Gd₄Mo₇O₂₇, a novel phase in the Gd₂O₃–MoO₃ system

The title compound, heptamolybdenum(VI) tetragadolin­ate(III), a novel phase in the the Gd₂O₃–MoO₃ system, has been prepared by pyrolysis of [Gd₂(H₂O)₁₂Mo₈O₂₇]·8H₂O at 1023 K for 2 h in air. The compound can be described as a layer structure consisting of {MoO₄}-, {Mo₃O₁₁}- and {Gd}-containing layers, which are stacked along the a direction. The {Mo₃O₁₁} group is composed of trigonal bipyramidal MoO₅ connected to two MoO₄ tetrahedra, with corner-sharing. The coordination polyhedra of square-antiprismatic GdO₈ and monocapped trigonal prismatic GdO₇ are dimerized to give {Gd₂O_n} (n = 12 and 13) groups which possess short Gd...Gd separations [3.6345 (4)–3.6404 (4) Å].

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](Mo-O) = 0.005 Å
• R factor = 0.039
• wR factor = 0.108
• Data-to-parameter ratio = 19.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

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Computing details

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: TEXSAN (Molecular Structure Corporation, 2000; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN (Molecular Structure Corporation, 2000; software used to prepare material for publication: TEXSAN (Molecular Structure Corporation, 2000.

(I)

Crystal data

Gd4Mo7O27	F(000) = 6128.0
Mr = 1732.56	Dx = 4.908 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.7107 Å
Hall symbol: -C 2yc	Cell parameters from 15047 reflections
a = 23.034 (2) Å	θ = 2.8–30.0°
b = 14.677 (2) Å	µ = 14.88 mm^−1
c = 14.348 (1) Å	T = 296 K
β = 104.816 (3)°	Block, colorless
V = 4689.4 (8) Å^3	0.15 × 0.11 × 0.11 mm
Z = 8

Data collection

Rigaku RAXIS-RAPID Imaging Plate diffractometer	5944 reflections with F^2 > 2σ(F^2)
Detector resolution: 10.00 pixels mm^-1	Rint = 0.048
ω scans	θmax = 30.0°
Absorption correction: numerical (Higashi, 1999)	h = 0→32
Tmin = 0.101, Tmax = 0.197	k = 0→20
24606 measured reflections	l = −20→19
6779 independent reflections

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + (0.05(Max(Fo^2,0) + 2Fc^2)/3)^2]
R[F^2 > 2σ(F^2)] = 0.039	(Δ/σ)max = 0.002
wR(F^2) = 0.108	Δρmax = 4.62 e Å^−3
S = 1.38	Δρmin = −3.57 e Å^−3
6778 reflections	Extinction correction: Zachariasen (1967) type 2 Gaussian isotropic
344 parameters	Extinction coefficient: 0.00217 (4)

