1	124.661 (13)
Dy1^vii—Dy1—Dy3^ii	66.554 (6)	Dy3^iii—Sb1—Dy1	69.677 (7)
Dy1^viii—Dy1—Dy3^ii	119.418 (4)	Dy2—Sb1—Dy1	139.196 (7)
Dy1^ix—Dy1—Dy3^ii	105.397 (5)	Dy1^viii—Sb1—Dy1	55.043 (8)
Dy3^i—Dy1—Dy3^ii	141.412 (7)	Dy1^xxii—Sb1—Dy1	81.609 (13)
Sb1—Dy1—Dy3^ii	167.854 (7)	Dy3^x—Sb1—Dy1^ix	124.662 (13)
O1—Dy2—Sb1	180.0	Dy3^i—Sb1—Dy1^ix	118.312 (12)
O1—Dy2—Sb2^x	85.395 (8)	Dy3^xi—Sb1—Dy1^ix	69.676 (7)
Sb1—Dy2—Sb2^x	94.605 (8)	Dy3^iii—Sb1—Dy1^ix	63.782 (7)
O1—Dy2—Sb2^i	85.395 (8)	Dy2—Sb1—Dy1^ix	139.195 (6)
Sb1—Dy2—Sb2^i	94.605 (8)	Dy1^viii—Sb1—Dy1^ix	81.609 (13)
Sb2^x—Dy2—Sb2^i	89.631 (1)	Dy1^xxii—Sb1—Dy1^ix	55.043 (8)
O1—Dy2—Sb2^xi	85.395 (8)	Dy1—Sb1—Dy1^ix	55.043 (8)
Sb1—Dy2—Sb2^xi	94.605 (8)	Dy3^xix—Sb2—Dy3	84.853 (8)
Sb2^x—Dy2—Sb2^xi	89.631 (1)	Dy3^xix—Sb2—Dy3^xviii	165.769 (12)
Sb2^i—Dy2—Sb2^xi	170.789 (16)	Dy3—Sb2—Dy3^xviii	80.961 (8)
O1—Dy2—Sb2^iii	85.395 (8)	Dy3^xix—Sb2—Dy2^xvi	88.902 (7)
Sb1—Dy2—Sb2^iii	94.605 (8)	Dy3—Sb2—Dy2^xvi	84.259 (9)
Sb2^x—Dy2—Sb2^iii	170.789 (16)	Dy3^xviii—Sb2—Dy2^xvi	88.555 (6)
Sb2^i—Dy2—Sb2^iii	89.630 (1)	Dy3^xix—Sb2—Dy3^xvii	92.183 (7)
Sb2^xi—Dy2—Sb2^iii	89.630 (1)	Dy3—Sb2—Dy3^xvii	84.060 (8)
O1—Dy2—Dy1^xii	39.113 (5)	Dy3^xviii—Sb2—Dy3^xvii	87.497 (8)
Sb1—Dy2—Dy1^xii	140.887 (5)	Dy2^xvi—Sb2—Dy3^xvii	168.122 (12)
Sb2^x—Dy2—Dy1^xii	55.689 (6)	Dy3^xix—Sb2—Dy1^xxiii	70.299 (7)
Sb2^i—Dy2—Dy1^xii	63.782 (6)	Dy3—Sb2—Dy1^xxiii	145.250 (9)
Sb2^xi—Dy2—Dy1^xii	108.494 (9)	Dy3^xviii—Sb2—Dy1^xxiii	121.912 (9)
Sb2^iii—Dy2—Dy1^xii	116.046 (10)	Dy2^xvi—Sb2—Dy1^xxiii	71.735 (8)
O1—Dy2—Dy1^xiii	39.113 (5)	Dy3^xvii—Sb2—Dy1^xxiii	119.702 (9)
Sb1—Dy2—Dy1^xiii	140.887 (5)	Dy3^xix—Sb2—Dy1^xxiv	119.599 (9)
Sb2^x—Dy2—Dy1^xiii	63.782 (6)	Dy3—Sb2—Dy1^xxiv	141.286 (9)
Sb2^i—Dy2—Dy1^xiii	116.047 (10)	Dy3^xviii—Sb2—Dy1^xxiv	73.222 (7)
Sb2^xi—Dy2—Dy1^xiii	55.688 (6)	Dy2^xvi—Sb2—Dy1^xxiv	122.570 (10)
Sb2^iii—Dy2—Dy1^xiii	108.493 (9)	Dy3^xvii—Sb2—Dy1^xxiv	66.749 (6)
Dy1^xii—Dy2—Dy1^xiii	52.986 (6)	Dy1^xxiii—Sb2—Dy1^xxiv	73.424 (7)
O1—Dy2—Dy1^xiv	39.114 (4)	Dy2—O1—Dy1^xii	103.86 (16)
Sb1—Dy2—Dy1^xiv	140.887 (5)	Dy2—O1—Dy1^xiii	103.86 (16)
Sb2^x—Dy2—Dy1^xiv	108.494 (9)	Dy1^xii—O1—Dy1^xiii	86.71 (8)
Sb2^i—Dy2—Dy1^xiv	55.688 (6)	Dy2—O1—Dy1^xiv	103.86 (16)
Sb2^xi—Dy2—Dy1^xiv	116.046 (10)	Dy1^xii—O1—Dy1^xiv	86.71 (8)
Sb2^iii—Dy2—Dy1^xiv	63.781 (6)	Dy1^xiii—O1—Dy1^xiv	152.3 (3)
Dy1^xii—Dy2—Dy1^xiv	52.985 (6)	Dy2—O1—Dy1^xv	103.86 (16)
Dy1^xiii—Dy2—Dy1^xiv	78.227 (9)	Dy1^xii—O1—Dy1^xv	152.3 (3)
O1—Dy2—Dy1^xv	39.114 (5)	Dy1^xiii—O1—Dy1^xv	86.71 (8)
Sb1—Dy2—Dy1^xv	140.886 (5)	Dy1^xiv—O1—Dy1^xv	86.71 (8)
Sb2^x—Dy2—Dy1^xv	116.047 (10)	Dy1^xvi—O2—Dy1^xx	129.05 (14)
Sb2^i—Dy2—Dy1^xv	108.493 (9)	Dy1^xvi—O2—Dy3	107.40 (11)
Sb2^xi—Dy2—Dy1^xv	63.781 (6)	Dy1^xx—O2—Dy3	110.57 (11)
Sb2^iii—Dy2—Dy1^xv	55.688 (6)	Dy1^xvi—O2—Dy1^xxi	97.17 (10)
Dy1^xii—Dy2—Dy1^xv	78.227 (9)	Dy1^xx—O2—Dy1^xxi	95.88 (10)
Dy1^xiii—Dy2—Dy1^xv	52.985 (6)	Dy3—O2—Dy1^xxi	115.54 (12)

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