Special details

Refinement. Refinement using reflections with F² > -10.0 σ(F²). The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Gd(1)	0.11465 (1)	0.94156 (2)	0.14469 (2)	0.00925 (7)
Gd(2)	0.62225 (1)	0.80732 (2)	−0.06296 (2)	0.00899 (7)
Gd(3)	0.61114 (1)	0.94038 (2)	0.14541 (2)	0.00921 (7)
Gd(4)	0.38042 (1)	0.69462 (2)	0.06521 (2)	0.00984 (7)
Mo(1)	0.25560 (2)	0.80117 (3)	0.16578 (4)	0.0099 (1)
Mo(2)	0.22995 (2)	0.88003 (3)	0.38708 (4)	0.0106 (1)
Mo(3)	0.23504 (2)	0.59750 (3)	0.29825 (4)	0.0107 (1)
Mo(4)	0.56999 (2)	1.05445 (3)	−0.10012 (4)	0.0097 (1)
Mo(5)	−0.06886 (2)	0.94988 (3)	0.10152 (4)	0.0098 (1)
Mo(6)	0.06131 (2)	0.69567 (3)	0.14512 (4)	0.0094 (1)
Mo(7)	0.56210 (2)	0.69421 (3)	0.14586 (4)	0.0097 (1)
O(1)	0.5791 (2)	0.9741 (3)	0.2866 (3)	0.020 (1)
O(2)	0.5900 (2)	0.7855 (3)	0.0866 (3)	0.016 (1)
O(3)	0.5899 (2)	0.9543 (3)	−0.0254 (3)	0.0115 (9)
O(4)	0.6002 (2)	0.7932 (4)	−0.2341 (4)	0.024 (1)
O(5)	0.6005 (2)	0.6541 (3)	−0.0587 (4)	0.019 (1)
O(6)	0.1990 (2)	0.8789 (3)	0.2568 (3)	0.0147 (10)
O(7)	0.3847 (2)	0.8488 (3)	0.0598 (3)	0.016 (1)
O(8)	0.4001 (3)	0.6987 (4)	0.2320 (4)	0.027 (1)
O(9)	0.0747 (2)	1.0873 (3)	0.1023 (4)	0.020 (1)
O(10)	0.0868 (2)	0.9721 (4)	0.2896 (3)	0.024 (1)
O(11)	0.0870 (2)	0.7878 (3)	0.0820 (3)	0.016 (1)
O(12)	0.1952 (2)	1.0459 (3)	0.1563 (4)	0.019 (1)
O(13)	0.0079 (2)	0.9342 (3)	0.1207 (4)	0.019 (1)
O(14)	0.2459 (2)	0.7153 (3)	0.2609 (4)	0.020 (1)
O(15)	0.7034 (2)	0.7161 (3)	−0.0662 (4)	0.019 (1)
O(16)	0.6947 (2)	0.9030 (3)	−0.1151 (4)	0.021 (1)
O(17)	0.5163 (2)	0.7981 (3)	−0.1277 (4)	0.022 (1)
O(18)	0.6888 (2)	0.8735 (3)	0.0817 (3)	0.0152 (10)
O(19)	0.5052 (2)	0.9183 (3)	0.1124 (4)	0.018 (1)
O(20)	0.5768 (2)	1.0886 (3)	0.1027 (4)	0.020 (1)
O(21)	0.4845 (2)	0.7071 (3)	0.1282 (4)	0.022 (1)
O(22)	0.6955 (2)	1.0383 (3)	0.1964 (4)	0.022 (1)
O(23)	0.6866 (2)	0.8761 (3)	0.2853 (3)	0.016 (1)
O(24)	0.2860 (2)	0.7268 (3)	0.0976 (3)	0.0157 (10)
O(25)	0.1948 (2)	0.8495 (3)	0.0776 (3)	0.017 (1)
O(26)	0.0931 (2)	0.9504 (3)	−0.0246 (3)	0.0124 (10)
O(27)	0.2052 (2)	0.9758 (3)	0.4309 (4)	0.023 (1)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd(1)	0.0084 (1)	0.0099 (1)	0.0090 (1)	0.00012 (8)	0.0015 (1)	0.00032 (9)
Gd(2)	0.0077 (1)	0.0096 (1)	0.0097 (1)	−0.00016 (8)	0.0025 (1)	−0.00106 (9)
Gd(3)	0.0083 (1)	0.0098 (1)	0.0095 (1)	0.00081 (8)	0.0022 (1)	−0.00027 (9)
Gd(4)	0.0092 (1)	0.0107 (1)	0.0095 (2)	0.00068 (9)	0.0021 (1)	−0.00091 (9)
Mo(1)	0.0074 (2)	0.0121 (2)	0.0099 (2)	−0.0009 (2)	0.0016 (2)	−0.0006 (2)
Mo(2)	0.0069 (2)	0.0139 (2)	0.0106 (2)	0.0005 (2)	0.0014 (2)	0.0010 (2)
Mo(3)	0.0093 (2)	0.0096 (2)	0.0135 (2)	0.0005 (2)	0.0034 (2)	0.0007 (2)
Mo(4)	0.0085 (2)	0.0097 (2)	0.0107 (2)	0.0008 (2)	0.0023 (2)	0.0014 (2)
Mo(5)	0.0092 (2)	0.0101 (2)	0.0101 (2)	0.0005 (2)	0.0023 (2)	0.0013 (2)
Mo(6)	0.0079 (2)	0.0105 (2)	0.0097 (2)	−0.0002 (2)	0.0023 (2)	0.0004 (2)
Mo(7)	0.0081 (2)	0.0112 (2)	0.0098 (2)	−0.0003 (2)	0.0022 (2)	0.0002 (2)
O(1)	0.019 (2)	0.026 (2)	0.015 (2)	0.003 (2)	0.007 (2)	0.000 (2)
O(2)	0.018 (2)	0.013 (2)	0.019 (2)	0.000 (2)	0.008 (2)	−0.002 (2)
O(3)	0.017 (2)	0.010 (2)	0.008 (2)	0.003 (2)	0.004 (2)	0.000 (1)
O(4)	0.023 (3)	0.038 (3)	0.012 (2)	0.002 (2)	0.003 (2)	−0.003 (2)
O(5)	0.014 (2)	0.013 (2)	0.028 (3)	−0.002 (2)	0.003 (2)	0.000 (2)
O(6)	0.014 (2)	0.018 (2)	0.010 (2)	0.002 (2)	0.001 (2)	0.002 (2)
O(7)	0.016 (2)	0.013 (2)	0.021 (2)	0.001 (2)	0.005 (2)	−0.001 (2)
O(8)	0.023 (3)	0.046 (3)	0.013 (2)	0.006 (2)	0.004 (2)	0.000 (2)
O(9)	0.022 (2)	0.014 (2)	0.026 (3)	0.003 (2)	0.008 (2)	0.005 (2)
O(10)	0.023 (2)	0.037 (3)	0.012 (2)	−0.001 (2)	0.005 (2)	−0.003 (2)
O(11)	0.024 (2)	0.014 (2)	0.014 (2)	−0.002 (2)	0.008 (2)	0.001 (2)
O(12)	0.015 (2)	0.021 (2)	0.022 (2)	−0.003 (2)	0.006 (2)	0.001 (2)
O(13)	0.010 (2)	0.025 (2)	0.023 (2)	−0.001 (2)	0.004 (2)	0.000 (2)
O(14)	0.021 (2)	0.015 (2)	0.028 (3)	0.000 (2)	0.012 (2)	0.000 (2)
O(15)	0.010 (2)	0.024 (2)	0.024 (2)	0.001 (2)	0.006 (2)	−0.009 (2)
O(16)	0.026 (2)	0.017 (2)	0.027 (3)	−0.006 (2)	0.019 (2)	−0.003 (2)
O(17)	0.009 (2)	0.025 (2)	0.030 (3)	0.003 (2)	0.002 (2)	−0.003 (2)
O(18)	0.006 (2)	0.020 (2)	0.018 (2)	−0.001 (2)	0.002 (2)	−0.002 (2)
O(19)	0.010 (2)	0.020 (2)	0.022 (2)	0.001 (2)	0.004 (2)	−0.001 (2)
O(20)	0.025 (2)	0.014 (2)	0.022 (2)	0.004 (2)	0.008 (2)	0.003 (2)
O(21)	0.009 (2)	0.024 (2)	0.032 (3)	0.002 (2)	0.003 (2)	−0.002 (2)
O(22)	0.024 (2)	0.022 (2)	0.019 (2)	−0.007 (2)	0.005 (2)	−0.001 (2)
O(23)	0.012 (2)	0.023 (2)	0.015 (2)	0.004 (2)	0.004 (2)	0.002 (2)
O(24)	0.008 (2)	0.023 (2)	0.017 (2)	0.003 (2)	0.005 (2)	−0.005 (2)
O(25)	0.013 (2)	0.019 (2)	0.015 (2)	0.003 (2)	0.000 (2)	−0.002 (2)
O(26)	0.017 (2)	0.010 (2)	0.010 (2)	0.004 (2)	0.005 (2)	0.001 (1)
O(27)	0.023 (2)	0.025 (2)	0.022 (2)	0.007 (2)	0.006 (2)	−0.007 (2)

Geometric parameters (Å, º)

Gd(1)—O(9)	2.346 (4)	Gd(4)—O(11)^i	2.428 (5)
Gd(1)—O(26)	2.355 (4)	Mo(1)—O(24)	1.729 (4)
Gd(1)—O(6)	2.368 (4)	Mo(1)—O(23)^ii	1.732 (4)
Gd(1)—O(10)	2.371 (5)	Mo(1)—O(25)	1.777 (4)
Gd(1)—O(12)	2.379 (4)	Mo(1)—O(14)	1.913 (5)
Gd(1)—O(13)	2.396 (5)	Mo(1)—O(6)	2.362 (4)
Gd(1)—O(11)	2.452 (4)	Mo(2)—O(27)	1.697 (4)
Gd(1)—O(25)	2.659 (4)	Mo(2)—O(15)^iii	1.738 (4)
Gd(2)—O(5)	2.309 (4)	Mo(2)—O(18)^ii	1.811 (4)
Gd(2)—O(15)	2.310 (4)	Mo(2)—O(6)	1.823 (4)
Gd(2)—O(17)	2.383 (5)	Mo(3)—O(16)^iii	1.732 (4)
Gd(2)—O(4)	2.386 (5)	Mo(3)—O(22)^iv	1.743 (5)
Gd(2)—O(3)	2.388 (4)	Mo(3)—O(12)^v	1.745 (4)
Gd(2)—O(16)	2.441 (4)	Mo(3)—O(14)	1.845 (5)
Gd(2)—O(18)	2.444 (4)	Mo(4)—O(1)^vi	1.742 (5)
Gd(2)—O(2)	2.464 (5)	Mo(4)—O(19)^vii	1.743 (4)
Gd(3)—O(20)	2.342 (4)	Mo(4)—O(7)^vii	1.769 (4)
Gd(3)—O(22)	2.377 (5)	Mo(4)—O(3)	1.808 (4)
Gd(3)—O(1)	2.378 (5)	Mo(5)—O(5)^i	1.734 (4)
Gd(3)—O(3)	2.382 (4)	Mo(5)—O(13)	1.734 (5)
Gd(3)—O(19)	2.385 (4)	Mo(5)—O(10)^viii	1.745 (5)
Gd(3)—O(18)	2.417 (4)	Mo(5)—O(26)^ix	1.832 (4)
Gd(3)—O(2)	2.431 (4)	Mo(6)—O(17)^i	1.743 (5)
Gd(3)—O(23)	2.481 (4)	Mo(6)—O(4)^iii	1.743 (5)
Gd(4)—O(7)	2.268 (4)	Mo(6)—O(20)^iv	1.755 (5)
Gd(4)—O(8)	2.320 (6)	Mo(6)—O(11)	1.810 (4)
Gd(4)—O(26)^i	2.329 (4)	Mo(7)—O(9)^x	1.741 (5)
Gd(4)—O(21)	2.343 (5)	Mo(7)—O(8)^ii	1.747 (6)
Gd(4)—O(24)	2.384 (4)	Mo(7)—O(21)	1.750 (5)
Gd(4)—O(25)^i	2.409 (4)	Mo(7)—O(2)	1.792 (5)
O(9)—Gd(1)—O(26)	73.6 (2)	O(26)^i—Gd(4)—O(24)	122.7 (2)
O(9)—Gd(1)—O(6)	136.8 (2)	O(26)^i—Gd(4)—O(25)^i	73.7 (2)
O(9)—Gd(1)—O(10)	83.0 (2)	O(26)^i—Gd(4)—O(11)^i	73.8 (2)
O(9)—Gd(1)—O(12)	71.2 (2)	O(21)—Gd(4)—O(24)	143.5 (2)
O(9)—Gd(1)—O(13)	71.6 (2)	O(21)—Gd(4)—O(25)^i	142.3 (2)
O(9)—Gd(1)—O(11)	134.1 (2)	O(21)—Gd(4)—O(11)^i	79.3 (2)
O(9)—Gd(1)—O(25)	129.2 (2)	O(24)—Gd(4)—O(25)^i	74.1 (2)
O(26)—Gd(1)—O(6)	129.9 (2)	O(24)—Gd(4)—O(11)^i	130.4 (2)
O(26)—Gd(1)—O(10)	149.5 (2)	O(25)^i—Gd(4)—O(11)^i	66.7 (2)
O(26)—Gd(1)—O(12)	89.5 (2)	O(24)—Mo(1)—O(23)^ii	104.4 (2)
O(26)—Gd(1)—O(13)	85.2 (2)	O(24)—Mo(1)—O(25)	102.0 (2)
O(26)—Gd(1)—O(11)	72.9 (1)	O(24)—Mo(1)—O(14)	97.2 (2)
O(26)—Gd(1)—O(25)	68.7 (1)	O(24)—Mo(1)—O(6)	168.1 (2)
O(6)—Gd(1)—O(10)	80.6 (2)	O(23)^ii—Mo(1)—O(25)	114.8 (2)
O(6)—Gd(1)—O(12)	73.3 (2)	O(23)^ii—Mo(1)—O(14)	110.4 (2)
O(6)—Gd(1)—O(13)	135.5 (2)	O(23)^ii—Mo(1)—O(6)	86.9 (2)
O(6)—Gd(1)—O(11)	89.0 (2)	O(25)—Mo(1)—O(14)	123.8 (2)
O(6)—Gd(1)—O(25)	61.5 (1)	O(25)—Mo(1)—O(6)	75.8 (2)
O(10)—Gd(1)—O(12)	101.4 (2)	O(14)—Mo(1)—O(6)	75.0 (2)
O(10)—Gd(1)—O(13)	68.7 (2)	O(27)—Mo(2)—O(15)^iii	110.2 (2)
O(10)—Gd(1)—O(11)	113.2 (2)	O(27)—Mo(2)—O(18)^ii	112.1 (2)
O(10)—Gd(1)—O(25)	141.5 (2)	O(27)—Mo(2)—O(6)	107.9 (2)
O(12)—Gd(1)—O(13)	142.4 (2)	O(15)^iii—Mo(2)—O(18)^ii	107.7 (2)
O(12)—Gd(1)—O(11)	138.0 (2)	O(15)^iii—Mo(2)—O(6)	107.7 (2)
O(12)—Gd(1)—O(25)	75.6 (2)	O(18)^ii—Mo(2)—O(6)	111.2 (2)
O(13)—Gd(1)—O(11)	75.3 (2)	O(16)^iii—Mo(3)—O(22)^iv	109.8 (2)
O(13)—Gd(1)—O(25)	135.0 (2)	O(16)^iii—Mo(3)—O(12)^v	110.0 (2)
O(11)—Gd(1)—O(25)	62.5 (1)	O(16)^iii—Mo(3)—O(14)	110.5 (2)
O(5)—Gd(2)—O(15)	67.6 (2)	O(22)^iv—Mo(3)—O(12)^v	109.3 (2)
O(5)—Gd(2)—O(17)	75.4 (2)	O(22)^iv—Mo(3)—O(14)	107.7 (2)
O(5)—Gd(2)—O(4)	87.2 (2)	O(12)^v—Mo(3)—O(14)	109.6 (2)
O(5)—Gd(2)—O(3)	142.3 (2)	O(1)^vi—Mo(4)—O(19)^vii	108.4 (2)
O(5)—Gd(2)—O(16)	137.6 (2)	O(1)^vi—Mo(4)—O(7)^vii	107.2 (2)
O(5)—Gd(2)—O(18)	117.3 (2)	O(1)^vi—Mo(4)—O(3)	106.5 (2)
O(5)—Gd(2)—O(2)	74.6 (2)	O(19)^vii—Mo(4)—O(7)^vii	109.7 (2)
O(15)—Gd(2)—O(17)	135.5 (2)	O(19)^vii—Mo(4)—O(3)	109.9 (2)
O(15)—Gd(2)—O(4)	83.6 (2)	O(7)^vii—Mo(4)—O(3)	114.8 (2)
O(15)—Gd(2)—O(3)	146.0 (2)	O(5)^i—Mo(5)—O(13)	105.0 (2)
O(15)—Gd(2)—O(16)	72.9 (2)	O(5)^i—Mo(5)—O(10)^viii	107.9 (2)
O(15)—Gd(2)—O(18)	85.0 (2)	O(5)^i—Mo(5)—O(26)^ix	117.0 (2)
O(15)—Gd(2)—O(2)	111.6 (2)	O(13)—Mo(5)—O(10)^viii	110.4 (2)
O(17)—Gd(2)—O(4)	70.5 (2)	O(13)—Mo(5)—O(26)^ix	110.1 (2)
O(17)—Gd(2)—O(3)	78.0 (2)	O(10)^viii—Mo(5)—O(26)^ix	106.5 (2)
O(17)—Gd(2)—O(16)	128.7 (2)	O(17)^i—Mo(6)—O(4)^iii	112.7 (3)
O(17)—Gd(2)—O(18)	135.4 (2)	O(17)^i—Mo(6)—O(20)^iv	106.8 (2)
O(17)—Gd(2)—O(2)	79.9 (2)	O(17)^i—Mo(6)—O(11)	110.2 (2)
O(4)—Gd(2)—O(3)	108.3 (2)	O(4)^iii—Mo(6)—O(20)^iv	109.3 (2)
O(4)—Gd(2)—O(16)	73.5 (2)	O(4)^iii—Mo(6)—O(11)	106.0 (2)
O(4)—Gd(2)—O(18)	146.2 (2)	O(20)^iv—Mo(6)—O(11)	112.0 (2)
O(4)—Gd(2)—O(2)	148.5 (2)	O(9)^x—Mo(7)—O(8)^ii	107.9 (3)
O(3)—Gd(2)—O(16)	80.0 (2)	O(9)^x—Mo(7)—O(21)	107.7 (2)
O(3)—Gd(2)—O(18)	67.3 (1)	O(9)^x—Mo(7)—O(2)	113.0 (2)
O(3)—Gd(2)—O(2)	74.9 (1)	O(8)^ii—Mo(7)—O(21)	111.7 (3)
O(16)—Gd(2)—O(18)	72.7 (2)	O(8)^ii—Mo(7)—O(2)	107.5 (2)
O(16)—Gd(2)—O(2)	136.4 (2)	O(21)—Mo(7)—O(2)	109.1 (2)
O(18)—Gd(2)—O(2)	64.9 (2)	Mo(4)^xi—O(1)—Gd(3)	151.9 (3)
O(20)—Gd(3)—O(22)	73.4 (2)	Mo(7)—O(2)—Gd(3)	126.8 (2)
O(20)—Gd(3)—O(1)	82.7 (2)	Mo(7)—O(2)—Gd(2)	137.3 (2)
O(20)—Gd(3)—O(3)	71.6 (2)	Gd(3)—O(2)—Gd(2)	95.9 (2)
O(20)—Gd(3)—O(19)	79.3 (2)	Mo(4)—O(3)—Gd(3)	129.3 (2)
O(20)—Gd(3)—O(18)	120.8 (2)	Mo(4)—O(3)—Gd(2)	130.3 (2)
O(20)—Gd(3)—O(2)	138.9 (2)	Gd(3)—O(3)—Gd(2)	99.3 (2)
O(20)—Gd(3)—O(23)	133.2 (2)	Mo(6)^xii—O(4)—Gd(2)	159.2 (3)
O(22)—Gd(3)—O(1)	91.1 (2)	Mo(5)^i—O(5)—Gd(2)	157.3 (3)
O(22)—Gd(3)—O(3)	101.6 (2)	Mo(2)—O(6)—Mo(1)	116.4 (2)
O(22)—Gd(3)—O(19)	149.0 (2)	Mo(2)—O(6)—Gd(1)	137.0 (2)
O(22)—Gd(3)—O(18)	74.7 (2)	Mo(1)—O(6)—Gd(1)	106.6 (2)
O(22)—Gd(3)—O(2)	138.4 (2)	Mo(4)^vii—O(7)—Gd(4)	144.8 (2)
O(22)—Gd(3)—O(23)	68.4 (2)	Mo(7)^ii—O(8)—Gd(4)	161.7 (3)
O(1)—Gd(3)—O(3)	146.3 (2)	Mo(7)^xiii—O(9)—Gd(1)	145.0 (3)
O(1)—Gd(3)—O(19)	70.9 (2)	Mo(5)^viii—O(10)—Gd(1)	158.2 (3)
O(1)—Gd(3)—O(18)	145.9 (2)	Mo(6)—O(11)—Gd(4)^i	136.7 (2)
O(1)—Gd(3)—O(2)	114.3 (2)	Mo(6)—O(11)—Gd(1)	126.2 (2)
O(1)—Gd(3)—O(23)	72.2 (2)	Gd(4)^i—O(11)—Gd(1)	96.5 (2)
O(3)—Gd(3)—O(19)	82.9 (2)	Mo(3)^xiv—O(12)—Gd(1)	158.9 (3)
O(3)—Gd(3)—O(18)	67.8 (2)	Mo(5)—O(13)—Gd(1)	169.7 (3)
O(3)—Gd(3)—O(2)	75.7 (2)	Mo(3)—O(14)—Mo(1)	150.9 (3)
O(3)—Gd(3)—O(23)	141.5 (1)	Mo(2)^xii—O(15)—Gd(2)	147.6 (3)
O(19)—Gd(3)—O(18)	133.5 (2)	Mo(3)^xii—O(16)—Gd(2)	138.8 (2)
O(19)—Gd(3)—O(2)	72.5 (2)	Mo(6)^i—O(17)—Gd(2)	164.5 (3)
O(19)—Gd(3)—O(23)	125.3 (2)	Mo(2)^ii—O(18)—Gd(3)	134.6 (2)
O(18)—Gd(3)—O(2)	65.8 (1)	Mo(2)^ii—O(18)—Gd(2)	128.0 (2)
O(18)—Gd(3)—O(23)	73.7 (1)	Gd(3)—O(18)—Gd(2)	96.8 (1)
O(2)—Gd(3)—O(23)	87.8 (2)	Mo(4)^vii—O(19)—Gd(3)	158.3 (3)
O(7)—Gd(4)—O(8)	90.6 (2)	Mo(6)^xv—O(20)—Gd(3)	145.7 (3)
O(7)—Gd(4)—O(26)^i	152.5 (2)	Mo(7)—O(21)—Gd(4)	162.5 (3)
O(7)—Gd(4)—O(21)	83.4 (2)	Mo(3)^xv—O(22)—Gd(3)	140.4 (3)
O(7)—Gd(4)—O(24)	81.9 (2)	Mo(1)^ii—O(23)—Gd(3)	151.2 (2)
O(7)—Gd(4)—O(25)^i	105.5 (2)	Mo(1)—O(24)—Gd(4)	139.2 (2)
O(7)—Gd(4)—O(11)^i	80.7 (2)	Mo(1)—O(25)—Gd(4)^i	139.7 (2)
O(8)—Gd(4)—O(26)^i	106.7 (2)	Mo(1)—O(25)—Gd(1)	116.0 (2)
O(8)—Gd(4)—O(21)	71.9 (2)	Gd(4)^i—O(25)—Gd(1)	91.7 (1)
O(8)—Gd(4)—O(24)	75.0 (2)	Mo(5)^ix—O(26)—Gd(4)^i	129.6 (2)
O(8)—Gd(4)—O(25)^i	142.4 (2)	Mo(5)^ix—O(26)—Gd(1)	128.1 (2)
O(8)—Gd(4)—O(11)^i	150.7 (2)	Gd(4)^i—O(26)—Gd(1)	102.0 (2)
O(26)^i—Gd(4)—O(21)	82.0 (2)

Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x+1, y, −z+1/2; (iii) x−1/2, −y+3/2, z+1/2; (iv) x−1/2, y−1/2, z; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, −y+2, z−1/2; (vii) −x+1, −y+2, −z; (viii) −x, y, −z+1/2; (ix) −x, −y+2, −z; (x) x+1/2, y−1/2, z; (xi) x, −y+2, z+1/2; (xii) x+1/2, −y+3/2, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) −x+1/2, y+1/2, −z+1/2; (xv) x+1/2, y+1/2, z.